Supporting information
CCDC references: 2074914; 2074913; 2074912; 2074911; 2074910
For all structures, data collection: COLLECT (Nonius, 2000); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997). Program(s) used to solve structure: SIR92 (Altomare et al., 1994) for (I); SHELXS97 (Sheldrick, 2008) for (II), (IV), (V); PATTY and DIRDIF94 (Beurskens et al., 1992, 1994) for (III). For all structures, program(s) used to refine structure: SHELXL2018 (Sheldrick, 2015); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL2018 (Sheldrick, 2015), Mercury (Macrae et al., 2020) and PLATON (Spek, 2020).
[Sn(C4H9)2(C14H11N2O3)2]·0.5C6H12 | F(000) = 1624 |
Mr = 785.49 | Dx = 1.424 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 9.4028 (1) Å | Cell parameters from 84811 reflections |
b = 25.1718 (2) Å | θ = 2.0–30.0° |
c = 15.5008 (1) Å | µ = 0.75 mm−1 |
β = 93.3046 (3)° | T = 160 K |
V = 3662.71 (5) Å3 | Prism, orange |
Z = 4 | 0.25 × 0.17 × 0.12 mm |
Nonius KappaCCD area detector diffractometer | 10708 independent reflections |
Radiation source: Nonius FR590 sealed tube generator | 7109 reflections with I > 2σ(I) |
Horizontally mounted graphite crystal monochromator | Rint = 0.066 |
Detector resolution: 9 pixels mm-1 | θmax = 30.0°, θmin = 2.6° |
φ and ω scans with κ offsets | h = −13→13 |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | k = −35→35 |
Tmin = 0.854, Tmax = 0.917 | l = −21→21 |
90950 measured reflections |
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)] = 0.040 | Hydrogen site location: mixed |
wR(F2) = 0.110 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0545P)2 + 1.0512P] where P = (Fo2 + 2Fc2)/3 |
10702 reflections | (Δ/σ)max = 0.001 |
623 parameters | Δρmax = 0.90 e Å−3 |
645 restraints | Δρmin = −0.63 e Å−3 |
Experimental. Data collection and full structure determination done by Prof. Anthony Linden: anthony.linden@chem.uzh.ch Solvent used: petrolum ether Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: on a glass fibre Mosaicity (deg.): 0.504 (1) Frames collected: 817 Seconds exposure per frame: 33 Degrees rotation per frame: 1.1 Crystal-detector distance (mm): 39.0 Client: Tushar Basubaul Sample code: TSBB-2 (L0218) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. The asymmetric unit contains one molecule of the Sn-complex, plus one half of a cyclohexane molecule. The cyclohexane molecule sits about a crystallographic centre of inversion. One of the carboxylate ligands is disordered in its entirety over two conformations, the difference arising from a reversal of the direction of the zig-zag at the N=N bond. Two positions were defined for all atoms of this ligand, except for the carboxylate O atom bound strongly with the Sn-atom, which is not significantly disordered. Refinement of constrained site occupation factors for the two orientations yielded a value of 0.563 (5) for the major conformation. Similarity restraints were applied to the chemically equivalent bond lengths and angles of all atoms in the carboxylate ligands, including those of the ordered ligand. Furthermore, neighbouring atoms within and between each conformation of the disordered ligand were restrained to have similar atomic displacement parameters. The geometry of the cyclohexane molecule is poor because of possible disorder, as indicated by the enlarged atomic displacement parameters, but no attempt was made to resolve the disorder; the C-C distances within the solvent molecule were restrained to 1.52 (1) Å. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Sn1 | 1.14355 (2) | 0.40458 (2) | 0.17524 (2) | 0.03777 (7) | |
O1 | 0.99456 (19) | 0.45491 (7) | 0.22890 (10) | 0.0422 (4) | |
O2 | 1.01081 (19) | 0.48431 (7) | 0.09670 (11) | 0.0459 (4) | |
O3 | 0.8742 (2) | 0.57069 (8) | 0.04591 (11) | 0.0452 (4) | |
H3 | 0.922 (4) | 0.5455 (14) | 0.045 (2) | 0.069 (12)* | |
N1 | 0.6414 (2) | 0.57079 (8) | 0.36788 (13) | 0.0389 (5) | |
N2 | 0.5572 (2) | 0.60765 (8) | 0.38296 (13) | 0.0385 (5) | |
C1 | 0.9573 (3) | 0.48839 (10) | 0.16860 (14) | 0.0375 (5) | |
C2 | 0.8560 (2) | 0.53078 (9) | 0.18696 (14) | 0.0354 (5) | |
C3 | 0.8204 (3) | 0.56998 (10) | 0.12480 (15) | 0.0364 (5) | |
C4 | 0.7271 (3) | 0.61062 (10) | 0.14413 (16) | 0.0414 (6) | |
H4 | 0.704542 | 0.637386 | 0.102346 | 0.050* | |
C5 | 0.6672 (3) | 0.61257 (10) | 0.22263 (16) | 0.0401 (6) | |
H5 | 0.604374 | 0.640728 | 0.235119 | 0.048* | |
C6 | 0.6987 (3) | 0.57297 (10) | 0.28457 (15) | 0.0359 (5) | |
C7 | 0.7924 (3) | 0.53284 (9) | 0.26635 (15) | 0.0358 (5) | |
H7 | 0.814077 | 0.506154 | 0.308404 | 0.043* | |
C8 | 0.4993 (3) | 0.60429 (9) | 0.46625 (15) | 0.0370 (5) | |
C9 | 0.3989 (3) | 0.64256 (10) | 0.48359 (16) | 0.0404 (6) | |
H9 | 0.374403 | 0.668761 | 0.441186 | 0.049* | |
C10 | 0.3330 (3) | 0.64347 (11) | 0.56202 (17) | 0.0442 (6) | |
C11 | 0.3726 (3) | 0.60474 (11) | 0.62258 (17) | 0.0475 (7) | |
H11 | 0.330706 | 0.604756 | 0.676913 | 0.057* | |
C12 | 0.4716 (3) | 0.56619 (11) | 0.60530 (17) | 0.0474 (6) | |
H12 | 0.495179 | 0.539636 | 0.647273 | 0.057* | |
C13 | 0.5368 (3) | 0.56584 (10) | 0.52760 (16) | 0.0419 (6) | |
H13 | 0.606252 | 0.539696 | 0.516368 | 0.050* | |
C27 | 0.2235 (3) | 0.68518 (13) | 0.5788 (2) | 0.0584 (8) | |
H271 | 0.184768 | 0.678779 | 0.635272 | 0.088* | |
H272 | 0.146349 | 0.683583 | 0.533646 | 0.088* | |
H273 | 0.268068 | 0.720375 | 0.578592 | 0.088* | |
O4 | 1.16131 (18) | 0.37375 (7) | 0.30096 (11) | 0.0428 (4) | |
O5A | 1.335 (2) | 0.3262 (13) | 0.2380 (11) | 0.038 (3) | 0.437 (5) |
O6A | 1.4503 (15) | 0.2495 (6) | 0.3328 (6) | 0.0458 (18) | 0.437 (5) |
H6A | 1.426681 | 0.265078 | 0.286191 | 0.069* | 0.437 (5) |
N3A | 1.1171 (13) | 0.3174 (6) | 0.5944 (7) | 0.0364 (18) | 0.437 (5) |
N4A | 1.1244 (5) | 0.2927 (2) | 0.6633 (3) | 0.0403 (12) | 0.437 (5) |
C14A | 1.263 (3) | 0.3393 (10) | 0.3002 (11) | 0.035 (2) | 0.437 (5) |
C15A | 1.276 (2) | 0.3105 (7) | 0.3838 (9) | 0.0336 (17) | 0.437 (5) |
C16A | 1.3711 (14) | 0.2678 (5) | 0.3955 (6) | 0.0361 (17) | 0.437 (5) |
C17A | 1.3879 (9) | 0.2418 (3) | 0.4754 (5) | 0.0358 (15) | 0.437 (5) |
H171 | 1.455009 | 0.213821 | 0.483992 | 0.043* | 0.437 (5) |
C18A | 1.3061 (8) | 0.2576 (3) | 0.5407 (4) | 0.0292 (13) | 0.437 (5) |
H181 | 1.316526 | 0.239976 | 0.594895 | 0.035* | 0.437 (5) |
C19A | 1.2077 (8) | 0.2987 (3) | 0.5299 (4) | 0.0309 (14) | 0.437 (5) |
C20A | 1.1937 (12) | 0.3254 (4) | 0.4520 (6) | 0.0303 (16) | 0.437 (5) |
H201 | 1.128234 | 0.354046 | 0.444884 | 0.036* | 0.437 (5) |
C21A | 1.0284 (8) | 0.3130 (3) | 0.7254 (5) | 0.0394 (15) | 0.437 (5) |
C22A | 0.9380 (17) | 0.3551 (7) | 0.7085 (9) | 0.047 (2) | 0.437 (5) |
H221 | 0.938030 | 0.372809 | 0.654406 | 0.057* | 0.437 (5) |
C23A | 0.846 (3) | 0.3720 (12) | 0.7709 (13) | 0.0523 (19) | 0.437 (5) |
C24A | 0.8551 (14) | 0.3465 (5) | 0.8502 (8) | 0.056 (2) | 0.437 (5) |
H241 | 0.795821 | 0.358344 | 0.893955 | 0.067* | 0.437 (5) |
C25A | 0.9464 (10) | 0.3049 (4) | 0.8683 (6) | 0.0552 (18) | 0.437 (5) |
H25A | 0.948616 | 0.288099 | 0.923288 | 0.066* | 0.437 (5) |
C26A | 1.0355 (8) | 0.2874 (3) | 0.8057 (6) | 0.0447 (16) | 0.437 (5) |
H261 | 1.099738 | 0.258732 | 0.817100 | 0.054* | 0.437 (5) |
C28A | 0.7532 (13) | 0.4206 (5) | 0.7581 (10) | 0.059 (2) | 0.437 (5) |
H281 | 0.665835 | 0.411168 | 0.724009 | 0.089* | 0.437 (5) |
H282 | 0.804899 | 0.447936 | 0.727597 | 0.089* | 0.437 (5) |
H283 | 0.728524 | 0.434321 | 0.814542 | 0.089* | 0.437 (5) |
O5B | 1.3096 (18) | 0.3282 (9) | 0.2321 (9) | 0.038 (2) | 0.563 (5) |
O6B | 1.4630 (12) | 0.2517 (4) | 0.3081 (5) | 0.0430 (13) | 0.563 (5) |
H6B | 1.437641 | 0.272918 | 0.268220 | 0.064* | 0.563 (5) |
N3B | 1.1851 (4) | 0.28580 (16) | 0.6084 (2) | 0.0382 (10) | 0.563 (5) |
N4B | 1.0894 (10) | 0.3200 (5) | 0.6092 (5) | 0.0395 (15) | 0.563 (5) |
C14B | 1.253 (2) | 0.3355 (7) | 0.3023 (9) | 0.034 (2) | 0.563 (5) |
C15B | 1.2916 (16) | 0.3040 (5) | 0.3807 (7) | 0.0325 (14) | 0.563 (5) |
C16B | 1.3935 (10) | 0.2631 (4) | 0.3785 (5) | 0.0335 (14) | 0.563 (5) |
C17B | 1.4235 (7) | 0.2322 (3) | 0.4516 (4) | 0.0376 (13) | 0.563 (5) |
H172 | 1.493150 | 0.204936 | 0.450500 | 0.045* | 0.563 (5) |
C18B | 1.3532 (6) | 0.2410 (2) | 0.5249 (4) | 0.0350 (11) | 0.563 (5) |
H182 | 1.373890 | 0.219341 | 0.574244 | 0.042* | 0.563 (5) |
C19B | 1.2507 (6) | 0.2814 (3) | 0.5287 (3) | 0.0314 (12) | 0.563 (5) |
C20B | 1.2228 (9) | 0.3132 (3) | 0.4569 (5) | 0.0328 (14) | 0.563 (5) |
H202 | 1.156312 | 0.341497 | 0.459372 | 0.039* | 0.563 (5) |
C21B | 1.0245 (7) | 0.3227 (3) | 0.6912 (4) | 0.0404 (13) | 0.563 (5) |
C22B | 0.9174 (13) | 0.3598 (5) | 0.6964 (7) | 0.0474 (17) | 0.563 (5) |
H222 | 0.890803 | 0.380898 | 0.647321 | 0.057* | 0.563 (5) |
C23B | 0.847 (3) | 0.3667 (9) | 0.7726 (10) | 0.0531 (17) | 0.563 (5) |
C24B | 0.8824 (11) | 0.3341 (4) | 0.8423 (6) | 0.0554 (18) | 0.563 (5) |
H242 | 0.833196 | 0.337597 | 0.893834 | 0.067* | 0.563 (5) |
C25B | 0.9873 (8) | 0.2969 (3) | 0.8375 (5) | 0.0541 (15) | 0.563 (5) |
H252 | 1.011694 | 0.275187 | 0.886349 | 0.065* | 0.563 (5) |
C26B | 1.0593 (6) | 0.2902 (2) | 0.7617 (5) | 0.0465 (12) | 0.563 (5) |
H263 | 1.131037 | 0.263793 | 0.758446 | 0.056* | 0.563 (5) |
C28B | 0.7288 (11) | 0.4068 (4) | 0.7728 (8) | 0.071 (2) | 0.563 (5) |
H284 | 0.754429 | 0.434989 | 0.814503 | 0.107* | 0.563 (5) |
H285 | 0.641172 | 0.389335 | 0.789138 | 0.107* | 0.563 (5) |
H286 | 0.713613 | 0.422241 | 0.714997 | 0.107* | 0.563 (5) |
C29 | 1.0163 (3) | 0.34748 (10) | 0.10760 (16) | 0.0412 (6) | |
H291 | 0.978564 | 0.362721 | 0.052015 | 0.049* | |
H292 | 1.075319 | 0.316216 | 0.094748 | 0.049* | |
C30 | 0.8923 (3) | 0.32999 (11) | 0.16058 (16) | 0.0429 (6) | |
H301 | 0.930799 | 0.315112 | 0.216247 | 0.051* | |
H302 | 0.834154 | 0.361491 | 0.173503 | 0.051* | |
C31 | 0.7970 (3) | 0.28867 (11) | 0.11466 (17) | 0.0444 (6) | |
H311 | 0.757029 | 0.303476 | 0.059265 | 0.053* | |
H312 | 0.854462 | 0.257036 | 0.101545 | 0.053* | |
C32 | 0.6759 (3) | 0.27222 (14) | 0.1699 (2) | 0.0600 (8) | |
H321 | 0.715235 | 0.256159 | 0.223728 | 0.090* | |
H322 | 0.614986 | 0.246356 | 0.138249 | 0.090* | |
H323 | 0.619406 | 0.303553 | 0.183397 | 0.090* | |
C33 | 1.3355 (3) | 0.44608 (11) | 0.16023 (18) | 0.0474 (6) | |
H331 | 1.312307 | 0.483083 | 0.142993 | 0.057* | |
H332 | 1.389692 | 0.447418 | 0.216890 | 0.057* | |
C34 | 1.4310 (3) | 0.42214 (11) | 0.09390 (18) | 0.0450 (6) | |
H341 | 1.447514 | 0.384176 | 0.107854 | 0.054* | |
H342 | 1.380992 | 0.424035 | 0.035994 | 0.054* | |
C35 | 1.5724 (3) | 0.44980 (13) | 0.0910 (2) | 0.0536 (7) | |
H351 | 1.626598 | 0.444800 | 0.147116 | 0.064* | |
H352 | 1.556030 | 0.488363 | 0.082824 | 0.064* | |
C36 | 1.6606 (3) | 0.42936 (15) | 0.0192 (2) | 0.0639 (8) | |
H361 | 1.679330 | 0.391364 | 0.027768 | 0.096* | |
H362 | 1.751182 | 0.448674 | 0.020065 | 0.096* | |
H363 | 1.608370 | 0.434816 | −0.036627 | 0.096* | |
C37 | 0.9061 (6) | 0.5119 (2) | 0.5726 (4) | 0.149 (3) | |
H371 | 0.948957 | 0.493958 | 0.624624 | 0.179* | |
H372 | 0.822029 | 0.532405 | 0.589114 | 0.179* | |
C38 | 1.0160 (4) | 0.54900 (15) | 0.5328 (3) | 0.0857 (12) | |
H381 | 0.963940 | 0.572510 | 0.490655 | 0.103* | |
H382 | 1.057966 | 0.571923 | 0.579548 | 0.103* | |
C39 | 1.1321 (5) | 0.5243 (2) | 0.4897 (3) | 0.1039 (15) | |
H391 | 1.188027 | 0.552653 | 0.463175 | 0.125* | |
H392 | 1.195644 | 0.506552 | 0.533944 | 0.125* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sn1 | 0.03821 (10) | 0.04234 (12) | 0.03366 (10) | 0.00372 (7) | 0.00971 (7) | 0.00012 (7) |
O1 | 0.0486 (10) | 0.0441 (10) | 0.0349 (9) | 0.0126 (8) | 0.0111 (8) | 0.0026 (8) |
O2 | 0.0468 (10) | 0.0604 (12) | 0.0316 (9) | 0.0075 (9) | 0.0107 (8) | 0.0006 (8) |
O3 | 0.0548 (12) | 0.0512 (12) | 0.0307 (9) | 0.0075 (10) | 0.0120 (8) | 0.0062 (8) |
N1 | 0.0425 (12) | 0.0396 (12) | 0.0354 (11) | 0.0001 (9) | 0.0097 (9) | −0.0034 (9) |
N2 | 0.0390 (11) | 0.0406 (12) | 0.0368 (11) | −0.0005 (9) | 0.0098 (9) | −0.0027 (9) |
C1 | 0.0387 (13) | 0.0442 (14) | 0.0298 (12) | 0.0005 (11) | 0.0040 (10) | −0.0001 (10) |
C2 | 0.0351 (12) | 0.0407 (13) | 0.0305 (12) | −0.0014 (10) | 0.0043 (9) | −0.0033 (10) |
C3 | 0.0399 (13) | 0.0389 (13) | 0.0308 (12) | −0.0033 (10) | 0.0055 (10) | 0.0015 (10) |
C4 | 0.0506 (15) | 0.0387 (13) | 0.0352 (13) | 0.0013 (11) | 0.0045 (11) | 0.0046 (10) |
C5 | 0.0462 (15) | 0.0353 (13) | 0.0393 (14) | 0.0013 (11) | 0.0069 (11) | −0.0022 (11) |
C6 | 0.0376 (13) | 0.0374 (13) | 0.0334 (12) | −0.0039 (10) | 0.0084 (10) | −0.0028 (10) |
C7 | 0.0405 (13) | 0.0358 (13) | 0.0314 (12) | −0.0004 (10) | 0.0045 (10) | 0.0025 (9) |
C8 | 0.0368 (13) | 0.0404 (14) | 0.0342 (12) | −0.0040 (10) | 0.0065 (10) | −0.0051 (10) |
C9 | 0.0427 (14) | 0.0412 (14) | 0.0380 (13) | −0.0019 (11) | 0.0080 (11) | −0.0025 (11) |
C10 | 0.0423 (14) | 0.0505 (16) | 0.0406 (14) | −0.0029 (12) | 0.0087 (11) | −0.0089 (12) |
C11 | 0.0535 (17) | 0.0553 (17) | 0.0346 (13) | −0.0057 (13) | 0.0111 (12) | −0.0065 (12) |
C12 | 0.0578 (17) | 0.0490 (16) | 0.0360 (14) | −0.0013 (13) | 0.0070 (12) | 0.0023 (12) |
C13 | 0.0439 (14) | 0.0425 (15) | 0.0397 (14) | 0.0005 (11) | 0.0052 (11) | −0.0034 (11) |
C27 | 0.0598 (18) | 0.0632 (19) | 0.0541 (18) | 0.0109 (15) | 0.0194 (14) | −0.0048 (15) |
O4 | 0.0445 (10) | 0.0474 (11) | 0.0369 (9) | 0.0082 (8) | 0.0057 (8) | 0.0012 (8) |
O5A | 0.031 (6) | 0.055 (5) | 0.028 (4) | 0.010 (4) | 0.008 (4) | 0.006 (3) |
O6A | 0.051 (4) | 0.051 (3) | 0.037 (5) | 0.005 (3) | 0.017 (4) | 0.011 (4) |
N3A | 0.035 (4) | 0.041 (3) | 0.033 (3) | 0.000 (3) | 0.007 (3) | 0.001 (3) |
N4A | 0.044 (2) | 0.044 (2) | 0.034 (2) | −0.004 (2) | 0.009 (2) | 0.0025 (19) |
C14A | 0.036 (4) | 0.039 (4) | 0.032 (4) | −0.003 (4) | 0.006 (3) | 0.002 (3) |
C15A | 0.031 (4) | 0.035 (4) | 0.035 (3) | −0.001 (3) | 0.004 (3) | −0.002 (3) |
C16A | 0.034 (4) | 0.042 (3) | 0.033 (3) | −0.004 (3) | 0.015 (3) | −0.002 (3) |
C17A | 0.035 (3) | 0.036 (3) | 0.037 (4) | 0.003 (3) | 0.011 (3) | 0.002 (3) |
C18A | 0.029 (3) | 0.030 (4) | 0.029 (3) | 0.000 (3) | 0.009 (3) | −0.002 (3) |
C19A | 0.032 (3) | 0.029 (3) | 0.032 (2) | 0.001 (2) | 0.003 (2) | −0.001 (2) |
C20A | 0.030 (4) | 0.033 (4) | 0.029 (3) | 0.004 (3) | 0.005 (2) | 0.001 (2) |
C21A | 0.037 (3) | 0.045 (3) | 0.037 (4) | −0.002 (3) | 0.007 (3) | −0.001 (3) |
C22A | 0.045 (4) | 0.053 (4) | 0.043 (4) | −0.003 (3) | 0.002 (3) | −0.009 (3) |
C23A | 0.047 (3) | 0.061 (4) | 0.050 (3) | −0.005 (3) | 0.010 (3) | −0.017 (3) |
C24A | 0.049 (4) | 0.063 (5) | 0.057 (4) | −0.006 (3) | 0.016 (3) | −0.015 (4) |
C25A | 0.058 (4) | 0.058 (4) | 0.052 (4) | −0.008 (3) | 0.023 (3) | −0.009 (3) |
C26A | 0.047 (4) | 0.049 (3) | 0.039 (4) | 0.002 (3) | 0.009 (3) | 0.000 (3) |
C28A | 0.050 (4) | 0.063 (5) | 0.067 (5) | 0.007 (4) | 0.020 (3) | −0.010 (4) |
O5B | 0.037 (5) | 0.047 (4) | 0.031 (3) | 0.002 (4) | 0.004 (3) | −0.001 (3) |
O6B | 0.046 (3) | 0.050 (2) | 0.035 (3) | 0.0119 (19) | 0.018 (3) | 0.009 (3) |
N3B | 0.039 (2) | 0.041 (2) | 0.0348 (19) | −0.0003 (16) | 0.0087 (15) | 0.0036 (16) |
N4B | 0.043 (4) | 0.043 (3) | 0.034 (3) | −0.003 (3) | 0.006 (2) | 0.000 (2) |
C14B | 0.034 (3) | 0.037 (3) | 0.033 (3) | −0.005 (3) | 0.005 (3) | −0.004 (3) |
C15B | 0.033 (3) | 0.037 (3) | 0.028 (2) | −0.001 (2) | 0.007 (2) | 0.000 (2) |
C16B | 0.032 (3) | 0.038 (3) | 0.032 (3) | −0.001 (2) | 0.011 (2) | −0.001 (2) |
C17B | 0.036 (3) | 0.036 (3) | 0.041 (3) | 0.000 (2) | 0.005 (2) | 0.001 (2) |
C18B | 0.035 (3) | 0.034 (3) | 0.037 (3) | 0.005 (2) | 0.005 (2) | 0.003 (2) |
C19B | 0.030 (3) | 0.033 (3) | 0.032 (2) | 0.001 (2) | 0.004 (2) | 0.002 (2) |
C20B | 0.030 (3) | 0.033 (3) | 0.036 (2) | 0.002 (2) | 0.003 (2) | −0.004 (2) |
C21B | 0.042 (2) | 0.042 (3) | 0.038 (3) | −0.008 (2) | 0.007 (2) | −0.007 (2) |
C22B | 0.044 (4) | 0.053 (3) | 0.045 (3) | 0.002 (3) | 0.004 (3) | −0.013 (3) |
C23B | 0.045 (3) | 0.065 (4) | 0.050 (3) | −0.002 (3) | 0.007 (3) | −0.018 (3) |
C24B | 0.054 (4) | 0.062 (4) | 0.052 (3) | −0.007 (3) | 0.010 (3) | −0.013 (3) |
C25B | 0.057 (4) | 0.059 (3) | 0.048 (4) | −0.002 (3) | 0.014 (3) | 0.003 (3) |
C26B | 0.048 (3) | 0.051 (3) | 0.042 (3) | −0.005 (2) | 0.010 (2) | 0.002 (3) |
C28B | 0.066 (4) | 0.086 (5) | 0.064 (4) | 0.007 (4) | 0.017 (3) | −0.013 (4) |
C29 | 0.0446 (14) | 0.0470 (15) | 0.0325 (12) | 0.0051 (11) | 0.0080 (10) | −0.0024 (11) |
C30 | 0.0454 (15) | 0.0493 (15) | 0.0345 (13) | 0.0006 (12) | 0.0077 (11) | −0.0012 (11) |
C31 | 0.0435 (14) | 0.0481 (15) | 0.0414 (14) | 0.0049 (12) | 0.0008 (11) | −0.0033 (12) |
