Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802018123/lh6005sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802018123/lh6005Isup2.hkl |
CCDC reference: 200756
Data collection: SMART (Bruker, 1997-1999); cell refinement: SMART; data reduction: SHELXTL (Sheldrick, 1997a); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997b); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997b); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
C29H36BNO4S | Z = 4 |
Mr = 505.46 | F(000) = 1080 |
Triclinic, P1 | Dx = 1.198 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 12.7798 (9) Å | Cell parameters from 9524 reflections |
b = 14.4877 (10) Å | θ = 2.3–33.2° |
c = 16.5149 (12) Å | µ = 0.15 mm−1 |
α = 66.858 (2)° | T = 173 K |
β = 86.916 (2)° | Block, colourless |
γ = 85.396 (2)° | 0.45 × 0.40 × 0.35 mm |
V = 2801.8 (3) Å3 |
Bruker SMART CCD diffractometer | 11889 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.022 |
Graphite monochromator | θmax = 32.5°, θmin = 1.5° |
φ and ω scans | h = −19→18 |
30001 measured reflections | k = −21→21 |
19380 independent reflections | l = −23→24 |
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)] = 0.053 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.154 | H-atom parameters constrained |
S = 0.95 | w = 1/[σ2(Fo2) + (0.0893P)2] where P = (Fo2 + 2Fc2)/3 |
19380 reflections | (Δ/σ)max = 0.001 |
665 parameters | Δρmax = 0.70 e Å−3 |
0 restraints | Δρmin = −0.47 e Å−3 |
Experimental. Crystal decay was monitored by repeating the initial 50 frames at the end of the data collection and analyzing duplicate reflections. |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
B1 | 0.14125 (12) | 0.68127 (12) | 0.03085 (11) | 0.0323 (3) | |
O2 | 0.06318 (7) | 0.62688 (8) | 0.02094 (7) | 0.0372 (2) | |
C3 | −0.03566 (11) | 0.66417 (11) | 0.05065 (10) | 0.0357 (3) | |
C4 | 0.00418 (10) | 0.71241 (11) | 0.11228 (10) | 0.0356 (3) | |
O5 | 0.10832 (7) | 0.74323 (8) | 0.07371 (7) | 0.0386 (2) | |
C6 | −0.10372 (13) | 0.57574 (13) | 0.09626 (13) | 0.0498 (4) | |
H6A | −0.1173 | 0.5448 | 0.0550 | 0.075* | |
H6B | −0.1705 | 0.5995 | 0.1157 | 0.075* | |
H6C | −0.0672 | 0.5260 | 0.1474 | 0.075* | |
C7 | −0.08874 (14) | 0.74103 (14) | −0.03088 (12) | 0.0508 (4) | |
H7A | −0.0432 | 0.7966 | −0.0600 | 0.076* | |
H7B | −0.1557 | 0.7670 | −0.0137 | 0.076* | |
H7C | −0.1016 | 0.7090 | −0.0715 | 0.076* | |
C8 | 0.02242 (13) | 0.63737 (14) | 0.20695 (11) | 0.0489 (4) | |
H8A | 0.0674 | 0.5796 | 0.2063 | 0.073* | |
H8B | −0.0451 | 0.6144 | 0.2358 | 0.073* | |
H8C | 0.0566 | 0.6701 | 0.2394 | 0.073* | |
C9 | −0.06323 (12) | 0.80449 (13) | 0.11121 (13) | 0.0480 (4) | |
H9A | −0.0397 | 0.8254 | 0.1566 | 0.072* | |
H9B | −0.1368 | 0.7879 | 0.1231 | 0.072* | |
H9C | −0.0566 | 0.8595 | 0.0533 | 0.072* | |
C10 | 0.25727 (10) | 0.67107 (10) | −0.00098 (9) | 0.0304 (3) | |
C11 | 0.33440 (10) | 0.72446 (9) | 0.01642 (9) | 0.0274 (2) | |
H11 | 0.3150 | 0.7679 | 0.0462 | 0.033* | |
C12 | 0.43864 (10) | 0.71447 (9) | −0.00936 (8) | 0.0259 (2) | |
C13 | 0.46888 (11) | 0.64937 (10) | −0.05117 (9) | 0.0327 (3) | |
H13 | 0.5403 | 0.6422 | −0.0682 | 0.039* | |
C14 | 0.39358 (12) | 0.59475 (11) | −0.06784 (10) | 0.0370 (3) | |
