+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 16:41:52 on 17-Apr-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SOT039 in P-1 CELL 0.71069 8.6080 15.2120 15.2570 67.786 84.475 73.886 ZERR 2.00 0.0050 0.0050 0.0050 0.005 0.005 0.005 LATT 1 SFAC C H N O S UNIT 68 62 14 24 4 V = 1776.79 F(000) = 824.0 Mu = 0.23 mm-1 Cell Wt = 1587.56 Rho = 1.484 SHEL 7 0.84 EQIV $1 X, Y, Z-1 HTAB N4 O12_$1 HTAB N5 O12_$1 FMAP 2 PLAN 25 HTAB ACTA TEMP -153 SIZE 0.15 0.1 0.02 L.S. 4 WGHT 0.048000 EXTI 0.002525 FVAR 0.12244 C1 1 0.186915 0.492621 0.135089 11.00000 0.02088 0.01906 = 0.02750 -0.00732 -0.00057 -0.00549 AFIX 43 H1 2 0.217907 0.456729 0.199646 11.00000 -1.20000 AFIX 0 C2 1 0.049882 0.569798 0.110514 11.00000 0.02024 0.02102 = 0.02732 -0.01300 0.00651 -0.00661 C3 1 -0.002423 0.625010 0.018391 11.00000 0.01896 0.01672 = 0.03680 -0.01218 -0.00255 -0.00183 AFIX 43 H3 2 -0.097159 0.678246 0.002910 11.00000 -1.20000 AFIX 0 C4 1 0.093439 0.597102 -0.049977 11.00000 0.01826 0.02044 = 0.02650 -0.00670 -0.00188 -0.00524 C5 1 0.231340 0.520440 -0.030789 11.00000 0.02022 0.02164 = 0.02631 -0.01020 0.00046 -0.00779 AFIX 43 H5 2 0.291746 0.503827 -0.080377 11.00000 -1.20000 AFIX 0 C6 1 0.279656 0.468044 0.063218 11.00000 0.01819 0.01589 = 0.02896 -0.00566 0.00263 -0.00242 C7 1 0.519836 0.345066 0.036862 11.00000 0.02034 0.02110 = 0.02334 -0.01119 0.00254 -0.00550 C8 1 0.645419 0.256211 0.090162 11.00000 0.02162 0.01896 = 0.01820 -0.00726 -0.00088 -0.00209 C9 1 0.679295 0.202379 0.185158 11.00000 0.01593 0.02319 = 0.02649 -0.01185 0.00066 -0.00611 C10 1 0.827885 0.131384 0.190464 11.00000 0.02044 0.02123 = 0.01895 -0.00829 -0.00136 -0.00442 C11 1 0.878814 0.143799 0.097841 11.00000 0.01880 0.02113 = 0.02100 -0.00788 0.00180 -0.00825 C12 1 1.022297 0.084429 0.066531 11.00000 0.01876 0.02540 = 0.01936 -0.00905 -0.00083 -0.00618 C13 1 1.184620 0.076095 -0.074223 11.00000 0.01968 0.02297 = 0.02186 -0.00955 0.00279 -0.00326 C14 1 1.203719 0.130868 -0.168905 11.00000 0.02063 0.02484 = 0.02480 -0.00925 -0.00077 -0.00452 AFIX 43 H14 2 1.125249 0.190295 -0.200879 11.00000 -1.20000 AFIX 0 C15 1 1.338364 0.097577 -0.215680 11.00000 0.02306 0.02484 = 0.02126 -0.00845 0.00172 -0.00794 C16 1 1.457487 0.012121 -0.173404 11.00000 0.01850 0.02686 = 0.02613 -0.01470 0.00214 -0.00580 AFIX 43 H16 2 1.550886 -0.008797 -0.206415 11.00000 -1.20000 AFIX 0 C17 1 1.431491 -0.040114 -0.080871 11.00000 0.01741 0.02110 = 0.02771 -0.01233 -0.00062 -0.00253 C18 1 1.299233 -0.011896 -0.029839 11.00000 0.02074 0.02213 = 0.02299 -0.01100 0.00082 -0.00517 AFIX 43 H18 2 1.286597 -0.051657 0.034245 11.00000 -1.20000 AFIX 0 C19 1 0.576280 0.214746 0.266017 11.00000 0.02366 0.02138 = 0.01878 -0.00653 0.00396 -0.00202 C20 1 0.631992 0.240621 0.333052 11.00000 0.01918 0.03710 = 0.02393 -0.01217 0.00355 -0.00739 AFIX 43 H20 2 0.738716 0.248156 0.328712 11.00000 -1.20000 AFIX 0 C21 1 0.533276 0.255463 0.405953 11.00000 0.03798 0.03774 = 0.02697 -0.01810 -0.00196 -0.00667 AFIX 43 H21 2 0.571897 0.273478 0.451299 11.00000 -1.20000 AFIX 0 C22 1 0.378198 0.244021 0.412694 11.00000 0.03220 0.03996 = 0.02591 -0.01522 0.00690 -0.00516 AFIX 43 H22 2 0.310265 0.254250 0.462738 11.00000 -1.20000 AFIX 0 C23 1 0.322172 0.217980 0.347445 11.00000 0.02268 0.04154 = 0.02752 -0.01560 0.00485 -0.00864 AFIX 43 H23 2 0.215370 0.210507 0.352099 11.00000 -1.20000 AFIX 0 C24 1 0.421182 0.202569 0.274774 11.00000 0.02538 0.02832 = 0.02200 -0.01138 0.00031 -0.00593 AFIX 43 H24 2 0.382349 0.183415 0.230371 11.00000 -1.20000 AFIX 0 C25 1 0.911245 0.056872 0.279699 11.00000 0.02241 0.02441 = 0.01903 -0.01148 -0.00007 -0.00043 C26 1 1.070387 0.048281 0.298816 11.00000 0.02075 0.02611 = 0.02491 -0.01058 0.00151 -0.00119 AFIX 43 H26 2 1.128741 0.089804 0.253979 11.00000 -1.20000 AFIX 0 C27 1 1.144630 -0.020468 0.382872 11.00000 0.03049 0.03232 = 0.03004 -0.01324 -0.00853 0.00179 AFIX 43 H27 2 1.253576 -0.026043 0.395554 11.00000 -1.20000 AFIX 0 C28 1 1.059896 -0.080984 0.448307 11.00000 0.04449 0.02835 = 0.03040 -0.00855 -0.01227 0.00626 AFIX 43 H28 2 1.111650 -0.128780 0.505431 11.00000 -1.20000 AFIX 0 C29 1 0.900681 -0.072487 0.431272 11.00000 0.05114 0.02630 = 0.02526 -0.00233 -0.00184 -0.01439 AFIX 43 H29 2 0.842636 -0.114087 0.476278 11.00000 -1.20000 AFIX 0 C30 1 0.826616 -0.002326 0.347485 11.00000 0.02824 0.02852 = 0.02747 -0.01095 -0.00136 -0.00698 AFIX 