C32 | 0.0463 (16) | 0.068 (2) | 0.066 (2) | −0.0095 (14) | 0.0066 (14) | −0.0134 (16) |
C33 | 0.0475 (15) | 0.0461 (15) | 0.0491 (15) | −0.0055 (12) | 0.0080 (12) | −0.0029 (12) |
C34 | 0.0393 (14) | 0.0487 (15) | 0.0473 (15) | −0.0024 (12) | 0.0043 (11) | −0.0005 (12) |
C35 | 0.0438 (15) | 0.0635 (19) | 0.0539 (17) | −0.0032 (13) | 0.0059 (13) | 0.0034 (14) |
C36 | 0.0453 (17) | 0.081 (2) | 0.067 (2) | 0.0053 (16) | 0.0131 (15) | 0.0117 (18) |
C37 | 0.113 (4) | 0.210 (7) | 0.119 (4) | 0.063 (5) | −0.036 (4) | −0.073 (5) |
C38 | 0.081 (3) | 0.069 (2) | 0.109 (3) | 0.007 (2) | 0.022 (2) | 0.003 (2) |
C39 | 0.098 (3) | 0.125 (4) | 0.090 (3) | 0.032 (3) | 0.011 (3) | −0.001 (3) |
Sn1—O1 | 2.0961 (16) | C26A—H261 | 0.9500 |
Sn1—O2 | 2.6252 (18) | C28A—H281 | 0.9800 |
Sn1—O4 | 2.0954 (17) | C28A—H282 | 0.9800 |
Sn1—O5A | 2.81 (3) | C28A—H283 | 0.9800 |
Sn1—O5B | 2.60 (2) | O5B—C14B | 1.253 (4) |
Sn1—C29 | 2.110 (3) | O6B—C16B | 1.336 (6) |
Sn1—C33 | 2.110 (3) | O6B—H6B | 0.8400 |
Sn1—O3i | 3.4786 (17) | N3B—N4B | 1.246 (8) |
O1—C1 | 1.292 (3) | N3B—C19B | 1.418 (6) |
O2—C1 | 1.253 (2) | N4B—C21B | 1.444 (8) |
O3—C3 | 1.350 (3) | C14B—C15B | 1.480 (8) |
O3—H3 | 0.78 (3) | C15B—C20B | 1.398 (8) |
N1—N2 | 1.250 (3) | C15B—C16B | 1.407 (8) |
N1—C6 | 1.429 (3) | C16B—C17B | 1.389 (8) |
N2—C8 | 1.433 (3) | C17B—C18B | 1.366 (7) |
C1—C2 | 1.469 (3) | C17B—H172 | 0.9500 |
C2—C7 | 1.400 (3) | C18B—C19B | 1.405 (7) |
C2—C3 | 1.406 (3) | C18B—H182 | 0.9500 |
C3—C4 | 1.392 (4) | C19B—C20B | 1.383 (7) |
C4—C5 | 1.371 (3) | C20B—H202 | 0.9500 |
C4—H4 | 0.9500 | C21B—C22B | 1.377 (8) |
C5—C6 | 1.404 (3) | C21B—C26B | 1.390 (7) |
C5—H5 | 0.9500 | C22B—C23B | 1.397 (9) |
C6—C7 | 1.380 (3) | C22B—H222 | 0.9500 |
C7—H7 | 0.9500 | C23B—C24B | 1.381 (9) |
C8—C9 | 1.386 (3) | C23B—C28B | 1.503 (10) |
C8—C13 | 1.388 (3) | C24B—C25B | 1.366 (9) |
C9—C10 | 1.396 (3) | C24B—H242 | 0.9500 |
C9—H9 | 0.9500 | C25B—C26B | 1.401 (8) |
C10—C11 | 1.389 (4) | C25B—H252 | 0.9500 |
C10—C27 | 1.504 (4) | C26B—H263 | 0.9500 |
C11—C12 | 1.382 (4) | C28B—H284 | 0.9800 |
C11—H11 | 0.9500 | C28B—H285 | 0.9800 |
C12—C13 | 1.383 (3) | C28B—H286 | 0.9800 |
C12—H12 | 0.9500 | C29—C30 | 1.529 (3) |
C13—H13 | 0.9500 | C29—H291 | 0.9900 |
C27—H271 | 0.9800 | C29—H292 | 0.9900 |
C27—H272 | 0.9800 | C30—C31 | 1.522 (4) |
C27—H273 | 0.9800 | C30—H301 | 0.9900 |
O4—C14B | 1.291 (4) | C30—H302 | 0.9900 |
O4—C14A | 1.291 (4) | C31—C32 | 1.521 (4) |
O5A—C14A | 1.254 (4) | C31—H311 | 0.9900 |
O6A—C16A | 1.340 (9) | C31—H312 | 0.9900 |
O6A—H6A | 0.8400 | C32—H321 | 0.9800 |
N3A—N4A | 1.233 (10) | C32—H322 | 0.9800 |
N3A—C19A | 1.430 (10) | C32—H323 | 0.9800 |
N4A—C21A | 1.450 (8) | C33—C34 | 1.527 (4) |
C14A—C15A | 1.485 (11) | C33—H331 | 0.9900 |
C15A—C20A | 1.395 (10) | C33—H332 | 0.9900 |
C15A—C16A | 1.405 (10) | C34—C35 | 1.504 (4) |
C16A—C17A | 1.401 (10) | C34—H341 | 0.9900 |
C17A—C18A | 1.365 (8) | C34—H342 | 0.9900 |
C17A—H171 | 0.9500 | C35—C36 | 1.516 (4) |
C18A—C19A | 1.393 (8) | C35—H351 | 0.9900 |
C18A—H181 | 0.9500 | C35—H352 | 0.9900 |
C19A—C20A | 1.382 (9) | C36—H361 | 0.9800 |
C20A—H201 | 0.9500 | C36—H362 | 0.9800 |
C21A—C22A | 1.375 (10) | C36—H363 | 0.9800 |
C21A—C26A | 1.399 (9) | C37—C39ii | 1.360 (5) |
C22A—C23A | 1.401 (11) | C37—C38 | 1.546 (6) |
C22A—H221 | 0.9500 | C37—H371 | 0.9900 |
C23A—C24A | 1.386 (11) | C37—H372 | 0.9900 |
C23A—C28A | 1.508 (11) | C38—C39 | 1.453 (5) |
C24A—C25A | 1.374 (11) | C38—H381 | 0.9900 |
C24A—H241 | 0.9500 | C38—H382 | 0.9900 |
C25A—C26A | 1.390 (9) | C39—H391 | 0.9900 |
C25A—H25A | 0.9500 | C39—H392 | 0.9900 |
O1—Sn1—O2 | 53.93 (5) | C23A—C28A—H283 | 109.5 |
O1—Sn1—O4 | 82.76 (6) | H281—C28A—H283 | 109.5 |
O1—Sn1—O5A | 135.8 (3) | H282—C28A—H283 | 109.5 |
O1—Sn1—O5B | 135.6 (2) | C14B—O5B—Sn1 | 84.7 (9) |
O1—Sn1—C29 | 103.65 (9) | C16B—O6B—H6B | 109.5 |
O1—Sn1—C33 | 109.89 (9) | N4B—N3B—C19B | 114.4 (5) |
O2—Sn1—O4 | 136.44 (6) | N3B—N4B—C21B | 112.5 (7) |
O2—Sn1—O5A | 167.5 (4) | O5B—C14B—O4 | 114.3 (11) |
O2—Sn1—O5B | 169.5 (3) | O5B—C14B—C15B | 122.5 (10) |
O2—Sn1—C29 | 92.83 (8) | O4—C14B—C15B | 123.1 (8) |
O2—Sn1—C33 | 87.56 (9) | C20B—C15B—C16B | 119.4 (7) |
O4—Sn1—O5A | 53.3 (3) | C20B—C15B—C14B | 120.1 (7) |
O4—Sn1—O5B | 52.9 (2) | C16B—C15B—C14B | 120.5 (6) |
O4—Sn1—C29 | 102.85 (9) | O6B—C16B—C17B | 117.4 (6) |
O4—Sn1—C33 | 105.25 (9) | O6B—C16B—C15B | 122.8 (7) |
O5A—Sn1—C29 | 91.6 (6) | C17B—C16B—C15B | 119.7 (6) |
O5A—Sn1—C33 | 81.4 (6) | C18B—C17B—C16B | 120.2 (5) |
O5B—Sn1—C29 | 88.7 (5) | C18B—C17B—H172 | 119.9 |
O5B—Sn1—C33 | 84.4 (5) | C16B—C17B—H172 | 119.9 |
C29—Sn1—C33 | 138.31 (10) | C17B—C18B—C19B | 121.2 (5) |
C1—O1—Sn1 | 105.49 (14) | C17B—C18B—H182 | 119.4 |
C1—O2—Sn1 | 81.66 (14) | C19B—C18B—H182 | 119.4 |
C3—O3—H3 | 105 (3) | C20B—C19B—C18B | 119.0 (5) |
N2—N1—C6 | 114.6 (2) | C20B—C19B—N3B | 125.8 (6) |
N1—N2—C8 | 113.7 (2) | C18B—C19B—N3B | 115.3 (5) |
O2—C1—O1 | 118.9 (2) | C19B—C20B—C15B | 120.5 (6) |
O2—C1—C2 | 122.0 (2) | C19B—C20B—H202 | 119.7 |
O1—C1—C2 | 119.07 (19) | C15B—C20B—H202 | 119.7 |
C7—C2—C3 | 118.7 (2) | C22B—C21B—C26B | 119.6 (6) |
C7—C2—C1 | 120.8 (2) | C22B—C21B—N4B | 115.5 (7) |
C3—C2—C1 | 120.6 (2) | C26B—C21B—N4B | 124.9 (6) |
O3—C3—C4 | 117.3 (2) | C21B—C22B—C23B | 121.1 (8) |
O3—C3—C2 | 122.9 (2) | C21B—C22B—H222 | 119.5 |
C4—C3—C2 | 119.8 (2) | C23B—C22B—H222 | 119.5 |
C5—C4—C3 | 120.9 (2) | C24B—C23B—C22B | 118.9 (8) |
C5—C4—H4 | 119.5 | C24B—C23B—C28B | 122.8 (8) |
C3—C4—H4 | 119.5 | C22B—C23B—C28B | 118.1 (9) |
C4—C5—C6 | 120.0 (2) | C25B—C24B—C23B | 120.4 (8) |
C4—C5—H5 | 120.0 | C25B—C24B—H242 | 119.8 |
C6—C5—H5 | 120.0 | C23B—C24B—H242 | 119.8 |
C7—C6—C5 | 119.5 (2) | C24B—C25B—C26B | 120.9 (7) |
C7—C6—N1 | 115.8 (2) | C24B—C25B—H252 | 119.6 |
C5—C6—N1 | 124.7 (2) | C26B—C25B—H252 | 119.6 |
C6—C7—C2 | 121.1 (2) | C21B—C26B—C25B | 119.1 (6) |
C6—C7—H7 | 119.4 | C21B—C26B—H263 | 120.5 |
C2—C7—H7 | 119.4 | C25B—C26B—H263 | 120.5 |
C9—C8—C13 | 120.1 (2) | C23B—C28B—H284 | 109.5 |
C9—C8—N2 | 115.6 (2) | C23B—C28B—H285 | 109.5 |
C13—C8—N2 | 124.3 (2) | H284—C28B—H285 | 109.5 |
C8—C9—C10 | 121.4 (2) | C23B—C28B—H286 | 109.5 |
C8—C9—H9 | 119.3 | H284—C28B—H286 | 109.5 |
C10—C9—H9 | 119.3 | H285—C28B—H286 | 109.5 |
C11—C10—C9 | 117.5 (2) | C30—C29—Sn1 | 110.95 (16) |
C11—C10—C27 | 122.2 (2) | C30—C29—H291 | 109.4 |
C9—C10—C27 | 120.3 (3) | Sn1—C29—H291 | 109.4 |
C12—C11—C10 | 121.3 (2) | C30—C29—H292 | 109.4 |
C12—C11—H11 | 119.4 | Sn1—C29—H292 | 109.4 |
C10—C11—H11 | 119.4 | H291—C29—H292 | 108.0 |
C11—C12—C13 | 120.7 (3) | C31—C30—C29 | 113.1 (2) |
C11—C12—H12 | 119.6 | C31—C30—H301 | 109.0 |
C13—C12—H12 | 119.6 | C29—C30—H301 | 109.0 |
C12—C13—C8 | 119.0 (2) | C31—C30—H302 | 109.0 |
C12—C13—H13 | 120.5 | C29—C30—H302 | 109.0 |
C8—C13—H13 | 120.5 | H301—C30—H302 | 107.8 |
C10—C27—H271 | 109.5 | C32—C31—C30 | 111.2 (2) |
C10—C27—H272 | 109.5 | C32—C31—H311 | 109.4 |
H271—C27—H272 | 109.5 | C30—C31—H311 | 109.4 |
C10—C27—H273 | 109.5 | C32—C31—H312 | 109.4 |
H271—C27—H273 | 109.5 | C30—C31—H312 | 109.4 |
H272—C27—H273 | 109.5 | H311—C31—H312 | 108.0 |
C14B—O4—Sn1 | 108.0 (5) | C31—C32—H321 | 109.5 |
C14A—O4—Sn1 | 105.1 (6) | C31—C32—H322 | 109.5 |
C14A—O5A—Sn1 | 73.6 (12) | H321—C32—H322 | 109.5 |
C16A—O6A—H6A | 109.5 | C31—C32—H323 | 109.5 |
N4A—N3A—C19A | 115.7 (9) | H321—C32—H323 | 109.5 |
N3A—N4A—C21A | 113.1 (7) | H322—C32—H323 | 109.5 |
O5A—C14A—O4 | 128.0 (15) | C34—C33—Sn1 | 114.74 (18) |
O5A—C14A—C15A | 121.5 (13) | C34—C33—H331 | 108.6 |
O4—C14A—C15A | 110.0 (9) | Sn1—C33—H331 | 108.6 |
C20A—C15A—C16A | 119.0 (9) | C34—C33—H332 | 108.6 |
C20A—C15A—C14A | 120.6 (9) | Sn1—C33—H332 | 108.6 |
C16A—C15A—C14A | 120.3 (8) | H331—C33—H332 | 107.6 |
O6A—C16A—C17A | 116.3 (8) | C35—C34—C33 | 113.1 (2) |
O6A—C16A—C15A | 123.1 (9) | C35—C34—H341 | 109.0 |
C17A—C16A—C15A | 120.6 (8) | C33—C34—H341 | 109.0 |
C18A—C17A—C16A | 118.7 (7) | C35—C34—H342 | 109.0 |
C18A—C17A—H171 | 120.6 | C33—C34—H342 | 109.0 |
C16A—C17A—H171 | 120.7 | H341—C34—H342 | 107.8 |
C17A—C18A—C19A | 121.8 (6) | C34—C35—C36 | 112.8 (3) |
C17A—C18A—H181 | 119.1 | C34—C35—H351 | 109.0 |
C19A—C18A—H181 | 119.1 | C36—C35—H351 | 109.0 |
C20A—C19A—C18A | 119.7 (6) | C34—C35—H352 | 109.0 |
C20A—C19A—N3A | 114.9 (7) | C36—C35—H352 | 109.0 |
C18A—C19A—N3A | 125.4 (7) | H351—C35—H352 | 107.8 |
C19A—C20A—C15A | 120.1 (8) | C35—C36—H361 | 109.5 |
C19A—C20A—H201 | 119.9 | C35—C36—H362 | 109.5 |
C15A—C20A—H201 | 119.9 | H361—C36—H362 | 109.5 |
C22A—C21A—C26A | 121.5 (8) | C35—C36—H363 | 109.5 |
C22A—C21A—N4A | 123.1 (8) | H361—C36—H363 | 109.5 |
C26A—C21A—N4A | 115.4 (7) | H362—C36—H363 | 109.5 |
C21A—C22A—C23A | 120.2 (11) | C39ii—C37—C38 | 106.1 (5) |
C21A—C22A—H221 | 119.9 | C39ii—C37—H371 | 110.5 |
C23A—C22A—H221 | 119.9 | C38—C37—H371 | 110.5 |
C24A—C23A—C22A | 117.5 (10) | C39ii—C37—H372 | 110.5 |
C24A—C23A—C28A | 119.9 (10) | C38—C37—H372 | 110.5 |
C22A—C23A—C28A | 122.1 (11) | H371—C37—H372 | 108.7 |
C25A—C24A—C23A | 122.8 (10) | C39—C38—C37 | 117.5 (4) |
C25A—C24A—H241 | 118.6 | C39—C38—H381 | 107.9 |
C23A—C24A—H241 | 118.6 | C37—C38—H381 | 107.9 |
C24A—C25A—C26A | 119.6 (9) | C39—C38—H382 | 107.9 |
C24A—C25A—H25A | 120.2 | C37—C38—H382 | 107.9 |
C26A—C25A—H25A | 120.2 | H381—C38—H382 | 107.2 |
C25A—C26A—C21A | 118.4 (8) | C37ii—C39—C38 | 116.0 (4) |
C25A—C26A—H261 | 120.8 | C37ii—C39—H391 | 108.3 |
C21A—C26A—H261 | 120.8 | C38—C39—H391 | 108.3 |
C23A—C28A—H281 | 109.5 | C37ii—C39—H392 | 108.3 |
C23A—C28A—H282 | 109.5 | C38—C39—H392 | 108.3 |
H281—C28A—H282 | 109.5 | H391—C39—H392 | 107.4 |
C6—N1—N2—C8 | 179.1 (2) | N3A—C19A—C20A—C15A | −179.4 (15) |
Sn1—O2—C1—O1 | −0.6 (2) | C16A—C15A—C20A—C19A | 1 (2) |
Sn1—O2—C1—C2 | 178.0 (2) | C14A—C15A—C20A—C19A | −179 (2) |
Sn1—O1—C1—O2 | 0.7 (3) | N3A—N4A—C21A—C22A | 0.5 (16) |
Sn1—O1—C1—C2 | −177.90 (18) | N3A—N4A—C21A—C26A | −178.1 (10) |
O2—C1—C2—C7 | 176.8 (2) | C26A—C21A—C22A—C23A | −3 (3) |
O1—C1—C2—C7 | −4.6 (4) | N4A—C21A—C22A—C23A | 179 (2) |
O2—C1—C2—C3 | −2.9 (4) | C21A—C22A—C23A—C24A | 3 (5) |
O1—C1—C2—C3 | 175.7 (2) | C21A—C22A—C23A—C28A | 175 (2) |
C7—C2—C3—O3 | −178.8 (2) | C22A—C23A—C24A—C25A | −2 (4) |
C1—C2—C3—O3 | 0.9 (4) | C28A—C23A—C24A—C25A | −174 (2) |
C7—C2—C3—C4 | 2.0 (4) | C23A—C24A—C25A—C26A | 1 (2) |
C1—C2—C3—C4 | −178.3 (2) | C24A—C25A—C26A—C21A | −0.3 (14) |
O3—C3—C4—C5 | 179.6 (2) | C22A—C21A—C26A—C25A | 1.3 (15) |
C2—C3—C4—C5 | −1.1 (4) | N4A—C21A—C26A—C25A | 179.9 (7) |
C3—C4—C5—C6 | −0.6 (4) | C19B—N3B—N4B—C21B | 179.3 (7) |
C4—C5—C6—C7 | 1.3 (4) | Sn1—O5B—C14B—O4 | −2.1 (19) |
C4—C5—C6—N1 | −179.3 (2) | Sn1—O5B—C14B—C15B | −180 (2) |
N2—N1—C6—C7 | 179.8 (2) | Sn1—O4—C14B—O5B | 3 (2) |
N2—N1—C6—C5 | 0.4 (4) | Sn1—O4—C14B—C15B | −179.5 (19) |
C5—C6—C7—C2 | −0.3 (4) | O5B—C14B—C15B—C20B | −179 (2) |
N1—C6—C7—C2 | −179.8 (2) | O4—C14B—C15B—C20B | 4 (3) |
C3—C2—C7—C6 | −1.3 (4) | O5B—C14B—C15B—C16B | −2 (3) |
C1—C2—C7—C6 | 179.0 (2) | O4—C14B—C15B—C16B | −179.1 (18) |
N1—N2—C8—C9 | −176.3 (2) | C20B—C15B—C16B—O6B | 179.6 (12) |
N1—N2—C8—C13 | 3.3 (4) | C14B—C15B—C16B—O6B | 2 (2) |
C13—C8—C9—C10 | −0.3 (4) | C20B—C15B—C16B—C17B | 0.6 (18) |
N2—C8—C9—C10 | 179.3 (2) | C14B—C15B—C16B—C17B | −176.8 (16) |
C8—C9—C10—C11 | 0.5 (4) | O6B—C16B—C17B—C18B | −178.2 (8) |
C8—C9—C10—C27 | −179.5 (3) | C15B—C16B—C17B—C18B | 0.8 (13) |
C9—C10—C11—C12 | −1.1 (4) | C16B—C17B—C18B—C19B | −0.7 (9) |
C27—C10—C11—C12 | 178.9 (3) | C17B—C18B—C19B—C20B | −0.9 (9) |
C10—C11—C12—C13 | 1.5 (4) | C17B—C18B—C19B—N3B | 179.5 (5) |
C11—C12—C13—C8 | −1.2 (4) | N4B—N3B—C19B—C20B | 4.0 (10) |
C9—C8—C13—C12 | 0.6 (4) | N4B—N3B—C19B—C18B | −176.5 (8) |
N2—C8—C13—C12 | −178.9 (2) | C18B—C19B—C20B—C15B | 2.3 (12) |
C19A—N3A—N4A—C21A | −179.0 (10) | N3B—C19B—C20B—C15B | −178.1 (9) |
Sn1—O5A—C14A—O4 | 1 (3) | C16B—C15B—C20B—C19B | −2.2 (17) |
Sn1—O5A—C14A—C15A | 173 (3) | C14B—C15B—C20B—C19B | 175.2 (16) |
Sn1—O4—C14A—O5A | −1 (4) | N3B—N4B—C21B—C22B | −179.9 (10) |
Sn1—O4—C14A—C15A | −174.0 (19) | N3B—N4B—C21B—C26B | −2.0 (14) |
O5A—C14A—C15A—C20A | −179 (3) | C26B—C21B—C22B—C23B | 3 (2) |
O4—C14A—C15A—C20A | −6 (4) | N4B—C21B—C22B—C23B | −179 (2) |
O5A—C14A—C15A—C16A | 1 (4) | C21B—C22B—C23B—C24B | −3 (4) |
O4—C14A—C15A—C16A | 174 (2) | C21B—C22B—C23B—C28B | −178.4 (15) |
C20A—C15A—C16A—O6A | 177.7 (15) | C22B—C23B—C24B—C25B | 2 (3) |
C14A—C15A—C16A—O6A | −3 (3) | C28B—C23B—C24B—C25B | 177.4 (18) |
C20A—C15A—C16A—C17A | −2 (2) | C23B—C24B—C25B—C26B | −1.3 (19) |
C14A—C15A—C16A—C17A | 177 (2) | C22B—C21B—C26B—C25B | −1.8 (11) |
O6A—C16A—C17A—C18A | −177.7 (10) | N4B—C21B—C26B—C25B | −179.6 (8) |
C15A—C16A—C17A—C18A | 2.4 (18) | C24B—C25B—C26B—C21B | 1.1 (11) |
C16A—C17A—C18A—C19A | −0.4 (12) | Sn1—C29—C30—C31 | −179.94 (18) |
C17A—C18A—C19A—C20A | −1.4 (11) | C29—C30—C31—C32 | 179.6 (2) |
C17A—C18A—C19A—N3A | 179.4 (11) | Sn1—C33—C34—C35 | −174.66 (19) |
N4A—N3A—C19A—C20A | 177.4 (11) | C33—C34—C35—C36 | −174.4 (2) |
N4A—N3A—C19A—C18A | −3.5 (19) | C39ii—C37—C38—C39 | −48.3 (6) |
C18A—C19A—C20A—C15A | 1.4 (16) | C37—C38—C39—C37ii | 53.0 (7) |
Symmetry codes: (i) −x+2, −y+1, −z; (ii) −x+2, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3···O2 | 0.78 (3) | 1.91 (3) | 2.623 (3) | 153 (3) |
O3—H3···O2i | 0.78 (3) | 2.44 (3) | 2.872 (3) | 117 (3) |
O6A—H6A···O5A | 0.84 | 1.90 | 2.62 (3) | 144 |
O6B—H6B···O5B | 0.84 | 1.90 | 2.64 (2) | 146 |
Symmetry code: (i) −x+2, −y+1, −z. |
[Sn(C7H7)2(C13H8BrN2O3)2] | F(000) = 1864 |
Mr = 941.19 | Dx = 1.686 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 13.6816 (1) Å | Cell parameters from 89697 reflections |
b = 12.5767 (1) Å | θ = 2.0–30.0° |
c = 22.5401 (2) Å | µ = 2.90 mm−1 |
β = 107.0174 (6)° | T = 160 K |
V = 3708.65 (5) Å3 | Tablet, orange |
Z = 4 | 0.25 × 0.15 × 0.10 mm |
Nonius KappaCCD area detector diffractometer | 10845 independent reflections |
Radiation source: Nonius FR590 sealed tube generator | 8598 reflections with I > 2σ(I) |
Horizontally mounted graphite crystal monochromator | Rint = 0.059 |
Detector resolution: 9 pixels mm-1 | θmax = 30.0°, θmin = 2.0° |
φ and ω scans with κ offsets | h = −19→19 |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | k = −17→16 |
Tmin = 0.652, Tmax = 0.843 | l = −31→31 |
107473 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.032 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.076 | w = 1/[σ2(Fo2) + (0.0342P)2 + 2.2611P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max = 0.002 |
10845 reflections | Δρmax = 0.69 e Å−3 |
487 parameters | Δρmin = −0.87 e Å−3 |
0 restraints | Extinction correction: SHELXL2018 (Sheldrick 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00044 (10) |
Experimental. Data collection and full structure determination done by Prof. Anthony Linden: anthony.linden@chem.uzh.ch Solvent used: benzene Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: on a glass fibre Mosaicity (deg.): 0.497 (1) Frames collected: 621 Seconds exposure per frame: 42 Degrees rotation per frame: 1.4 Crystal-detector distance (mm): 33.0 Client: Tushar Basu Sample code: TSBB-116 (L0503) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Sn1 | 1.12288 (2) | 0.92949 (2) | 0.21744 (2) | 0.02364 (5) | |
Br1 | 0.35337 (2) | 0.38616 (2) | −0.16642 (2) | 0.04522 (8) | |
Br2 | 0.24024 (2) | 1.11571 (2) | −0.12676 (2) | 0.04297 (7) | |
O1 | 1.03424 (11) | 0.81362 (11) | 0.15792 (7) | 0.0267 (3) | |
O2 | 1.18264 (11) | 0.73803 (12) | 0.20301 (7) | 0.0295 (3) | |
O3 | 1.21624 (12) | 0.54381 (14) | 0.17681 (8) | 0.0341 (4) | |
H3 | 1.227 (2) | 0.600 (2) | 0.1896 (14) | 0.043 (9)* | |
O4 | 0.99008 (11) | 1.02063 (12) | 0.17848 (7) | 0.0287 (3) | |
O5 | 1.10390 (12) | 1.12542 (12) | 0.23962 (7) | 0.0336 (4) | |
O6 | 1.06615 (14) | 1.32629 (15) | 0.24788 (9) | 0.0413 (4) | |
H6 | 1.095 (2) | 1.273 (3) | 0.2523 (14) | 0.048 (9)* | |
N1 | 0.81504 (14) | 0.53194 (15) | 0.02420 (8) | 0.0293 (4) | |
N2 | 0.79016 (14) | 0.44594 (15) | −0.00499 (9) | 0.0312 (4) | |
N3 | 0.67967 (13) | 1.26118 (15) | 0.08248 (8) | 0.0290 (4) | |
N4 | 0.66500 (14) | 1.17649 (15) | 0.05176 (9) | 0.0304 (4) | |
C1 | 1.09302 (15) | 0.73155 (16) | 0.16653 (9) | 0.0241 (4) | |
C2 | 1.05433 (16) | 0.63236 (16) | 0.13312 (9) | 0.0246 (4) | |
C3 | 1.11879 (16) | 0.54387 (17) | 0.13959 (10) | 0.0275 (4) | |
C4 | 1.08292 (18) | 0.45075 (18) | 0.10642 (11) | 0.0336 (5) | |
H4 | 1.126847 | 0.390942 | 0.110629 | 0.040* | |
C5 | 0.98481 (18) | 0.44523 (18) | 0.06788 (11) | 0.0326 (5) | |
H5 | 0.961411 | 0.381945 | 0.045143 | 0.039* | |
C6 | 0.91881 (16) | 0.53244 (18) | 0.06183 (10) | 0.0283 (4) | |