H14 | 0.4139 | 0.5497 | −0.0958 | 0.044* | |
C15 | 0.28925 (11) | 0.60618 (11) | −0.04372 (10) | 0.0357 (3) | |
H15 | 0.2385 | 0.5695 | −0.0563 | 0.043* | |
N16 | 0.51763 (8) | 0.77257 (8) | 0.00597 (7) | 0.0274 (2) | |
C17 | 0.49271 (11) | 0.88294 (10) | −0.02315 (10) | 0.0348 (3) | |
H17A | 0.5560 | 0.9157 | −0.0186 | 0.042* | |
H17B | 0.4370 | 0.8956 | 0.0160 | 0.042* | |
C18 | 0.45633 (12) | 0.92800 (10) | −0.11691 (10) | 0.0384 (3) | |
C19 | 0.52441 (14) | 0.92240 (13) | −0.18480 (12) | 0.0494 (4) | |
C20 | 0.4885 (2) | 0.96409 (16) | −0.27202 (13) | 0.0694 (6) | |
H20 | 0.5340 | 0.9608 | −0.3184 | 0.083* | |
C21 | 0.3878 (2) | 1.00988 (15) | −0.29168 (15) | 0.0731 (7) | |
C22 | 0.32352 (17) | 1.01483 (13) | −0.22404 (15) | 0.0644 (6) | |
H22 | 0.2551 | 1.0466 | −0.2374 | 0.077* | |
C23 | 0.35412 (13) | 0.97539 (11) | −0.13671 (12) | 0.0462 (4) | |
C24 | 0.63405 (15) | 0.87235 (16) | −0.16619 (14) | 0.0651 (5) | |
H24A | 0.6697 | 0.8982 | −0.1291 | 0.098* | |
H24B | 0.6737 | 0.8870 | −0.2218 | 0.098* | |
H24C | 0.6298 | 0.7995 | −0.1356 | 0.098* | |
C25 | 0.3513 (3) | 1.0495 (2) | −0.38704 (16) | 0.1133 (12) | |
H25A | 0.2815 | 1.0266 | −0.3881 | 0.170* | |
H25B | 0.4010 | 1.0241 | −0.4219 | 0.170* | |
H25C | 0.3482 | 1.1232 | −0.4121 | 0.170* | |
C26 | 0.27535 (14) | 0.98581 (13) | −0.06869 (15) | 0.0590 (5) | |
H26A | 0.2106 | 1.0213 | −0.0978 | 0.089* | |
H26B | 0.3046 | 1.0240 | −0.0387 | 0.089* | |
H26C | 0.2598 | 0.9189 | −0.0255 | 0.089* | |
S1 | 0.58378 (2) | 0.71587 (2) | 0.09789 (2) | 0.02926 (8) | |
O3 | 0.61769 (8) | 0.61721 (7) | 0.10263 (7) | 0.0367 (2) | |
O4 | 0.65996 (7) | 0.78399 (8) | 0.09776 (7) | 0.0380 (2) | |
C27 | 0.49113 (10) | 0.70372 (10) | 0.18393 (9) | 0.0286 (3) | |
C28 | 0.47353 (11) | 0.77985 (10) | 0.21548 (10) | 0.0333 (3) | |
H28 | 0.5164 | 0.8355 | 0.1955 | 0.040* | |
C29 | 0.39218 (12) | 0.77331 (11) | 0.27682 (10) | 0.0387 (3) | |
H29 | 0.3803 | 0.8248 | 0.2989 | 0.046* | |
C30 | 0.32773 (11) | 0.69213 (12) | 0.30650 (9) | 0.0370 (3) | |
C31 | 0.34725 (12) | 0.61660 (11) | 0.27442 (10) | 0.0366 (3) | |
H31 | 0.3044 | 0.5608 | 0.2945 | 0.044* | |
C32 | 0.42840 (11) | 0.62119 (10) | 0.21338 (9) | 0.0331 (3) | |
H32 | 0.4410 | 0.5691 | 0.1920 | 0.040* | |
C33 | 0.23807 (14) | 0.68650 (15) | 0.37209 (12) | 0.0524 (4) | |
H33A | 0.1787 | 0.6568 | 0.3583 | 0.079* | |
H33B | 0.2162 | 0.7544 | 0.3686 | 0.079* | |
H33C | 0.2614 | 0.6447 | 0.4318 | 0.079* | |
B41 | 0.38932 (12) | 0.32720 (11) | 0.33425 (11) | 0.0306 (3) | |
O42 | 0.41170 (8) | 0.27175 (9) | 0.42095 (7) | 0.0436 (3) | |
C43 | 0.51416 (11) | 0.30026 (12) | 0.43611 (11) | 0.0396 (3) | |
C44 | 0.56476 (11) | 0.34166 (12) | 0.34137 (11) | 0.0397 (3) | |
O45 | 0.47209 (7) | 0.37786 (7) | 0.28548 (7) | 0.0373 (2) | |
C46 | 0.49194 (17) | 0.38018 (18) | 0.47444 (16) | 0.0711 (6) | |
H46A | 0.4537 | 0.4390 | 0.4317 | 0.107* | |
H46B | 0.5584 | 0.4002 | 0.4875 | 0.107* | |
H46C | 0.4494 | 0.3528 | 0.5288 | 0.107* | |
C47 | 0.57327 (13) | 0.20790 (14) | 0.50099 (12) | 0.0541 (5) | |
H47A | 0.5373 | 0.1868 | 0.5587 | 0.081* | |
H47B | 0.6450 | 0.2241 | 0.5062 | 0.081* | |
H47C | 0.5758 | 0.1533 | 0.4799 | 0.081* | |
C48 | 0.63457 (15) | 0.42870 (16) | 0.32180 (16) | 0.0736 (7) | |