43 H30 2 0.716086 0.005295 0.336356 11.00000 -1.20000 AFIX 0 C31 1 0.766267 0.525901 0.485285 11.00000 0.03311 0.03458 = 0.05494 -0.01438 0.00055 -0.01064 AFIX 137 H31A 2 0.664904 0.572814 0.490444 11.00000 -1.50000 H31B 2 0.834467 0.560743 0.437141 11.00000 -1.50000 H31C 2 0.823161 0.494366 0.546469 11.00000 -1.50000 AFIX 0 C32 1 0.924326 0.359708 0.458417 11.00000 0.03522 0.03606 = 0.05379 -0.01468 0.00934 -0.00205 AFIX 137 H32A 2 0.967140 0.335685 0.522897 11.00000 -1.50000 H32B 2 0.992537 0.398205 0.414059 11.00000 -1.50000 H32C 2 0.923933 0.303648 0.441594 11.00000 -1.50000 AFIX 0 C33 1 0.728970 0.204404 0.735073 11.00000 0.09866 0.03692 = 0.04620 -0.00918 -0.02496 -0.02369 AFIX 137 H33A 2 0.831011 0.154157 0.739416 11.00000 -1.50000 H33B 2 0.675983 0.223193 0.674214 11.00000 -1.50000 H33C 2 0.658059 0.177952 0.786777 11.00000 -1.50000 AFIX 0 C34 1 0.567925 0.376078 0.745050 11.00000 0.04138 0.09753 = 0.04424 -0.03547 -0.02014 0.03112 AFIX 137 H34A 2 0.508351 0.335510 0.794378 11.00000 -1.50000 H34B 2 0.516881 0.396321 0.683312 11.00000 -1.50000 H34C 2 0.566433 0.434558 0.758229 11.00000 -1.50000 AFIX 0 N1 3 -0.046873 0.592669 0.187946 11.00000 0.02589 0.02668 = 0.03568 -0.01487 0.00337 -0.00262 N2 3 0.041328 0.650584 -0.148892 11.00000 0.02117 0.02510 = 0.03224 -0.00830 -0.00333 -0.00685 N3 3 0.415310 0.387263 0.092006 11.00000 0.02482 0.02525 = 0.02006 -0.00823 -0.00215 0.00222 AFIX 43 H3A 2 0.435906 0.360254 0.153245 11.00000 -1.20000 AFIX 0 N4 3 0.765449 0.220674 0.037850 11.00000 0.02006 0.01959 = 0.01753 -0.00680 -0.00023 -0.00341 AFIX 43 H4 2 0.769706 0.243315 -0.024378 11.00000 -1.20000 AFIX 0 N5 3 1.049330 0.115217 -0.029082 11.00000 0.01779 0.02374 = 0.02341 -0.00754 -0.00036 0.00282 AFIX 43 H5A 2 0.974188 0.164410 -0.065616 11.00000 -1.20000 AFIX 0 N6 3 1.355064 0.158518 -0.315632 11.00000 0.03023 0.03377 = 0.02599 -0.01497 0.00439 -0.00738 N7 3 1.552493 -0.132738 -0.030884 11.00000 0.01975 0.02383 = 0.03161 -0.01404 -0.00119 -0.00294 O1 4 0.005157 0.547527 0.269042 11.00000 0.03870 0.03095 = 0.02690 -0.00923 0.00528 -0.00394 O2 4 -0.175499 0.656428 0.166179 11.00000 0.02359 0.04262 = 0.04738 -0.02221 0.00255 0.00446 O3 4 -0.078591 0.720790 -0.167143 11.00000 0.03533 0.03092 = 0.03723 -0.00569 -0.00930 0.00335 O4 4 0.119002 0.621523 -0.209530 11.00000 0.03587 0.03601 = 0.02517 -0.00719 0.00088 0.00009 O5 4 0.514748 0.379332 -0.049231 11.00000 0.02878 0.02820 = 0.02284 -0.00788 0.00149 -0.00149 O6 4 1.110241 0.011226 0.123245 11.00000 0.02766 0.02627 = 0.02263 -0.00439 -0.00013 0.00792 O7 4 1.249498 0.233934 -0.352333 11.00000 0.04930 0.03298 = 0.02459 -0.00177 0.00462 0.00490 O8 4 1.474384 0.129014 -0.358020 11.00000 0.03520 0.05367 = 0.02891 -0.01114 0.00876 -0.00423 O9 4 1.666331 -0.162049 -0.076740 11.00000 0.02214 0.03857 = 0.03863 -0.02174 -0.00035 0.00515 O10 4 1.534487 -0.174776 0.053887 11.00000 0.03089 0.02746 = 0.02931 -0.00743 -0.00210 -0.00033 O11 4 0.635573 0.378049 0.533939 11.00000 0.03341 0.03595 = 0.03322 -0.00652 0.00074 -0.01526 O12 4 0.833139 0.274996 0.843365 11.00000 0.02344 0.03331 = 0.02062 -0.01050 -0.00320 0.00099 S1 5 0.723421 0.435227 0.452424 11.00000 0.03179 0.03357 = 0.03040 -0.00552 -0.00416 -0.00724 S2 5 0.768053 0.307967 0.743675 11.00000 0.02744 0.02734 = 0.02322 -0.00764 -0.00231 -0.00336 HKLF 4 Covalent radii and connectivity table for 02SOT039 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - C2 C6 C2 - C1 C3 N1 C3 - C2 C4 C4 - C5 C3 N2 C5 - C4 C6 C6 - C5 C1 N3 C7 - O5 N3 C8 C8 - N4 C9 C7 C9 - C8 C10 C19 C10 - C11 C9 C25 C11 - N4 C10 C12 C12 - O6 N5 C11 C13 - C14 C18 N5 C14 - C15 C13 C15 - C14 C16 N6 C16 - C17 C15 C17 - C16 C18 N7 C18 - C17 C13 C19 - C24 C20 C9 C20 - C21 C19 C21 - C20 C22 C22 - C23 C21 C23 - C22 C24 C24 - C23 C19 C25 - C30 C26 C10 C26 - C27 C25 C27 - C28 C26 C28 - C29 C27 C29 - C28 C30 C30 - C25 C29 C31 - S1 C32 - S1 C33 - S2 C34 - S2 N1 - O1 O2 C2 N2 - O3 O4 C4 N3 - C7 C6 N4 - C8 C11 N5 - C12 C13 N6 - O7 O8 C15 N7 - O10 O9 C17 O1 - N1 O2 - N1 O3 - N2 O4 - N2 O5 - C7 O6 - C12 O7 - N6 O8 - N6 O9 - N7 O10 - N7 O11 - S1 O12 - S2 S1 - O11 C31 C32 S2 - O12 C34 C33 Operators for generating equivalent atoms: $1 x, y, z-1 22373 Reflections read, of which 2874 rejected -10 =< h =< 10, -18 =< k =< 18, -18 =< l =< 18, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -1 1 0 42.40 1.70 2 12.69 -2 3 2 42.34 0.87 