C7 | 0.95369 (16) | 0.62502 (16) | 0.09410 (9) | 0.0261 (4) | |
H7 | 0.909103 | 0.684281 | 0.089839 | 0.031* | |
C8 | 0.68605 (16) | 0.43989 (17) | −0.04158 (10) | 0.0282 (4) | |
C9 | 0.66170 (19) | 0.35179 (19) | −0.08038 (11) | 0.0353 (5) | |
H9 | 0.713574 | 0.302189 | −0.081361 | 0.042* | |
C10 | 0.56283 (18) | 0.33562 (19) | −0.11754 (11) | 0.0347 (5) | |
H10 | 0.546201 | 0.275366 | −0.144009 | 0.042* | |
C11 | 0.48879 (17) | 0.40869 (18) | −0.11544 (10) | 0.0312 (5) | |
C12 | 0.51050 (17) | 0.49732 (18) | −0.07683 (10) | 0.0316 (5) | |
H12 | 0.458157 | 0.546255 | −0.075751 | 0.038* | |
C13 | 0.61031 (17) | 0.51274 (18) | −0.03988 (10) | 0.0313 (5) | |
H13 | 0.626884 | 0.573038 | −0.013445 | 0.038* | |
C14 | 1.01655 (16) | 1.11307 (17) | 0.20191 (10) | 0.0270 (4) | |
C15 | 0.94456 (15) | 1.20272 (16) | 0.18346 (9) | 0.0246 (4) | |
C16 | 0.97321 (17) | 1.30496 (17) | 0.20791 (10) | 0.0295 (4) | |
C17 | 0.90408 (19) | 1.38837 (18) | 0.19048 (11) | 0.0348 (5) | |
H17 | 0.922534 | 1.457432 | 0.207046 | 0.042* | |
C18 | 0.80892 (18) | 1.37121 (18) | 0.14927 (11) | 0.0312 (5) | |
H18 | 0.762175 | 1.428724 | 0.137696 | 0.037* | |
C19 | 0.78022 (16) | 1.27034 (17) | 0.12426 (9) | 0.0258 (4) | |
C20 | 0.84821 (15) | 1.18649 (17) | 0.14157 (9) | 0.0252 (4) | |
H20 | 0.829109 | 1.117652 | 0.124835 | 0.030* | |
C21 | 0.56306 (16) | 1.16501 (18) | 0.01224 (10) | 0.0289 (4) | |
C22 | 0.47863 (17) | 1.21300 (19) | 0.02333 (11) | 0.0338 (5) | |
H22 | 0.487192 | 1.256449 | 0.058965 | 0.041* | |
C23 | 0.38202 (18) | 1.1977 (2) | −0.01744 (12) | 0.0371 (5) | |
H23 | 0.324028 | 1.230242 | −0.010048 | 0.045* | |
C24 | 0.37124 (17) | 1.13422 (18) | −0.06909 (11) | 0.0326 (5) | |
C25 | 0.45375 (19) | 1.0834 (2) | −0.07959 (11) | 0.0382 (5) | |
H25 | 0.444656 | 1.038832 | −0.114839 | 0.046* | |
C26 | 0.55027 (19) | 1.0977 (2) | −0.03824 (12) | 0.0364 (5) | |
H26 | 0.607427 | 1.061489 | −0.044466 | 0.044* | |
C27 | 1.23394 (17) | 0.9824 (2) | 0.17457 (11) | 0.0345 (5) | |
H271 | 1.274498 | 1.040539 | 0.199706 | 0.041* | |
H272 | 1.281210 | 0.923037 | 0.174009 | 0.041* | |
C28 | 1.18727 (16) | 1.02131 (18) | 0.10939 (10) | 0.0289 (4) | |
C29 | 1.15565 (19) | 1.1265 (2) | 0.09827 (11) | 0.0367 (5) | |
H29 | 1.163412 | 1.173705 | 0.132262 | 0.044* | |
C30 | 1.1131 (2) | 1.1634 (2) | 0.03845 (12) | 0.0470 (7) | |
H30 | 1.091423 | 1.235306 | 0.031672 | 0.056* | |
C31 | 1.1021 (2) | 1.0965 (3) | −0.01115 (13) | 0.0511 (7) | |
H31 | 1.073282 | 1.122162 | −0.052203 | 0.061* | |
C32 | 1.1324 (2) | 0.9933 (3) | −0.00152 (13) | 0.0537 (8) | |
H32 | 1.124292 | 0.946947 | −0.035900 | 0.064* | |
C33 | 1.1756 (2) | 0.9551 (2) | 0.05899 (13) | 0.0436 (6) | |
H33 | 1.197067 | 0.883071 | 0.065309 | 0.052* | |
C34 | 1.11013 (17) | 0.88479 (18) | 0.30603 (10) | 0.0295 (5) | |
H341 | 1.177731 | 0.861067 | 0.332684 | 0.035* | |
H342 | 1.089104 | 0.947379 | 0.325971 | 0.035* | |
C35 | 1.03402 (16) | 0.79736 (17) | 0.30103 (9) | 0.0262 (4) | |
C36 | 1.06646 (18) | 0.69271 (18) | 0.31317 (11) | 0.0316 (5) | |
H36 | 1.137571 | 0.677401 | 0.326086 | 0.038* | |
C37 | 0.9968 (2) | 0.6103 (2) | 0.30672 (12) | 0.0387 (5) | |
H37 | 1.020131 | 0.539084 | 0.314606 | 0.046* | |
C38 | 0.89273 (19) | 0.6322 (2) | 0.28872 (11) | 0.0376 (5) | |
H38 | 0.844633 | 0.576106 | 0.284560 | 0.045* | |
C39 | 0.85972 (18) | 0.7355 (2) | 0.27695 (10) | 0.0355 (5) | |
H39 | 0.788575 | 0.750619 | 0.264705 | 0.043* | |
C40 | 0.92922 (17) | 0.81773 (19) | 0.28278 (10) | 0.0308 (5) | |
H40 | 0.905311 | 0.888640 | 0.274277 | 0.037* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sn1 | 0.02239 (7) | 0.01846 (7) | 0.02550 (7) | −0.00111 (5) | −0.00014 (5) | 0.00225 (5) |
Br1 | 0.03174 (13) | 0.03595 (14) | 0.05510 (16) | −0.00582 (10) | −0.00740 (11) | −0.00544 (11) |
Br2 | 0.03208 (13) | 0.04611 (16) | 0.04141 (14) | −0.00977 (11) | −0.00380 (10) | 0.00158 (11) |
O1 | 0.0273 (7) | 0.0195 (7) | 0.0282 (7) | 0.0003 (6) | 0.0004 (6) | −0.0008 (6) |
O2 | 0.0267 (7) | 0.0252 (8) | 0.0304 (8) | −0.0004 (6) | −0.0010 (6) | −0.0007 (6) |
O3 | 0.0263 (8) | 0.0271 (9) | 0.0392 (9) | 0.0044 (7) | −0.0054 (7) | −0.0047 (7) |
O4 | 0.0254 (7) | 0.0202 (7) | 0.0346 (8) | 0.0010 (6) | −0.0005 (6) | −0.0005 (6) |
O5 | 0.0284 (8) | 0.0264 (8) | 0.0360 (8) | −0.0014 (6) | −0.0063 (6) | 0.0032 (6) |
O6 | 0.0376 (9) | 0.0239 (9) | 0.0475 (10) | −0.0030 (7) | −0.0112 (8) | −0.0047 (7) |
N1 | 0.0283 (9) | 0.0261 (9) | 0.0290 (9) | −0.0018 (7) | 0.0013 (7) | −0.0022 (7) |
N2 | 0.0278 (9) | 0.0276 (10) | 0.0329 (10) | −0.0019 (7) | 0.0007 (7) | −0.0043 (7) |
N3 | 0.0253 (9) | 0.0277 (10) | 0.0311 (9) | 0.0030 (7) | 0.0038 (7) | 0.0010 (7) |
N4 | 0.0270 (9) | 0.0289 (10) | 0.0316 (9) | 0.0032 (7) | 0.0028 (7) | −0.0013 (7) |
C1 | 0.0254 (10) | 0.0224 (10) | 0.0225 (9) | 0.0000 (8) | 0.0041 (7) | −0.0003 (7) |
C2 | 0.0259 (10) | 0.0215 (10) | 0.0238 (9) | −0.0012 (8) | 0.0032 (8) | 0.0011 (7) |
C3 | 0.0235 (10) | 0.0259 (11) | 0.0294 (10) | 0.0019 (8) | 0.0020 (8) | 0.0003 (8) |
C4 | 0.0292 (11) | 0.0256 (12) | 0.0416 (13) | 0.0052 (9) | 0.0033 (9) | −0.0048 (9) |
C5 | 0.0322 (11) | 0.0255 (11) | 0.0355 (12) | 0.0004 (9) | 0.0028 (9) | −0.0079 (9) |
C6 | 0.0254 (10) | 0.0280 (11) | 0.0276 (10) | −0.0003 (8) | 0.0019 (8) | −0.0004 (8) |
C7 | 0.0265 (10) | 0.0214 (10) | 0.0270 (10) | 0.0012 (8) | 0.0024 (8) | 0.0013 (8) |
C8 | 0.0276 (10) | 0.0247 (11) | 0.0280 (10) | −0.0039 (8) | 0.0016 (8) | 0.0004 (8) |
C9 | 0.0357 (12) | 0.0250 (11) | 0.0402 (13) | 0.0013 (9) | 0.0035 (10) | −0.0042 (9) |
C10 | 0.0354 (12) | 0.0247 (11) | 0.0372 (12) | −0.0061 (9) | 0.0000 (10) | −0.0049 (9) |
C11 | 0.0275 (11) | 0.0288 (12) | 0.0319 (11) | −0.0066 (9) | 0.0001 (9) | 0.0029 (9) |
C12 | 0.0291 (11) | 0.0296 (12) | 0.0340 (11) | −0.0008 (9) | 0.0059 (9) | −0.0014 (9) |
C13 | 0.0311 (11) | 0.0276 (12) | 0.0326 (11) | −0.0027 (9) | 0.0051 (9) | −0.0046 (9) |
C14 | 0.0276 (10) | 0.0213 (10) | 0.0282 (10) | −0.0017 (8) | 0.0018 (8) | 0.0025 (8) |
C15 | 0.0261 (10) | 0.0199 (10) | 0.0245 (9) | −0.0011 (8) | 0.0026 (8) | −0.0001 (7) |
C16 | 0.0304 (11) | 0.0244 (11) | 0.0284 (10) | −0.0034 (9) | 0.0005 (8) | −0.0010 (8) |
C17 | 0.0417 (13) | 0.0190 (10) | 0.0390 (12) | −0.0016 (9) | 0.0044 (10) | −0.0053 (9) |
C18 | 0.0332 (11) | 0.0230 (11) | 0.0362 (12) | 0.0051 (9) | 0.0082 (9) | −0.0004 (9) |
C19 | 0.0253 (10) | 0.0270 (11) | 0.0230 (9) | 0.0016 (8) | 0.0035 (8) | −0.0001 (8) |
C20 | 0.0262 (10) | 0.0209 (10) | 0.0261 (10) | 0.0000 (8) | 0.0039 (8) | −0.0007 (8) |
C21 | 0.0271 (10) | 0.0262 (11) | 0.0293 (11) | −0.0006 (9) | 0.0020 (8) | 0.0004 (8) |
C22 | 0.0307 (11) | 0.0328 (12) | 0.0350 (12) | 0.0011 (9) | 0.0048 (9) | −0.0064 (9) |
C23 | 0.0265 (11) | 0.0364 (13) | 0.0451 (14) | 0.0014 (10) | 0.0051 (10) | −0.0054 (10) |
C24 | 0.0277 (11) | 0.0296 (12) | 0.0339 (11) | −0.0059 (9) | −0.0010 (9) | 0.0026 (9) |
C25 | 0.0392 (13) | 0.0402 (14) | 0.0330 (12) | −0.0060 (11) | 0.0071 (10) | −0.0088 (10) |
C26 | 0.0324 (12) | 0.0358 (13) | 0.0410 (13) | 0.0004 (10) | 0.0105 (10) | −0.0084 (10) |
C27 | 0.0256 (11) | 0.0349 (13) | 0.0386 (12) | −0.0025 (9) | 0.0024 (9) | 0.0129 (10) |
C28 | 0.0229 (10) | 0.0300 (12) | 0.0331 (11) | 0.0002 (9) | 0.0069 (8) | 0.0052 (9) |
C29 | 0.0399 (13) | 0.0337 (13) | 0.0346 (12) | 0.0034 (10) | 0.0080 (10) | 0.0069 (10) |
C30 | 0.0483 (15) | 0.0506 (17) | 0.0422 (14) | 0.0141 (13) | 0.0135 (12) | 0.0193 (12) |
C31 | 0.0479 (16) | 0.070 (2) | 0.0322 (13) | 0.0005 (14) | 0.0074 (11) | 0.0115 (13) |
C32 | 0.0634 (19) | 0.066 (2) | 0.0359 (14) | −0.0111 (16) | 0.0215 (13) | −0.0134 (13) |
C33 | 0.0518 (16) | 0.0363 (14) | 0.0482 (15) | 0.0037 (12) | 0.0234 (13) | −0.0030 (11) |
C34 | 0.0322 (11) | 0.0263 (11) | 0.0261 (10) | −0.0051 (9) | 0.0024 (8) | −0.0019 (8) |
C35 | 0.0296 (10) | 0.0254 (11) | 0.0220 (9) | −0.0021 (8) | 0.0050 (8) | −0.0015 (8) |
C36 | 0.0305 (11) | 0.0281 (11) | 0.0357 (12) | 0.0009 (9) | 0.0090 (9) | 0.0041 (9) |
C37 | 0.0447 (14) | 0.0257 (12) | 0.0461 (14) | −0.0028 (10) | 0.0141 (11) | 0.0042 (10) |
C38 | 0.0384 (13) | 0.0363 (13) | 0.0392 (13) | −0.0131 (10) | 0.0134 (10) | −0.0024 (10) |
C39 | 0.0275 (11) | 0.0452 (15) | 0.0329 (12) | −0.0034 (10) | 0.0072 (9) | −0.0028 (10) |
C40 | 0.0315 (11) | 0.0279 (11) | 0.0309 (11) | 0.0010 (9) | 0.0060 (9) | −0.0006 (9) |
Sn1—O1 | 2.1077 (14) | C16—C17 | 1.390 (3) |
Sn1—O2 | 2.5939 (15) | C17—C18 | 1.377 (3) |
Sn1—O4 | 2.1100 (14) | C17—H17 | 0.9500 |
Sn1—O5 | 2.5426 (16) | C18—C19 | 1.397 (3) |
Sn1—C27 | 2.132 (2) | C18—H18 | 0.9500 |
Sn1—C34 | 2.130 (2) | C19—C20 | 1.385 (3) |
Sn1—O3i | 3.0858 (16) | C20—H20 | 0.9500 |
Br1—C11 | 1.894 (2) | C21—C26 | 1.388 (3) |
Br2—C24 | 1.895 (2) | C21—C22 | 1.389 (3) |
O1—C1 | 1.288 (2) | C22—C23 | 1.385 (3) |
O2—C1 | 1.263 (2) | C22—H22 | 0.9500 |
O3—C3 | 1.352 (3) | C23—C24 | 1.383 (3) |
O3—H3 | 0.77 (3) | C23—H23 | 0.9500 |
O4—C14 | 1.284 (3) | C24—C25 | 1.377 (4) |
O5—C14 | 1.257 (2) | C25—C26 | 1.387 (3) |
O6—C16 | 1.353 (3) | C25—H25 | 0.9500 |
O6—H6 | 0.76 (3) | C26—H26 | 0.9500 |
N1—N2 | 1.260 (3) | C27—C28 | 1.502 (3) |
N1—C6 | 1.425 (3) | C27—H271 | 0.9900 |
N2—C8 | 1.424 (3) | C27—H272 | 0.9900 |
N3—N4 | 1.254 (3) | C28—C33 | 1.379 (3) |
N3—C19 | 1.426 (3) | C28—C29 | 1.392 (3) |
N4—C21 | 1.425 (3) | C29—C30 | 1.383 (3) |
C1—C2 | 1.473 (3) | C29—H29 | 0.9500 |
C2—C3 | 1.401 (3) | C30—C31 | 1.372 (4) |
C2—C7 | 1.403 (3) | C30—H30 | 0.9500 |
C3—C4 | 1.399 (3) | C31—C32 | 1.360 (5) |
C4—C5 | 1.371 (3) | C31—H31 | 0.9500 |
C4—H4 | 0.9500 | C32—C33 | 1.403 (4) |
C5—C6 | 1.402 (3) | C32—H32 | 0.9500 |
C5—H5 | 0.9500 | C33—H33 | 0.9500 |
C6—C7 | 1.382 (3) | C34—C35 | 1.496 (3) |
C7—H7 | 0.9500 | C34—H341 | 0.9900 |
C8—C9 | 1.390 (3) | C34—H342 | 0.9900 |
C8—C13 | 1.392 (3) | C35—C36 | 1.390 (3) |
C9—C10 | 1.382 (3) | C35—C40 | 1.395 (3) |
C9—H9 | 0.9500 | C36—C37 | 1.387 (3) |
C10—C11 | 1.379 (3) | C36—H36 | 0.9500 |
C10—H10 | 0.9500 | C37—C38 | 1.389 (4) |
C11—C12 | 1.392 (3) | C37—H37 | 0.9500 |
C12—C13 | 1.389 (3) | C38—C39 | 1.376 (4) |
C12—H12 | 0.9500 | C38—H38 | 0.9500 |
C13—H13 | 0.9500 | C39—C40 | 1.385 (3) |
C14—C15 | 1.475 (3) | C39—H39 | 0.9500 |
C15—C20 | 1.394 (3) | C40—H40 | 0.9500 |
C15—C16 | 1.409 (3) | ||
O1—Sn1—O2 | 54.69 (5) | C17—C16—C15 | 119.34 (19) |
O1—Sn1—O4 | 81.12 (6) | C18—C17—C16 | 120.2 (2) |
O1—Sn1—O5 | 136.25 (5) | C18—C17—H17 | 119.9 |
O1—Sn1—C27 | 106.31 (8) | C16—C17—H17 | 119.9 |
O1—Sn1—C34 | 102.97 (7) | C17—C18—C19 | 120.9 (2) |
O2—Sn1—O4 | 135.78 (5) | C17—C18—H18 | 119.6 |
O2—Sn1—O5 | 168.06 (5) | C19—C18—H18 | 119.6 |
O2—Sn1—C27 | 86.57 (8) | C20—C19—C18 | 119.44 (19) |
O2—Sn1—C34 | 89.30 (7) | C20—C19—N3 | 124.27 (19) |
O4—Sn1—O5 | 55.27 (5) | C18—C19—N3 | 116.27 (19) |
O4—Sn1—C27 | 106.44 (7) | C19—C20—C15 | 120.24 (19) |
O4—Sn1—C34 | 103.69 (8) | C19—C20—H20 | 119.9 |
O5—Sn1—C27 | 85.08 (8) | C15—C20—H20 | 119.9 |
O5—Sn1—C34 | 91.74 (7) | C26—C21—C22 | 120.0 (2) |
C27—Sn1—C34 | 140.54 (9) | C26—C21—N4 | 116.1 (2) |
O1—Sn1—O3i | 164.01 (5) | C22—C21—N4 | 123.8 (2) |
O4—Sn1—O3i | 113.64 (5) | C23—C22—C21 | 120.2 (2) |
C34—Sn1—O3i | 68.56 (7) | C23—C22—H22 | 119.9 |
C27—Sn1—O3i | 76.28 (7) | C21—C22—H22 | 119.9 |
O5—Sn1—O3i | 59.16 (5) | C24—C23—C22 | 119.0 (2) |
O2—Sn1—O3i | 110.47 (5) | C24—C23—H23 | 120.5 |
C1—O1—Sn1 | 103.93 (12) | C22—C23—H23 | 120.5 |
C1—O2—Sn1 | 81.95 (12) | C25—C24—C23 | 121.5 (2) |
C3—O3—Sn1ii | 146.18 (14) | C25—C24—Br2 | 118.91 (18) |
C3—O3—H3 | 106 (2) | C23—C24—Br2 | 119.64 (18) |
Sn1ii—O3—H3 | 97 (2) | C24—C25—C26 | 119.4 (2) |
C14—O4—Sn1 | 102.46 (12) | C24—C25—H25 | 120.3 |
C14—O5—Sn1 | 83.04 (12) | C26—C25—H25 | 120.3 |
C16—O6—H6 | 105 (2) | C25—C26—C21 | 119.8 (2) |
N2—N1—C6 | 112.60 (18) | C25—C26—H26 | 120.1 |
N1—N2—C8 | 114.82 (18) | C21—C26—H26 | 120.1 |
N4—N3—C19 | 113.63 (18) | C28—C27—Sn1 | 112.94 (14) |
N3—N4—C21 | 113.59 (18) | C28—C27—H271 | 109.0 |
O2—C1—O1 | 119.38 (18) | Sn1—C27—H271 | 109.0 |
O2—C1—C2 | 121.50 (18) | C28—C27—H272 | 109.0 |
O1—C1—C2 | 119.12 (17) | Sn1—C27—H272 | 109.0 |
C3—C2—C7 | 119.04 (19) | H271—C27—H272 | 107.8 |
C3—C2—C1 | 119.90 (18) | C33—C28—C29 | 118.1 (2) |
C7—C2—C1 | 121.06 (19) | C33—C28—C27 | 121.5 (2) |
O3—C3—C4 | 117.35 (19) | C29—C28—C27 | 120.4 (2) |
O3—C3—C2 | 122.80 (19) | C30—C29—C28 | 120.9 (2) |
C4—C3—C2 | 119.85 (19) | C30—C29—H29 | 119.5 |
C5—C4—C3 | 120.4 (2) | C28—C29—H29 | 119.5 |
C5—C4—H4 | 119.8 | C31—C30—C29 | 120.2 (3) |
C3—C4—H4 | 119.8 | C31—C30—H30 | 119.9 |
C4—C5—C6 | 120.4 (2) | C29—C30—H30 | 119.9 |
C4—C5—H5 | 119.8 | C32—C31—C30 | 120.0 (3) |
C6—C5—H5 | 119.8 | C32—C31—H31 | 120.0 |
C7—C6—C5 | 119.6 (2) | C30—C31—H31 | 120.0 |
C7—C6—N1 | 116.58 (19) | C31—C32—C33 | 120.3 (3) |
C5—C6—N1 | 123.8 (2) | C31—C32—H32 | 119.9 |
C6—C7—C2 | 120.65 (19) | C33—C32—H32 | 119.9 |
C6—C7—H7 | 119.7 | C28—C33—C32 | 120.5 (3) |
C2—C7—H7 | 119.7 | C28—C33—H33 | 119.7 |
C9—C8—C13 | 119.9 (2) | C32—C33—H33 | 119.7 |
C9—C8—N2 | 115.0 (2) | C35—C34—Sn1 | 111.69 (14) |
C13—C8—N2 | 125.13 (19) | C35—C34—H341 | 109.3 |
C10—C9—C8 | 120.7 (2) | Sn1—C34—H341 | 109.3 |
C10—C9—H9 | 119.7 | C35—C34—H342 | 109.3 |
C8—C9—H9 | 119.7 | Sn1—C34—H342 | 109.3 |
C11—C10—C9 | 118.7 (2) | H341—C34—H342 | 107.9 |
C11—C10—H10 | 120.7 | C36—C35—C40 | 118.3 (2) |
C9—C10—H10 | 120.7 | C36—C35—C34 | 120.4 (2) |
C10—C11—C12 | 122.1 (2) | C40—C35—C34 | 121.3 (2) |
C10—C11—Br1 | 118.52 (17) | C37—C36—C35 | 121.1 (2) |
C12—C11—Br1 | 119.42 (18) | C37—C36—H36 | 119.4 |
C13—C12—C11 | 118.6 (2) | C35—C36—H36 | 119.4 |
C13—C12—H12 | 120.7 | C36—C37—C38 | 119.8 (2) |
C11—C12—H12 | 120.7 | C36—C37—H37 | 120.1 |
C12—C13—C8 | 120.0 (2) | C38—C37—H37 | 120.1 |
C12—C13—H13 | 120.0 | C39—C38—C37 | 119.6 (2) |
C8—C13—H13 | 120.0 | C39—C38—H38 | 120.2 |
O5—C14—O4 | 119.19 (19) | C37—C38—H38 | 120.2 |
O5—C14—C15 | 121.37 (19) | C38—C39—C40 | 120.6 (2) |
O4—C14—C15 | 119.44 (18) | C38—C39—H39 | 119.7 |
C20—C15—C16 | 119.90 (19) | C40—C39—H39 | 119.7 |
C20—C15—C14 | 120.02 (18) | C39—C40—C35 | 120.6 (2) |
C16—C15—C14 | 120.08 (18) | C39—C40—H40 | 119.7 |
O6—C16—C17 | 117.9 (2) | C35—C40—H40 | 119.7 |
O6—C16—C15 | 122.8 (2) | ||
C6—N1—N2—C8 | 177.82 (18) | C20—C15—C16—O6 | −178.8 (2) |
C19—N3—N4—C21 | 177.10 (18) | C14—C15—C16—O6 | 0.9 (3) |
Sn1—O2—C1—O1 | 1.81 (17) | C20—C15—C16—C17 | 0.9 (3) |
Sn1—O2—C1—C2 | −178.70 (19) | C14—C15—C16—C17 | −179.4 (2) |
Sn1—O1—C1—O2 | −2.3 (2) | O6—C16—C17—C18 | 179.1 (2) |
Sn1—O1—C1—C2 | 178.23 (15) | C15—C16—C17—C18 | −0.6 (4) |
O2—C1—C2—C3 | −2.6 (3) | C16—C17—C18—C19 | −0.1 (4) |
O1—C1—C2—C3 | 176.92 (19) | C17—C18—C19—C20 | 0.5 (3) |
O2—C1—C2—C7 | 178.11 (19) | C17—C18—C19—N3 | 179.5 (2) |
O1—C1—C2—C7 | −2.4 (3) | N4—N3—C19—C20 | −15.1 (3) |
Sn1ii—O3—C3—C4 | −52.7 (3) | N4—N3—C19—C18 | 166.0 (2) |
Sn1ii—O3—C3—C2 | 127.6 (2) | C18—C19—C20—C15 | −0.2 (3) |
C7—C2—C3—O3 | −179.1 (2) | N3—C19—C20—C15 | −179.07 (19) |
C1—C2—C3—O3 | 1.6 (3) | C16—C15—C20—C19 | −0.5 (3) |
C7—C2—C3—C4 | 1.2 (3) | C14—C15—C20—C19 | 179.8 (2) |
C1—C2—C3—C4 | −178.1 (2) | N3—N4—C21—C26 | 156.8 (2) |
O3—C3—C4—C5 | 179.9 (2) | N3—N4—C21—C22 | −26.1 (3) |
C2—C3—C4—C5 | −0.4 (4) | C26—C21—C22—C23 | −2.9 (4) |
C3—C4—C5—C6 | −0.8 (4) | N4—C21—C22—C23 | −180.0 (2) |
C4—C5—C6—C7 | 1.2 (4) | C21—C22—C23—C24 | −0.1 (4) |
C4—C5—C6—N1 | −178.1 (2) | C22—C23—C24—C25 | 2.2 (4) |
N2—N1—C6—C7 | 178.1 (2) | C22—C23—C24—Br2 | −178.11 (19) |
N2—N1—C6—C5 | −2.6 (3) | C23—C24—C25—C26 | −1.4 (4) |
C5—C6—C7—C2 | −0.3 (3) | Br2—C24—C25—C26 | 179.0 (2) |
N1—C6—C7—C2 | 178.98 (19) | C24—C25—C26—C21 | −1.6 (4) |
C3—C2—C7—C6 | −0.8 (3) | C22—C21—C26—C25 | 3.8 (4) |
C1—C2—C7—C6 | 178.5 (2) | N4—C21—C26—C25 | −179.0 (2) |
N1—N2—C8—C9 | 171.5 (2) | Sn1—C27—C28—C33 | −94.1 (2) |
N1—N2—C8—C13 | −9.8 (3) | Sn1—C27—C28—C29 | 86.8 (2) |
C13—C8—C9—C10 | 0.1 (4) | C33—C28—C29—C30 | 0.5 (4) |
N2—C8—C9—C10 | 178.9 (2) | C27—C28—C29—C30 | 179.6 (2) |
C8—C9—C10—C11 | 0.1 (4) | C28—C29—C30—C31 | −0.5 (4) |
C9—C10—C11—C12 | −0.5 (4) | C29—C30—C31—C32 | 0.5 (4) |
C9—C10—C11—Br1 | −179.97 (19) | C30—C31—C32—C33 | −0.4 (5) |
C10—C11—C12—C13 | 0.7 (4) | C29—C28—C33—C32 | −0.5 (4) |
Br1—C11—C12—C13 | −179.82 (17) | C27—C28—C33—C32 | −179.6 (2) |
C11—C12—C13—C8 | −0.5 (3) | C31—C32—C33—C28 | 0.4 (4) |
C9—C8—C13—C12 | 0.1 (3) | Sn1—C34—C35—C36 | 99.9 (2) |
N2—C8—C13—C12 | −178.5 (2) | Sn1—C34—C35—C40 | −78.5 (2) |
Sn1—O5—C14—O4 | 1.63 (19) | C40—C35—C36—C37 | 0.7 (3) |
Sn1—O5—C14—C15 | −177.6 (2) | C34—C35—C36—C37 | −177.8 (2) |
Sn1—O4—C14—O5 | −2.0 (2) | C35—C36—C37—C38 | −0.9 (4) |