H48A | 0.6602 | 0.4517 | 0.2605 | 0.110* | |
H48B | 0.6944 | 0.4063 | 0.3612 | 0.110* | |
H48C | 0.5940 | 0.4842 | 0.3312 | 0.110* | |
C49 | 0.62164 (14) | 0.25964 (16) | 0.31660 (13) | 0.0628 (5) | |
H49A | 0.5760 | 0.2039 | 0.3303 | 0.094* | |
H49B | 0.6862 | 0.2351 | 0.3501 | 0.094* | |
H49C | 0.6393 | 0.2871 | 0.2534 | 0.094* | |
C50 | 0.27959 (10) | 0.33402 (9) | 0.29480 (9) | 0.0282 (3) | |
C51 | 0.19536 (10) | 0.28411 (10) | 0.34882 (9) | 0.0280 (3) | |
H51 | 0.2058 | 0.2456 | 0.4097 | 0.034* | |
C52 | 0.09691 (10) | 0.29090 (9) | 0.31343 (8) | 0.0266 (2) | |
C53 | 0.08054 (11) | 0.34785 (10) | 0.22402 (9) | 0.0316 (3) | |
H53 | 0.0137 | 0.3518 | 0.1999 | 0.038* | |
C54 | 0.16252 (11) | 0.39879 (11) | 0.17047 (9) | 0.0342 (3) | |
H54 | 0.1511 | 0.4387 | 0.1099 | 0.041* | |
C55 | 0.26116 (11) | 0.39148 (10) | 0.20524 (9) | 0.0318 (3) | |
H55 | 0.3168 | 0.4258 | 0.1679 | 0.038* | |
N56 | 0.00865 (8) | 0.24059 (8) | 0.36798 (7) | 0.0290 (2) | |
C57 | 0.02199 (11) | 0.12956 (10) | 0.41631 (9) | 0.0338 (3) | |
H57A | −0.0440 | 0.1044 | 0.4489 | 0.041* | |
H57B | 0.0782 | 0.1132 | 0.4597 | 0.041* | |
C58 | 0.05001 (11) | 0.07761 (10) | 0.35348 (9) | 0.0321 (3) | |
C59 | 0.14733 (11) | 0.02270 (10) | 0.35927 (10) | 0.0365 (3) | |
C60 | 0.17181 (13) | −0.02151 (11) | 0.29893 (12) | 0.0466 (4) | |
H60 | 0.2374 | −0.0587 | 0.3031 | 0.056* | |
C61 | 0.10496 (15) | −0.01373 (12) | 0.23331 (12) | 0.0494 (4) | |
C62 | 0.00727 (14) | 0.03778 (12) | 0.23025 (11) | 0.0457 (4) | |
H62 | −0.0409 | 0.0418 | 0.1869 | 0.055* | |
C63 | −0.02180 (11) | 0.08367 (11) | 0.28926 (10) | 0.0370 (3) | |
C64 | 0.22829 (12) | 0.01101 (12) | 0.42726 (12) | 0.0476 (4) | |
H64A | 0.2894 | −0.0307 | 0.4200 | 0.071* | |
H64B | 0.1974 | −0.0212 | 0.4865 | 0.071* | |
H64C | 0.2503 | 0.0774 | 0.4191 | 0.071* | |
C65 | 0.1384 (2) | −0.05698 (18) | 0.16480 (17) | 0.0803 (7) | |
H65A | 0.2110 | −0.0414 | 0.1452 | 0.121* | |
H65B | 0.0921 | −0.0273 | 0.1143 | 0.121* | |
H65C | 0.1336 | −0.1301 | 0.1908 | 0.121* | |
C66 | −0.12841 (12) | 0.14024 (13) | 0.28138 (13) | 0.0487 (4) | |
H66A | −0.1202 | 0.2126 | 0.2512 | 0.073* | |
H66B | −0.1594 | 0.1260 | 0.3403 | 0.073* | |
H66C | −0.1745 | 0.1187 | 0.2475 | 0.073* | |
S41 | −0.06228 (3) | 0.30523 (3) | 0.41700 (2) | 0.03295 (9) | |
O43 | −0.08324 (8) | 0.40487 (8) | 0.35193 (7) | 0.0422 (2) | |
O44 | −0.14806 (8) | 0.24440 (9) | 0.46190 (7) | 0.0428 (3) | |
C67 | 0.01950 (10) | 0.31377 (11) | 0.49663 (9) | 0.0321 (3) | |
C68 | 0.07568 (13) | 0.39891 (12) | 0.47572 (11) | 0.0426 (3) | |
H68 | 0.0648 | 0.4550 | 0.4216 | 0.051* | |
C69 | 0.14836 (14) | 0.40100 (14) | 0.53539 (12) | 0.0493 (4) | |
H69 | 0.1868 | 0.4590 | 0.5213 | 0.059* | |
C70 | 0.16532 (13) | 0.31931 (14) | 0.61510 (11) | 0.0460 (4) | |
C71 | 0.10639 (13) | 0.23641 (13) | 0.63466 (10) | 0.0443 (4) | |
H71 | 0.1160 | 0.1809 | 0.6894 | 0.053* | |
C72 | 0.03362 (11) | 0.23191 (12) | 0.57673 (10) | 0.0374 (3) | |
H72 | −0.0056 | 0.1743 | 0.5915 | 0.045* | |
C73 | 0.24717 (16) | 0.32258 (19) | 0.67715 (13) | 0.0672 (6) | |
H73A | 0.2441 | 0.2629 | 0.7323 | 0.101* | |
H73B | 0.2330 | 0.3832 | 0.6896 | 0.101* | |
H73C | 0.3172 | 0.3237 | 0.6496 | 0.101* |
U11 | U22 | U33 | U12 | U13 | U23 | |