3 12.39 -8 -1 4 37.95 0.92 5 7.86 -5 3 5 32.93 0.92 3 12.79 4 Inconsistent equivalents 6028 Unique reflections, of which 0 suppressed R(int) = 0.1126 R(sigma) = 0.1403 Friedel opposites merged Maximum memory for data reduction = 3955 / 61971 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 5302 / 662792 wR2 = 0.1242 before cycle 1 for 6028 data and 501 / 501 parameters GooF = S = 0.909; Restrained GooF = 0.909 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12244 0.00023 0.002 OSF 2 0.00253 0.00059 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.007 for U23 S2 Max. shift = 0.000 A for H34B Max. dU = 0.000 for O3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5302 / 662792 wR2 = 0.1242 before cycle 2 for 6028 data and 501 / 501 parameters GooF = S = 0.909; Restrained GooF = 0.909 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12244 0.00023 -0.003 OSF 2 0.00252 0.00059 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for OSF Max. shift = 0.000 A for H34B Max. dU = 0.000 for O3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5302 / 662792 wR2 = 0.1242 before cycle 3 for 6028 data and 501 / 501 parameters GooF = S = 0.909; Restrained GooF = 0.909 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12244 0.00023 0.002 OSF 2 0.00253 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for OSF Max. shift = 0.000 A for H31A Max. dU = 0.000 for C31 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5302 / 662792 wR2 = 0.1242 before cycle 4 for 6028 data and 501 / 501 parameters GooF = S = 0.909; Restrained GooF = 0.909 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12244 0.00023 0.000 OSF 2 0.00253 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U33 S2 Max. shift = 0.000 A for N6 Max. dU = 0.000 for O9 Largest correlation matrix elements -0.562 U23 N7 / U33 N7 -0.524 U23 C2 / U33 C2 -0.511 U23 O9 / U33 O9 -0.542 U23 N1 / U33 N1 -0.522 U23 C9 / U33 C9 -0.506 U23 C25 / U33 C25 -0.535 U23 C16 / U33 C16 -0.521 U23 C7 / U33 C7 -0.504 U23 C12 / U33 C12 -0.535 U23 C34 / U33 C34 -0.521 U23 C5 / U33 C5 -0.503 U23 C3 / U33 C3 -0.533 U23 C34 / U22 C34 -0.518 U23 C13 / U33 C13 -0.502 U23 C26 / U33 C26 -0.532 U23 O9 / U22 O9 -0.514 U23 C27 / U33 C27 -0.501 U23 C8 / U33 C8 -0.530 U23 C17 / U33 C17 -0.513 U23 C21 / U33 C21 -0.529 U23 N6 / U22 N6 -0.513 U23 C21 / U22 C21 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.2179 0.4567 0.1996 43 0.950 0.000 C1 C2 C6 H3 -0.0972 0.6782 0.0029 43 0.950 0.000 C3 C2 C4 H5 0.2917 0.5038 -0.0804 43 0.950 0.000 C5 C4 C6 H14 1.1252 0.1903 -0.2009 43 0.950 0.000 C14 C15 C13 H16 1.5509 -0.0088 -0.2064 43 0.950 0.000 C16 C17 C15 H18 1.2866 -0.0517 0.0342 43 0.950 0.000 C18 C17 C13 H20 0.7387 0.2482 0.3287 43 0.950 0.000 C20 C21 C19 H21 0.5719 0.2735 0.4513 43 0.950 0.000 C21 C20 C22 H22 0.3103 0.2542 0.4627 43 0.950 0.000 C22 C23 C21 H23 0.2154 0.2105 0.3521 43 0.950 0.000 C23 C22 C24 H24 0.3823 0.1834 0.2304 43 0.950 0.000 C24 C23 C19 H26 1.1287 0.0898 0.2540 43 0.950 0.000 C26 C27 C25 H27 1.2536 -0.0260 0.3956 43 0.950 0.000 C27 C28 C26 H28 1.1117 -0.1288 0.5054 43 0.950 0.000 C28 C29 C27 H29 0.8426 -0.1141 0.4763 43 0.950 0.000 C29 C28 C30 H30 0.7161 0.0053 0.3364 43 0.950 0.000 C30 C25 C29 H31A 0.6649 0.5728 0.4904 137 0.980 0.000 C31 S1 H31A H31B 0.8345 0.5607 0.4371 137 0.980 0.000 C31 S1 H31A H31C 0.8232 0.4944 0.5465 137 0.980 0.000 C31 S1 H31A H32A 0.9671 0.3357 0.5229 137 0.980 0.000 C32 S1 H32A H32B 0.9925 0.3982 0.4141 137 0.980 0.000 C32 S1 H32A H32C 0.9239 0.3036 0.4416 137 0.980 0.000 C32 S1 H32A H33A 0.8310 0.1542 0.7394 137 0.980 0.000 C33 S2 H33A H33B 0.6760 0.2232 0.6742 137 0.980 0.000 C33 S2 H33A H33C 0.6581 0.1780 0.7868 137 0.980 0.000 C33 S2 H33A H34A 0.5084 0.3355 0.7944 137 0.980 0.000 C34 S2 H34A H34B 0.5169 0.3963 0.6833 137 0.980 0.000 C34 S2 H34A H34C 0.5664 0.4346 0.7582 137 0.980 0.000 C34 S2 H34A H3A 0.4359 0.3603 0.1532 43 0.880 0.000 N3 C7 C6 H4 0.7697 0.2433 -0.0244 43 0.880 0.000 N4 C8 C11 H5A 0.9742 0.1644 -0.0656 43 0.880 0.000 N5 C12 C13 02SOT039 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.18691 0.49262 0.13509 1.00000 0.02088 0.01906 0.02750 -0.00732 -0.00057 -0.00549 0.02274 0.00528 0.00045 0.00028 0.00028 0.00000 0.00222 0.00217 0.00234 0.00182 0.00163 0.00182 0.00090 H1 0.21791 0.45673 0.19965 1.00000 0.02729 0.00000 0.00000 C2 0.04988 0.56980 0.11051 1.00000 0.02024 