Sn1—O4—C14—C15 | 177.22 (16) | C36—C37—C38—C39 | 0.5 (4) |
O5—C14—C15—C20 | −180.0 (2) | C37—C38—C39—C40 | 0.1 (4) |
O4—C14—C15—C20 | 0.8 (3) | C38—C39—C40—C35 | −0.4 (3) |
O5—C14—C15—C16 | 0.3 (3) | C36—C35—C40—C39 | 0.0 (3) |
O4—C14—C15—C16 | −178.9 (2) | C34—C35—C40—C39 | 178.4 (2) |
Symmetry codes: (i) −x+5/2, y+1/2, −z+1/2; (ii) −x+5/2, y−1/2, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3···O2 | 0.77 (3) | 1.89 (3) | 2.586 (2) | 152 (3) |
O3—H3···O5ii | 0.77 (3) | 2.42 (3) | 2.818 (2) | 114 (3) |
O6—H6···O5 | 0.76 (3) | 1.89 (3) | 2.596 (2) | 153 (3) |
Symmetry code: (ii) −x+5/2, y−1/2, −z+1/2. |
[Sn(C7H7)2(C12H12NO3)2(H2O)]·2C6H6 | F(000) = 1888 |
Mr = 911.62 | Dx = 1.358 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 23.6530 (5) Å | Cell parameters from 125492 reflections |
b = 10.1034 (2) Å | θ = 2.0–30.0° |
c = 20.5952 (4) Å | µ = 0.63 mm−1 |
β = 115.0715 (12)° | T = 160 K |
V = 4458.02 (16) Å3 | Tablet, colorless |
Z = 4 | 0.25 × 0.22 × 0.10 mm |
Nonius KappaCCD area detector diffractometer | 6506 independent reflections |
Radiation source: Nonius FR590 sealed tube generator | 5193 reflections with I > 2σ(I) |
Horizontally mounted graphite crystal monochromator | Rint = 0.101 |
Detector resolution: 9 pixels mm-1 | θmax = 30.0°, θmin = 2.2° |
ω scans with κ offsets | h = −32→32 |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | k = −14→14 |
Tmin = 0.753, Tmax = 0.943 | l = −28→29 |
58583 measured reflections |
Refinement on F2 | Primary atom site location: heavy-atom method |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.056 | Hydrogen site location: mixed |
wR(F2) = 0.148 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0943P)2 + 4.7027P] where P = (Fo2 + 2Fc2)/3 |
6506 reflections | (Δ/σ)max < 0.001 |
228 parameters | Δρmax = 1.06 e Å−3 |
2 restraints | Δρmin = −2.17 e Å−3 |
Experimental. Data collection and full structure determination done by Prof. Anthony Linden: anthony.linden@chem.uzh.ch Solvent used: benzene Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: on a glass fibre Mosaicity (deg.): 1.053 (1) Frames collected: 0 Seconds exposure per frame: 33 Degrees rotation per frame: 0.0 Crystal-detector distance (mm): 0.0 Client: Tushar Basu Sample code: TSBB-192 (L0711) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. The asymmetric unit contains one half of a molecule of the Sn-complex, which sits across a two-fold axis, plus a highly disordered benzene molecule. The disordered solvent molecule could not be modelled adequately, so its contribution to the diffraction data was removed using the SQUEEZE routine of the program PLATON. When the solvent molecule is excluded from the model, there are four cavities of 324 Å3 per unit cell. The total number of electrons contributing to each void was calculated by the SQUEEZE routine to be approximately 85 e. A benzene molecule has 42 e, which suggests that the cavities have two molecules of benzene (one per asymmetric unit) and this approximation was used in the subsequent calculation of the empirical formula, formula weight, density, linear absorption coefficient and F(000). Based on the assumption, the overall ratio of Sn-complex molecules to benzene is 1:2. |
x | y | z | Uiso*/Ueq | ||
Sn1 | 0.000000 | 0.20944 (3) | 0.250000 | 0.01902 (10) | |
O1 | −0.06248 (9) | 0.0370 (2) | 0.19456 (11) | 0.0248 (4) | |
O2 | −0.10242 (10) | 0.2366 (2) | 0.16188 (12) | 0.0247 (4) | |
O3 | 0.000000 | 0.4408 (3) | 0.250000 | 0.0353 (8) | |
H3 | 0.0301 (14) | 0.476 (4) | 0.2841 (16) | 0.051 (13)* | |
O10 | −0.43538 (10) | −0.1170 (2) | −0.14546 (12) | 0.0303 (5) | |
N1 | −0.34338 (12) | −0.1205 (3) | −0.01611 (14) | 0.0255 (5) | |
H1 | −0.3581 (18) | −0.084 (4) | −0.055 (2) | 0.033 (10)* | |
C1 | −0.10849 (13) | 0.1113 (3) | 0.15772 (15) | 0.0213 (6) | |
C2 | −0.16937 (13) | 0.0487 (3) | 0.11166 (15) | 0.0222 (6) | |
C3 | −0.17658 (13) | −0.0879 (3) | 0.11204 (16) | 0.0239 (6) | |
H3A | −0.142047 | −0.141854 | 0.140536 | 0.029* | |
C4 | −0.23372 (14) | −0.1456 (3) | 0.07121 (17) | 0.0261 (6) | |
H4 | −0.238480 | −0.238854 | 0.071822 | 0.031* | |
C5 | −0.28419 (13) | −0.0668 (3) | 0.02923 (15) | 0.0236 (6) | |
C6 | −0.27703 (14) | 0.0703 (3) | 0.02811 (17) | 0.0268 (6) | |
H6 | −0.311396 | 0.124213 | −0.000880 | 0.032* | |
C7 | −0.21968 (14) | 0.1274 (3) | 0.06939 (17) | 0.0277 (6) | |
H7 | −0.214750 | 0.220631 | 0.068782 | 0.033* | |
C8 | −0.37763 (15) | −0.2072 (3) | −0.00003 (18) | 0.0291 (7) | |
C9 | −0.43476 (15) | −0.2480 (3) | −0.05114 (18) | 0.0263 (6) | |
H9 | −0.457607 | −0.310895 | −0.037549 | 0.032* | |
C10 | −0.46156 (15) | −0.2012 (3) | −0.12320 (18) | 0.0258 (6) | |
C11 | −0.52313 (16) | −0.2589 (4) | −0.17386 (18) | 0.0322 (7) | |
H11A | −0.547018 | −0.285054 | −0.146995 | 0.048* | |
H11B | −0.515815 | −0.336583 | −0.197729 | 0.048* | |
H11C | −0.546698 | −0.192478 | −0.209889 | 0.048* | |
C12 | −0.3541 (2) | −0.2594 (6) | 0.0753 (2) | 0.0541 (12) | |
H12A | −0.323563 | −0.329840 | 0.082306 | 0.081* | |
H12B | −0.389126 | −0.294807 | 0.083429 | 0.081* | |
H12C | −0.334203 | −0.187465 | 0.109331 | 0.081* | |
C13 | 0.04032 (16) | 0.2193 (4) | 0.17412 (18) | 0.0316 (7) | |
H13A | 0.069539 | 0.295146 | 0.187002 | 0.038* | |
H13B | 0.065092 | 0.137904 | 0.178904 | 0.038* | |
C14 | −0.00517 (15) | 0.2337 (3) | 0.09721 (17) | 0.0253 (6) | |
C15 | −0.03435 (18) | 0.1238 (4) | 0.0575 (2) | 0.0372 (8) | |
H15 | −0.024141 | 0.038632 | 0.078874 | 0.045* | |
C16 | −0.0783 (2) | 0.1349 (5) | −0.0130 (2) | 0.0474 (10) | |
H16 | −0.097970 | 0.058061 | −0.039592 | 0.057* | |
C17 | −0.0931 (2) | 0.2581 (6) | −0.0441 (2) | 0.0494 (11) | |
H17 | −0.124052 | 0.267139 | −0.091927 | 0.059* | |
C18 | −0.06295 (19) | 0.3685 (4) | −0.0056 (2) | 0.0436 (10) | |
H18 | −0.071962 | 0.453215 | −0.027685 | 0.052* | |
C19 | −0.01989 (18) | 0.3569 (4) | 0.06461 (19) | 0.0346 (8) | |
H19 | −0.000091 | 0.433880 | 0.090941 | 0.042* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sn1 | 0.01201 (14) | 0.02281 (16) | 0.01816 (14) | 0.000 | 0.00244 (10) | 0.000 |
O1 | 0.0133 (10) | 0.0248 (11) | 0.0282 (10) | −0.0007 (8) | 0.0008 (8) | −0.0012 (9) |
O2 | 0.0183 (10) | 0.0220 (11) | 0.0292 (11) | −0.0009 (8) | 0.0057 (9) | −0.0012 (9) |
O3 | 0.039 (2) | 0.0160 (15) | 0.0325 (18) | 0.000 | −0.0025 (16) | 0.000 |
O10 | 0.0229 (11) | 0.0344 (13) | 0.0259 (11) | −0.0022 (10) | 0.0030 (9) | 0.0022 (10) |
N1 | 0.0153 (12) | 0.0317 (14) | 0.0215 (12) | −0.0003 (10) | 0.0002 (10) | 0.0034 (11) |
C1 | 0.0156 (13) | 0.0229 (14) | 0.0236 (13) | −0.0010 (11) | 0.0067 (11) | −0.0015 (11) |
C2 | 0.0161 (13) | 0.0283 (15) | 0.0198 (12) | −0.0009 (11) | 0.0052 (11) | −0.0017 (11) |
C3 | 0.0141 (13) | 0.0286 (15) | 0.0240 (13) | 0.0037 (11) | 0.0033 (11) | −0.0021 (12) |
C4 | 0.0204 (14) | 0.0228 (15) | 0.0304 (15) | −0.0019 (12) | 0.0061 (12) | −0.0057 (13) |
C5 | 0.0158 (13) | 0.0309 (16) | 0.0211 (13) | −0.0027 (11) | 0.0050 (11) | −0.0020 (12) |
C6 | 0.0139 (13) | 0.0311 (16) | 0.0294 (15) | 0.0016 (12) | 0.0034 (12) | 0.0091 (13) |
C7 | 0.0212 (15) | 0.0269 (15) | 0.0294 (15) | −0.0012 (12) | 0.0055 (12) | 0.0051 (13) |
C8 | 0.0205 (15) | 0.0376 (18) | 0.0271 (15) | −0.0012 (13) | 0.0079 (12) | 0.0009 (13) |
C9 | 0.0209 (15) | 0.0276 (14) | 0.0288 (15) | −0.0022 (12) | 0.0089 (12) | 0.0002 (13) |
C10 | 0.0190 (14) | 0.0257 (15) | 0.0282 (15) | 0.0012 (12) | 0.0057 (12) | −0.0040 (12) |
C11 | 0.0206 (16) | 0.0419 (19) | 0.0277 (16) | −0.0037 (14) | 0.0039 (13) | −0.0031 (14) |
C12 | 0.032 (2) | 0.091 (3) | 0.0306 (19) | −0.021 (2) | 0.0044 (16) | 0.017 (2) |
C13 | 0.0213 (15) | 0.046 (2) | 0.0287 (16) | −0.0012 (14) | 0.0116 (13) | −0.0015 (14) |
C14 | 0.0218 (15) | 0.0290 (17) | 0.0265 (15) | 0.0010 (12) | 0.0118 (12) | −0.0011 (12) |
C15 | 0.045 (2) | 0.0318 (18) | 0.0383 (18) | −0.0037 (16) | 0.0206 (17) | −0.0007 (16) |
C16 | 0.046 (2) | 0.062 (3) | 0.0314 (18) | −0.016 (2) | 0.0139 (17) | −0.0117 (19) |
C17 | 0.034 (2) | 0.086 (3) | 0.0244 (17) | 0.008 (2) | 0.0086 (15) | 0.003 (2) |
C18 | 0.047 (2) | 0.050 (2) | 0.042 (2) | 0.0243 (19) | 0.0264 (18) | 0.0200 (19) |
C19 | 0.043 (2) | 0.0318 (19) | 0.0389 (18) | 0.0051 (15) | 0.0266 (17) | 0.0031 (15) |
Sn1—O1 | 2.257 (2) | C9—C10 | 1.425 (5) |
Sn1—O2 | 2.348 (2) | C9—H9 | 0.9500 |
Sn1—O3 | 2.337 (3) | C10—C11 | 1.504 (4) |
Sn1—C13 | 2.150 (3) | C11—H11A | 0.9800 |
O1—C1 | 1.274 (4) | C11—H11B | 0.9800 |
O2—C1 | 1.273 (4) | C11—H11C | 0.9800 |
O3—H3 | 0.838 (7) | C12—H12A | 0.9800 |
O10—C10 | 1.248 (4) | C12—H12B | 0.9800 |
N1—C5 | 1.421 (4) | C12—H12C | 0.9800 |
N1—C8 | 1.327 (4) | C13—C14 | 1.498 (5) |
N1—H1 | 0.82 (4) | C13—H13A | 0.9900 |
C1—C2 | 1.489 (4) | C13—H13B | 0.9900 |
C2—C7 | 1.389 (4) | C14—C15 | 1.378 (5) |
C2—C3 | 1.391 (4) | C14—C19 | 1.388 (5) |
C3—C4 | 1.382 (4) | C15—C16 | 1.386 (5) |
C3—H3A | 0.9500 | C15—H15 | 0.9500 |
C4—C5 | 1.390 (4) | C16—C17 | 1.376 (7) |
C4—H4 | 0.9500 | C16—H16 | 0.9500 |
C5—C6 | 1.397 (5) | C17—C18 | 1.380 (7) |
C6—C7 | 1.385 (4) | C17—H17 | 0.9500 |
C6—H6 | 0.9500 | C18—C19 | 1.376 (5) |
C7—H7 | 0.9500 | C18—H18 | 0.9500 |
C8—C9 | 1.378 (5) | C19—H19 | 0.9500 |
C8—C12 | 1.505 (5) | ||
O1—Sn1—O1i | 78.94 (11) | C9—C8—C12 | 119.9 (3) |
O1—Sn1—O2 | 57.26 (8) | C8—C9—C10 | 123.8 (3) |
O1—Sn1—O2i | 136.18 (8) | C8—C9—H9 | 118.1 |
O1—Sn1—O3 | 140.53 (5) | C10—C9—H9 | 118.1 |
O1—Sn1—C13 | 93.73 (11) | O10—C10—C9 | 122.5 (3) |
O1—Sn1—C13i | 90.36 (11) | O10—C10—C11 | 119.6 (3) |
O2—Sn1—O2i | 166.56 (11) | C9—C10—C11 | 117.8 (3) |
O2—Sn1—O3 | 83.28 (6) | C10—C11—H11A | 109.5 |
O2—Sn1—C13 | 93.61 (11) | C10—C11—H11B | 109.5 |
O2—Sn1—C13i | 85.77 (11) | H11A—C11—H11B | 109.5 |
O3—Sn1—C13 | 87.35 (10) | C10—C11—H11C | 109.5 |
C13—Sn1—C13i | 174.7 (2) | H11A—C11—H11C | 109.5 |
C1—O1—Sn1 | 93.31 (18) | H11B—C11—H11C | 109.5 |
C1—O2—Sn1 | 89.18 (17) | C8—C12—H12A | 109.5 |
Sn1—O3—H3 | 115 (3) | C8—C12—H12B | 109.5 |
Sn1—O3—H3i | 115 (3) | H12A—C12—H12B | 109.5 |
H3—O3—H3i | 130 (7) | C8—C12—H12C | 109.5 |
C8—N1—C5 | 128.6 (3) | H12A—C12—H12C | 109.5 |
C8—N1—H1 | 120 (3) | H12B—C12—H12C | 109.5 |
C5—N1—H1 | 111 (3) | C14—C13—Sn1 | 115.6 (2) |
O2—C1—O1 | 120.1 (3) | C14—C13—H13A | 108.4 |
O2—C1—C2 | 121.1 (3) | Sn1—C13—H13A | 108.4 |
O1—C1—C2 | 118.7 (3) | C14—C13—H13B | 108.4 |
C7—C2—C3 | 119.8 (3) | Sn1—C13—H13B | 108.4 |
C7—C2—C1 | 119.8 (3) | H13A—C13—H13B | 107.4 |
C3—C2—C1 | 120.4 (3) | C15—C14—C19 | 118.4 (3) |
C4—C3—C2 | 120.4 (3) | C15—C14—C13 | 120.3 (3) |
C4—C3—H3A | 119.8 | C19—C14—C13 | 121.3 (3) |
C2—C3—H3A | 119.8 | C14—C15—C16 | 121.4 (4) |
C3—C4—C5 | 119.9 (3) | C14—C15—H15 | 119.3 |
C3—C4—H4 | 120.1 | C16—C15—H15 | 119.3 |
C5—C4—H4 | 120.1 | C17—C16—C15 | 119.4 (4) |
C4—C5—C6 | 120.0 (3) | C17—C16—H16 | 120.3 |
C4—C5—N1 | 122.5 (3) | C15—C16—H16 | 120.3 |
C6—C5—N1 | 117.4 (3) | C16—C17—C18 | 119.7 (4) |
C7—C6—C5 | 119.8 (3) | C16—C17—H17 | 120.1 |
C7—C6—H6 | 120.1 | C18—C17—H17 | 120.1 |
C5—C6—H6 | 120.1 | C19—C18—C17 | 120.5 (4) |
C6—C7—C2 | 120.2 (3) | C19—C18—H18 | 119.7 |
C6—C7—H7 | 119.9 | C17—C18—H18 | 119.7 |
C2—C7—H7 | 119.9 | C18—C19—C14 | 120.5 (4) |
N1—C8—C9 | 120.8 (3) | C18—C19—H19 | 119.8 |
N1—C8—C12 | 119.4 (3) | C14—C19—H19 | 119.8 |
Sn1—O2—C1—O1 | −3.3 (3) | C3—C2—C7—C6 | 0.5 (5) |
Sn1—O2—C1—C2 | 175.1 (2) | C1—C2—C7—C6 | −177.9 (3) |
Sn1—O1—C1—O2 | 3.4 (3) | C5—N1—C8—C9 | 179.5 (3) |
Sn1—O1—C1—C2 | −175.0 (2) | C5—N1—C8—C12 | 0.6 (6) |
O2—C1—C2—C7 | 3.5 (4) | N1—C8—C9—C10 | −0.6 (5) |
O1—C1—C2—C7 | −178.1 (3) | C12—C8—C9—C10 | 178.2 (4) |
O2—C1—C2—C3 | −174.9 (3) | C8—C9—C10—O10 | −1.2 (5) |
O1—C1—C2—C3 | 3.5 (4) | C8—C9—C10—C11 | 177.5 (3) |
C7—C2—C3—C4 | −0.7 (5) | Sn1—C13—C14—C15 | −83.5 (4) |
C1—C2—C3—C4 | 177.7 (3) | Sn1—C13—C14—C19 | 95.3 (3) |
C2—C3—C4—C5 | 0.3 (5) | C19—C14—C15—C16 | −1.2 (5) |
C3—C4—C5—C6 | 0.3 (5) | C13—C14—C15—C16 | 177.7 (3) |
C3—C4—C5—N1 | 177.4 (3) | C14—C15—C16—C17 | 0.0 (6) |
C8—N1—C5—C4 | 51.0 (5) | C15—C16—C17—C18 | 1.8 (6) |
C8—N1—C5—C6 | −131.8 (4) | C16—C17—C18—C19 | −2.6 (6) |
C4—C5—C6—C7 | −0.6 (5) | C17—C18—C19—C14 | 1.4 (5) |
N1—C5—C6—C7 | −177.8 (3) | C15—C14—C19—C18 | 0.4 (5) |
C5—C6—C7—C2 | 0.2 (5) | C13—C14—C19—C18 | −178.4 (3) |
Symmetry code: (i) −x, y, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O10 | 0.82 (4) | 2.01 (4) | 2.631 (3) | 132 (4) |
O3—H3···O10ii | 0.84 (1) | 1.95 (2) | 2.712 (3) | 151 (4) |
Symmetry code: (ii) x+1/2, −y+1/2, z+1/2. |
[Sn4(C4H9)8(C15H13N2O3)4O2]·2C2H6O | F(000) = 2192 |
Mr = 2132.88 | Dx = 1.422 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 11.8395 (1) Å | Cell parameters from 171311 reflections |
b = 24.2855 (3) Å | θ = 2.0–27.5° |
c = 17.3557 (2) Å | µ = 1.06 mm−1 |
β = 93.2962 (7)° | T = 160 K |
V = 4982.00 (9) Å3 | Tablet, orange |
Z = 2 | 0.35 × 0.20 × 0.15 mm |
Nonius KappaCCD area detector diffractometer | 11376 independent reflections |
Radiation source: Nonius FR590 sealed tube generator | 9553 reflections with I > 2σ(I) |
Horizontally mounted graphite crystal monochromator | Rint = 0.049 |
Detector resolution: 9 pixels mm-1 | θmax = 27.5°, θmin = 2.1° |
φ and ω scans with κ offsets | h = −15→15 |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | k = −31→31 |
Tmin = 0.829, Tmax = 0.922 | l = −22→22 |
94026 measured reflections |
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)] = 0.033 | Hydrogen site location: mixed |
wR(F2) = 0.077 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0278P)2 + 6.8029P] where P = (Fo2 + 2Fc2)/3 |
11371 reflections | (Δ/σ)max = 0.001 |
628 parameters | Δρmax = 0.91 e Å−3 |
144 restraints | Δρmin = −0.93 e Å−3 |
Experimental. Data collection and full structure determination done by Prof. Anthony Linden: anthony.linden@chem.uzh.ch Solvent used: toluene Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: on a glass fibre Mosaicity (deg.): 0.746 (1) Frames collected: 718 Seconds exposure per frame: 60 Degrees rotation per frame: 1.0 Crystal-detector distance (mm): 38.0 Client: Tushar Basu-Baul Sample code: TSBB-304 (L1014) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. The Sn-complex molecule sits across a crystallographic centre of inversion and the asymmetric includes a molecule of EtOH. Two butyl groups at the same Sn atom are disordered over two conformations. Two sets of overlapping positions were defined for the atoms of one methylene group in one ligand and for all atoms of the other disordered butyl group and the site occupation factors of the major conformations of these groups refined to 0.846 (6) and 0.683 (5), respectively. Similarity restraints were applied to the chemically equivalent bond lengths and angles involving all disordered C-atoms, while neighbouring atoms within and between each conformation of the disordered butyl groups were restrained to have similar atomic displacement parameters. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Sn1 | 0.05001 (2) | 0.37049 (2) | 0.45148 (2) | 0.03285 (6) | |
Sn2 | 0.08779 (2) | 0.52372 (2) | 0.43610 (2) | 0.02578 (5) | |
O1 | 0.19192 (17) | 0.47981 (8) | 0.34877 (12) | 0.0416 (5) | |
O2 | 0.1733 (3) | 0.39106 (10) | 0.36369 (17) | 0.0832 (10) | |
O3 | 0.86222 (19) | 0.39724 (10) | −0.16369 (12) | 0.0469 (5) | |
H3 | 0.893 (3) | 0.3655 (15) | −0.159 (2) | 0.055 (11)* | |
O4 | −0.07448 (14) | 0.36432 (7) | 0.53976 (10) | 0.0289 (4) | |
O5 | −0.06043 (16) | 0.27469 (8) | 0.51891 (12) | 0.0375 (4) | |
O6 | −0.96252 (16) | 0.32178 (10) | 0.86854 (13) | 0.0446 (5) | |
H6 | −0.966 (3) | 0.3262 (17) | 0.921 (2) | 0.076 (13)* | |
O7 | 0.02343 (14) | 0.45122 (7) | 0.47392 (10) | 0.0263 (4) | |
N1 | 0.49994 (19) | 0.38861 (10) | 0.08500 (13) | 0.0346 (5) | |
N2 | 0.5496 (2) | 0.42950 (10) | 0.05843 (13) | 0.0366 (5) | |
N3 | −0.52091 (18) | 0.28868 (10) | 0.69716 (13) | 0.0356 (5) | |
N4 | −0.53547 (19) | 0.31997 (11) | 0.75336 (13) | 0.0377 (5) | |
C1 | 0.2124 (2) | 0.43154 (13) | 0.33106 (16) | 0.0367 (6) | |
C2 | 0.2894 (2) | 0.42124 (12) | 0.26719 (15) | 0.0342 (6) | |
C3 | 0.3003 (3) | 0.36865 (13) | 0.23750 (18) | 0.0438 (7) | |
H31 | 0.260555 | 0.338821 | 0.258794 | 0.053* | |
C4 | 0.3693 (3) | 0.35950 (13) | 0.17654 (17) | 0.0413 (7) | |
H4 | 0.375730 | 0.323563 | 0.155619 | 0.050* | |
C5 | 0.4283 (2) | 0.40272 (12) | 0.14652 (15) | 0.0330 (6) | |
C6 | 0.4202 (2) | 0.45534 (13) | 0.17723 (16) | 0.0384 (6) | |
H61 | 0.462926 | 0.484808 | 0.157705 | 0.046* | |
C7 | 0.3490 (2) | 0.46434 (12) | 0.23667 (16) | 0.0375 (6) | |
H7 | 0.341064 | 0.500458 | 0.256670 | 0.045* | |