B1 | 0.0276 (7) | 0.0334 (8) | 0.0368 (8) | −0.0103 (6) | 0.0022 (6) | −0.0133 (7) |
O2 | 0.0269 (5) | 0.0436 (6) | 0.0472 (6) | −0.0131 (4) | 0.0051 (4) | −0.0230 (5) |
C3 | 0.0248 (6) | 0.0418 (8) | 0.0420 (8) | −0.0092 (5) | 0.0022 (6) | −0.0170 (7) |
C4 | 0.0228 (6) | 0.0430 (8) | 0.0439 (8) | −0.0066 (5) | 0.0026 (6) | −0.0198 (7) |
O5 | 0.0246 (5) | 0.0463 (6) | 0.0529 (7) | −0.0109 (4) | 0.0049 (4) | −0.0270 (5) |
C6 | 0.0323 (8) | 0.0518 (10) | 0.0666 (12) | −0.0196 (7) | 0.0076 (8) | −0.0223 (9) |
C7 | 0.0435 (9) | 0.0613 (11) | 0.0458 (10) | −0.0052 (8) | −0.0085 (8) | −0.0178 (8) |
C8 | 0.0403 (9) | 0.0649 (11) | 0.0408 (9) | 0.0018 (8) | −0.0011 (7) | −0.0208 (8) |
C9 | 0.0333 (8) | 0.0514 (10) | 0.0657 (11) | −0.0038 (7) | 0.0050 (7) | −0.0302 (9) |
C10 | 0.0275 (6) | 0.0309 (6) | 0.0325 (7) | −0.0100 (5) | 0.0042 (5) | −0.0113 (5) |
C11 | 0.0255 (6) | 0.0254 (6) | 0.0319 (7) | −0.0059 (5) | 0.0038 (5) | −0.0115 (5) |
C12 | 0.0242 (6) | 0.0239 (6) | 0.0278 (6) | −0.0071 (4) | 0.0038 (5) | −0.0076 (5) |
C13 | 0.0305 (7) | 0.0344 (7) | 0.0345 (7) | −0.0065 (5) | 0.0084 (5) | −0.0151 (6) |
C14 | 0.0409 (8) | 0.0361 (7) | 0.0404 (8) | −0.0093 (6) | 0.0075 (6) | −0.0215 (6) |
C15 | 0.0372 (7) | 0.0351 (7) | 0.0391 (8) | −0.0149 (6) | 0.0045 (6) | −0.0173 (6) |
N16 | 0.0248 (5) | 0.0253 (5) | 0.0310 (6) | −0.0081 (4) | 0.0023 (4) | −0.0090 (4) |
C17 | 0.0349 (7) | 0.0257 (6) | 0.0436 (8) | −0.0095 (5) | −0.0017 (6) | −0.0117 (6) |
C18 | 0.0392 (8) | 0.0256 (6) | 0.0437 (8) | −0.0142 (6) | −0.0062 (6) | −0.0035 (6) |
C19 | 0.0516 (10) | 0.0405 (9) | 0.0441 (9) | −0.0243 (7) | 0.0032 (8) | −0.0002 (7) |
C20 | 0.0921 (16) | 0.0628 (13) | 0.0420 (10) | −0.0477 (12) | 0.0092 (10) | −0.0015 (9) |
C21 | 0.0901 (16) | 0.0505 (11) | 0.0564 (12) | −0.0406 (11) | −0.0304 (12) | 0.0135 (9) |
C22 | 0.0651 (12) | 0.0377 (9) | 0.0720 (14) | −0.0196 (8) | −0.0295 (11) | 0.0049 (9) |
C23 | 0.0458 (9) | 0.0241 (7) | 0.0626 (11) | −0.0109 (6) | −0.0139 (8) | −0.0072 (7) |
C24 | 0.0535 (11) | 0.0685 (13) | 0.0593 (12) | −0.0208 (9) | 0.0280 (9) | −0.0105 (10) |
C25 | 0.141 (3) | 0.108 (2) | 0.0565 (14) | −0.0707 (19) | −0.0401 (16) | 0.0215 (14) |
C26 | 0.0422 (9) | 0.0366 (9) | 0.0967 (16) | 0.0047 (7) | −0.0109 (10) | −0.0244 (10) |
S1 | 0.02204 (14) | 0.02987 (16) | 0.03509 (18) | −0.00359 (11) | 0.00137 (12) | −0.01176 (14) |
O3 | 0.0303 (5) | 0.0344 (5) | 0.0451 (6) | 0.0030 (4) | −0.0002 (4) | −0.0162 (5) |
O4 | 0.0244 (5) | 0.0436 (6) | 0.0467 (6) | −0.0106 (4) | 0.0000 (4) | −0.0171 (5) |
C27 | 0.0252 (6) | 0.0293 (6) | 0.0295 (6) | −0.0007 (5) | −0.0011 (5) | −0.0099 (5) |
C28 | 0.0334 (7) | 0.0314 (7) | 0.0360 (7) | −0.0045 (5) | −0.0017 (6) | −0.0134 (6) |
C29 | 0.0423 (8) | 0.0398 (8) | 0.0382 (8) | −0.0006 (6) | 0.0016 (6) | −0.0204 (7) |
C30 | 0.0342 (7) | 0.0448 (8) | 0.0284 (7) | −0.0005 (6) | 0.0024 (6) | −0.0112 (6) |
C31 | 0.0362 (7) | 0.0329 (7) | 0.0347 (7) | −0.0079 (6) | 0.0046 (6) | −0.0065 (6) |
C32 | 0.0339 (7) | 0.0277 (6) | 0.0357 (7) | −0.0040 (5) | 0.0035 (6) | −0.0103 (6) |
C33 | 0.0496 (10) | 0.0645 (11) | 0.0435 (9) | −0.0075 (8) | 0.0162 (8) | −0.0230 (9) |
B41 | 0.0248 (7) | 0.0279 (7) | 0.0349 (8) | −0.0038 (5) | 0.0035 (6) | −0.0078 (6) |