0.02102 0.02732 -0.01300 0.00651 -0.00661 0.02180 0.00526 0.00044 0.00028 0.00027 0.00000 0.00220 0.00221 0.00246 0.00191 0.00166 0.00186 0.00090 C3 -0.00242 0.62501 0.01839 1.00000 0.01896 0.01672 0.03680 -0.01218 -0.00255 -0.00183 0.02385 0.00515 0.00045 0.00028 0.00028 0.00000 0.00222 0.00214 0.00262 0.00195 0.00173 0.00176 0.00093 H3 -0.09716 0.67825 0.00291 1.00000 0.02862 0.00000 0.00000 C4 0.09344 0.59710 -0.04998 1.00000 0.01826 0.02044 0.02650 -0.00670 -0.00188 -0.00524 0.02213 0.00522 0.00044 0.00028 0.00027 0.00000 0.00216 0.00221 0.00234 0.00183 0.00159 0.00182 0.00089 C5 0.23134 0.52044 -0.03079 1.00000 0.02022 0.02164 0.02631 -0.01020 0.00046 -0.00779 0.02182 0.00507 0.00044 0.00028 0.00027 0.00000 0.00219 0.00219 0.00244 0.00189 0.00161 0.00183 0.00090 H5 0.29175 0.50383 -0.08038 1.00000 0.02618 0.00000 0.00000 C6 0.27966 0.46804 0.06322 1.00000 0.01819 0.01589 0.02896 -0.00566 0.00263 -0.00242 0.02241 0.00537 0.00044 0.00027 0.00027 0.00000 0.00221 0.00209 0.00243 0.00184 0.00168 0.00178 0.00091 C7 0.51984 0.34507 0.03686 1.00000 0.02034 0.02110 0.02334 -0.01119 0.00254 -0.00550 0.02082 0.00526 0.00044 0.00028 0.00028 0.00000 0.00222 0.00221 0.00251 0.00193 0.00164 0.00179 0.00089 C8 0.64542 0.25621 0.09016 1.00000 0.02162 0.01896 0.01820 -0.00726 -0.00088 -0.00209 0.02008 0.00508 0.00044 0.00027 0.00025 0.00000 0.00223 0.00214 0.00225 0.00179 0.00158 0.00176 0.00088 C9 0.67929 0.20238 0.18516 1.00000 0.01593 0.02319 0.02649 -0.01185 0.00066 -0.00611 0.02086 0.00506 0.00044 0.00028 0.00026 0.00000 0.00213 0.00224 0.00240 0.00190 0.00157 0.00179 0.00089 C10 0.82789 0.13138 0.19046 1.00000 0.02044 0.02123 0.01895 -0.00829 -0.00136 -0.00442 0.02004 0.00501 0.00044 0.00027 0.00025 0.00000 0.00219 0.00217 0.00222 0.00177 0.00156 0.00179 0.00087 C11 0.87881 0.14380 0.09784 1.00000 0.01880 0.02113 0.02100 -0.00788 0.00180 -0.00825 0.01973 0.00507 0.00043 0.00028 0.00025 0.00000 0.00215 0.00217 0.00226 0.00178 0.00157 0.00179 0.00087 C12 1.02230 0.08443 0.06653 1.00000 0.01876 0.02540 0.01936 -0.00905 -0.00083 -0.00618 0.02076 0.00506 0.00045 0.00029 0.00026 0.00000 0.00213 0.00231 0.00233 0.00192 0.00159 0.00186 0.00088 C13 1.18462 0.07610 -0.07422 1.00000 0.01968 0.02297 0.02186 -0.00955 0.00279 -0.00326 0.02179 0.00521 0.00044 0.00028 0.00026 0.00000 0.00224 0.00222 0.00233 0.00188 0.00159 0.00181 0.00090 C14 1.20372 0.13087 -0.16890 1.00000 0.02063 0.02484 0.02480 -0.00925 -0.00077 -0.00452 0.02362 0.00514 0.00045 0.00029 0.00027 0.00000 0.00227 0.00227 0.00242 0.00191 0.00162 0.00182 0.00092 H14 1.12525 0.19030 -0.20088 1.00000 0.02834 0.00000 0.00000 C15 1.33836 0.09758 -0.21568 1.00000 0.02306 0.02484 0.02126 -0.00845 0.00172 -0.00794 0.02281 0.00513 0.00044 0.00028 0.00026 0.00000 0.00231 0.00229 0.00231 0.00187 0.00165 0.00191 0.00091 C16 1.45749 0.01212 -0.17340 1.00000 0.01850 0.02686 0.02613 -0.01470 0.00214 -0.00580 0.02249 0.00505 0.00045 0.00028 0.00027 0.00000 0.00217 0.00236 0.00242 0.00198 0.00161 0.00188 0.00091 H16 1.55089 -0.00880 -0.20642 1.00000 0.02699 0.00000 0.00000 C17 1.43149 -0.04011 -0.08087 1.00000 0.01741 0.02110 0.02771 -0.01233 -0.00062 -0.00253 0.02153 0.00510 0.00043 0.00028 0.00027 0.00000 0.00217 0.00220 0.00248 0.00191 0.00164 0.00177 0.00090 C18 1.29923 -0.01190 -0.02984 1.00000 0.02074 0.02213 0.02299 -0.01100 0.00082 -0.00517 0.02127 0.00503 0.00044 0.00028 0.00027 0.00000 0.00220 0.00222 0.00224 0.00183 0.00161 0.00182 0.00088 H18 1.28660 -0.05166 0.03425 1.00000 0.02552 0.00000 0.00000 C19 0.57628 0.21475 0.26602 1.00000 0.02366 0.02138 0.01878 -0.00653 0.00396 -0.00202 0.02264 0.00547 0.00045 0.00028 0.00026 0.00000 0.00227 0.00220 0.00217 0.00179 0.00158 0.00181 0.00091 C20 0.63199 0.24062 0.33305 1.00000 0.01918 0.03710 0.02393 -0.01217 0.00355 -0.00739 0.02668 0.00560 0.00046 0.00030 0.00026 0.00000 0.00226 0.00262 0.00238 0.00202 0.00168 0.00198 0.00098 H20 0.73872 0.24816 0.32871 1.00000 0.03202 0.00000 0.00000 C21 0.53328 0.25546 0.40595 1.00000 0.03798 0.03774 0.02697 -0.01810 -0.00196 -0.00667 0.03287 0.00600 0.00052 0.00031 0.00028 0.00000 0.00281 0.00269 0.00255 0.00214 0.00190 0.00218 0.00106 H21 0.57190 0.27348 0.45130 1.00000 0.03944 0.00000 0.00000 C22 0.37820 0.24402 0.41269 1.00000 0.03220 0.03996 0.02591 -0.01522 0.00690 -0.00516 0.03314 0.00599 0.00050 0.00032 0.00029 0.00000 0.00263 0.00273 0.00249 0.00214 