C8 | 0.6245 (2) | 0.41710 (12) | −0.00080 (15) | 0.0335 (6) | |
C9 | 0.6373 (2) | 0.36544 (12) | −0.03379 (14) | 0.0323 (6) | |
H9 | 0.591369 | 0.335693 | −0.018730 | 0.039* | |
C10 | 0.7166 (2) | 0.35691 (12) | −0.08854 (15) | 0.0338 (6) | |
C11 | 0.7829 (2) | 0.40186 (12) | −0.10944 (15) | 0.0347 (6) | |
C12 | 0.7715 (2) | 0.45410 (12) | −0.07742 (16) | 0.0372 (6) | |
C13 | 0.6898 (2) | 0.46103 (12) | −0.02381 (16) | 0.0376 (6) | |
H13 | 0.678300 | 0.496499 | −0.002518 | 0.045* | |
C14 | −0.1081 (2) | 0.31416 (11) | 0.54896 (14) | 0.0290 (5) | |
C15 | −0.2107 (2) | 0.30627 (11) | 0.59369 (14) | 0.0282 (5) | |
C16 | −0.2756 (2) | 0.25913 (11) | 0.58262 (15) | 0.0331 (6) | |
H16 | −0.250333 | 0.230332 | 0.550798 | 0.040* | |
C17 | −0.3774 (2) | 0.25384 (12) | 0.61792 (16) | 0.0353 (6) | |
H17 | −0.423231 | 0.222120 | 0.608842 | 0.042* | |
C18 | −0.4119 (2) | 0.29533 (11) | 0.66666 (15) | 0.0317 (6) | |
C19 | −0.3446 (2) | 0.34171 (11) | 0.68061 (16) | 0.0339 (6) | |
H19 | −0.366960 | 0.369375 | 0.715311 | 0.041* | |
C20 | −0.2452 (2) | 0.34710 (12) | 0.64359 (16) | 0.0335 (6) | |
H20 | −0.199796 | 0.378994 | 0.652214 | 0.040* | |
C21 | −0.6464 (2) | 0.31876 (12) | 0.78052 (16) | 0.0353 (6) | |
C22 | −0.7403 (2) | 0.29662 (12) | 0.73911 (15) | 0.0342 (6) | |
H22 | −0.731344 | 0.279902 | 0.690359 | 0.041* | |
C23 | −0.8464 (2) | 0.29884 (12) | 0.76852 (15) | 0.0341 (6) | |
C24 | −0.8561 (2) | 0.32229 (12) | 0.84176 (16) | 0.0340 (6) | |
C25 | −0.7646 (2) | 0.34633 (12) | 0.88293 (16) | 0.0367 (6) | |
C26 | −0.6596 (2) | 0.34449 (13) | 0.85090 (16) | 0.0384 (6) | |
H26 | −0.595981 | 0.361054 | 0.877554 | 0.046* | |
C27 | 0.7332 (3) | 0.30115 (12) | −0.12382 (17) | 0.0417 (7) | |
H271 | 0.805858 | 0.285805 | −0.104178 | 0.063* | |
H272 | 0.732898 | 0.304692 | −0.180080 | 0.063* | |
H273 | 0.671797 | 0.276597 | −0.110190 | 0.063* | |
C28 | 0.8491 (3) | 0.50027 (14) | −0.0985 (2) | 0.0493 (8) | |
H281 | 0.925568 | 0.493058 | −0.076133 | 0.074* | |
H282 | 0.821345 | 0.535095 | −0.078167 | 0.074* | |
H283 | 0.850778 | 0.502670 | −0.154743 | 0.074* | |
C29 | −0.9499 (2) | 0.27881 (15) | 0.72325 (18) | 0.0467 (8) | |
H291 | −1.002889 | 0.309436 | 0.714349 | 0.070* | |
H292 | −0.986017 | 0.249706 | 0.752224 | 0.070* | |
H293 | −0.928331 | 0.264165 | 0.673558 | 0.070* | |
C30 | −0.7776 (3) | 0.37509 (15) | 0.95911 (19) | 0.0510 (8) | |
H301 | −0.837317 | 0.402949 | 0.952971 | 0.076* | |
H302 | −0.706064 | 0.392894 | 0.975839 | 0.076* | |
H303 | −0.797867 | 0.348070 | 0.997917 | 0.076* | |
C31 | −0.0504 (3) | 0.33948 (15) | 0.35816 (19) | 0.0621 (10) | |
H311 | −0.019966 | 0.354021 | 0.310265 | 0.074* | 0.846 (6) |
H312 | −0.040346 | 0.299023 | 0.357445 | 0.074* | 0.846 (6) |
H313 | 0.003673 | 0.319310 | 0.327125 | 0.074* | 0.154 (6) |
H314 | −0.097015 | 0.310760 | 0.381464 | 0.074* | 0.154 (6) |
C32A | −0.1746 (3) | 0.35092 (16) | 0.35450 (19) | 0.0482 (10) | 0.846 (6) |
H321 | −0.186547 | 0.390964 | 0.360917 | 0.058* | 0.846 (6) |
H322 | −0.208716 | 0.331909 | 0.397941 | 0.058* | 0.846 (6) |
C32B | −0.1307 (9) | 0.3665 (5) | 0.2985 (9) | 0.048 (3) | 0.154 (6) |
H323 | −0.154143 | 0.402744 | 0.318202 | 0.057* | 0.154 (6) |
H324 | −0.090353 | 0.372993 | 0.250881 | 0.057* | 0.154 (6) |
C33 | −0.2352 (3) | 0.33224 (16) | 0.2787 (2) | 0.0650 (10) | |
H331 | −0.207086 | 0.353506 | 0.235028 | 0.078* | 0.846 (6) |
H332 | −0.220096 | 0.292717 | 0.269771 | 0.078* | 0.846 (6) |
H333 | −0.227730 | 0.322244 | 0.223896 | 0.078* | 0.154 (6) |
H334 | −0.220917 | 0.297728 | 0.308001 | 0.078* | 0.154 (6) |
C34 | −0.3584 (4) | 0.34142 (18) | 0.2837 (3) | 0.0750 (12) | |
H341 | −0.384999 | 0.321324 | 0.328195 | 0.112* | |
H342 | −0.398658 | 0.328149 | 0.236420 | 0.112* | |
H343 | −0.372987 | 0.380847 | 0.289956 | 0.112* | |
C35A | 0.1923 (5) | 0.3365 (3) | 0.5137 (3) | 0.0520 (11) | 0.683 (5) |
H351 | 0.256182 | 0.362739 | 0.512478 | 0.062* | 0.683 (5) |
H352 | 0.174183 | 0.331603 | 0.568242 | 0.062* | 0.683 (5) |
C36A | 0.2283 (3) | 0.28175 (18) | 0.4817 (3) | 0.0561 (11) | 0.683 (5) |
H361 | 0.215317 | 0.282017 | 0.424886 | 0.067* | 0.683 (5) |
H362 | 0.181177 | 0.252161 | 0.502419 | 0.067* | 0.683 (5) |
C37A | 0.3522 (3) | 0.2694 (2) | 0.5023 (3) | 0.0584 (11) | 0.683 (5) |
H371 | 0.368956 | 0.277667 | 0.557674 | 0.070* | 0.683 (5) |
H372 | 0.366059 | 0.229671 | 0.494476 | 0.070* | 0.683 (5) |
C38A | 0.4320 (5) | 0.3023 (3) | 0.4547 (4) | 0.0740 (14) | 0.683 (5) |
H381 | 0.414469 | 0.295236 | 0.399770 | 0.111* | 0.683 (5) |
H382 | 0.510245 | 0.291322 | 0.468471 | 0.111* | 0.683 (5) |
H383 | 0.422915 | 0.341678 | 0.465264 | 0.111* | 0.683 (5) |
C35B | 0.1813 (8) | 0.3411 (7) | 0.5291 (5) | 0.0499 (18) | 0.317 (5) |
H353 | 0.180419 | 0.365466 | 0.574715 | 0.060* | 0.317 (5) |
H354 | 0.155412 | 0.304566 | 0.546319 | 0.060* | 0.317 (5) |
C36B | 0.3053 (7) | 0.3336 (4) | 0.5138 (6) | 0.0556 (13) | 0.317 (5) |
H363 | 0.335371 | 0.368597 | 0.493995 | 0.067* | 0.317 (5) |
H364 | 0.348202 | 0.324812 | 0.562901 | 0.067* | 0.317 (5) |
C37B | 0.3229 (7) | 0.2882 (5) | 0.4560 (7) | 0.0624 (14) | 0.317 (5) |
H373 | 0.268332 | 0.293180 | 0.411172 | 0.075* | 0.317 (5) |
H374 | 0.306460 | 0.252346 | 0.480111 | 0.075* | 0.317 (5) |
C38B | 0.4416 (9) | 0.2867 (6) | 0.4277 (9) | 0.069 (2) | 0.317 (5) |
H384 | 0.455717 | 0.320455 | 0.398989 | 0.104* | 0.317 (5) |
H385 | 0.449236 | 0.254724 | 0.393922 | 0.104* | 0.317 (5) |
H386 | 0.496459 | 0.283802 | 0.472014 | 0.104* | 0.317 (5) |
C39 | −0.0139 (2) | 0.55226 (11) | 0.33912 (15) | 0.0341 (6) | |
H391 | −0.063498 | 0.582067 | 0.356541 | 0.041* | |
H392 | 0.036437 | 0.568497 | 0.301596 | 0.041* | |
C40 | −0.0874 (3) | 0.50922 (12) | 0.29784 (17) | 0.0408 (7) | |
H401 | −0.136548 | 0.491785 | 0.335113 | 0.049* | |
H402 | −0.038530 | 0.480228 | 0.277378 | 0.049* | |
C41 | −0.1604 (3) | 0.53376 (16) | 0.2320 (2) | 0.0556 (9) | |
H411 | −0.204804 | 0.564561 | 0.252264 | 0.067* | |
H412 | −0.110612 | 0.549153 | 0.193499 | 0.067* | |
C42 | −0.2410 (4) | 0.4931 (2) | 0.1921 (3) | 0.0872 (15) | |
H421 | −0.197718 | 0.464150 | 0.167801 | 0.131* | |
H422 | −0.288684 | 0.512244 | 0.152600 | 0.131* | |
H423 | −0.288924 | 0.476569 | 0.230118 | 0.131* | |
C43 | 0.2440 (2) | 0.53863 (12) | 0.49912 (17) | 0.0366 (6) | |
H431 | 0.296430 | 0.556690 | 0.464588 | 0.044* | |
H432 | 0.230664 | 0.564508 | 0.541729 | 0.044* | |
C44 | 0.3002 (2) | 0.48697 (13) | 0.53277 (18) | 0.0417 (7) | |
H441 | 0.244056 | 0.465861 | 0.560869 | 0.050* | |
H442 | 0.324509 | 0.463603 | 0.490002 | 0.050* | |
C45 | 0.4017 (3) | 0.49905 (16) | 0.5872 (2) | 0.0636 (10) | |
H451 | 0.377820 | 0.522706 | 0.629762 | 0.076* | |
H452 | 0.458541 | 0.519662 | 0.559023 | 0.076* | |
C46 | 0.4560 (4) | 0.44683 (19) | 0.6211 (3) | 0.0981 (18) | |
H461 | 0.400622 | 0.426645 | 0.649966 | 0.147* | |
H462 | 0.521129 | 0.456675 | 0.655762 | 0.147* | |
H463 | 0.481311 | 0.423588 | 0.579210 | 0.147* | |
O8 | −0.0246 (2) | 0.16675 (10) | 0.50888 (14) | 0.0595 (7) | |
H8 | −0.032 (4) | 0.2013 (19) | 0.528 (3) | 0.084 (14)* | |
C47 | −0.0545 (3) | 0.12520 (15) | 0.5618 (2) | 0.0549 (9) | |
H471 | −0.040073 | 0.088507 | 0.539589 | 0.066* | |
H472 | −0.136335 | 0.127863 | 0.570249 | 0.066* | |
C48 | 0.0098 (4) | 0.13068 (18) | 0.6355 (2) | 0.0752 (12) | |
H481 | −0.010756 | 0.165217 | 0.660340 | 0.113* | |
H482 | 0.090894 | 0.130889 | 0.626875 | 0.113* | |
H483 | −0.007377 | 0.099619 | 0.668940 | 0.113* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sn1 | 0.03794 (11) | 0.02823 (10) | 0.03422 (10) | 0.00428 (8) | 0.01800 (8) | 0.00162 (7) |
Sn2 | 0.02240 (9) | 0.02967 (10) | 0.02597 (9) | 0.00093 (7) | 0.00740 (6) | 0.00225 (7) |
O1 | 0.0458 (12) | 0.0420 (12) | 0.0398 (11) | 0.0046 (9) | 0.0260 (9) | −0.0031 (9) |
O2 | 0.117 (2) | 0.0470 (13) | 0.0948 (19) | 0.0125 (14) | 0.0868 (18) | 0.0092 (13) |
O3 | 0.0464 (13) | 0.0545 (14) | 0.0422 (12) | 0.0101 (11) | 0.0240 (10) | 0.0074 (10) |
O4 | 0.0293 (9) | 0.0298 (9) | 0.0285 (9) | −0.0024 (7) | 0.0102 (7) | −0.0004 (7) |
O5 | 0.0395 (11) | 0.0287 (10) | 0.0460 (11) | −0.0028 (8) | 0.0171 (9) | −0.0038 (8) |
O6 | 0.0283 (10) | 0.0646 (14) | 0.0419 (12) | 0.0000 (9) | 0.0122 (9) | −0.0002 (11) |
O7 | 0.0267 (9) | 0.0238 (8) | 0.0297 (9) | 0.0022 (7) | 0.0121 (7) | 0.0017 (7) |
N1 | 0.0319 (12) | 0.0415 (13) | 0.0315 (12) | 0.0047 (10) | 0.0104 (9) | 0.0013 (10) |
N2 | 0.0360 (12) | 0.0425 (13) | 0.0322 (12) | 0.0065 (10) | 0.0110 (10) | 0.0002 (10) |
N3 | 0.0277 (11) | 0.0430 (13) | 0.0371 (12) | −0.0018 (10) | 0.0099 (9) | 0.0032 (10) |
N4 | 0.0294 (12) | 0.0519 (15) | 0.0326 (12) | −0.0011 (10) | 0.0089 (9) | 0.0018 (11) |
C1 | 0.0348 (14) | 0.0470 (17) | 0.0294 (14) | 0.0086 (13) | 0.0121 (11) | 0.0071 (12) |
C2 | 0.0327 (14) | 0.0431 (16) | 0.0277 (13) | 0.0094 (12) | 0.0105 (11) | 0.0047 (11) |
C3 | 0.0462 (17) | 0.0426 (17) | 0.0451 (17) | 0.0056 (14) | 0.0238 (14) | 0.0059 (13) |
C4 | 0.0438 (16) | 0.0405 (16) | 0.0413 (16) | 0.0053 (13) | 0.0180 (13) | −0.0039 (13) |
C5 | 0.0302 (13) | 0.0425 (16) | 0.0270 (13) | 0.0063 (11) | 0.0079 (10) | 0.0000 (11) |
C6 | 0.0364 (15) | 0.0445 (16) | 0.0355 (15) | −0.0003 (12) | 0.0134 (12) | 0.0005 (12) |
C7 | 0.0372 (15) | 0.0418 (16) | 0.0348 (15) | 0.0017 (12) | 0.0130 (12) | −0.0048 (12) |
C8 | 0.0327 (14) | 0.0411 (15) | 0.0276 (13) | 0.0075 (12) | 0.0092 (10) | 0.0024 (11) |
C9 | 0.0327 (14) | 0.0401 (15) | 0.0245 (12) | 0.0025 (11) | 0.0046 (10) | 0.0043 (11) |
C10 | 0.0334 (14) | 0.0407 (15) | 0.0275 (13) | 0.0070 (12) | 0.0045 (11) | 0.0003 (11) |
C11 | 0.0314 (13) | 0.0490 (17) | 0.0246 (13) | 0.0082 (12) | 0.0089 (10) | 0.0057 (11) |
C12 | 0.0353 (15) | 0.0427 (16) | 0.0344 (15) | 0.0014 (12) | 0.0088 (12) | 0.0054 (12) |
C13 | 0.0429 (16) | 0.0367 (15) | 0.0340 (15) | 0.0050 (12) | 0.0100 (12) | 0.0006 (12) |
C14 | 0.0286 (13) | 0.0303 (14) | 0.0281 (13) | 0.0011 (10) | 0.0027 (10) | 0.0004 (10) |
C15 | 0.0235 (12) | 0.0332 (13) | 0.0282 (12) | −0.0014 (10) | 0.0049 (10) | 0.0046 (10) |
C16 | 0.0314 (13) | 0.0361 (14) | 0.0326 (14) | −0.0020 (11) | 0.0079 (11) | −0.0030 (11) |
C17 | 0.0290 (13) | 0.0386 (15) | 0.0391 (15) | −0.0074 (11) | 0.0077 (11) | 0.0001 (12) |
C18 | 0.0252 (12) | 0.0385 (15) | 0.0319 (13) | −0.0009 (11) | 0.0065 (10) | 0.0052 (11) |
C19 | 0.0329 (14) | 0.0369 (15) | 0.0328 (14) | 0.0008 (11) | 0.0101 (11) | −0.0012 (11) |
C20 | 0.0295 (13) | 0.0356 (14) | 0.0361 (14) | −0.0038 (11) | 0.0090 (11) | 0.0026 (11) |
C21 | 0.0251 (13) | 0.0464 (16) | 0.0352 (14) | −0.0003 (12) | 0.0082 (11) | 0.0027 (12) |
C22 | 0.0321 (14) | 0.0412 (15) | 0.0298 (13) | −0.0002 (12) | 0.0060 (11) | 0.0004 (11) |
C23 | 0.0284 (13) | 0.0419 (15) | 0.0320 (14) | −0.0010 (11) | 0.0026 (11) | 0.0068 (12) |
C24 | 0.0261 (13) | 0.0413 (15) | 0.0353 (14) | 0.0022 (11) | 0.0090 (11) | 0.0056 (12) |
C25 | 0.0324 (14) | 0.0448 (16) | 0.0338 (14) | 0.0005 (12) | 0.0077 (11) | −0.0002 (12) |
C26 | 0.0313 (14) | 0.0508 (17) | 0.0333 (14) | −0.0026 (12) | 0.0044 (11) | 0.0001 (13) |
C27 | 0.0492 (17) | 0.0429 (16) | 0.0339 (15) | 0.0047 (13) | 0.0108 (13) | −0.0043 (12) |
C28 | 0.0472 (18) | 0.0511 (19) | 0.0510 (19) | −0.0071 (15) | 0.0144 (15) | 0.0035 (15) |
C29 | 0.0358 (16) | 0.066 (2) | 0.0387 (16) | −0.0102 (15) | 0.0038 (12) | 0.0011 (15) |
C30 | 0.0418 (17) | 0.069 (2) | 0.0424 (17) | −0.0033 (16) | 0.0095 (14) | −0.0133 (16) |
C31 | 0.097 (3) | 0.052 (2) | 0.0355 (17) | 0.006 (2) | −0.0037 (18) | −0.0078 (15) |
C32A | 0.066 (3) | 0.043 (2) | 0.0354 (19) | −0.0070 (18) | 0.0004 (17) | −0.0079 (16) |
C32B | 0.064 (5) | 0.045 (5) | 0.034 (5) | −0.008 (5) | −0.001 (5) | −0.006 (5) |
C33 | 0.077 (3) | 0.049 (2) | 0.067 (2) | 0.0024 (19) | −0.014 (2) | −0.0099 (18) |
C34 | 0.082 (3) | 0.066 (3) | 0.074 (3) | 0.006 (2) | −0.023 (2) | −0.011 (2) |
C35A | 0.0279 (19) | 0.040 (2) | 0.089 (3) | 0.0098 (17) | 0.006 (2) | 0.000 (2) |
C36A | 0.0394 (19) | 0.047 (2) | 0.082 (3) | 0.0142 (17) | 0.0011 (19) | −0.007 (2) |
C37A | 0.043 (2) | 0.059 (2) | 0.074 (3) | 0.0158 (18) | 0.0034 (19) | −0.009 (2) |
C38A | 0.059 (2) | 0.078 (3) | 0.085 (4) | 0.015 (2) | 0.003 (3) | −0.002 (3) |
C35B | 0.027 (3) | 0.035 (3) | 0.087 (4) | 0.009 (3) | 0.006 (3) | 0.000 (3) |
C36B | 0.037 (2) | 0.048 (3) | 0.082 (3) | 0.012 (2) | 0.004 (2) | −0.003 (2) |
C37B | 0.048 (2) | 0.059 (3) | 0.081 (3) | 0.016 (2) | 0.005 (3) | −0.005 (3) |
C38B | 0.058 (4) | 0.065 (4) | 0.085 (5) | 0.020 (4) | 0.006 (4) | −0.009 (4) |
C39 | 0.0365 (14) | 0.0352 (15) | 0.0304 (14) | 0.0007 (12) | −0.0008 (11) | 0.0057 (11) |
C40 | 0.0456 (17) | 0.0414 (16) | 0.0350 (15) | −0.0039 (13) | −0.0025 (12) | −0.0002 (12) |
C41 | 0.059 (2) | 0.065 (2) | 0.0413 (18) | −0.0038 (17) | −0.0136 (16) | 0.0034 (16) |
C42 | 0.090 (3) | 0.102 (4) | 0.065 (3) | −0.020 (3) | −0.034 (2) | −0.004 (3) |
C43 | 0.0253 (13) | 0.0379 (15) | 0.0464 (16) | −0.0003 (11) | 0.0001 (11) | −0.0015 (12) |
C44 | 0.0316 (14) | 0.0448 (17) | 0.0478 (17) | 0.0073 (12) | −0.0052 (12) | −0.0026 (13) |
C45 | 0.048 (2) | 0.060 (2) | 0.080 (3) | 0.0170 (17) | −0.0227 (18) | −0.016 (2) |
C46 | 0.089 (3) | 0.079 (3) | 0.118 (4) | 0.034 (3) | −0.063 (3) | −0.017 (3) |
O8 | 0.0842 (18) | 0.0429 (13) | 0.0552 (15) | 0.0171 (12) | 0.0370 (13) | 0.0126 (11) |
C47 | 0.060 (2) | 0.054 (2) | 0.051 (2) | 0.0039 (17) | 0.0091 (16) | 0.0125 (16) |
C48 | 0.091 (3) | 0.073 (3) | 0.062 (3) | −0.001 (2) | 0.006 (2) | −0.010 (2) |
Sn1—O2 | 2.227 (2) | C30—H302 | 0.9800 |
Sn1—O4 | 2.1914 (16) | C30—H303 | 0.9800 |
Sn1—O5 | 2.9442 (18) | C31—C32A | 1.494 (4) |
Sn1—O7 | 2.0270 (16) | C31—C32B | 1.515 (5) |
Sn1—C31 | 2.094 (3) | C31—H311 | 0.9900 |
Sn1—C35A | 2.115 (4) | C31—H312 | 0.9900 |
Sn1—C35B | 2.121 (5) | C31—H313 | 0.9900 |
Sn2—O1 | 2.2736 (18) | C31—H314 | 0.9900 |
Sn2—O4i | 2.7571 (18) | C32A—C33 | 1.531 (3) |
Sn2—O7 | 2.0418 (16) | C32A—H321 | 0.9900 |
Sn2—O7i | 2.1864 (16) | C32A—H322 | 0.9900 |
Sn2—C39 | 2.128 (3) | C32B—C33 | 1.514 (5) |
Sn2—C43 | 2.125 (3) | C32B—H323 | 0.9900 |
O1—C1 | 1.239 (3) | C32B—H324 | 0.9900 |
O2—C1 | 1.237 (4) | C33—C34 | 1.484 (6) |
O3—C11 | 1.372 (3) | C33—H331 | 0.9900 |
O3—H3 | 0.85 (4) | C33—H332 | 0.9900 |
O4—C14 | 1.294 (3) | C33—H333 | 0.9900 |
O5—C14 | 1.243 (3) | C33—H334 | 0.9900 |
O6—C24 | 1.368 (3) | C34—H341 | 0.9800 |
O6—H6 | 0.93 (4) | C34—H342 | 0.9800 |
N1—N2 | 1.255 (3) | C34—H343 | 0.9800 |
N1—C5 | 1.442 (3) | C35A—C36A | 1.512 (4) |
N2—C8 | 1.428 (3) | C35A—H351 | 0.9900 |
N3—N4 | 1.256 (3) | C35A—H352 | 0.9900 |
N3—C18 | 1.432 (3) | C36A—C37A | 1.519 (4) |
N4—C21 | 1.421 (3) | C36A—H361 | 0.9900 |
C1—C2 | 1.497 (3) | C36A—H362 | 0.9900 |
C2—C7 | 1.385 (4) | C37A—C38A | 1.518 (4) |
C2—C3 | 1.386 (4) | C37A—H371 | 0.9900 |
C3—C4 | 1.391 (4) | C37A—H372 | 0.9900 |
C3—H31 | 0.9500 | C38A—H381 | 0.9800 |
C4—C5 | 1.380 (4) | C38A—H382 | 0.9800 |
C4—H4 | 0.9500 | C38A—H383 | 0.9800 |
C5—C6 | 1.390 (4) | C35B—C36B | 1.518 (5) |
C6—C7 | 1.386 (4) | C35B—H353 | 0.9900 |
C6—H61 | 0.9500 | C35B—H354 | 0.9900 |
C7—H7 | 0.9500 | C36B—C37B | 1.513 (4) |
C8—C13 | 1.389 (4) | C36B—H363 | 0.9900 |
C8—C9 | 1.391 (4) | C36B—H364 | 0.9900 |
C9—C10 | 1.389 (4) | C37B—C38B | 1.515 (4) |
C9—H9 | 0.9500 | C37B—H373 | 0.9900 |
C10—C11 | 1.404 (4) | C37B—H374 | 0.9900 |
C10—C27 | 1.504 (4) | C38B—H384 | 0.9800 |
C11—C12 | 1.395 (4) | C38B—H385 | 0.9800 |
C12—C13 | 1.391 (4) | C38B—H386 | 0.9800 |
C12—C28 | 1.508 (4) | C39—C40 | 1.513 (4) |
C13—H13 | 0.9500 | C39—H391 | 0.9900 |
C14—C15 | 1.491 (3) | C39—H392 | 0.9900 |
C15—C16 | 1.386 (4) | C40—C41 | 1.514 (4) |
C15—C20 | 1.393 (4) | C40—H401 | 0.9900 |
C16—C17 | 1.390 (4) | C40—H402 | 0.9900 |
C16—H16 | 0.9500 | C41—C42 | 1.513 (5) |
C17—C18 | 1.392 (4) | C41—H411 | 0.9900 |
C17—H17 | 0.9500 | C41—H412 | 0.9900 |
C18—C19 | 1.393 (4) | C42—H421 | 0.9800 |
C19—C20 | 1.379 (4) | C42—H422 | 0.9800 |
C19—H19 | 0.9500 | C42—H423 | 0.9800 |
C20—H20 | 0.9500 | C43—C44 | 1.521 (4) |
C21—C26 | 1.389 (4) | C43—H431 | 0.9900 |
C21—C22 | 1.397 (4) | C43—H432 | 0.9900 |
C22—C23 | 1.383 (4) | C44—C45 | 1.514 (4) |
C22—H22 | 0.9500 | C44—H441 | 0.9900 |
C23—C24 | 1.404 (4) | C44—H442 | 0.9900 |
C23—C29 | 1.498 (4) | C45—C46 | 1.524 (5) |
C24—C25 | 1.392 (4) | C45—H451 | 0.9900 |
C25—C26 | 1.392 (4) | C45—H452 | 0.9900 |
C25—C30 | 1.511 (4) | C46—H461 | 0.9800 |
C26—H26 | 0.9500 | C46—H462 | 0.9800 |
C27—H271 | 0.9800 | C46—H463 | 0.9800 |
C27—H272 | 0.9800 | O8—C47 | 1.423 (4) |
C27—H273 | 0.9800 | O8—H8 | 0.91 (5) |
C28—H281 | 0.9800 | C47—C48 | 1.457 (5) |