O42 | 0.0260 (5) | 0.0571 (7) | 0.0352 (6) | −0.0101 (5) | 0.0006 (4) | −0.0036 (5) |
C43 | 0.0263 (7) | 0.0458 (8) | 0.0423 (8) | −0.0042 (6) | −0.0021 (6) | −0.0121 (7) |
C44 | 0.0226 (6) | 0.0404 (8) | 0.0427 (8) | −0.0029 (5) | −0.0027 (6) | −0.0013 (7) |
O45 | 0.0226 (4) | 0.0364 (5) | 0.0398 (6) | −0.0056 (4) | −0.0003 (4) | −0.0001 (4) |
C46 | 0.0606 (12) | 0.0895 (16) | 0.0808 (15) | 0.0157 (11) | −0.0209 (11) | −0.0535 (14) |
C47 | 0.0380 (8) | 0.0606 (11) | 0.0454 (10) | −0.0061 (8) | −0.0095 (7) | 0.0006 (8) |
C48 | 0.0385 (9) | 0.0614 (12) | 0.0878 (15) | −0.0237 (9) | −0.0208 (10) | 0.0125 (11) |
C49 | 0.0408 (9) | 0.0811 (14) | 0.0571 (12) | 0.0205 (9) | 0.0017 (8) | −0.0217 (11) |
C50 | 0.0242 (6) | 0.0268 (6) | 0.0313 (7) | −0.0050 (5) | 0.0040 (5) | −0.0090 (5) |
C51 | 0.0253 (6) | 0.0299 (6) | 0.0258 (6) | −0.0038 (5) | 0.0018 (5) | −0.0075 (5) |
C52 | 0.0242 (6) | 0.0287 (6) | 0.0249 (6) | −0.0052 (5) | 0.0050 (5) | −0.0084 (5) |
C53 | 0.0300 (6) | 0.0341 (7) | 0.0284 (7) | −0.0049 (5) | −0.0013 (5) | −0.0093 (6) |
C54 | 0.0380 (7) | 0.0353 (7) | 0.0254 (6) | −0.0086 (6) | 0.0029 (5) | −0.0068 (6) |
C55 | 0.0302 (6) | 0.0309 (7) | 0.0314 (7) | −0.0083 (5) | 0.0078 (5) | −0.0090 (6) |
N56 | 0.0241 (5) | 0.0337 (6) | 0.0276 (5) | −0.0064 (4) | 0.0061 (4) | −0.0102 (5) |
C57 | 0.0303 (7) | 0.0344 (7) | 0.0308 (7) | −0.0077 (5) | 0.0063 (5) | −0.0060 (6) |
C58 | 0.0299 (6) | 0.0285 (6) | 0.0322 (7) | −0.0097 (5) | 0.0078 (5) | −0.0053 (5) |
C59 | 0.0325 (7) | 0.0269 (6) | 0.0413 (8) | −0.0091 (5) | 0.0085 (6) | −0.0037 (6) |
C60 | 0.0404 (8) | 0.0319 (8) | 0.0660 (11) | −0.0101 (6) | 0.0172 (8) | −0.0185 (8) |
C61 | 0.0585 (10) | 0.0390 (8) | 0.0571 (11) | −0.0220 (7) | 0.0221 (8) | −0.0251 (8) |
C62 | 0.0531 (10) | 0.0429 (9) | 0.0449 (9) | −0.0241 (7) | 0.0072 (7) | −0.0185 (7) |
C63 | 0.0342 (7) | 0.0333 (7) | 0.0400 (8) | −0.0128 (6) | 0.0050 (6) | −0.0091 (6) |
C64 | 0.0349 (8) | 0.0417 (9) | 0.0530 (10) | −0.0007 (6) | −0.0008 (7) | −0.0045 (7) |
C65 | 0.0859 (16) | 0.0874 (16) | 0.0994 (18) | −0.0329 (13) | 0.0326 (14) | −0.0696 (15) |
C66 | 0.0352 (8) | 0.0538 (10) | 0.0596 (11) | −0.0070 (7) | −0.0078 (7) | −0.0230 (9) |
S41 | 0.02245 (15) | 0.0435 (2) | 0.03243 (18) | −0.00136 (13) | 0.00290 (13) | −0.01494 (15) |
O43 | 0.0358 (5) | 0.0457 (6) | 0.0412 (6) | 0.0085 (5) | −0.0042 (5) | −0.0144 (5) |
O44 | 0.0243 (5) | 0.0650 (7) | 0.0415 (6) | −0.0112 (5) | 0.0101 (4) | −0.0231 (6) |
C67 | 0.0265 (6) | 0.0402 (7) | 0.0303 (7) | −0.0033 (5) | 0.0040 (5) | −0.0150 (6) |
C68 | 0.0465 (9) | 0.0403 (8) | 0.0398 (8) | −0.0072 (7) | 0.0011 (7) | −0.0140 (7) |
C69 | 0.0515 (10) | 0.0535 (10) | 0.0474 (10) | −0.0196 (8) | 0.0009 (8) | −0.0217 (8) |
C70 | 0.0369 (8) | 0.0700 (11) | 0.0367 (8) | −0.0108 (7) | 0.0041 (6) | −0.0262 (8) |
C71 | 0.0418 (8) | 0.0578 (10) | 0.0288 (7) | −0.0066 (7) | 0.0020 (6) | −0.0118 (7) |
C72 | 0.0339 (7) | 0.0453 (8) | 0.0305 (7) | −0.0070 (6) | 0.0065 (6) | −0.0121 (6) |
C73 | 0.0519 (11) | 0.1100 (17) | 0.0458 (11) | −0.0244 (11) | −0.0028 (9) | −0.0329 (11) |
B1—O2 | 1.3741 (17) | B41—O45 | 1.3692 (17) |
B1—O5 | 1.3750 (18) | B41—O42 | 1.3713 (19) |
B1—C10 | 1.562 (2) | B41—C50 | 1.558 (2) |