0.00182 0.00213 0.00106 H22 0.31027 0.25425 0.46274 1.00000 0.03977 0.00000 0.00000 C23 0.32217 0.21798 0.34744 1.00000 0.02268 0.04154 0.02752 -0.01560 0.00485 -0.00864 0.02997 0.00578 0.00048 0.00031 0.00028 0.00000 0.00234 0.00273 0.00248 0.00213 0.00174 0.00205 0.00101 H23 0.21537 0.21051 0.35210 1.00000 0.03597 0.00000 0.00000 C24 0.42118 0.20257 0.27477 1.00000 0.02538 0.02832 0.02200 -0.01138 0.00031 -0.00593 0.02482 0.00547 0.00046 0.00029 0.00026 0.00000 0.00236 0.00237 0.00233 0.00192 0.00166 0.00191 0.00093 H24 0.38235 0.18342 0.23037 1.00000 0.02979 0.00000 0.00000 C25 0.91125 0.05687 0.27970 1.00000 0.02241 0.02441 0.01903 -0.01148 -0.00007 -0.00043 0.02209 0.00527 0.00045 0.00028 0.00026 0.00000 0.00228 0.00225 0.00220 0.00186 0.00162 0.00184 0.00090 C26 1.07039 0.04828 0.29882 1.00000 0.02075 0.02611 0.02491 -0.01058 0.00151 -0.00119 0.02471 0.00537 0.00045 0.00029 0.00027 0.00000 0.00233 0.00235 0.00238 0.00195 0.00166 0.00187 0.00094 H26 1.12874 0.08980 0.25398 1.00000 0.02966 0.00000 0.00000 C27 1.14463 -0.02047 0.38287 1.00000 0.03049 0.03232 0.03004 -0.01324 -0.00853 0.00179 0.03193 0.00584 0.00052 0.00031 0.00029 0.00000 0.00254 0.00257 0.00263 0.00219 0.00192 0.00211 0.00106 H27 1.25358 -0.02604 0.39555 1.00000 0.03831 0.00000 0.00000 C28 1.05990 -0.08098 0.44831 1.00000 0.04449 0.02835 0.03040 -0.00855 -0.01227 0.00626 0.03759 0.00636 0.00055 0.00032 0.00031 0.00000 0.00302 0.00255 0.00266 0.00217 0.00208 0.00225 0.00114 H28 1.11165 -0.12878 0.50543 1.00000 0.04511 0.00000 0.00000 C29 0.90068 -0.07249 0.43127 1.00000 0.05114 0.02630 0.02526 -0.00233 -0.00184 -0.01439 0.03533 0.00604 0.00056 0.00031 0.00029 0.00000 0.00306 0.00247 0.00255 0.00204 0.00199 0.00222 0.00108 H29 0.84264 -0.11409 0.47628 1.00000 0.04239 0.00000 0.00000 C30 0.82662 -0.00233 0.34748 1.00000 0.02824 0.02852 0.02747 -0.01095 -0.00136 -0.00698 0.02785 0.00553 0.00049 0.00029 0.00027 0.00000 0.00242 0.00245 0.00247 0.00203 0.00179 0.00199 0.00097 H30 0.71609 0.00530 0.33636 1.00000 0.03343 0.00000 0.00000 C31 0.76627 0.52590 0.48528 1.00000 0.03311 0.03458 0.05494 -0.01438 0.00055 -0.01064 0.04113 0.00620 0.00054 0.00033 0.00034 0.00000 0.00270 0.00274 0.00318 0.00239 0.00209 0.00224 0.00117 H31A 0.66490 0.57281 0.49044 1.00000 0.06170 0.00000 0.00000 H31B 0.83447 0.56074 0.43714 1.00000 0.06170 0.00000 0.00000 H31C 0.82316 0.49437 0.54647 1.00000 0.06170 0.00000 0.00000 C32 0.92433 0.35971 0.45842 1.00000 0.03522 0.03606 0.05379 -0.01468 0.00934 -0.00205 0.04446 0.00711 0.00053 0.00034 0.00034 0.00000 0.00286 0.00281 0.00322 0.00243 0.00216 0.00228 0.00123 H32A 0.96714 0.33568 0.52290 1.00000 0.06669 0.00000 0.00000 H32B 0.99254 0.39821 0.41406 1.00000 0.06669 0.00000 0.00000 H32C 0.92393 0.30365 0.44159 1.00000 0.06669 0.00000 0.00000 C33 0.72897 0.20440 0.73507 1.00000 0.09866 0.03692 0.04620 -0.00918 -0.02496 -0.02369 0.05931 0.00663 0.00072 0.00035 0.00036 0.00000 0.00460 0.00307 0.00334 0.00255 0.00292 0.00310 0.00158 H33A 0.83101 0.15416 0.73942 1.00000 0.08897 0.00000 0.00000 H33B 0.67598 0.22319 0.67421 1.00000 0.08897 0.00000 0.00000 H33C 0.65806 0.17795 0.78678 1.00000 0.08897 0.00000 0.00000 C34 0.56793 0.37608 0.74505 1.00000 0.04138 0.09753 0.04424 -0.03547 -0.02014 0.03112 0.06732 0.00816 0.00060 0.00046 0.00036 0.00000 0.00332 0.00460 0.00327 0.00321 0.00238 0.00300 0.00178 H34A 0.50835 0.33551 0.79438 1.00000 0.10098 0.00000 0.00000 H34B 0.51688 0.39632 0.68331 1.00000 0.10098 0.00000 0.00000 H34C 0.56643 0.43456 0.75823 1.00000 0.10098 0.00000 0.00000 N1 -0.04687 0.59267 0.18795 1.00000 0.02589 0.02668 0.03568 -0.01487 0.00337 -0.00262 0.02952 0.00486 0.00042 0.00026 0.00026 0.00000 0.00215 0.00201 0.00239 0.00182 0.00161 0.00174 0.00083 N2 0.04133 0.65058 -0.14889 1.00000 0.02117 0.02510 0.03224 -0.00830 -0.00333 -0.00685 0.02642 0.00445 0.00039 0.00025 0.00023 0.00000 0.00202 0.00200 0.00219 0.00169 0.00153 0.00173 0.00079 N3 0.41531 0.38726 0.09201 1.00000 0.02482 0.02525 0.02006 -0.00823 -0.00215 0.00222 0.02513 0.00445 0.00037 0.00023 0.00022 0.00000 0.00193 0.00191 0.00183 0.00154 0.00136 0.00155 0.00078 H3A 0.43591 0.36025 0.15324 1.00000 0.03015 0.00000 0.00000 N4 0.76545 0.22067 0.03785 1.00000 0.02006 0.01959 0.01753 -0.00680 -0.00023 -0.00341 0.01942 0.00406 0.00035 0.00022 0.00021 0.00000 0.00182 0.00178 0.00175 0.00145 0.00130 0.00144 0.00072 H4 0.76971 