C28—H282 | 0.9800 | C47—H471 | 0.9900 |
C28—H283 | 0.9800 | C47—H472 | 0.9900 |
C29—H291 | 0.9800 | C48—H481 | 0.9800 |
C29—H292 | 0.9800 | C48—H482 | 0.9800 |
C29—H293 | 0.9800 | C48—H483 | 0.9800 |
C30—H301 | 0.9800 | ||
O2—Sn1—O4 | 170.96 (8) | C32A—C31—Sn1 | 118.7 (2) |
O2—Sn1—O5 | 140.62 (7) | C32B—C31—Sn1 | 132.8 (6) |
O2—Sn1—O7 | 91.70 (8) | C32A—C31—H311 | 107.6 |
O2—Sn1—C31 | 85.24 (14) | Sn1—C31—H311 | 107.6 |
O2—Sn1—C35A | 84.4 (2) | C32A—C31—H312 | 107.6 |
O2—Sn1—C35B | 91.4 (3) | Sn1—C31—H312 | 107.6 |
O4—Sn1—O5 | 48.40 (6) | H311—C31—H312 | 107.1 |
O4—Sn1—O7 | 79.26 (6) | C32B—C31—H313 | 104.0 |
O4—Sn1—C31 | 98.12 (12) | Sn1—C31—H313 | 104.0 |
O4—Sn1—C35A | 99.5 (2) | C32B—C31—H314 | 104.0 |
O4—Sn1—C35B | 91.8 (3) | Sn1—C31—H314 | 104.0 |
O5—Sn1—O7 | 127.63 (6) | H313—C31—H314 | 105.5 |
O5—Sn1—C31 | 77.16 (12) | C31—C32A—C33 | 113.1 (3) |
O5—Sn1—C35A | 81.2 (2) | C31—C32A—H321 | 109.0 |
O5—Sn1—C35B | 78.9 (5) | C33—C32A—H321 | 109.0 |
O7—Sn1—C31 | 114.14 (11) | C31—C32A—H322 | 109.0 |
O7—Sn1—C35A | 114.02 (18) | C33—C32A—H322 | 109.0 |
O7—Sn1—C35B | 108.7 (4) | H321—C32A—H322 | 107.8 |
C31—Sn1—C35A | 130.91 (17) | C33—C32B—C31 | 112.9 (5) |
C31—Sn1—C35B | 137.1 (4) | C33—C32B—H323 | 109.0 |
O1—Sn2—O4i | 127.00 (6) | C31—C32B—H323 | 109.0 |
O1—Sn2—O7 | 92.10 (7) | C33—C32B—H324 | 109.0 |
O1—Sn2—O7i | 168.16 (7) | C31—C32B—H324 | 109.0 |
O1—Sn2—C39 | 85.96 (10) | H323—C32B—H324 | 107.8 |
O1—Sn2—C43 | 86.21 (10) | C34—C33—C32B | 134.2 (8) |
O4i—Sn2—O7 | 140.89 (6) | C34—C33—C32A | 108.6 (3) |
O4i—Sn2—O7i | 64.84 (5) | C34—C33—H331 | 110.0 |
O4i—Sn2—C39 | 76.37 (8) | C32A—C33—H331 | 110.0 |
O4i—Sn2—C43 | 79.00 (9) | C34—C33—H332 | 110.0 |
O7—Sn2—O7i | 76.07 (7) | C32A—C33—H332 | 110.0 |
O7—Sn2—C39 | 109.29 (9) | H331—C33—H332 | 108.4 |
O7i—Sn2—C39 | 97.91 (9) | C34—C33—H333 | 103.6 |
O7—Sn2—C43 | 108.14 (9) | C32B—C33—H333 | 103.6 |
O7i—Sn2—C43 | 97.29 (9) | C34—C33—H334 | 103.6 |
C39—Sn2—C43 | 141.97 (11) | C32B—C33—H334 | 103.6 |
C1—O1—Sn2 | 136.90 (17) | H333—C33—H334 | 105.3 |
C1—O2—Sn1 | 140.2 (2) | C33—C34—H341 | 109.5 |
C11—O3—H3 | 108 (2) | C33—C34—H342 | 109.5 |
C14—O4—Sn1 | 112.01 (15) | H341—C34—H342 | 109.5 |
C14—O4—Sn2i | 152.71 (15) | C33—C34—H343 | 109.5 |
Sn1—O4—Sn2i | 94.90 (6) | H341—C34—H343 | 109.5 |
C14—O5—Sn1 | 77.29 (14) | H342—C34—H343 | 109.5 |
C24—O6—H6 | 116 (2) | C36A—C35A—Sn1 | 112.9 (3) |
Sn1—O7—Sn2 | 135.02 (8) | C36A—C35A—H351 | 109.0 |
Sn1—O7—Sn2i | 120.87 (8) | Sn1—C35A—H351 | 109.0 |
Sn2—O7—Sn2i | 103.93 (7) | C36A—C35A—H352 | 109.0 |
N2—N1—C5 | 113.1 (2) | Sn1—C35A—H352 | 109.0 |
N1—N2—C8 | 114.9 (2) | H351—C35A—H352 | 107.8 |
N4—N3—C18 | 112.7 (2) | C35A—C36A—C37A | 112.1 (4) |
N3—N4—C21 | 114.6 (2) | C35A—C36A—H361 | 109.2 |
O2—C1—O1 | 123.7 (2) | C37A—C36A—H361 | 109.2 |
O2—C1—C2 | 117.8 (3) | C35A—C36A—H362 | 109.2 |
O1—C1—C2 | 118.6 (2) | C37A—C36A—H362 | 109.2 |
C7—C2—C3 | 119.6 (2) | H361—C36A—H362 | 107.9 |
C7—C2—C1 | 120.2 (3) | C38A—C37A—C36A | 113.0 (5) |
C3—C2—C1 | 120.2 (3) | C38A—C37A—H371 | 109.0 |
C2—C3—C4 | 120.1 (3) | C36A—C37A—H371 | 109.0 |
C2—C3—H31 | 120.0 | C38A—C37A—H372 | 109.0 |
C4—C3—H31 | 120.0 | C36A—C37A—H372 | 109.0 |
C5—C4—C3 | 119.9 (3) | H371—C37A—H372 | 107.8 |
C5—C4—H4 | 120.1 | C37A—C38A—H381 | 109.5 |
C3—C4—H4 | 120.1 | C37A—C38A—H382 | 109.5 |
C4—C5—C6 | 120.4 (2) | H381—C38A—H382 | 109.5 |
C4—C5—N1 | 115.5 (2) | C37A—C38A—H383 | 109.5 |
C6—C5—N1 | 124.0 (2) | H381—C38A—H383 | 109.5 |
C7—C6—C5 | 119.3 (3) | H382—C38A—H383 | 109.5 |
C7—C6—H61 | 120.4 | C36B—C35B—Sn1 | 127.6 (7) |
C5—C6—H61 | 120.4 | C36B—C35B—H353 | 105.4 |
C2—C7—C6 | 120.7 (3) | Sn1—C35B—H353 | 105.4 |
C2—C7—H7 | 119.7 | C36B—C35B—H354 | 105.4 |
C6—C7—H7 | 119.7 | Sn1—C35B—H354 | 105.4 |
C13—C8—C9 | 119.9 (2) | H353—C35B—H354 | 106.0 |
C13—C8—N2 | 115.1 (2) | C37B—C36B—C35B | 111.9 (5) |
C9—C8—N2 | 125.0 (2) | C37B—C36B—H363 | 109.2 |
C10—C9—C8 | 120.6 (3) | C35B—C36B—H363 | 109.2 |
C10—C9—H9 | 119.7 | C37B—C36B—H364 | 109.2 |
C8—C9—H9 | 119.7 | C35B—C36B—H364 | 109.2 |
C9—C10—C11 | 118.1 (3) | H363—C36B—H364 | 107.9 |
C9—C10—C27 | 121.5 (3) | C36B—C37B—C38B | 113.5 (6) |
C11—C10—C27 | 120.5 (2) | C36B—C37B—H373 | 108.9 |
O3—C11—C12 | 115.7 (3) | C38B—C37B—H373 | 108.9 |
O3—C11—C10 | 121.9 (3) | C36B—C37B—H374 | 108.9 |
C12—C11—C10 | 122.4 (2) | C38B—C37B—H374 | 108.9 |
C13—C12—C11 | 117.6 (3) | H373—C37B—H374 | 107.7 |
C13—C12—C28 | 121.9 (3) | C37B—C38B—H384 | 109.5 |
C11—C12—C28 | 120.4 (3) | C37B—C38B—H385 | 109.5 |
C8—C13—C12 | 121.3 (3) | H384—C38B—H385 | 109.5 |
C8—C13—H13 | 119.4 | C37B—C38B—H386 | 109.5 |
C12—C13—H13 | 119.4 | H384—C38B—H386 | 109.5 |
O5—C14—O4 | 121.6 (2) | H385—C38B—H386 | 109.5 |
O5—C14—C15 | 121.5 (2) | C40—C39—Sn2 | 115.66 (19) |
O4—C14—C15 | 116.8 (2) | C40—C39—H391 | 108.4 |
C16—C15—C20 | 119.6 (2) | Sn2—C39—H391 | 108.4 |
C16—C15—C14 | 119.7 (2) | C40—C39—H392 | 108.4 |
C20—C15—C14 | 120.6 (2) | Sn2—C39—H392 | 108.4 |
C15—C16—C17 | 120.2 (3) | H391—C39—H392 | 107.4 |
C15—C16—H16 | 119.9 | C39—C40—C41 | 111.9 (3) |
C17—C16—H16 | 119.9 | C39—C40—H401 | 109.2 |
C16—C17—C18 | 119.6 (3) | C41—C40—H401 | 109.2 |
C16—C17—H17 | 120.2 | C39—C40—H402 | 109.2 |
C18—C17—H17 | 120.2 | C41—C40—H402 | 109.2 |
C17—C18—C19 | 120.4 (2) | H401—C40—H402 | 107.9 |
C17—C18—N3 | 116.4 (2) | C42—C41—C40 | 114.0 (3) |
C19—C18—N3 | 123.1 (2) | C42—C41—H411 | 108.8 |
C20—C19—C18 | 119.4 (3) | C40—C41—H411 | 108.8 |
C20—C19—H19 | 120.3 | C42—C41—H412 | 108.8 |
C18—C19—H19 | 120.3 | C40—C41—H412 | 108.8 |
C19—C20—C15 | 120.7 (3) | H411—C41—H412 | 107.7 |
C19—C20—H20 | 119.6 | C41—C42—H421 | 109.5 |
C15—C20—H20 | 119.6 | C41—C42—H422 | 109.5 |
C26—C21—C22 | 120.0 (2) | H421—C42—H422 | 109.5 |
C26—C21—N4 | 115.8 (2) | C41—C42—H423 | 109.5 |
C22—C21—N4 | 124.1 (2) | H421—C42—H423 | 109.5 |
C23—C22—C21 | 120.5 (3) | H422—C42—H423 | 109.5 |
C23—C22—H22 | 119.7 | C44—C43—Sn2 | 113.95 (19) |
C21—C22—H22 | 119.7 | C44—C43—H431 | 108.8 |
C22—C23—C24 | 118.2 (2) | Sn2—C43—H431 | 108.8 |
C22—C23—C29 | 121.7 (3) | C44—C43—H432 | 108.8 |
C24—C23—C29 | 120.0 (2) | Sn2—C43—H432 | 108.8 |
O6—C24—C25 | 122.3 (2) | H431—C43—H432 | 107.7 |
O6—C24—C23 | 115.4 (2) | C45—C44—C43 | 113.2 (3) |
C25—C24—C23 | 122.2 (2) | C45—C44—H441 | 108.9 |
C26—C25—C24 | 117.9 (3) | C43—C44—H441 | 108.9 |
C26—C25—C30 | 120.2 (3) | C45—C44—H442 | 108.9 |
C24—C25—C30 | 121.8 (2) | C43—C44—H442 | 108.9 |
C21—C26—C25 | 120.9 (3) | H441—C44—H442 | 107.7 |
C21—C26—H26 | 119.5 | C44—C45—C46 | 112.4 (3) |
C25—C26—H26 | 119.5 | C44—C45—H451 | 109.1 |
C10—C27—H271 | 109.5 | C46—C45—H451 | 109.1 |
C10—C27—H272 | 109.5 | C44—C45—H452 | 109.1 |
H271—C27—H272 | 109.5 | C46—C45—H452 | 109.1 |
C10—C27—H273 | 109.5 | H451—C45—H452 | 107.8 |
H271—C27—H273 | 109.5 | C45—C46—H461 | 109.5 |
H272—C27—H273 | 109.5 | C45—C46—H462 | 109.5 |
C12—C28—H281 | 109.5 | H461—C46—H462 | 109.5 |
C12—C28—H282 | 109.5 | C45—C46—H463 | 109.5 |
H281—C28—H282 | 109.5 | H461—C46—H463 | 109.5 |
C12—C28—H283 | 109.5 | H462—C46—H463 | 109.5 |
H281—C28—H283 | 109.5 | C47—O8—H8 | 113 (3) |
H282—C28—H283 | 109.5 | O8—C47—C48 | 111.4 (3) |
C23—C29—H291 | 109.5 | O8—C47—H471 | 109.3 |
C23—C29—H292 | 109.5 | C48—C47—H471 | 109.3 |
H291—C29—H292 | 109.5 | O8—C47—H472 | 109.3 |
C23—C29—H293 | 109.5 | C48—C47—H472 | 109.3 |
H291—C29—H293 | 109.5 | H471—C47—H472 | 108.0 |
H292—C29—H293 | 109.5 | C47—C48—H481 | 109.5 |
C25—C30—H301 | 109.5 | C47—C48—H482 | 109.5 |
C25—C30—H302 | 109.5 | H481—C48—H482 | 109.5 |
H301—C30—H302 | 109.5 | C47—C48—H483 | 109.5 |
C25—C30—H303 | 109.5 | H481—C48—H483 | 109.5 |
H301—C30—H303 | 109.5 | H482—C48—H483 | 109.5 |
H302—C30—H303 | 109.5 | ||
C5—N1—N2—C8 | 177.9 (2) | O5—C14—C15—C16 | −20.6 (4) |
C18—N3—N4—C21 | 174.0 (2) | O4—C14—C15—C16 | 156.1 (2) |
Sn1—O2—C1—O1 | 6.9 (7) | O5—C14—C15—C20 | 162.7 (3) |
Sn1—O2—C1—C2 | −173.7 (3) | O4—C14—C15—C20 | −20.6 (4) |
Sn2—O1—C1—O2 | −0.4 (5) | C20—C15—C16—C17 | 3.3 (4) |
Sn2—O1—C1—C2 | −179.79 (19) | C14—C15—C16—C17 | −173.4 (2) |
O2—C1—C2—C7 | −170.1 (3) | C15—C16—C17—C18 | −2.3 (4) |
O1—C1—C2—C7 | 9.3 (4) | C16—C17—C18—C19 | −0.5 (4) |
O2—C1—C2—C3 | 10.8 (5) | C16—C17—C18—N3 | 176.2 (2) |
O1—C1—C2—C3 | −169.8 (3) | N4—N3—C18—C17 | 164.6 (2) |
C7—C2—C3—C4 | −1.0 (5) | N4—N3—C18—C19 | −18.8 (4) |
C1—C2—C3—C4 | 178.0 (3) | C17—C18—C19—C20 | 2.2 (4) |
C2—C3—C4—C5 | 1.1 (5) | N3—C18—C19—C20 | −174.3 (3) |
C3—C4—C5—C6 | 0.6 (5) | C18—C19—C20—C15 | −1.2 (4) |
C3—C4—C5—N1 | 178.3 (3) | C16—C15—C20—C19 | −1.6 (4) |
N2—N1—C5—C4 | 178.4 (3) | C14—C15—C20—C19 | 175.1 (2) |
N2—N1—C5—C6 | −4.0 (4) | N3—N4—C21—C26 | 168.2 (3) |
C4—C5—C6—C7 | −2.2 (4) | N3—N4—C21—C22 | −15.6 (4) |
N1—C5—C6—C7 | −179.7 (3) | C26—C21—C22—C23 | −1.6 (4) |
C3—C2—C7—C6 | −0.6 (4) | N4—C21—C22—C23 | −177.7 (3) |
C1—C2—C7—C6 | −179.7 (3) | C21—C22—C23—C24 | −2.0 (4) |
C5—C6—C7—C2 | 2.2 (4) | C21—C22—C23—C29 | 175.9 (3) |
N1—N2—C8—C13 | −172.6 (2) | C22—C23—C24—O6 | −178.1 (2) |
N1—N2—C8—C9 | 5.7 (4) | C29—C23—C24—O6 | 3.9 (4) |
C13—C8—C9—C10 | 1.4 (4) | C22—C23—C24—C25 | 4.3 (4) |
N2—C8—C9—C10 | −176.8 (3) | C29—C23—C24—C25 | −173.6 (3) |
C8—C9—C10—C11 | −0.1 (4) | O6—C24—C25—C26 | 179.7 (3) |
C8—C9—C10—C27 | 178.9 (3) | C23—C24—C25—C26 | −2.9 (4) |
C9—C10—C11—O3 | −179.2 (2) | O6—C24—C25—C30 | −1.9 (5) |
C27—C10—C11—O3 | 1.8 (4) | C23—C24—C25—C30 | 175.5 (3) |
C9—C10—C11—C12 | −0.1 (4) | C22—C21—C26—C25 | 3.1 (4) |
C27—C10—C11—C12 | −179.1 (3) | N4—C21—C26—C25 | 179.4 (3) |
O3—C11—C12—C13 | 178.2 (3) | C24—C25—C26—C21 | −0.9 (4) |
C10—C11—C12—C13 | −1.0 (4) | C30—C25—C26—C21 | −179.3 (3) |
O3—C11—C12—C28 | −4.3 (4) | Sn1—C31—C32A—C33 | 172.7 (3) |
C10—C11—C12—C28 | 176.6 (3) | Sn1—C31—C32B—C33 | −141.5 (7) |
C9—C8—C13—C12 | −2.5 (4) | C31—C32B—C33—C34 | 120.3 (10) |
N2—C8—C13—C12 | 175.8 (3) | C31—C32A—C33—C34 | 175.5 (3) |
C11—C12—C13—C8 | 2.3 (4) | Sn1—C35A—C36A—C37A | 156.1 (4) |
C28—C12—C13—C8 | −175.2 (3) | C35A—C36A—C37A—C38A | −75.5 (7) |
Sn1—O5—C14—O4 | −7.2 (2) | Sn1—C35B—C36B—C37B | −67.6 (15) |
Sn1—O5—C14—C15 | 169.3 (2) | C35B—C36B—C37B—C38B | 169.0 (12) |
Sn1—O4—C14—O5 | 10.2 (3) | Sn2—C39—C40—C41 | 177.4 (2) |
Sn2i—O4—C14—O5 | −179.9 (2) | C39—C40—C41—C42 | −176.2 (3) |
Sn1—O4—C14—C15 | −166.49 (17) | Sn2—C43—C44—C45 | −171.4 (2) |
Sn2i—O4—C14—C15 | 3.5 (5) | C43—C44—C45—C46 | 179.3 (4) |
Symmetry code: (i) −x, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3···O6ii | 0.85 (4) | 2.05 (4) | 2.801 (3) | 146 (3) |
O6—H6···O8iii | 0.93 (4) | 1.71 (4) | 2.599 (3) | 159 (4) |
O8—H8···O5 | 0.91 (5) | 1.82 (5) | 2.663 (3) | 154 (4) |
Symmetry codes: (ii) x+2, y, z−1; (iii) x−1, −y+1/2, z+1/2. |
[Sn4(C4H9)8(C10H10NO3)4O2] | Z = 2 |
Mr = 1732.41 | F(000) = 1768 |
Triclinic, P1 | Dx = 1.446 Mg m−3 |
a = 12.0054 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 14.7309 (4) Å | Cell parameters from 106136 reflections |
c = 23.9132 (6) Å | θ = 2.0–25.0° |
α = 76.3707 (18)° | µ = 1.30 mm−1 |
β = 75.5206 (16)° | T = 160 K |
γ = 88.1609 (16)° | Plate, yellow |
V = 3977.81 (18) Å3 | 0.25 × 0.20 × 0.05 mm |
Nonius KappaCCD area detector diffractometer | 14030 independent reflections |
Radiation source: Nonius FR590 sealed tube generator | 8004 reflections with I > 2σ(I) |
Horizontally mounted graphite crystal monochromator | Rint = 0.107 |
Detector resolution: 9 pixels mm-1 | θmax = 25.0°, θmin = 2.0° |
φ and ω scans with κ offsets | h = −14→14 |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | k = −17→17 |
Tmin = 0.358, Tmax = 0.537 | l = −28→28 |
68065 measured reflections |
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) = 0.114 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0465P)2 + 1.4894P] where P = (Fo2 + 2Fc2)/3 |
14030 reflections | (Δ/σ)max = 0.001 |
859 parameters | Δρmax = 1.20 e Å−3 |
0 restraints | Δρmin = −1.11 e Å−3 |
Experimental. Data collection and full structure determination done by Prof. Anthony Linden: anthony.linden@chem.uzh.ch Solvent used: hexane / chloroform Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: on a glass fibre Mosaicity (deg.): 0.885 (1) Frames collected: 539 Seconds exposure per frame: 16 Degrees rotation per frame: 1.1 Crystal-detector distance (mm): 33.8 Client: Tushar Basu Sample code: TSBB-71 (L0403) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Sn1 | 0.38021 (3) | 0.02573 (3) | 0.23737 (2) | 0.03287 (12) | |
Sn2 | 0.38814 (3) | 0.28443 (3) | 0.22852 (2) | 0.03121 (12) | |
Sn3 | 0.60632 (3) | 0.15581 (3) | 0.26223 (2) | 0.03134 (12) | |
Sn4 | 0.61477 (3) | 0.41241 (3) | 0.25625 (2) | 0.03435 (13) | |
O1 | 0.5272 (3) | −0.0175 (3) | 0.27270 (16) | 0.0351 (10) | |
O2 | 0.4760 (4) | −0.1604 (3) | 0.27374 (19) | 0.0491 (12) | |
O3 | 0.8718 (4) | −0.0556 (3) | 0.1265 (2) | 0.0649 (14) | |
H3 | 0.845980 | −0.084544 | 0.162059 | 0.097* | |
O4 | 0.2463 (3) | 0.0988 (3) | 0.19408 (17) | 0.0392 (10) | |
O5 | 0.2152 (3) | 0.2340 (3) | 0.22109 (18) | 0.0400 (10) | |
O6 | −0.1493 (4) | 0.0000 (3) | 0.3391 (2) | 0.0546 (12) | |
H6 | −0.113764 | 0.032733 | 0.305975 | 0.082* | |
O7 | 0.4375 (3) | 0.1493 (2) | 0.24415 (15) | 0.0324 (10) | |
O8 | 0.5543 (3) | 0.2917 (2) | 0.24699 (17) | 0.0348 (10) | |
O9 | 0.4733 (3) | 0.4609 (3) | 0.21652 (17) | 0.0372 (10) | |
O10 | 0.5336 (4) | 0.5998 (3) | 0.2193 (2) | 0.0501 (12) | |
O11 | 0.1346 (4) | 0.4953 (3) | 0.3665 (2) | 0.0639 (14) | |
H11 | 0.154235 | 0.528340 | 0.331607 | 0.096* | |
O12 | 0.7414 (3) | 0.3336 (3) | 0.30478 (17) | 0.0419 (11) | |
O13 | 0.7794 (3) | 0.2045 (3) | 0.27115 (18) | 0.0397 (10) | |
O14 | 1.1290 (4) | 0.4380 (3) | 0.1734 (2) | 0.0595 (13) | |
H14 | 1.097150 | 0.402687 | 0.206286 | 0.089* | |
N1 | 0.7526 (4) | −0.1796 (3) | 0.2140 (2) | 0.0432 (14) | |
N2 | −0.0146 (4) | 0.0327 (4) | 0.2316 (2) | 0.0420 (13) | |
N3 | 0.2564 (4) | 0.6223 (4) | 0.2797 (3) | 0.0482 (14) | |
N4 | 0.9972 (4) | 0.3938 (4) | 0.2827 (2) | 0.0422 (13) | |
C1 | 0.5443 (6) | −0.1067 (4) | 0.2818 (3) | 0.0371 (15) | |
C2 | 0.6454 (5) | −0.1407 (4) | 0.3060 (3) | 0.0430 (16) | |
H21 | 0.619058 | −0.165257 | 0.349583 | 0.052* | |
H22 | 0.700041 | −0.087644 | 0.298497 | 0.052* | |
C3 | 0.7073 (6) | −0.2173 (4) | 0.2778 (3) | 0.0510 (18) | |
H31 | 0.771145 | −0.240606 | 0.296234 | 0.061* | |
H32 | 0.652973 | −0.270324 | 0.284672 | 0.061* | |
C4 | 0.7150 (5) | −0.2121 (4) | 0.1774 (3) | 0.0442 (17) | |
H4 | 0.661028 | −0.263207 | 0.192023 | 0.053* | |
C5 | 0.7517 (6) | −0.1739 (4) | 0.1147 (3) | 0.0471 (17) | |
C6 | 0.8268 (6) | −0.0944 (5) | 0.0907 (3) | 0.0536 (19) | |
C7 | 0.8536 (8) | −0.0556 (6) | 0.0308 (4) | 0.081 (3) | |
H7 | 0.902099 | −0.001185 | 0.015103 | 0.098* | |
C8 | 0.8113 (8) | −0.0944 (7) | −0.0066 (4) | 0.087 (3) | |
H8 | 0.830824 | −0.066773 | −0.048047 | 0.104* | |
C9 | 0.7398 (8) | −0.1742 (7) | 0.0157 (4) | 0.084 (3) | |
H9 | 0.711990 | −0.201968 | −0.010488 | 0.101* | |
C10 | 0.7100 (7) | −0.2121 (6) | 0.0756 (4) | 0.068 (2) | |
H10 | 0.659773 | −0.265579 | 0.090837 | 0.082* | |
C11 | 0.1872 (5) | 0.1706 (4) | 0.1998 (2) | 0.0293 (14) | |
C12 | 0.0828 (5) | 0.1821 (4) | 0.1759 (3) | 0.0374 (15) | |
H121 | 0.103123 | 0.223926 | 0.135549 | 0.045* | |
H122 | 0.023434 | 0.213047 | 0.201325 | 0.045* | |
C13 | 0.0318 (5) | 0.0912 (4) | 0.1724 (3) | 0.0447 (17) | |
H131 | −0.030228 | 0.105022 | 0.151281 | 0.054* | |
H132 | 0.092047 | 0.057270 | 0.149501 | 0.054* | |
C14 | 0.0147 (5) | −0.0521 (4) | 0.2431 (3) | 0.0417 (16) | |
H141 | 0.067197 | −0.074667 | 0.212852 | 0.050* | |
C15 | −0.0285 (5) | −0.1157 (4) | 0.3004 (3) | 0.0427 (16) | |
C16 | −0.1085 (5) | −0.0879 (4) | 0.3464 (3) | 0.0470 (17) | |
C17 | −0.1522 (6) | −0.1512 (5) | 0.4001 (3) | 0.0556 (19) | |
H17 | −0.208156 | −0.133009 | 0.430990 | 0.067* | |
C18 | −0.1123 (7) | −0.2420 (5) | 0.4079 (4) | 0.066 (2) | |
H18 | −0.141016 | −0.285644 | 0.444647 | 0.079* | |
C19 | −0.0322 (7) | −0.2697 (5) | 0.3634 (4) | 0.069 (2) | |
H19 | −0.006126 | −0.332012 | 0.369458 | 0.083* | |
C20 | 0.0099 (6) | −0.2069 (5) | 0.3103 (3) | 0.0523 (18) | |
H20 | 0.066025 | −0.225865 | 0.279839 | 0.063* | |
C21 | 0.2455 (5) | −0.0351 (4) | 0.3123 (3) | 0.0433 (16) | |
H211 | 0.181242 | 0.008841 | 0.315108 | 0.052* | |
H212 | 0.216866 | −0.092719 | 0.305395 | 0.052* | |
C22 | 0.2778 (5) | −0.0595 (5) | 0.3717 (3) | 0.0496 (18) | |
H221 | 0.303150 | −0.001849 | 0.379999 | 0.060* | |
H222 | 0.343214 | −0.102311 | 0.369154 | 0.060* | |
C23 | 0.1767 (6) | −0.1063 (5) | 0.4234 (3) | 0.066 (2) | |
H231 | 0.111218 | −0.063578 | 0.425921 | 0.079* | |
H232 | 0.151524 | −0.164077 | 0.415209 | 0.079* | |