O2—C3 | 1.4699 (17) | O42—C43 | 1.4667 (17) |
C3—C7 | 1.520 (2) | C43—C47 | 1.519 (2) |
C3—C6 | 1.522 (2) | C43—C46 | 1.525 (2) |
C3—C4 | 1.567 (2) | C43—C44 | 1.563 (2) |
C4—O5 | 1.4687 (16) | C44—O45 | 1.4721 (17) |
C4—C9 | 1.523 (2) | C44—C49 | 1.523 (2) |
C4—C8 | 1.531 (2) | C44—C48 | 1.523 (2) |
C6—H6A | 0.9800 | C46—H46A | 0.9800 |
C6—H6B | 0.9800 | C46—H46B | 0.9800 |
C6—H6C | 0.9800 | C46—H46C | 0.9800 |
C7—H7A | 0.9800 | C47—H47A | 0.9800 |
C7—H7B | 0.9800 | C47—H47B | 0.9800 |
C7—H7C | 0.9800 | C47—H47C | 0.9800 |
C8—H8A | 0.9800 | C48—H48A | 0.9800 |
C8—H8B | 0.9800 | C48—H48B | 0.9800 |
C8—H8C | 0.9800 | C48—H48C | 0.9800 |
C9—H9A | 0.9800 | C49—H49A | 0.9800 |
C9—H9B | 0.9800 | C49—H49B | 0.9800 |
C9—H9C | 0.9800 | C49—H49C | 0.9800 |
C10—C15 | 1.4064 (19) | C50—C55 | 1.4051 (19) |
C10—C11 | 1.4071 (17) | C50—C51 | 1.4114 (17) |
C11—C12 | 1.3905 (17) | C51—C52 | 1.3959 (17) |
C11—H11 | 0.9500 | C51—H51 | 0.9500 |
C12—C13 | 1.3929 (17) | C52—C53 | 1.3974 (18) |
C12—N16 | 1.4571 (15) | C52—N56 | 1.4565 (16) |
C13—C14 | 1.3963 (19) | C53—C54 | 1.3913 (19) |
C13—H13 | 0.9500 | C53—H53 | 0.9500 |
C14—C15 | 1.387 (2) | C54—C55 | 1.3924 (19) |
C14—H14 | 0.9500 | C54—H54 | 0.9500 |
C15—H15 | 0.9500 | C55—H55 | 0.9500 |
N16—C17 | 1.4899 (17) | N56—C57 | 1.4884 (18) |
N16—S1 | 1.6555 (11) | N56—S41 | 1.6537 (11) |
C17—C18 | 1.508 (2) | C57—C58 | 1.5172 (19) |
C17—H17A | 0.9900 | C57—H57A | 0.9900 |
C17—H17B | 0.9900 | C57—H57B | 0.9900 |
C18—C19 | 1.406 (3) | C58—C59 | 1.408 (2) |
C18—C23 | 1.418 (2) | C58—C63 | 1.412 (2) |
C19—C20 | 1.412 (3) | C59—C60 | 1.392 (2) |
C19—C24 | 1.514 (3) | C59—C64 | 1.519 (2) |
C20—C21 | 1.393 (3) | C60—C61 | 1.380 (3) |
C20—H20 | 0.9500 | C60—H60 | 0.9500 |
C21—C22 | 1.372 (3) | C61—C62 | 1.395 (3) |
C21—C25 | 1.534 (3) | C61—C65 | 1.522 (2) |
C22—C23 | 1.392 (3) | C62—C63 | 1.400 (2) |
C22—H22 | 0.9500 | C62—H62 | 0.9500 |
C23—C26 | 1.512 (3) | C63—C66 | 1.517 (2) |
C24—H24A | 0.9800 | C64—H64A | 0.9800 |
C24—H24B | 0.9800 | C64—H64B | 0.9800 |
C24—H24C | 0.9800 | C64—H64C | 0.9800 |
C25—H25A | 0.9800 | C65—H65A | 0.9800 |
C25—H25B | 0.9800 | C65—H65B | 0.9800 |
C25—H25C | 0.9800 | C65—H65C | 0.9800 |
C26—H26A | 0.9800 | C66—H66A | 0.9800 |
C26—H26B | 0.9800 | C66—H66B | 0.9800 |
C26—H26C | 0.9800 | C66—H66C | 0.9800 |
S1—O3 | 1.4328 (10) | S41—O43 | 1.4354 (11) |
S1—O4 | 1.4402 (10) | S41—O44 | 1.4430 (11) |
S1—C27 | 1.7629 (14) | S41—C67 | 1.7701 (14) |
C27—C28 | 1.3921 (18) | C67—C68 | 1.392 (2) |
C27—C32 | 1.4012 (19) | C67—C72 | 1.395 (2) |
C28—C29 | 1.394 (2) | C68—C69 | 1.400 (2) |
C28—H28 | 0.9500 | C68—H68 | 0.9500 |
C29—C30 | 1.400 (2) | C69—C70 | 1.395 (2) |
C29—H29 | 0.9500 | C69—H69 | 0.9500 |
C30—C31 | 1.392 (2) | C70—C71 | 1.389 (2) |
C30—C33 | 1.518 (2) | C70—C73 | 1.519 (2) |
C31—C32 | 1.394 (2) | C71—C72 | 1.392 (2) |
C31—H31 | 0.9500 | C71—H71 | 0.9500 |
C32—H32 | 0.9500 | C72—H72 | 0.9500 |
C33—H33A | 0.9800 | C73—H73A | 0.9800 |
C33—H33B | 0.9800 | C73—H73B | 0.9800 |
C33—H33C | 0.9800 | C73—H73C | 0.9800 |
O2—B1—O5 | 113.71 (12) | O45—B41—O42 | 113.71 (12) |
O2—B1—C10 | 123.08 (13) | O45—B41—C50 | 122.82 (13) |
O5—B1—C10 | 123.18 (12) | O42—B41—C50 | 123.46 (12) |
B1—O2—C3 | 106.96 (11) | B41—O42—C43 | 106.90 (11) |