0.24332 -0.02438 1.00000 0.02330 0.00000 0.00000 N5 1.04933 0.11522 -0.02908 1.00000 0.01779 0.02374 0.02341 -0.00754 -0.00036 0.00282 0.02372 0.00433 0.00036 0.00023 0.00022 0.00000 0.00183 0.00188 0.00197 0.00154 0.00133 0.00148 0.00077 H5A 0.97419 0.16441 -0.06562 1.00000 0.02847 0.00000 0.00000 N6 1.35506 0.15852 -0.31563 1.00000 0.03023 0.03377 0.02599 -0.01497 0.00439 -0.00738 0.02929 0.00464 0.00043 0.00026 0.00023 0.00000 0.00218 0.00225 0.00206 0.00179 0.00162 0.00186 0.00082 N7 1.55249 -0.13274 -0.03088 1.00000 0.01975 0.02383 0.03161 -0.01404 -0.00119 -0.00294 0.02438 0.00444 0.00038 0.00024 0.00025 0.00000 0.00199 0.00191 0.00228 0.00176 0.00150 0.00157 0.00077 O1 0.00516 0.54753 0.26904 1.00000 0.03870 0.03095 0.02690 -0.00923 0.00528 -0.00394 0.03408 0.00415 0.00035 0.00021 0.00020 0.00000 0.00186 0.00173 0.00182 0.00146 0.00135 0.00146 0.00072 O2 -0.17550 0.65643 0.16618 1.00000 0.02359 0.04262 0.04738 -0.02221 0.00255 0.00446 0.03912 0.00412 0.00034 0.00022 0.00021 0.00000 0.00178 0.00193 0.00196 0.00157 0.00133 0.00159 0.00077 O3 -0.07859 0.72079 -0.16714 1.00000 0.03533 0.03092 0.03723 -0.00569 -0.00930 0.00335 0.03846 0.00406 0.00035 0.00021 0.00020 0.00000 0.00194 0.00175 0.00187 0.00144 0.00135 0.00158 0.00076 O4 0.11900 0.62152 -0.20953 1.00000 0.03587 0.03601 0.02517 -0.00719 0.00088 0.00009 0.03567 0.00414 0.00035 0.00021 0.00019 0.00000 0.00181 0.00179 0.00168 0.00142 0.00132 0.00146 0.00073 O5 0.51475 0.37933 -0.04923 1.00000 0.02878 0.02820 0.02284 -0.00788 0.00149 -0.00149 0.02844 0.00380 0.00031 0.00020 0.00019 0.00000 0.00168 0.00161 0.00174 0.00135 0.00118 0.00132 0.00067 O6 1.11024 0.01123 0.12324 1.00000 0.02766 0.02627 0.02263 -0.00439 -0.00013 0.00792 0.03012 0.00395 0.00033 0.00020 0.00018 0.00000 0.00161 0.00161 0.00158 0.00133 0.00119 0.00134 0.00068 O7 1.24950 0.23393 -0.35233 1.00000 0.04930 0.03298 0.02459 -0.00177 0.00462 0.00490 0.04200 0.00457 0.00038 0.00022 0.00019 0.00000 0.00209 0.00185 0.00172 0.00144 0.00139 0.00166 0.00080 O8 1.47438 0.12901 -0.35802 1.00000 0.03520 0.05367 0.02891 -0.01114 0.00876 -0.00423 0.04270 0.00438 0.00036 0.00023 0.00020 0.00000 0.00194 0.00218 0.00176 0.00158 0.00137 0.00165 0.00082 O9 1.66633 -0.16205 -0.07674 1.00000 0.02214 0.03857 0.03863 -0.02174 -0.00035 0.00515 0.03358 0.00388 0.00032 0.00021 0.00019 0.00000 0.00166 0.00181 0.00179 0.00150 0.00128 0.00138 0.00071 O10 1.53449 -0.17478 0.05389 1.00000 0.03089 0.02746 0.02931 -0.00743 -0.00210 -0.00033 0.03154 0.00387 0.00032 0.00020 0.00021 0.00000 0.00173 0.00165 0.00187 0.00143 0.00127 0.00135 0.00069 O11 0.63557 0.37805 0.53394 1.00000 0.03341 0.03595 0.03322 -0.00652 0.00074 -0.01526 0.03477 0.00383 0.00033 0.00021 0.00019 0.00000 0.00175 0.00175 0.00173 0.00141 0.00126 0.00145 0.00072 O12 0.83314 0.27500 0.84337 1.00000 0.02344 0.03331 0.02062 -0.01050 -0.00320 0.00099 0.02718 0.00360 0.00030 0.00020 0.00017 0.00000 0.00155 0.00167 0.00152 0.00128 0.00110 0.00128 0.00066 S1 0.72342 0.43523 0.45242 1.00000 0.03179 0.03357 0.03040 -0.00552 -0.00416 -0.00724 0.03378 0.00155 0.00013 0.00008 0.00008 0.00000 0.00066 0.00067 0.00065 0.00053 0.00046 0.00053 0.00030 S2 0.76805 0.30797 0.74368 1.00000 0.02744 0.02734 0.02322 -0.00764 -0.00231 -0.00336 0.02714 0.00146 0.00012 0.00008 0.00007 0.00000 0.00061 0.00061 0.00060 0.00048 0.00042 0.00048 0.00027 Final Structure Factor Calculation for 02SOT039 in P-1 Total number of l.s. parameters = 501 Maximum vector length = 511 Memory required = 4801 / 24017 wR2 = 0.1242 before cycle 5 for 6028 data and 0 / 501 parameters GooF = S = 0.909; Restrained GooF = 0.909 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0559 for 3187 Fo > 4sig(Fo) and 0.1424 for all 6028 data wR2 = 0.1242, GooF = S = 0.909, Restrained GooF = 0.909 for all data Occupancy sum of asymmetric unit = 55.00 for non-hydrogen and 31.00 for hydrogen atoms Principal mean square atomic displacements U 0.0286 0.0208 0.0189 C1 0.0310 0.0191 0.0154 C2 0.0373 0.0200 0.0143 C3 0.0284 0.0204 0.0176 C4 0.0264 0.0223 0.0168 C5 0.0331 0.0191 0.0150 C6 0.0250 0.0204 0.0170 C7 0.0249 0.0179 0.0174 C8 0.0273 0.0201 0.0151 C9 0.0227 0.0202 0.0173 C10 0.0227 0.0208 0.0157 C11 0.0254 0.0200 0.0168 C12 0.0256 0.0232 0.0165 C13 0.0259 0.0246 0.0204 C14 0.0255 0.0226 0.0203 C15 0.0301 0.0197 0.0176 C16 0.0287 0.0197 0.0162 C17 0.0246 0.0210 0.0182 C18 0.0318 