C24 | 0.2094 (7) | −0.1304 (6) | 0.4828 (3) | 0.084 (3) | |
H241 | 0.279177 | −0.167172 | 0.479287 | 0.126* | |
H242 | 0.146329 | −0.166835 | 0.513454 | 0.126* | |
H243 | 0.223472 | −0.072666 | 0.493938 | 0.126* | |
C25 | 0.4506 (5) | −0.0064 (4) | 0.1540 (2) | 0.0407 (16) | |
H251 | 0.471649 | 0.052939 | 0.123549 | 0.049* | |
H252 | 0.522337 | −0.040680 | 0.155886 | 0.049* | |
C26 | 0.3726 (6) | −0.0638 (4) | 0.1340 (3) | 0.0496 (18) | |
H261 | 0.358661 | −0.125890 | 0.162134 | 0.060* | |
H262 | 0.297587 | −0.033041 | 0.136507 | 0.060* | |
C27 | 0.4171 (7) | −0.0777 (6) | 0.0726 (3) | 0.072 (2) | |
H271 | 0.493625 | −0.105990 | 0.069738 | 0.086* | |
H272 | 0.428022 | −0.015677 | 0.044452 | 0.086* | |
C28 | 0.3427 (8) | −0.1376 (5) | 0.0534 (3) | 0.085 (3) | |
H281 | 0.342861 | −0.202373 | 0.075968 | 0.128* | |
H282 | 0.372584 | −0.134524 | 0.010877 | 0.128* | |
H283 | 0.263859 | −0.115082 | 0.060624 | 0.128* | |
C29 | 0.2925 (5) | 0.3094 (4) | 0.3104 (2) | 0.0396 (16) | |
H291 | 0.344545 | 0.336341 | 0.328884 | 0.048* | |
H292 | 0.233134 | 0.355677 | 0.302931 | 0.048* | |
C30 | 0.2344 (5) | 0.2202 (4) | 0.3532 (3) | 0.0448 (17) | |
H301 | 0.172808 | 0.199677 | 0.337725 | 0.054* | |
H302 | 0.291712 | 0.170452 | 0.354718 | 0.054* | |
C31 | 0.1826 (6) | 0.2317 (5) | 0.4159 (3) | 0.0548 (19) | |
H311 | 0.131501 | 0.285862 | 0.414280 | 0.066* | |
H312 | 0.244997 | 0.244653 | 0.433478 | 0.066* | |
C32 | 0.1134 (7) | 0.1439 (6) | 0.4555 (3) | 0.088 (3) | |
H321 | 0.056695 | 0.127225 | 0.436131 | 0.132* | |
H322 | 0.073700 | 0.156392 | 0.493900 | 0.132* | |
H323 | 0.165755 | 0.092183 | 0.461656 | 0.132* | |
C33 | 0.4293 (5) | 0.3434 (4) | 0.1358 (2) | 0.0404 (16) | |
H331 | 0.365938 | 0.384474 | 0.126804 | 0.048* | |
H332 | 0.499367 | 0.383659 | 0.125534 | 0.048* | |
C34 | 0.4495 (6) | 0.2764 (4) | 0.0953 (3) | 0.0494 (18) | |
H341 | 0.380680 | 0.234594 | 0.105779 | 0.059* | |
H342 | 0.515290 | 0.236991 | 0.102394 | 0.059* | |
C35 | 0.4742 (6) | 0.3249 (5) | 0.0293 (3) | 0.065 (2) | |
H351 | 0.475464 | 0.277138 | 0.006190 | 0.077* | |
H352 | 0.410879 | 0.367490 | 0.022702 | 0.077* | |
C36 | 0.5858 (6) | 0.3796 (6) | 0.0066 (3) | 0.079 (3) | |
H361 | 0.582268 | 0.431327 | 0.026348 | 0.118* | |
H362 | 0.599666 | 0.404677 | −0.036349 | 0.118* | |
H363 | 0.648580 | 0.338785 | 0.015073 | 0.118* | |
C37 | 0.5619 (5) | 0.0987 (4) | 0.3557 (2) | 0.0356 (15) | |
H371 | 0.494429 | 0.055586 | 0.365742 | 0.043* | |
H372 | 0.626666 | 0.061251 | 0.366409 | 0.043* | |
C38 | 0.5335 (5) | 0.1705 (4) | 0.3940 (2) | 0.0381 (15) | |
H381 | 0.602607 | 0.210739 | 0.386683 | 0.046* | |
H382 | 0.471993 | 0.210820 | 0.381934 | 0.046* | |
C39 | 0.4949 (6) | 0.1253 (5) | 0.4595 (3) | 0.0544 (19) | |
H391 | 0.555918 | 0.084121 | 0.471401 | 0.065* | |
H392 | 0.425088 | 0.085813 | 0.466882 | 0.065* | |
C40 | 0.4685 (6) | 0.1967 (5) | 0.4977 (3) | 0.068 (2) | |
H401 | 0.536637 | 0.237104 | 0.489802 | 0.102* | |
H402 | 0.447513 | 0.164027 | 0.539809 | 0.102* | |
H403 | 0.404351 | 0.234778 | 0.488120 | 0.102* | |
C41 | 0.7007 (5) | 0.1298 (4) | 0.1803 (2) | 0.0364 (15) | |
H411 | 0.754476 | 0.078877 | 0.188434 | 0.044* | |
H412 | 0.646479 | 0.107701 | 0.160929 | 0.044* | |
C42 | 0.7696 (5) | 0.2149 (4) | 0.1371 (3) | 0.0433 (16) | |
H421 | 0.716977 | 0.267374 | 0.130883 | 0.052* | |
H422 | 0.827981 | 0.234357 | 0.155086 | 0.052* | |
C43 | 0.8301 (5) | 0.1957 (5) | 0.0769 (3) | 0.0477 (17) | |
H431 | 0.868498 | 0.135001 | 0.083301 | 0.057* | |
H432 | 0.771960 | 0.190993 | 0.054653 | 0.057* | |
C44 | 0.9186 (6) | 0.2716 (5) | 0.0401 (3) | 0.069 (2) | |
H441 | 0.879946 | 0.330760 | 0.030660 | 0.104* | |
H442 | 0.958892 | 0.254428 | 0.003235 | 0.104* | |
H443 | 0.974191 | 0.278586 | 0.062772 | 0.104* | |
C45 | 0.4637 (6) | 0.5509 (4) | 0.2090 (3) | 0.0391 (16) | |
C46 | 0.3637 (6) | 0.5915 (5) | 0.1857 (3) | 0.0522 (18) | |
H461 | 0.307152 | 0.540893 | 0.190781 | 0.063* | |
H462 | 0.390804 | 0.620252 | 0.142626 | 0.063* | |
C47 | 0.3054 (6) | 0.6647 (4) | 0.2175 (3) | 0.0533 (19) | |
H471 | 0.362281 | 0.714395 | 0.213773 | 0.064* | |
H472 | 0.243916 | 0.693754 | 0.198870 | 0.064* | |
C48 | 0.2906 (5) | 0.6530 (4) | 0.3187 (3) | 0.0477 (18) | |
H48 | 0.344980 | 0.703835 | 0.305337 | 0.057* | |
C49 | 0.2508 (6) | 0.6143 (4) | 0.3820 (3) | 0.0492 (18) | |
C50 | 0.1750 (6) | 0.5353 (5) | 0.4028 (3) | 0.0558 (19) | |
C51 | 0.1390 (7) | 0.4968 (6) | 0.4631 (4) | 0.074 (2) | |
H51 | 0.089415 | 0.442877 | 0.477315 | 0.089* | |
C52 | 0.1745 (8) | 0.5359 (7) | 0.5027 (4) | 0.088 (3) | |
H52 | 0.149068 | 0.508946 | 0.544147 | 0.106* | |
C53 | 0.2465 (8) | 0.6135 (7) | 0.4830 (4) | 0.086 (3) | |
H53 | 0.269119 | 0.641152 | 0.510726 | 0.104* | |
C54 | 0.2858 (7) | 0.6511 (5) | 0.4234 (4) | 0.071 (2) | |
H54 | 0.337937 | 0.703355 | 0.410022 | 0.086* | |
C55 | 0.8014 (5) | 0.2636 (4) | 0.2982 (2) | 0.0320 (14) | |
C56 | 0.8970 (5) | 0.2426 (4) | 0.3284 (3) | 0.0416 (16) | |
H561 | 0.959387 | 0.212966 | 0.303666 | 0.050* | |
H562 | 0.868522 | 0.197361 | 0.366945 | 0.050* | |
C57 | 0.9460 (5) | 0.3298 (4) | 0.3391 (3) | 0.0463 (17) | |
H571 | 0.883720 | 0.361065 | 0.362789 | 0.056* | |
H572 | 1.004904 | 0.311598 | 0.361872 | 0.056* | |
C58 | 0.9686 (5) | 0.4797 (5) | 0.2747 (3) | 0.0443 (17) | |
H58 | 0.916246 | 0.498929 | 0.306425 | 0.053* | |
C59 | 1.0122 (5) | 0.5489 (4) | 0.2197 (3) | 0.0439 (17) | |
C60 | 1.0894 (6) | 0.5256 (5) | 0.1713 (3) | 0.0486 (18) | |
C61 | 1.1278 (6) | 0.5926 (5) | 0.1191 (3) | 0.061 (2) | |
H61 | 1.178796 | 0.575992 | 0.085944 | 0.073* | |
C62 | 1.0929 (7) | 0.6824 (5) | 0.1149 (4) | 0.063 (2) | |
H62 | 1.120232 | 0.728209 | 0.078914 | 0.076* | |
C63 | 1.0179 (7) | 0.7071 (5) | 0.1628 (4) | 0.069 (2) | |
H63 | 0.994896 | 0.770025 | 0.159890 | 0.082* | |
C64 | 0.9769 (6) | 0.6408 (5) | 0.2146 (4) | 0.0572 (19) | |
H64 | 0.924062 | 0.657759 | 0.247072 | 0.069* | |
C65 | 0.5379 (5) | 0.4422 (4) | 0.3400 (2) | 0.0388 (15) | |
H651 | 0.458205 | 0.462367 | 0.340595 | 0.047* | |
H652 | 0.533589 | 0.384186 | 0.371469 | 0.047* | |
C66 | 0.6028 (6) | 0.5173 (4) | 0.3539 (3) | 0.0518 (18) | |
H661 | 0.685489 | 0.502701 | 0.346043 | 0.062* | |
H662 | 0.595041 | 0.577902 | 0.326605 | 0.062* | |
C67 | 0.5619 (7) | 0.5274 (5) | 0.4168 (3) | 0.062 (2) | |
H671 | 0.578024 | 0.469346 | 0.443892 | 0.074* | |
H672 | 0.477484 | 0.534837 | 0.426117 | 0.074* | |
C68 | 0.6181 (7) | 0.6098 (5) | 0.4283 (3) | 0.079 (3) | |
H681 | 0.701740 | 0.608241 | 0.413343 | 0.118* | |
H682 | 0.598895 | 0.606035 | 0.471086 | 0.118* | |
H683 | 0.589763 | 0.668154 | 0.407839 | 0.118* | |
C69 | 0.7591 (5) | 0.4686 (4) | 0.1851 (3) | 0.0467 (17) | |
H691 | 0.788968 | 0.524488 | 0.193602 | 0.056* | |
H692 | 0.820284 | 0.421914 | 0.184689 | 0.056* | |
C70 | 0.7376 (5) | 0.4962 (4) | 0.1236 (3) | 0.0443 (17) | |
H701 | 0.678541 | 0.544633 | 0.123013 | 0.053* | |
H702 | 0.706954 | 0.441030 | 0.114698 | 0.053* | |
C71 | 0.8458 (6) | 0.5334 (5) | 0.0757 (3) | 0.0531 (19) | |
H711 | 0.874022 | 0.590386 | 0.083620 | 0.064* | |
H712 | 0.906133 | 0.486212 | 0.077909 | 0.064* | |
C72 | 0.8279 (6) | 0.5567 (5) | 0.0135 (3) | 0.066 (2) | |
H721 | 0.799710 | 0.500705 | 0.005254 | 0.100* | |
H722 | 0.901014 | 0.578564 | −0.015310 | 0.100* | |
H723 | 0.771244 | 0.605815 | 0.010237 | 0.100* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sn1 | 0.0271 (2) | 0.0292 (2) | 0.0445 (3) | 0.00029 (18) | −0.0104 (2) | −0.01145 (19) |
Sn2 | 0.0260 (2) | 0.0288 (2) | 0.0400 (3) | 0.00371 (18) | −0.0085 (2) | −0.01030 (19) |
Sn3 | 0.0255 (2) | 0.0295 (2) | 0.0408 (3) | 0.00400 (18) | −0.00891 (19) | −0.01158 (19) |
Sn4 | 0.0289 (2) | 0.0294 (2) | 0.0472 (3) | 0.00047 (19) | −0.0108 (2) | −0.0122 (2) |
O1 | 0.027 (2) | 0.038 (3) | 0.042 (2) | 0.0035 (19) | −0.0121 (19) | −0.0107 (19) |
O2 | 0.049 (3) | 0.032 (2) | 0.066 (3) | 0.000 (2) | −0.012 (2) | −0.015 (2) |
O3 | 0.071 (4) | 0.050 (3) | 0.071 (3) | −0.016 (3) | −0.011 (3) | −0.015 (3) |
O4 | 0.032 (2) | 0.038 (2) | 0.054 (3) | 0.007 (2) | −0.018 (2) | −0.016 (2) |
O5 | 0.031 (2) | 0.038 (3) | 0.056 (3) | 0.004 (2) | −0.016 (2) | −0.016 (2) |
O6 | 0.047 (3) | 0.046 (3) | 0.063 (3) | 0.003 (2) | −0.001 (2) | −0.010 (2) |
O7 | 0.043 (2) | 0.026 (2) | 0.033 (2) | 0.0025 (18) | −0.0160 (19) | −0.0096 (17) |
O8 | 0.021 (2) | 0.031 (2) | 0.054 (3) | 0.0026 (17) | −0.0106 (19) | −0.0093 (19) |
O9 | 0.035 (2) | 0.028 (2) | 0.052 (3) | −0.0007 (19) | −0.015 (2) | −0.0107 (19) |
O10 | 0.046 (3) | 0.033 (3) | 0.074 (3) | 0.001 (2) | −0.017 (2) | −0.016 (2) |
O11 | 0.068 (4) | 0.053 (3) | 0.070 (3) | −0.007 (3) | −0.009 (3) | −0.020 (3) |
O12 | 0.035 (3) | 0.041 (3) | 0.054 (3) | 0.005 (2) | −0.017 (2) | −0.014 (2) |
O13 | 0.030 (2) | 0.041 (3) | 0.053 (3) | 0.0041 (19) | −0.014 (2) | −0.017 (2) |
O14 | 0.052 (3) | 0.054 (3) | 0.068 (3) | 0.005 (2) | 0.002 (3) | −0.024 (3) |
N1 | 0.040 (3) | 0.028 (3) | 0.059 (4) | 0.011 (2) | −0.008 (3) | −0.012 (3) |
N2 | 0.028 (3) | 0.043 (3) | 0.056 (4) | −0.001 (2) | −0.011 (3) | −0.013 (3) |
N3 | 0.041 (3) | 0.041 (3) | 0.068 (4) | 0.013 (3) | −0.020 (3) | −0.018 (3) |
N4 | 0.033 (3) | 0.047 (3) | 0.055 (4) | 0.001 (3) | −0.014 (3) | −0.025 (3) |
C1 | 0.062 (5) | 0.015 (3) | 0.040 (4) | 0.004 (3) | −0.022 (3) | −0.011 (3) |
C2 | 0.040 (4) | 0.043 (4) | 0.050 (4) | 0.017 (3) | −0.024 (3) | −0.007 (3) |
C3 | 0.043 (4) | 0.040 (4) | 0.065 (5) | 0.011 (3) | −0.012 (4) | −0.007 (3) |
C4 | 0.043 (4) | 0.030 (4) | 0.062 (5) | 0.007 (3) | −0.013 (4) | −0.017 (3) |
C5 | 0.048 (4) | 0.042 (4) | 0.056 (5) | 0.014 (3) | −0.014 (4) | −0.024 (4) |
C6 | 0.052 (5) | 0.049 (4) | 0.053 (5) | 0.004 (4) | −0.002 (4) | −0.012 (4) |
C7 | 0.104 (7) | 0.068 (6) | 0.057 (6) | −0.012 (5) | 0.004 (5) | −0.009 (5) |
C8 | 0.101 (8) | 0.098 (7) | 0.053 (5) | 0.017 (6) | −0.006 (5) | −0.019 (5) |
C9 | 0.087 (7) | 0.096 (7) | 0.087 (7) | 0.017 (6) | −0.032 (6) | −0.044 (6) |
C10 | 0.061 (5) | 0.071 (5) | 0.078 (6) | 0.008 (4) | −0.015 (5) | −0.032 (5) |
C11 | 0.025 (3) | 0.030 (3) | 0.027 (3) | 0.005 (3) | −0.001 (3) | −0.002 (3) |
C12 | 0.029 (3) | 0.045 (4) | 0.038 (4) | 0.003 (3) | −0.015 (3) | −0.006 (3) |
C13 | 0.033 (4) | 0.059 (4) | 0.049 (4) | 0.003 (3) | −0.019 (3) | −0.017 (4) |
C14 | 0.033 (4) | 0.047 (4) | 0.054 (4) | 0.000 (3) | −0.013 (3) | −0.026 (3) |
C15 | 0.032 (4) | 0.037 (4) | 0.062 (5) | 0.000 (3) | −0.016 (3) | −0.013 (3) |
C16 | 0.040 (4) | 0.037 (4) | 0.066 (5) | −0.001 (3) | −0.019 (4) | −0.010 (4) |
C17 | 0.041 (4) | 0.059 (5) | 0.061 (5) | −0.005 (4) | −0.010 (4) | −0.006 (4) |
C18 | 0.073 (6) | 0.042 (4) | 0.079 (6) | −0.007 (4) | −0.030 (5) | 0.006 (4) |
C19 | 0.058 (5) | 0.049 (5) | 0.111 (7) | 0.005 (4) | −0.039 (5) | −0.022 (5) |
C20 | 0.041 (4) | 0.045 (4) | 0.074 (5) | 0.004 (3) | −0.017 (4) | −0.018 (4) |
C21 | 0.038 (4) | 0.044 (4) | 0.045 (4) | −0.007 (3) | −0.008 (3) | −0.007 (3) |
C22 | 0.039 (4) | 0.053 (4) | 0.052 (4) | −0.001 (3) | −0.006 (3) | −0.010 (3) |
C23 | 0.052 (5) | 0.090 (6) | 0.044 (4) | −0.007 (4) | −0.001 (4) | −0.004 (4) |
C24 | 0.074 (6) | 0.114 (7) | 0.055 (5) | 0.007 (5) | −0.011 (5) | −0.008 (5) |
C25 | 0.045 (4) | 0.037 (4) | 0.039 (4) | 0.000 (3) | −0.007 (3) | −0.011 (3) |
C26 | 0.061 (5) | 0.041 (4) | 0.047 (4) | −0.009 (3) | −0.011 (4) | −0.013 (3) |
C27 | 0.079 (6) | 0.091 (6) | 0.061 (5) | 0.000 (5) | −0.022 (4) | −0.041 (5) |
C28 | 0.121 (8) | 0.072 (6) | 0.087 (6) | 0.008 (5) | −0.045 (6) | −0.044 (5) |
C29 | 0.035 (4) | 0.040 (4) | 0.050 (4) | 0.009 (3) | −0.011 (3) | −0.023 (3) |
C30 | 0.032 (4) | 0.057 (4) | 0.045 (4) | −0.001 (3) | −0.006 (3) | −0.014 (3) |
C31 | 0.039 (4) | 0.090 (6) | 0.042 (4) | 0.009 (4) | −0.011 (3) | −0.028 (4) |
C32 | 0.066 (6) | 0.128 (8) | 0.052 (5) | −0.013 (5) | 0.011 (4) | −0.009 (5) |
C33 | 0.045 (4) | 0.035 (3) | 0.040 (4) | 0.004 (3) | −0.012 (3) | −0.005 (3) |
C34 | 0.052 (4) | 0.050 (4) | 0.047 (4) | −0.006 (3) | −0.011 (3) | −0.014 (3) |
C35 | 0.060 (5) | 0.080 (5) | 0.057 (5) | −0.011 (4) | −0.013 (4) | −0.022 (4) |
C36 | 0.064 (5) | 0.108 (7) | 0.052 (5) | −0.007 (5) | −0.006 (4) | −0.006 (5) |
C37 | 0.031 (3) | 0.027 (3) | 0.046 (4) | −0.004 (3) | −0.007 (3) | −0.006 (3) |
C38 | 0.036 (4) | 0.037 (4) | 0.041 (4) | 0.002 (3) | −0.006 (3) | −0.014 (3) |
C39 | 0.058 (5) | 0.054 (4) | 0.051 (4) | −0.009 (4) | −0.011 (4) | −0.013 (4) |
C40 | 0.069 (5) | 0.086 (6) | 0.047 (4) | 0.002 (5) | −0.002 (4) | −0.027 (4) |
C41 | 0.024 (3) | 0.034 (3) | 0.056 (4) | 0.005 (3) | −0.009 (3) | −0.024 (3) |
C42 | 0.037 (4) | 0.041 (4) | 0.050 (4) | 0.002 (3) | −0.008 (3) | −0.009 (3) |
C43 | 0.044 (4) | 0.059 (4) | 0.042 (4) | 0.004 (3) | −0.017 (3) | −0.010 (3) |
C44 | 0.054 (5) | 0.095 (6) | 0.048 (5) | −0.008 (4) | −0.005 (4) | −0.005 (4) |
C45 | 0.049 (4) | 0.027 (4) | 0.041 (4) | 0.006 (3) | −0.014 (3) | −0.005 (3) |
C46 | 0.056 (5) | 0.049 (4) | 0.058 (4) | 0.015 (4) | −0.028 (4) | −0.012 (4) |
C47 | 0.048 (4) | 0.042 (4) | 0.068 (5) | 0.014 (3) | −0.023 (4) | −0.002 (4) |
C48 | 0.032 (4) | 0.033 (4) | 0.076 (5) | 0.005 (3) | −0.013 (4) | −0.010 (4) |
C49 | 0.041 (4) | 0.038 (4) | 0.070 (5) | 0.006 (3) | −0.016 (4) | −0.015 (4) |
C50 | 0.052 (5) | 0.052 (5) | 0.066 (5) | 0.017 (4) | −0.013 (4) | −0.023 (4) |
C51 | 0.073 (6) | 0.065 (5) | 0.081 (6) | 0.008 (4) | −0.012 (5) | −0.020 (5) |
C52 | 0.101 (8) | 0.084 (7) | 0.067 (6) | 0.020 (6) | −0.011 (6) | −0.003 (5) |
C53 | 0.102 (8) | 0.093 (7) | 0.082 (7) | 0.019 (6) | −0.040 (6) | −0.036 (6) |
C54 | 0.068 (6) | 0.063 (5) | 0.095 (7) | −0.003 (4) | −0.034 (5) | −0.024 (5) |
C55 | 0.032 (4) | 0.038 (4) | 0.030 (3) | 0.013 (3) | −0.013 (3) | −0.010 (3) |
C56 | 0.040 (4) | 0.044 (4) | 0.047 (4) | 0.007 (3) | −0.024 (3) | −0.010 (3) |
C57 | 0.035 (4) | 0.065 (5) | 0.047 (4) | −0.003 (3) | −0.018 (3) | −0.020 (4) |
C58 | 0.035 (4) | 0.052 (4) | 0.057 (4) | 0.002 (3) | −0.017 (3) | −0.030 (4) |
C59 | 0.028 (4) | 0.046 (4) | 0.061 (5) | −0.003 (3) | −0.014 (3) | −0.016 (4) |
C60 | 0.038 (4) | 0.047 (4) | 0.069 (5) | 0.000 (3) | −0.023 (4) | −0.021 (4) |
C61 | 0.049 (5) | 0.065 (5) | 0.069 (5) | 0.002 (4) | −0.017 (4) | −0.016 (4) |
C62 | 0.066 (5) | 0.057 (5) | 0.071 (6) | −0.004 (4) | −0.036 (5) | −0.003 (4) |
C63 | 0.055 (5) | 0.054 (5) | 0.114 (7) | 0.012 (4) | −0.047 (5) | −0.026 (5) |
C64 | 0.041 (4) | 0.052 (5) | 0.085 (6) | 0.006 (4) | −0.018 (4) | −0.027 (4) |
C65 | 0.037 (4) | 0.037 (4) | 0.047 (4) | 0.008 (3) | −0.016 (3) | −0.015 (3) |
C66 | 0.055 (5) | 0.049 (4) | 0.054 (4) | −0.002 (3) | −0.010 (4) | −0.018 (3) |
C67 | 0.088 (6) | 0.057 (5) | 0.048 (4) | −0.005 (4) | −0.022 (4) | −0.019 (4) |
C68 | 0.130 (8) | 0.058 (5) | 0.057 (5) | −0.017 (5) | −0.024 (5) | −0.027 (4) |
C69 | 0.028 (4) | 0.050 (4) | 0.058 (4) | −0.002 (3) | −0.006 (3) | −0.009 (3) |
C70 | 0.030 (4) | 0.047 (4) | 0.053 (4) | 0.002 (3) | −0.007 (3) | −0.010 (3) |
C71 | 0.046 (4) | 0.058 (5) | 0.050 (4) | −0.007 (4) | −0.004 (4) | −0.010 (4) |
C72 | 0.053 (5) | 0.076 (5) | 0.059 (5) | −0.017 (4) | 0.002 (4) | −0.008 (4) |
Sn1—O1 | 2.157 (4) | C29—C30 | 1.527 (8) |
Sn1—O2 | 2.962 (4) | C29—H291 | 0.9900 |
Sn1—O4 | 2.238 (4) | C29—H292 | 0.9900 |
Sn1—O7 | 2.021 (4) | C30—C31 | 1.518 (8) |
Sn1—C21 | 2.125 (5) | C30—H301 | 0.9900 |
Sn1—C25 | 2.118 (6) | C30—H302 | 0.9900 |
Sn2—O5 | 2.289 (4) | C31—C32 | 1.535 (9) |
Sn2—O7 | 2.035 (4) | C31—H311 | 0.9900 |
Sn2—O8 | 2.159 (4) | C31—H312 | 0.9900 |
Sn2—O9 | 2.749 (4) | C32—H321 | 0.9800 |
Sn2—C29 | 2.115 (5) | C32—H322 | 0.9800 |
Sn2—C33 | 2.119 (5) | C32—H323 | 0.9800 |
Sn3—O1 | 2.687 (4) | C33—C34 | 1.513 (8) |
Sn3—O7 | 2.185 (4) | C33—H331 | 0.9900 |
Sn3—O8 | 2.054 (4) | C33—H332 | 0.9900 |
Sn3—O13 | 2.295 (4) | C34—C35 | 1.529 (8) |
Sn3—C37 | 2.130 (5) | C34—H341 | 0.9900 |
Sn3—C41 | 2.117 (5) | C34—H342 | 0.9900 |
Sn4—O8 | 2.022 (4) | C35—C36 | 1.496 (9) |
Sn4—O9 | 2.170 (4) | C35—H351 | 0.9900 |
Sn4—O10 | 2.908 (4) | C35—H352 | 0.9900 |
Sn4—O12 | 2.267 (4) | C36—H361 | 0.9800 |
Sn4—C65 | 2.125 (6) | C36—H362 | 0.9800 |
Sn4—C69 | 2.129 (5) | C36—H363 | 0.9800 |
O1—C1 | 1.299 (6) | C37—C38 | 1.532 (7) |
O2—C1 | 1.236 (7) | C37—H371 | 0.9900 |
O3—C6 | 1.355 (8) | C37—H372 | 0.9900 |
O3—H3 | 0.8400 | C38—C39 | 1.509 (8) |
O4—C11 | 1.270 (6) | C38—H381 | 0.9900 |
O5—C11 | 1.254 (6) | C38—H382 | 0.9900 |
O6—C16 | 1.357 (7) | C39—C40 | 1.526 (9) |
O6—H6 | 0.8400 | C39—H391 | 0.9900 |
O9—C45 | 1.299 (7) | C39—H392 | 0.9900 |
O10—C45 | 1.230 (7) | C40—H401 | 0.9800 |
O11—C50 | 1.345 (8) | C40—H402 | 0.9800 |
O11—H11 | 0.8400 | C40—H403 | 0.9800 |