O2—C3—C7 | 107.12 (12) | O42—C43—C47 | 108.78 (13) |
O2—C3—C6 | 108.43 (12) | O42—C43—C46 | 106.48 (13) |
C7—C3—C6 | 110.65 (13) | C47—C43—C46 | 110.75 (15) |
O2—C3—C4 | 102.03 (10) | O42—C43—C44 | 102.37 (12) |
C7—C3—C4 | 112.94 (13) | C47—C43—C44 | 114.24 (14) |
C6—C3—C4 | 114.94 (13) | C46—C43—C44 | 113.49 (15) |
O5—C4—C9 | 109.23 (12) | O45—C44—C49 | 106.22 (13) |
O5—C4—C8 | 106.23 (12) | O45—C44—C48 | 108.92 (12) |
C9—C4—C8 | 110.70 (13) | C49—C44—C48 | 110.53 (16) |
O5—C4—C3 | 102.38 (11) | O45—C44—C43 | 102.31 (11) |
C9—C4—C3 | 113.79 (12) | C49—C44—C43 | 112.99 (14) |
C8—C4—C3 | 113.82 (12) | C48—C44—C43 | 115.09 (16) |
B1—O5—C4 | 106.24 (10) | B41—O45—C44 | 106.82 (11) |
C3—C6—H6A | 109.5 | C43—C46—H46A | 109.5 |
C3—C6—H6B | 109.5 | C43—C46—H46B | 109.5 |
H6A—C6—H6B | 109.5 | H46A—C46—H46B | 109.5 |
C3—C6—H6C | 109.5 | C43—C46—H46C | 109.5 |
H6A—C6—H6C | 109.5 | H46A—C46—H46C | 109.5 |
H6B—C6—H6C | 109.5 | H46B—C46—H46C | 109.5 |
C3—C7—H7A | 109.5 | C43—C47—H47A | 109.5 |
C3—C7—H7B | 109.5 | C43—C47—H47B | 109.5 |
H7A—C7—H7B | 109.5 | H47A—C47—H47B | 109.5 |
C3—C7—H7C | 109.5 | C43—C47—H47C | 109.5 |
H7A—C7—H7C | 109.5 | H47A—C47—H47C | 109.5 |
H7B—C7—H7C | 109.5 | H47B—C47—H47C | 109.5 |
C4—C8—H8A | 109.5 | C44—C48—H48A | 109.5 |
C4—C8—H8B | 109.5 | C44—C48—H48B | 109.5 |
H8A—C8—H8B | 109.5 | H48A—C48—H48B | 109.5 |
C4—C8—H8C | 109.5 | C44—C48—H48C | 109.5 |
H8A—C8—H8C | 109.5 | H48A—C48—H48C | 109.5 |
H8B—C8—H8C | 109.5 | H48B—C48—H48C | 109.5 |
C4—C9—H9A | 109.5 | C44—C49—H49A | 109.5 |
C4—C9—H9B | 109.5 | C44—C49—H49B | 109.5 |
H9A—C9—H9B | 109.5 | H49A—C49—H49B | 109.5 |
C4—C9—H9C | 109.5 | C44—C49—H49C | 109.5 |
H9A—C9—H9C | 109.5 | H49A—C49—H49C | 109.5 |
H9B—C9—H9C | 109.5 | H49B—C49—H49C | 109.5 |
C15—C10—C11 | 117.97 (12) | C55—C50—C51 | 118.28 (12) |
C15—C10—B1 | 122.08 (12) | C55—C50—B41 | 121.08 (12) |
C11—C10—B1 | 119.89 (12) | C51—C50—B41 | 120.62 (12) |
C12—C11—C10 | 120.81 (12) | C52—C51—C50 | 120.52 (12) |
C12—C11—H11 | 119.6 | C52—C51—H51 | 119.7 |
C10—C11—H11 | 119.6 | C50—C51—H51 | 119.7 |
C11—C12—C13 | 120.35 (11) | C51—C52—C53 | 120.24 (12) |
C11—C12—N16 | 120.66 (11) | C51—C52—N56 | 121.50 (11) |
C13—C12—N16 | 118.99 (11) | C53—C52—N56 | 118.25 (11) |
C12—C13—C14 | 119.56 (12) | C54—C53—C52 | 119.73 (12) |
C12—C13—H13 | 120.2 | C54—C53—H53 | 120.1 |
C14—C13—H13 | 120.2 | C52—C53—H53 | 120.1 |
C15—C14—C13 | 120.12 (13) | C53—C54—C55 | 120.26 (13) |
C15—C14—H14 | 119.9 | C53—C54—H54 | 119.9 |
C13—C14—H14 | 119.9 | C55—C54—H54 | 119.9 |
C14—C15—C10 | 121.17 (12) | C54—C55—C50 | 120.95 (12) |
C14—C15—H15 | 119.4 | C54—C55—H55 | 119.5 |
C10—C15—H15 | 119.4 | C50—C55—H55 | 119.5 |
C12—N16—C17 | 116.85 (10) | C52—N56—C57 | 117.37 (10) |
C12—N16—S1 | 115.83 (8) | C52—N56—S41 | 115.69 (8) |
C17—N16—S1 | 117.06 (9) | C57—N56—S41 | 117.44 (9) |
N16—C17—C18 | 110.92 (11) | N56—C57—C58 | 111.09 (11) |
N16—C17—H17A | 109.5 | N56—C57—H57A | 109.4 |
C18—C17—H17A | 109.5 | C58—C57—H57A | 109.4 |
N16—C17—H17B | 109.5 | N56—C57—H57B | 109.4 |
C18—C17—H17B | 109.5 | C58—C57—H57B | 109.4 |
H17A—C17—H17B | 108.0 | H57A—C57—H57B | 108.0 |
C19—C18—C23 | 120.05 (15) | C59—C58—C63 | 119.74 (13) |
C19—C18—C17 | 119.53 (14) | C59—C58—C57 | 120.22 (13) |