0.0199 0.0162 C19 0.0378 0.0248 0.0174 C20 0.0431 0.0355 0.0199 C21 0.0447 0.0354 0.0193 C22 0.0418 0.0284 0.0197 C23 0.0291 0.0253 0.0200 C24 0.0312 0.0204 0.0147 C25 0.0312 0.0253 0.0177 C26 0.0462 0.0283 0.0213 C27 0.0602 0.0331 0.0194 C28 0.0517 0.0344 0.0199 C29 0.0299 0.0282 0.0255 C30 0.0569 0.0353 0.0311 C31 0.0649 0.0415 0.0269 C32 0.1102 0.0366 0.0311 C33 0.1438 0.0378 0.0204 C34 0.0366 0.0321 0.0199 N1 0.0348 0.0250 0.0194 N2 0.0373 0.0201 0.0179 N3 0.0224 0.0184 0.0174 N4 0.0341 0.0235 0.0136 N5 0.0345 0.0326 0.0208 N6 0.0328 0.0217 0.0186 N7 0.0479 0.0295 0.0249 O1 0.0542 0.0460 0.0172 O2 0.0498 0.0450 0.0205 O3 0.0531 0.0291 0.0248 O4 0.0390 0.0238 0.0225 O5 0.0521 0.0233 0.0150 O6 0.0742 0.0304 0.0214 O7 0.0672 0.0383 0.0226 O8 0.0513 0.0339 0.0155 O9 0.0406 0.0314 0.0226 O10 0.0453 0.0337 0.0253 O11 0.0414 0.0218 0.0184 O12 0.0420 0.0336 0.0257 S1 0.0328 0.0269 0.0217 S2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.015 0.023 0.032 0.041 0.052 0.066 0.086 0.122 1.000 Number in group 647. 558. 606. 637. 591. 595. 585. 607. 604. 598. GooF 0.724 0.794 0.800 0.892 0.870 1.045 0.988 0.932 0.973 1.022 K 1.559 1.218 0.980 0.914 0.960 0.973 1.001 0.995 1.002 1.018 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.05 1.13 1.24 1.40 1.72 inf Number in group 627. 605. 592. 598. 596. 608. 598. 594. 608. 602. GooF 0.859 0.877 0.908 0.927 0.899 0.925 0.874 0.828 0.920 1.054 K 1.056 0.945 1.013 1.000 0.989 0.993 1.015 1.008 1.036 1.007 R1 0.391 0.377 0.274 0.196 0.162 0.119 0.094 0.083 0.072 0.039 Recommended weighting scheme: WGHT 0.0416 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 7 8 13 -55.05 179.69 4.41 0.051 0.89 -1 -1 14 -67.38 224.91 4.30 0.057 0.98 -4 6 4 402.28 163.43 4.01 0.049 1.38 -5 6 12 153.87 27.23 3.74 0.020 0.94 -6 5 8 164.16 286.46 3.60 0.064 1.02 5 -3 12 251.12 62.09 3.59 0.030 0.86 7 2 11 290.28 149.14 3.57 0.047 0.91 0 3 4 1486.66 1762.44 3.56 0.160 3.47 -2 4 6 2117.49 1807.84 3.44 0.162 1.93 -7 3 0 0.00 199.62 3.42 0.054 1.08 0 4 1 966.29 1146.84 3.34 0.129 3.62 1 0 8 118.33 219.39 3.33 0.056 1.72 2 4 5 459.57 573.57 3.31 0.091 2.51 -1 -4 5 6069.43 5189.47 3.29 0.274 1.88 8 14 3 0.00 170.88 3.24 0.050 0.86 -5 5 12 343.47 453.89 3.24 0.081 0.95 0 8 0 1714.37 1359.94 3.21 0.140 1.70 1 -1 12 242.61 390.35 3.17 0.075 1.12 -3 1 14 651.95 440.74 3.17 0.080 0.97 -2 11 14 67.38 170.65 3.14 0.050 0.91 -3 -4 2 917.54 1080.25 3.13 0.125 2.17 8 6 7 0.00 105.56 3.11 0.039 1.00 -4 0 13 359.31 177.21 3.05 0.051 0.97 -5 11 10 112.60 276.00 3.05 0.063 0.86 2 17 8 166.05 11.65 3.04 0.013 0.89 7 -1 2 -67.38 110.89 3.04 0.040 1.13 2 -5 3 1016.31 861.91 3.03 0.112 1.71 4 -6 10 169.43 42.48 3.02 0.025 0.88 1 -7 7 -38.90 63.36 3.02 0.030 1.16 2 -1 11 38.50 141.51 3.02 0.045 1.17 8 5 1 202.53 121.35 3.01 0.042 1.07 -5 7 11 83.86 174.23 3.01 0.050 0.96 -1 15 6 202.12 25.80 3.00 0.019 0.94 6 2 1 263.48 172.52 2.99 0.050 1.43 -1 2 5 1987.60 2279.55 2.98 0.182 2.75 0 0 8 1900.23 1623.48 2.98 0.153 1.77 3 1 0 2245.78 2567.30 2.97 0.193 2.85 1 9 15 53.96 170.34 2.95 0.050 0.99 -3 -9 10 472.97 127.38 2.92 0.043 0.88 -2 1 7 3802.52 3285.32 2.91 0.218 1.86 -3 -12 5 134.74 14.95 2.89 0.015 0.96 0 6 2 256.44 349.27 2.88 0.071 2.43 -2 -2 11 2523.90 2112.78 2.87 0.175 1.16 -3 3 13 193.32 53.05 2.87 0.028 1.05 -1 15 0 0.00 120.27 2.86 0.042 0.88 -2 -8 10 180.40 12.65 2.84 0.014 0.94 7 -1 9 84.42 0.45 2.84 0.003 0.91 3 8 16 -45.29 103.65 2.81 0.039 0.93 -3 13 4 213.65 93.56 2.81 0.037 0.95 4 3 11 323.75 238.02 2.81 0.059 1.18 Bond lengths and angles C1 - Distance Angles C2 1.3762 (0.0052) C6 1.3983 (0.0052) 118.73 (0.36) C1 - C2 C2 - Distance Angles C1 1.3762 (0.0052) C3 1.3795 (0.0054) 123.78 (0.34) N1 1.4734 (0.0049) 117.41 (0.35) 118.80 (0.35) C2 - C1 C3 C3 - Distance Angles C2 1.3795 (0.0054) C4 1.3870 (0.0053) 115.09 (0.36) C3 - C2 C4 - Distance Angles C5 1.3766 (0.0052) C3 1.3870 (0.0053) 124.42 (0.37) N2 1.4629 (0.0050) 117.81 (0.34) 117.74 (0.35) C4 - C5 C3 C5 - Distance Angles C4 1.3766 (0.0052) C6 1.3899 (0.0052) 118.09 (0.35) C5 - C4 C6 - Distance Angles C5 1.3899 (0.0052) C1 1.3983 (0.0052) 119.89 (0.36) N3 1.4002 (0.0047) 123.53 (0.34) 116.52 (0.35) C6 - C5 C1 C7 - Distance Angles O5 1.2164 (0.0044) N3 1.3680 (0.0047) 123.23 (0.35) C8 1.4778 (0.0052) 122.12 (0.32) 114.60 (0.34) C7 - O5 N3 C8 - Distance Angles N4 1.3617 (0.0046) C9 1.3812 (0.0052) 109.21 (0.32) C7 