O12—C55 | 1.257 (6) | C41—C42 | 1.535 (7) |
O13—C55 | 1.270 (7) | C41—H411 | 0.9900 |
O14—C60 | 1.355 (7) | C41—H412 | 0.9900 |
O14—H14 | 0.8400 | C42—C43 | 1.528 (8) |
N1—C4 | 1.267 (8) | C42—H421 | 0.9900 |
N1—C3 | 1.463 (8) | C42—H422 | 0.9900 |
N2—C14 | 1.273 (7) | C43—C44 | 1.516 (8) |
N2—C13 | 1.456 (7) | C43—H431 | 0.9900 |
N3—C48 | 1.283 (8) | C43—H432 | 0.9900 |
N3—C47 | 1.450 (8) | C44—H441 | 0.9800 |
N4—C58 | 1.283 (7) | C44—H442 | 0.9800 |
N4—C57 | 1.453 (7) | C44—H443 | 0.9800 |
C1—C2 | 1.496 (8) | C45—C46 | 1.498 (8) |
C2—C3 | 1.529 (8) | C46—C47 | 1.518 (8) |
C2—H21 | 0.9900 | C46—H461 | 0.9900 |
C2—H22 | 0.9900 | C46—H462 | 0.9900 |
C3—H31 | 0.9900 | C47—H471 | 0.9900 |
C3—H32 | 0.9900 | C47—H472 | 0.9900 |
C4—C5 | 1.430 (9) | C48—C49 | 1.446 (9) |
C4—H4 | 0.9500 | C48—H48 | 0.9500 |
C5—C10 | 1.395 (9) | C49—C54 | 1.387 (10) |
C5—C6 | 1.416 (9) | C49—C50 | 1.414 (9) |
C6—C7 | 1.370 (9) | C50—C51 | 1.382 (10) |
C7—C8 | 1.368 (11) | C51—C52 | 1.373 (11) |
C7—H7 | 0.9500 | C51—H51 | 0.9500 |
C8—C9 | 1.394 (11) | C52—C53 | 1.372 (11) |
C8—H8 | 0.9500 | C52—H52 | 0.9500 |
C9—C10 | 1.368 (10) | C53—C54 | 1.368 (11) |
C9—H9 | 0.9500 | C53—H53 | 0.9500 |
C10—H10 | 0.9500 | C54—H54 | 0.9500 |
C11—C12 | 1.493 (8) | C55—C56 | 1.489 (8) |
C12—C13 | 1.519 (8) | C56—C57 | 1.530 (8) |
C12—H121 | 0.9900 | C56—H561 | 0.9900 |
C12—H122 | 0.9900 | C56—H562 | 0.9900 |
C13—H131 | 0.9900 | C57—H571 | 0.9900 |
C13—H132 | 0.9900 | C57—H572 | 0.9900 |
C14—C15 | 1.447 (8) | C58—C59 | 1.449 (8) |
C14—H141 | 0.9500 | C58—H58 | 0.9500 |
C15—C20 | 1.392 (8) | C59—C64 | 1.392 (9) |
C15—C16 | 1.399 (9) | C59—C60 | 1.395 (9) |
C16—C17 | 1.388 (8) | C60—C61 | 1.380 (9) |
C17—C18 | 1.392 (9) | C61—C62 | 1.363 (9) |
C17—H17 | 0.9500 | C61—H61 | 0.9500 |
C18—C19 | 1.375 (10) | C62—C63 | 1.384 (10) |
C18—H18 | 0.9500 | C62—H62 | 0.9500 |
C19—C20 | 1.371 (9) | C63—C64 | 1.373 (10) |
C19—H19 | 0.9500 | C63—H63 | 0.9500 |
C20—H20 | 0.9500 | C64—H64 | 0.9500 |
C21—C22 | 1.525 (8) | C65—C66 | 1.517 (8) |
C21—H211 | 0.9900 | C65—H651 | 0.9900 |
C21—H212 | 0.9900 | C65—H652 | 0.9900 |
C22—C23 | 1.541 (8) | C66—C67 | 1.502 (8) |
C22—H221 | 0.9900 | C66—H661 | 0.9900 |
C22—H222 | 0.9900 | C66—H662 | 0.9900 |
C23—C24 | 1.527 (9) | C67—C68 | 1.518 (9) |
C23—H231 | 0.9900 | C67—H671 | 0.9900 |
C23—H232 | 0.9900 | C67—H672 | 0.9900 |
C24—H241 | 0.9800 | C68—H681 | 0.9800 |
C24—H242 | 0.9800 | C68—H682 | 0.9800 |
C24—H243 | 0.9800 | C68—H683 | 0.9800 |
C25—C26 | 1.512 (8) | C69—C70 | 1.516 (8) |
C25—H251 | 0.9900 | C69—H691 | 0.9900 |
C25—H252 | 0.9900 | C69—H692 | 0.9900 |
C26—C27 | 1.492 (8) | C70—C71 | 1.519 (8) |
C26—H261 | 0.9900 | C70—H701 | 0.9900 |
C26—H262 | 0.9900 | C70—H702 | 0.9900 |
C27—C28 | 1.495 (9) | C71—C72 | 1.514 (9) |
C27—H271 | 0.9900 | C71—H711 | 0.9900 |
C27—H272 | 0.9900 | C71—H712 | 0.9900 |
C28—H281 | 0.9800 | C72—H721 | 0.9800 |
C28—H282 | 0.9800 | C72—H722 | 0.9800 |
C28—H283 | 0.9800 | C72—H723 | 0.9800 |
O1—Sn1—O2 | 47.92 (13) | H291—C29—H292 | 107.9 |
O1—Sn1—O4 | 168.40 (14) | C31—C30—C29 | 113.6 (5) |
O1—Sn1—O7 | 78.96 (14) | C31—C30—H301 | 108.9 |
O1—Sn1—C21 | 99.87 (19) | C29—C30—H301 | 108.9 |
O1—Sn1—C25 | 95.4 (2) | C31—C30—H302 | 108.9 |
O2—Sn1—O4 | 142.74 (13) | C29—C30—H302 | 108.9 |
O2—Sn1—O7 | 126.82 (14) | H301—C30—H302 | 107.7 |
O2—Sn1—C21 | 80.07 (19) | C30—C31—C32 | 111.7 (6) |
O2—Sn1—C25 | 78.55 (19) | C30—C31—H311 | 109.3 |
O4—Sn1—O7 | 90.39 (14) | C32—C31—H311 | 109.3 |
O4—Sn1—C21 | 88.3 (2) | C30—C31—H312 | 109.3 |
O4—Sn1—C25 | 84.7 (2) | C32—C31—H312 | 109.3 |
O7—Sn1—C21 | 111.7 (2) | H311—C31—H312 | 107.9 |
O7—Sn1—C25 | 114.05 (18) | C31—C32—H321 | 109.5 |
C21—Sn1—C25 | 133.7 (2) | C31—C32—H322 | 109.5 |
O5—Sn2—O7 | 88.76 (14) | H321—C32—H322 | 109.5 |
O5—Sn2—O8 | 164.11 (14) | C31—C32—H323 | 109.5 |
O5—Sn2—O9 | 131.33 (13) | H321—C32—H323 | 109.5 |
O5—Sn2—C29 | 84.77 (19) | H322—C32—H323 | 109.5 |
O5—Sn2—C33 | 88.4 (2) | C34—C33—Sn2 | 117.1 (4) |
O7—Sn2—O8 | 76.01 (14) | C34—C33—H331 | 108.0 |
O7—Sn2—O9 | 139.90 (13) | Sn2—C33—H331 | 108.0 |
O7—Sn2—C29 | 107.64 (19) | C34—C33—H332 | 108.0 |
O7—Sn2—C33 | 109.61 (19) | Sn2—C33—H332 | 108.0 |
O8—Sn2—O9 | 64.10 (12) | H331—C33—H332 | 107.3 |
O8—Sn2—C29 | 95.4 (2) | C33—C34—C35 | 113.6 (5) |
O8—Sn2—C33 | 100.9 (2) | C33—C34—H341 | 108.9 |
O9—Sn2—C29 | 81.15 (17) | C35—C34—H341 | 108.9 |
O9—Sn2—C33 | 75.58 (18) | C33—C34—H342 | 108.9 |
C29—Sn2—C33 | 141.9 (2) | C35—C34—H342 | 108.9 |
O1—Sn3—O7 | 65.19 (12) | H341—C34—H342 | 107.7 |
O1—Sn3—O8 | 140.08 (13) | C36—C35—C34 | 113.4 (6) |
O1—Sn3—O13 | 129.85 (13) | C36—C35—H351 | 108.9 |
O1—Sn3—C37 | 76.61 (17) | C34—C35—H351 | 108.9 |
O1—Sn3—C41 | 79.64 (16) | C36—C35—H352 | 108.9 |
O7—Sn3—O8 | 75.04 (13) | C34—C35—H352 | 108.9 |
O7—Sn3—O13 | 164.68 (13) | H351—C35—H352 | 107.7 |
O7—Sn3—C37 | 99.74 (18) | C35—C36—H361 | 109.5 |
O7—Sn3—C41 | 95.43 (18) | C35—C36—H362 | 109.5 |
O8—Sn3—O13 | 90.05 (14) | H361—C36—H362 | 109.5 |
O8—Sn3—C37 | 108.06 (18) | C35—C36—H363 | 109.5 |
O8—Sn3—C41 | 108.35 (18) | H361—C36—H363 | 109.5 |
O13—Sn3—C37 | 88.07 (18) | H362—C36—H363 | 109.5 |
O13—Sn3—C41 | 85.82 (18) | C38—C37—Sn3 | 115.2 (4) |
C37—Sn3—C41 | 143.0 (2) | C38—C37—H371 | 108.5 |
O8—Sn4—O9 | 78.42 (14) | Sn3—C37—H371 | 108.5 |
O8—Sn4—O10 | 127.46 (14) | C38—C37—H372 | 108.5 |
O8—Sn4—O12 | 90.96 (14) | Sn3—C37—H372 | 108.5 |
O8—Sn4—C65 | 113.08 (19) | H371—C37—H372 | 107.5 |
O8—Sn4—C69 | 111.7 (2) | C39—C38—C37 | 112.5 (5) |
O9—Sn4—O10 | 49.09 (13) | C39—C38—H381 | 109.1 |
O9—Sn4—O12 | 168.21 (14) | C37—C38—H381 | 109.1 |
O9—Sn4—C65 | 95.69 (19) | C39—C38—H382 | 109.1 |
O9—Sn4—C69 | 101.3 (2) | C37—C38—H382 | 109.1 |
O10—Sn4—O12 | 141.50 (14) | H381—C38—H382 | 107.8 |
O10—Sn4—C65 | 79.04 (18) | C38—C39—C40 | 112.6 (5) |
O10—Sn4—C69 | 80.90 (19) | C38—C39—H391 | 109.1 |
O12—Sn4—C65 | 83.66 (19) | C40—C39—H391 | 109.1 |
O12—Sn4—C69 | 87.3 (2) | C38—C39—H392 | 109.1 |
C65—Sn4—C69 | 134.4 (2) | C40—C39—H392 | 109.1 |
C1—O1—Sn1 | 114.2 (4) | H391—C39—H392 | 107.8 |
C1—O1—Sn3 | 149.0 (4) | C39—C40—H401 | 109.5 |
Sn1—O1—Sn3 | 95.95 (13) | C39—C40—H402 | 109.5 |
C1—O2—Sn1 | 76.9 (3) | H401—C40—H402 | 109.5 |
C6—O3—H3 | 109.5 | C39—C40—H403 | 109.5 |
C11—O4—Sn1 | 133.7 (4) | H401—C40—H403 | 109.5 |
C11—O5—Sn2 | 133.1 (4) | H402—C40—H403 | 109.5 |
C16—O6—H6 | 109.5 | C42—C41—Sn3 | 114.3 (4) |
Sn1—O7—Sn2 | 136.7 (2) | C42—C41—H411 | 108.7 |
Sn1—O7—Sn3 | 118.47 (17) | Sn3—C41—H411 | 108.7 |
Sn2—O7—Sn3 | 104.34 (15) | C42—C41—H412 | 108.7 |
Sn2—O8—Sn3 | 104.61 (16) | Sn3—C41—H412 | 108.7 |
Sn2—O8—Sn4 | 120.77 (17) | H411—C41—H412 | 107.6 |
Sn3—O8—Sn4 | 134.05 (19) | C43—C42—C41 | 112.9 (5) |
Sn2—O9—Sn4 | 94.56 (13) | C43—C42—H421 | 109.0 |
C45—O9—Sn4 | 111.1 (4) | C41—C42—H421 | 109.0 |
C45—O9—Sn2 | 152.7 (4) | C43—C42—H422 | 109.0 |
C45—O10—Sn4 | 77.5 (3) | C41—C42—H422 | 109.0 |
C50—O11—H11 | 109.5 | H421—C42—H422 | 107.8 |
C55—O12—Sn4 | 133.0 (4) | C44—C43—C42 | 112.2 (6) |
C55—O13—Sn3 | 130.1 (4) | C44—C43—H431 | 109.2 |
C60—O14—H14 | 109.5 | C42—C43—H431 | 109.2 |
C4—N1—C3 | 119.7 (6) | C44—C43—H432 | 109.2 |
C14—N2—C13 | 119.0 (5) | C42—C43—H432 | 109.2 |
C48—N3—C47 | 118.3 (6) | H431—C43—H432 | 107.9 |
C58—N4—C57 | 118.7 (5) | C43—C44—H441 | 109.5 |
O2—C1—O1 | 120.9 (6) | C43—C44—H442 | 109.5 |
O2—C1—C2 | 122.5 (5) | H441—C44—H442 | 109.5 |
O1—C1—C2 | 116.6 (5) | C43—C44—H443 | 109.5 |
C1—C2—C3 | 111.7 (5) | H441—C44—H443 | 109.5 |
C1—C2—H21 | 109.3 | H442—C44—H443 | 109.5 |
C3—C2—H21 | 109.3 | O10—C45—O9 | 122.1 (6) |
C1—C2—H22 | 109.3 | O10—C45—C46 | 122.0 (5) |
C3—C2—H22 | 109.3 | O9—C45—C46 | 115.9 (6) |
H21—C2—H22 | 107.9 | C45—C46—C47 | 111.8 (6) |
N1—C3—C2 | 109.4 (5) | C45—C46—H461 | 109.3 |
N1—C3—H31 | 109.8 | C47—C46—H461 | 109.3 |
C2—C3—H31 | 109.8 | C45—C46—H462 | 109.3 |
N1—C3—H32 | 109.8 | C47—C46—H462 | 109.3 |
C2—C3—H32 | 109.8 | H461—C46—H462 | 107.9 |
H31—C3—H32 | 108.2 | N3—C47—C46 | 110.1 (5) |
N1—C4—C5 | 121.7 (6) | N3—C47—H471 | 109.6 |
N1—C4—H4 | 119.1 | C46—C47—H471 | 109.6 |
C5—C4—H4 | 119.1 | N3—C47—H472 | 109.6 |
C10—C5—C6 | 118.1 (7) | C46—C47—H472 | 109.6 |
C10—C5—C4 | 120.3 (7) | H471—C47—H472 | 108.1 |
C6—C5—C4 | 121.5 (6) | N3—C48—C49 | 123.4 (6) |
O3—C6—C7 | 119.5 (7) | N3—C48—H48 | 118.3 |
O3—C6—C5 | 120.6 (6) | C49—C48—H48 | 118.3 |
C7—C6—C5 | 119.9 (7) | C54—C49—C50 | 118.3 (7) |
C8—C7—C6 | 120.8 (8) | C54—C49—C48 | 122.3 (7) |
C8—C7—H7 | 119.6 | C50—C49—C48 | 119.3 (7) |
C6—C7—H7 | 119.6 | O11—C50—C51 | 117.5 (7) |
C7—C8—C9 | 120.4 (8) | O11—C50—C49 | 123.0 (7) |
C7—C8—H8 | 119.8 | C51—C50—C49 | 119.5 (8) |
C9—C8—H8 | 119.8 | C52—C51—C50 | 120.4 (8) |
C10—C9—C8 | 119.3 (8) | C52—C51—H51 | 119.8 |
C10—C9—H9 | 120.4 | C50—C51—H51 | 119.8 |
C8—C9—H9 | 120.4 | C53—C52—C51 | 120.5 (9) |
C9—C10—C5 | 121.5 (8) | C53—C52—H52 | 119.7 |
C9—C10—H10 | 119.3 | C51—C52—H52 | 119.7 |
C5—C10—H10 | 119.3 | C54—C53—C52 | 119.9 (9) |
O5—C11—O4 | 123.9 (5) | C54—C53—H53 | 120.1 |
O5—C11—C12 | 118.8 (5) | C52—C53—H53 | 120.1 |
O4—C11—C12 | 117.1 (5) | C53—C54—C49 | 121.3 (8) |
C11—C12—C13 | 114.2 (5) | C53—C54—H54 | 119.4 |
C11—C12—H121 | 108.7 | C49—C54—H54 | 119.4 |
C13—C12—H121 | 108.7 | O12—C55—O13 | 123.5 (5) |
C11—C12—H122 | 108.7 | O12—C55—C56 | 119.0 (5) |
C13—C12—H122 | 108.7 | O13—C55—C56 | 117.2 (5) |
H121—C12—H122 | 107.6 | C55—C56—C57 | 112.8 (5) |
N2—C13—C12 | 110.8 (5) | C55—C56—H561 | 109.0 |
N2—C13—H131 | 109.5 | C57—C56—H561 | 109.0 |
C12—C13—H131 | 109.5 | C55—C56—H562 | 109.0 |
N2—C13—H132 | 109.5 | C57—C56—H562 | 109.0 |
C12—C13—H132 | 109.5 | H561—C56—H562 | 107.8 |
H131—C13—H132 | 108.1 | N4—C57—C56 | 109.9 (5) |
N2—C14—C15 | 122.8 (6) | N4—C57—H571 | 109.7 |
N2—C14—H141 | 118.6 | C56—C57—H571 | 109.7 |
C15—C14—H141 | 118.6 | N4—C57—H572 | 109.7 |
C20—C15—C16 | 118.8 (6) | C56—C57—H572 | 109.7 |
C20—C15—C14 | 119.6 (6) | H571—C57—H572 | 108.2 |
C16—C15—C14 | 121.6 (6) | N4—C58—C59 | 123.3 (6) |
O6—C16—C17 | 118.1 (6) | N4—C58—H58 | 118.3 |
O6—C16—C15 | 121.4 (6) | C59—C58—H58 | 118.3 |
C17—C16—C15 | 120.5 (6) | C64—C59—C60 | 118.8 (6) |
C16—C17—C18 | 118.7 (7) | C64—C59—C58 | 119.8 (6) |
C16—C17—H17 | 120.7 | C60—C59—C58 | 121.4 (6) |
C18—C17—H17 | 120.7 | O14—C60—C61 | 117.8 (6) |
C19—C18—C17 | 121.4 (7) | O14—C60—C59 | 122.1 (6) |
C19—C18—H18 | 119.3 | C61—C60—C59 | 120.1 (7) |
C17—C18—H18 | 119.3 | C62—C61—C60 | 120.4 (7) |
C20—C19—C18 | 119.5 (7) | C62—C61—H61 | 119.8 |
C20—C19—H19 | 120.2 | C60—C61—H61 | 119.8 |
C18—C19—H19 | 120.2 | C61—C62—C63 | 120.3 (7) |
C19—C20—C15 | 121.0 (7) | C61—C62—H62 | 119.9 |
C19—C20—H20 | 119.5 | C63—C62—H62 | 119.9 |
C15—C20—H20 | 119.5 | C64—C63—C62 | 120.1 (7) |
C22—C21—Sn1 | 115.5 (4) | C64—C63—H63 | 120.0 |
C22—C21—H211 | 108.4 | C62—C63—H63 | 120.0 |
Sn1—C21—H211 | 108.4 | C63—C64—C59 | 120.3 (7) |
C22—C21—H212 | 108.4 | C63—C64—H64 | 119.8 |
Sn1—C21—H212 | 108.4 | C59—C64—H64 | 119.8 |
H211—C21—H212 | 107.5 | C66—C65—Sn4 | 113.4 (4) |
C21—C22—C23 | 112.3 (5) | C66—C65—H651 | 108.9 |
C21—C22—H221 | 109.1 | Sn4—C65—H651 | 108.9 |
C23—C22—H221 | 109.1 | C66—C65—H652 | 108.9 |
C21—C22—H222 | 109.1 | Sn4—C65—H652 | 108.9 |
C23—C22—H222 | 109.1 | H651—C65—H652 | 107.7 |
H221—C22—H222 | 107.9 | C67—C66—C65 | 113.9 (5) |
C24—C23—C22 | 112.1 (6) | C67—C66—H661 | 108.8 |
C24—C23—H231 | 109.2 | C65—C66—H661 | 108.8 |
C22—C23—H231 | 109.2 | C67—C66—H662 | 108.8 |
C24—C23—H232 | 109.2 | C65—C66—H662 | 108.8 |
C22—C23—H232 | 109.2 | H661—C66—H662 | 107.7 |
H231—C23—H232 | 107.9 | C66—C67—C68 | 113.4 (6) |
C23—C24—H241 | 109.5 | C66—C67—H671 | 108.9 |
C23—C24—H242 | 109.5 | C68—C67—H671 | 108.9 |
H241—C24—H242 | 109.5 | C66—C67—H672 | 108.9 |
C23—C24—H243 | 109.5 | C68—C67—H672 | 108.9 |
H241—C24—H243 | 109.5 | H671—C67—H672 | 107.7 |
H242—C24—H243 | 109.5 | C67—C68—H681 | 109.5 |
C26—C25—Sn1 | 115.3 (4) | C67—C68—H682 | 109.5 |
C26—C25—H251 | 108.4 | H681—C68—H682 | 109.5 |
Sn1—C25—H251 | 108.4 | C67—C68—H683 | 109.5 |
C26—C25—H252 | 108.4 | H681—C68—H683 | 109.5 |
Sn1—C25—H252 | 108.4 | H682—C68—H683 | 109.5 |
H251—C25—H252 | 107.5 | C70—C69—Sn4 | 116.3 (4) |
C27—C26—C25 | 115.3 (5) | C70—C69—H691 | 108.2 |
C27—C26—H261 | 108.5 | Sn4—C69—H691 | 108.2 |
C25—C26—H261 | 108.5 | C70—C69—H692 | 108.2 |
C27—C26—H262 | 108.5 | Sn4—C69—H692 | 108.2 |
C25—C26—H262 | 108.5 | H691—C69—H692 | 107.4 |
H261—C26—H262 | 107.5 | C69—C70—C71 | 112.5 (5) |
C26—C27—C28 | 115.7 (7) | C69—C70—H701 | 109.1 |
C26—C27—H271 | 108.4 | C71—C70—H701 | 109.1 |
C28—C27—H271 | 108.4 | C69—C70—H702 | 109.1 |
C26—C27—H272 | 108.4 | C71—C70—H702 | 109.1 |
C28—C27—H272 | 108.4 | H701—C70—H702 | 107.8 |
H271—C27—H272 | 107.4 | C72—C71—C70 | 113.5 (6) |
C27—C28—H281 | 109.5 | C72—C71—H711 | 108.9 |
C27—C28—H282 | 109.5 | C70—C71—H711 | 108.9 |
H281—C28—H282 | 109.5 | C72—C71—H712 | 108.9 |
C27—C28—H283 | 109.5 | C70—C71—H712 | 108.9 |
H281—C28—H283 | 109.5 | H711—C71—H712 | 107.7 |
H282—C28—H283 | 109.5 | C71—C72—H721 | 109.5 |
C30—C29—Sn2 | 112.0 (4) | C71—C72—H722 | 109.5 |
C30—C29—H291 | 109.2 | H721—C72—H722 | 109.5 |
Sn2—C29—H291 | 109.2 | C71—C72—H723 | 109.5 |
C30—C29—H292 | 109.2 | H721—C72—H723 | 109.5 |
Sn2—C29—H292 | 109.2 | H722—C72—H723 | 109.5 |
Sn1—O2—C1—O1 | 2.8 (5) | Sn3—C37—C38—C39 | 176.0 (4) |
Sn1—O2—C1—C2 | 178.7 (6) | C37—C38—C39—C40 | 179.1 (6) |
Sn1—O1—C1—O2 | −4.1 (7) | Sn3—C41—C42—C43 | −176.1 (4) |
Sn3—O1—C1—O2 | −169.8 (4) | C41—C42—C43—C44 | −166.9 (5) |
Sn1—O1—C1—C2 | 179.7 (4) | Sn4—O10—C45—O9 | −3.7 (5) |
Sn3—O1—C1—C2 | 14.1 (10) | Sn4—O10—C45—C46 | 177.5 (6) |
O2—C1—C2—C3 | 43.1 (8) | Sn4—O9—C45—O10 | 5.2 (7) |
O1—C1—C2—C3 | −140.8 (5) | Sn2—O9—C45—O10 | 164.3 (5) |
C4—N1—C3—C2 | −116.4 (6) | Sn4—O9—C45—C46 | −175.9 (4) |
C1—C2—C3—N1 | 62.4 (7) | Sn2—O9—C45—C46 | −16.9 (11) |
C3—N1—C4—C5 | 176.3 (5) | O10—C45—C46—C47 | −43.4 (9) |
N1—C4—C5—C10 | 179.1 (6) | O9—C45—C46—C47 | 137.8 (6) |
N1—C4—C5—C6 | −3.7 (10) | C48—N3—C47—C46 | 121.0 (7) |
C10—C5—C6—O3 | −178.6 (6) | C45—C46—C47—N3 | −63.9 (7) |
C4—C5—C6—O3 | 4.2 (10) | C47—N3—C48—C49 | −178.0 (5) |
C10—C5—C6—C7 | 1.9 (10) | N3—C48—C49—C54 | −177.5 (7) |
C4—C5—C6—C7 | −175.3 (7) | N3—C48—C49—C50 | 3.6 (10) |
O3—C6—C7—C8 | 178.6 (8) | C54—C49—C50—O11 | 178.9 (7) |
C5—C6—C7—C8 | −1.9 (12) | C48—C49—C50—O11 | −2.0 (10) |
C6—C7—C8—C9 | 0.1 (14) | C54—C49—C50—C51 | −0.6 (10) |
C7—C8—C9—C10 | 1.6 (14) | C48—C49—C50—C51 | 178.4 (6) |
C8—C9—C10—C5 | −1.5 (13) | O11—C50—C51—C52 | −178.2 (7) |
C6—C5—C10—C9 | −0.2 (11) | C49—C50—C51—C52 | 1.4 (12) |
C4—C5—C10—C9 | 177.0 (7) | C50—C51—C52—C53 | −0.2 (14) |
Sn2—O5—C11—O4 | 24.4 (8) | C51—C52—C53—C54 | −1.7 (14) |
Sn2—O5—C11—C12 | −151.2 (4) | C52—C53—C54—C49 | 2.4 (13) |
Sn1—O4—C11—O5 | 21.5 (8) | C50—C49—C54—C53 | −1.3 (11) |
Sn1—O4—C11—C12 | −162.8 (3) | C48—C49—C54—C53 | 179.7 (7) |
O5—C11—C12—C13 | −158.8 (5) | Sn4—O12—C55—O13 | −20.6 (8) |
O4—C11—C12—C13 | 25.3 (7) | Sn4—O12—C55—C56 | 165.5 (4) |
C14—N2—C13—C12 | −129.2 (6) | Sn3—O13—C55—O12 | −31.0 (8) |
C11—C12—C13—N2 | 66.6 (7) | Sn3—O13—C55—C56 | 143.1 (4) |
C13—N2—C14—C15 | −179.0 (5) | O12—C55—C56—C57 | −27.0 (8) |
N2—C14—C15—C20 | −178.2 (6) | O13—C55—C56—C57 | 158.6 (5) |
N2—C14—C15—C16 | 1.9 (10) | C58—N4—C57—C56 | 129.5 (6) |
C20—C15—C16—O6 | −179.7 (6) | C55—C56—C57—N4 | −63.6 (7) |
C14—C15—C16—O6 | 0.2 (10) | C57—N4—C58—C59 | −178.4 (5) |
C20—C15—C16—C17 | −2.5 (10) | N4—C58—C59—C64 | 180.0 (6) |
C14—C15—C16—C17 | 177.4 (6) | N4—C58—C59—C60 | −0.1 (10) |
O6—C16—C17—C18 | 179.1 (6) | C64—C59—C60—O14 | 178.9 (6) |
C15—C16—C17—C18 | 1.8 (10) | C58—C59—C60—O14 | −1.0 (10) |
C16—C17—C18—C19 | −0.7 (11) | C64—C59—C60—C61 | −1.3 (10) |
C17—C18—C19—C20 | 0.2 (12) | C58—C59—C60—C61 | 178.8 (6) |
C18—C19—C20—C15 | −0.9 (11) | O14—C60—C61—C62 | −178.5 (6) |
C16—C15—C20—C19 | 2.0 (10) | C59—C60—C61—C62 | 1.6 (11) |
C14—C15—C20—C19 | −177.9 (6) | C60—C61—C62—C63 | −0.5 (11) |
Sn1—C21—C22—C23 | −178.1 (5) | C61—C62—C63—C64 | −1.0 (11) |
C21—C22—C23—C24 | −179.8 (6) | C62—C63—C64—C59 | 1.4 (11) |
Sn1—C25—C26—C27 | 173.7 (5) | C60—C59—C64—C63 | −0.3 (10) |
C25—C26—C27—C28 | 177.7 (7) | C58—C59—C64—C63 | 179.7 (6) |
Sn2—C29—C30—C31 | 169.9 (4) | Sn4—C65—C66—C67 | −169.9 (5) |
C29—C30—C31—C32 | 173.5 (6) | C65—C66—C67—C68 | −173.5 (6) |
Sn2—C33—C34—C35 | 177.9 (4) | Sn4—C69—C70—C71 | −178.7 (4) |
C33—C34—C35—C36 | 66.6 (9) | C69—C70—C71—C72 | 177.0 (6) |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3···N1 | 0.84 | 1.83 | 2.575 (7) | 147 |
O6—H6···N2 | 0.84 | 1.88 | 2.616 (6) | 146 |
O11—H11···N3 | 0.84 | 1.87 | 2.602 (7) | 145 |
O14—H14···N4 | 0.84 | 1.90 | 2.637 (6) | 147 |