C23—C18—C17 | 120.43 (15) | C63—C58—C57 | 120.04 (12) |
C18—C19—C20 | 118.67 (18) | C60—C59—C58 | 118.72 (15) |
C18—C19—C24 | 121.54 (16) | C60—C59—C64 | 118.14 (14) |
C20—C19—C24 | 119.79 (19) | C58—C59—C64 | 123.13 (14) |
C21—C20—C19 | 121.5 (2) | C61—C60—C59 | 122.90 (15) |
C21—C20—H20 | 119.3 | C61—C60—H60 | 118.6 |
C19—C20—H20 | 119.3 | C59—C60—H60 | 118.6 |
C22—C21—C20 | 118.43 (19) | C60—C61—C62 | 117.80 (15) |
C22—C21—C25 | 122.4 (2) | C60—C61—C65 | 120.96 (18) |
C20—C21—C25 | 119.2 (3) | C62—C61—C65 | 121.20 (19) |
C21—C22—C23 | 122.95 (19) | C61—C62—C63 | 121.83 (16) |
C21—C22—H22 | 118.5 | C61—C62—H62 | 119.1 |
C23—C22—H22 | 118.5 | C63—C62—H62 | 119.1 |
C22—C23—C18 | 118.41 (19) | C62—C63—C58 | 118.93 (14) |
C22—C23—C26 | 117.46 (17) | C62—C63—C66 | 119.26 (14) |
C18—C23—C26 | 124.13 (16) | C58—C63—C66 | 121.79 (14) |
C19—C24—H24A | 109.5 | C59—C64—H64A | 109.5 |
C19—C24—H24B | 109.5 | C59—C64—H64B | 109.5 |
H24A—C24—H24B | 109.5 | H64A—C64—H64B | 109.5 |
C19—C24—H24C | 109.5 | C59—C64—H64C | 109.5 |
H24A—C24—H24C | 109.5 | H64A—C64—H64C | 109.5 |
H24B—C24—H24C | 109.5 | H64B—C64—H64C | 109.5 |
C21—C25—H25A | 109.5 | C61—C65—H65A | 109.5 |
C21—C25—H25B | 109.5 | C61—C65—H65B | 109.5 |
H25A—C25—H25B | 109.5 | H65A—C65—H65B | 109.5 |
C21—C25—H25C | 109.5 | C61—C65—H65C | 109.5 |
H25A—C25—H25C | 109.5 | H65A—C65—H65C | 109.5 |
H25B—C25—H25C | 109.5 | H65B—C65—H65C | 109.5 |
C23—C26—H26A | 109.5 | C63—C66—H66A | 109.5 |
C23—C26—H26B | 109.5 | C63—C66—H66B | 109.5 |
H26A—C26—H26B | 109.5 | H66A—C66—H66B | 109.5 |
C23—C26—H26C | 109.5 | C63—C66—H66C | 109.5 |
H26A—C26—H26C | 109.5 | H66A—C66—H66C | 109.5 |
H26B—C26—H26C | 109.5 | H66B—C66—H66C | 109.5 |
O3—S1—O4 | 119.97 (6) | O43—S41—O44 | 120.07 (7) |
O3—S1—N16 | 107.03 (6) | O43—S41—N56 | 107.25 (6) |
O4—S1—N16 | 106.59 (6) | O44—S41—N56 | 106.04 (6) |
O3—S1—C27 | 108.37 (6) | O43—S41—C67 | 107.92 (7) |
O4—S1—C27 | 108.63 (6) | O44—S41—C67 | 108.72 (7) |
N16—S1—C27 | 105.32 (6) | N56—S41—C67 | 106.01 (6) |
C28—C27—C32 | 120.73 (13) | C68—C67—C72 | 120.67 (13) |
C28—C27—S1 | 120.36 (11) | C68—C67—S41 | 119.46 (11) |
C32—C27—S1 | 118.59 (10) | C72—C67—S41 | 119.66 (11) |
C27—C28—C29 | 119.14 (13) | C67—C68—C69 | 119.24 (15) |
C27—C28—H28 | 120.4 | C67—C68—H68 | 120.4 |
C29—C28—H28 | 120.4 | C69—C68—H68 | 120.4 |
C28—C29—C30 | 121.16 (13) | C70—C69—C68 | 121.12 (15) |
C28—C29—H29 | 119.4 | C70—C69—H69 | 119.4 |
C30—C29—H29 | 119.4 | C68—C69—H69 | 119.4 |
C31—C30—C29 | 118.66 (13) | C71—C70—C69 | 118.12 (15) |
C31—C30—C33 | 120.52 (15) | C71—C70—C73 | 122.02 (17) |
C29—C30—C33 | 120.83 (14) | C69—C70—C73 | 119.85 (17) |
C30—C31—C32 | 121.26 (14) | C70—C71—C72 | 122.16 (15) |
C30—C31—H31 | 119.4 | C70—C71—H71 | 118.9 |
C32—C31—H31 | 119.4 | C72—C71—H71 | 118.9 |
C31—C32—C27 | 119.04 (13) | C71—C72—C67 | 118.66 (14) |
C31—C32—H32 | 120.5 | C71—C72—H72 | 120.7 |
C27—C32—H32 | 120.5 | C67—C72—H72 | 120.7 |
C30—C33—H33A | 109.5 | C70—C73—H73A | 109.5 |
C30—C33—H33B | 109.5 | C70—C73—H73B | 109.5 |
H33A—C33—H33B | 109.5 | H73A—C73—H73B | 109.5 |
C30—C33—H33C | 109.5 | C70—C73—H73C | 109.5 |
H33A—C33—H33C | 109.5 | H73A—C73—H73C | 109.5 |
H33B—C33—H33C | 109.5 | H73B—C73—H73C | 109.5 |