1.4778 (0.0052) 116.19 (0.32) 134.35 (0.34) C8 - N4 C9 C9 - Distance Angles C8 1.3812 (0.0052) C10 1.4128 (0.0051) 106.69 (0.32) C19 1.4886 (0.0051) 126.54 (0.34) 126.74 (0.34) C9 - C8 C10 C10 - Distance Angles C11 1.3963 (0.0050) C9 1.4128 (0.0051) 107.41 (0.32) C25 1.4910 (0.0052) 127.28 (0.35) 125.30 (0.33) C10 - C11 C9 C11 - Distance Angles N4 1.3736 (0.0047) C10 1.3963 (0.0050) 107.65 (0.32) C12 1.4706 (0.0052) 124.40 (0.32) 127.89 (0.34) C11 - N4 C10 C12 - Distance Angles O6 1.2212 (0.0044) N5 1.3712 (0.0047) 122.54 (0.35) C11 1.4706 (0.0052) 121.17 (0.34) 116.28 (0.32) C12 - O6 N5 C13 - Distance Angles C14 1.3886 (0.0052) C18 1.3906 (0.0052) 119.35 (0.34) N5 1.3984 (0.0046) 116.55 (0.34) 124.10 (0.34) C13 - C14 C18 C14 - Distance Angles C15 1.3774 (0.0052) C13 1.3886 (0.0052) 118.88 (0.36) C14 - C15 C15 - Distance Angles C14 1.3774 (0.0052) C16 1.3823 (0.0052) 123.57 (0.36) N6 1.4725 (0.0050) 117.14 (0.34) 119.28 (0.33) C15 - C14 C16 C16 - Distance Angles C17 1.3654 (0.0052) C15 1.3823 (0.0052) 115.30 (0.34) C16 - C17 C17 - Distance Angles C16 1.3654 (0.0052) C18 1.3774 (0.0051) 124.34 (0.36) N7 1.4757 (0.0049) 118.62 (0.32) 117.04 (0.34) C17 - C16 C18 C18 - Distance Angles C17 1.3774 (0.0051) C13 1.3906 (0.0052) 118.51 (0.36) C18 - C17 C19 - Distance Angles C24 1.3852 (0.0053) C20 1.3909 (0.0054) 118.66 (0.34) C9 1.4886 (0.0051) 120.38 (0.34) 120.94 (0.33) C19 - C24 C20 C20 - Distance Angles C21 1.3826 (0.0054) C19 1.3909 (0.0054) 120.52 (0.36) C20 - C21 C21 - Distance Angles C20 1.3826 (0.0054) C22 1.3827 (0.0058) 119.83 (0.38) C21 - C20 C22 - Distance Angles C23 1.3701 (0.0055) C21 1.3827 (0.0058) 120.23 (0.37) C22 - C23 C23 - Distance Angles C22 1.3701 (0.0055) C24 1.3836 (0.0053) 119.98 (0.38) C23 - C22 C24 - Distance Angles C23 1.3836 (0.0053) C19 1.3852 (0.0053) 120.76 (0.36) C24 - C23 C25 - Distance Angles C30 1.3878 (0.0054) C26 1.3883 (0.0052) 118.83 (0.35) C10 1.4910 (0.0052) 119.70 (0.35) 121.41 (0.35) C25 - C30 C26 C26 - Distance Angles C27 1.3855 (0.0055) C25 1.3883 (0.0052) 120.42 (0.38) C26 - C27 C27 - Distance Angles C28 1.3834 (0.0061) C26 1.3855 (0.0055) 119.91 (0.40) C27 - C28 C28 - Distance Angles C29 1.3811 (0.0061) C27 1.3834 (0.0061) 120.54 (0.40) C28 - C29 C29 - Distance Angles C28 1.3811 (0.0061) C30 1.3883 (0.0056) 119.10 (0.41) C29 - C28 C30 - Distance Angles C25 1.3878 (0.0054) C29 1.3883 (0.0056) 121.14 (0.39) C30 - C25 C31 - Distance Angles S1 1.7694 (0.0045) C31 - C32 - Distance Angles S1 1.7796 (0.0045) C32 - C33 - Distance Angles S2 1.7525 (0.0048) C33 - C34 - Distance Angles S2 1.7494 (0.0048) C34 - N1 - Distance Angles O1 1.2233 (0.0042) O2 1.2280 (0.0042) 124.34 (0.34) C2 1.4734 (0.0049) 118.48 (0.34) 117.18 (0.34) N1 - O1 O2 N2 - Distance Angles O3 1.2256 (0.0041) O4 1.2347 (0.0041) 123.39 (0.33) C4 1.4629 (0.0050) 118.41 (0.33) 118.18 (0.33) N2 - O3 O4 N3 - Distance Angles C7 1.3680 (0.0047) C6 1.4002 (0.0047) 128.13 (0.34) N3 - C7 N4 - Distance Angles C8 1.3617 (0.0046) C11 1.3736 (0.0047) 109.04 (0.30) N4 - C8 N5 - Distance Angles C12 1.3712 (0.0047) C13 1.3984 (0.0046) 126.38 (0.32) N5 - C12 N6 - Distance Angles O7 1.2202 (0.0042) O8 1.2289 (0.0041) 123.61 (0.34) C15 1.4725 (0.0050) 118.84 (0.32) 117.53 (0.34) N6 - O7 O8 N7 - Distance Angles O10 1.2234 (0.0039) O9 1.2288 (0.0040) 124.10 (0.32) C17 1.4757 (0.0049) 117.97 (0.30) 117.92 (0.33) N7 - O10 O9 O1 - Distance Angles N1 1.2233 (0.0042) O1 - O2 - Distance Angles N1 1.2280 (0.0042) O2 - O3 - Distance Angles N2 1.2256 (0.0041) O3 - O4 - Distance Angles N2 1.2347 (0.0041) O4 - O5 - Distance Angles C7 1.2164 (0.0044) O5 - O6 - Distance Angles C12 1.2212 (0.0044) O6 - O7 - Distance Angles N6 1.2202 (0.0042) O7 - O8 - Distance Angles N6 1.2289 (0.0041) O8 - O9 - Distance Angles N7 1.2288 (0.0040) O9 - O10 - Distance Angles N7 1.2234 (0.0039) O10 - O11 - Distance Angles S1 1.4970 (0.0029) O11 - O12 - Distance Angles S2 1.5199 (0.0027) O12 - S1 - Distance Angles O11 1.4970 (0.0029) C31 1.7694 (0.0045) 106.27 (0.20) C32 1.7796 (0.0045) 106.15 (0.20) 98.03 (0.23) S1 - O11 C31 S2 - Distance Angles O12 1.5199 (0.0027) C34 1.7494 (0.0048) 105.52 (0.19) C33 1.7525 (0.0048) 105.98 (0.20) 98.28 (0.31) S2 - O12 C34 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.95 2.812(4) 166.2 N4-H4...O12_$1 0.88 1.91 2.787(4) 172.5 N5-H5A...O12_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)