+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 15:45:48 on 02-Dec-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SRC410 in Cc CELL 0.71073 6.7778 20.1108 13.1963 90.000 96.674 90.000 ZERR 4.00 0.0003 0.0011 0.0009 0.000 0.002 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC C H O UNIT 88 80 24 V = 1786.56 F(000) = 800.0 Mu = 0.10 mm-1 Cell Wt = 1521.52 Rho = 1.414 MERG 2 SHEL 7 0.84 HTAB O3 O3 HTAB O6 O5 FMAP 2 PLAN 25 SIZE 0.10 0.10 0.20 ACTA BOND $H WGHT 0.06700 L.S. 10 TEMP -153.00 FVAR 0.27053 MOLE 1 O1 3 0.620040 0.208768 0.889349 11.00000 0.01703 0.02429 = 0.03659 0.00140 0.00604 0.00025 O2 3 0.763071 0.306304 0.899537 11.00000 0.01870 0.03164 = 0.04065 0.00206 0.00557 -0.00309 O3 3 0.567585 0.412787 0.900385 11.00000 0.02768 0.02587 = 0.05123 -0.00038 0.00603 -0.00358 AFIX 147 H3O 2 0.669055 0.388655 0.901993 11.00000 -1.50000 AFIX 0 C1 1 0.453536 0.167613 0.891732 11.00000 0.01688 0.02134 = 0.02221 0.00221 0.00341 -0.00254 C2 1 0.493232 0.100172 0.896357 11.00000 0.02538 0.02717 = 0.02851 -0.00209 0.00352 0.00081 AFIX 43 H2 2 0.626162 0.084538 0.900275 11.00000 -1.20000 AFIX 0 C3 1 0.338418 0.056049 0.895226 11.00000 0.03718 0.02008 = 0.03369 -0.00043 0.00003 0.00168 AFIX 43 H3 2 0.363511 0.009564 0.896989 11.00000 -1.20000 AFIX 0 C4 1 0.144560 0.079609 0.891489 11.00000 0.02989 0.02423 = 0.03569 0.00222 0.00122 -0.00587 AFIX 43 H4 2 0.037152 0.049233 0.891177 11.00000 -1.20000 AFIX 0 C5 1 0.108706 0.147188 0.888239 11.00000 0.01981 0.02590 = 0.03506 -0.00197 -0.00241 -0.00046 AFIX 43 H5 2 -0.023829 0.162823 0.886907 11.00000 -1.20000 AFIX 0 C6 1 0.263795 0.193300 0.886858 11.00000 0.02189 0.02630 = 0.01715 -0.00049 0.00091 0.00751 C7 1 0.223902 0.266267 0.879390 11.00000 0.02184 0.02727 = 0.02041 0.00303 0.00388 0.00057 AFIX 23 H7A 2 0.140909 0.279255 0.933120 11.00000 -1.20000 H7B 2 0.147626 0.276032 0.812444 11.00000 -1.20000 AFIX 0 C8 1 0.411250 0.307492 0.890730 11.00000 0.02280 0.01853 = 0.01838 -0.00043 0.00549 0.00041 C9 1 0.406067 0.374784 0.891110 11.00000 0.02401 0.02781 = 0.02219 -0.00191 0.00363 -0.00110 C10 1 0.217714 0.414269 0.879286 11.00000 0.03077 0.02840 = 0.03259 -0.00123 0.00577 0.00547 AFIX 137 H10A 2 0.223517 0.448311 0.932689 11.00000 -1.50000 H10B 2 0.104872 0.384636 0.885272 11.00000 -1.50000 H10C 2 0.201378 0.435723 0.812154 11.00000 -1.50000 AFIX 0 C11 1 0.604385 0.276502 0.894422 11.00000 0.02438 0.02329 = 0.02361 0.00061 0.00440 0.00311 MOLE 2 O4 3 0.336548 0.167932 0.627825 11.00000 0.02250 0.02165 = 0.03668 -0.00088 0.00442 -0.00482 O5 3 0.198117 0.266130 0.618879 11.00000 0.01738 0.03317 = 0.03769 -0.00220 0.00276 0.00279 O6 3 0.398807 0.371765 0.630303 11.00000 0.02595 0.02689 = 0.04443 -0.00224 0.00218 0.00497 AFIX 147 H6 2 0.295691 0.348281 0.622194 11.00000 -1.50000 AFIX 0 C12 1 0.503023 0.125979 0.632322 11.00000 0.02146 0.02497 = 0.02213 -0.00059 0.00151 -0.00125 C13 1 0.460024 0.059037 0.623669 11.00000 0.02911 0.02402 = 0.02969 0.00052 0.00405 -0.01018 AFIX 43 H13 2 0.326140 0.044136 0.614294 11.00000 -1.20000 AFIX 0 C14 1 0.615404 0.013837 0.628875 11.00000 0.03765 0.02125 = 0.03288 -0.00091 0.00195 -0.00250 AFIX 43 H14 2 0.588853 -0.032459 0.622688 11.00000 -1.20000 AFIX 0 C15 1 0.809597 0.036599 0.643154 11.00000 0.02714 0.02870 = 0.04081 0.00403 -0.00261 0.00383 AFIX 43 H15 2 0.916434 0.005754 0.648039 11.00000 -1.20000 AFIX 0 C16 1 0.848513 0.104075 0.650324 11.00000 0.02312 0.02467 = 0.02909 -0.00125 0.00060 0.00154 AFIX 43 H16 2 0.982309 0.119075 0.659359 11.00000 -1.20000 AFIX 0 C17 1 0.694596 0.150442 0.644510 11.00000 0.02321 0.01874 = 0.01820 -0.00199 0.00261 0.00049 C18 1 0.737097 0.223517 0.654414 11.00000 0.01712 0.02105 = 0.02397 -0.00260 0.00058 -0.00234 AFIX 23 H18A 2 0.824046 0.236811 0.602593 11.00000 -1.20000 H18B 2 0.809402 0.232519 0.722602 11.00000 -1.20000 AFIX 0 C19 1 0.550838 0.264674 0.640817 11.00000 0.01691 0.02425 = 0.02042 -0.00256 0.00123 0.00014 C20 1 0.558606 0.332437 0.641891 11.00000 0.01906 0.02785 = 0.02189 -0.00091 0.00431 -0.00046 C21 1 0.748554 0.370586 0.656775 11.00000 0.03142 0.02345 = 0.03665 -0.00305 0.00296 -0.00609 AFIX 137 H21A 2 0.799092 0.376738 0.590780 11.00000 -1.50000 H21B 2 0.846410 0.345969 0.702810 11.00000 -1.50000 H21C 2 0.724925 0.414110 0.686512 11.00000 -1.50000 AFIX 0 C22 1 0.358433 0.234880 0.628658 11.00000 0.02377 0.02830 = 0.02084 0.00131 0.00495 0.00235 HKLF 4 Covalent radii and connectivity table for 02SRC410 in Cc C 0.770 H 0.320 O 0.660 O1 - C11 C1 O2 - C11 O3 - C9 C1 - C6 C2 O1 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C1 C5 C7 C7 - C6 C8 C8 - C9 C11 C7 C9 - O3 C8 C10 C10 - C9 C11 - O2 O1 C8 O4 - C22 C12 O5 - C22 O6 - C20 C12 - C13 C17 O4 C13 - C12 C14 C14 - C15 C13 C15 - C16 C14 C16 - C15 C17 C17 - C12 C16 C18 C18 - C17 C19 C19 - C20 C22 C18 C20 - O6 C19 C21 C21 - C20 C22 - O5 O4 C19 Floating origin restraints generated 6549 Reflections read, of which 841 rejected -7 =< h =< 8, -23 =< k =< 22, -15 =< l =< 15, Max. 2-theta = 50.04 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -5 3 -4 144.22 1.97 3 77.21 -5 3 -2 42.41 1.45 2 19.69 -2 2 0 175.17 6.57 2 129.02 -6 6 0 32.26 1.44 2 8.04 -1 7 1 20.57 0.96 2 5.05 5 5 8 8.45 0.97 2 4.87 6 Inconsistent equivalents 2969 Unique reflections, of which 0 suppressed R(int) = 0.0487 R(sigma) = 0.0667 Friedel opposites not merged Maximum memory for data reduction = 2457 / 35391 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 = 3170 / 318294 wR2 = 0.1236 before cycle 1 for 2969 data and 257 / 257 parameters GooF = S = 1.044; Restrained GooF = 1.043 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0670 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27054 0.00073 0.008 OSF Mean shift/su = 0.001 Maximum = 0.008 for OSF Max. shift = 0.000 A for H10B Max. dU = 0.000 for C4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3170 / 318294 wR2 = 0.1236 before cycle 2 for 2969 data and 257 / 257 parameters GooF = S = 1.044; Restrained GooF = 1.043 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0670 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27054 0.00073 0.000 OSF Mean shift/su = 0.000 Maximum = 0.002 for U33 O2 Max. shift = 0.000 A for H21B Max. dU = 0.000 for C9 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3170 / 318294 wR2 = 0.1236 before cycle 3 for 2969 data and 257 / 257 parameters GooF = S = 1.044; Restrained GooF = 1.043 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0670 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27054 0.00073 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H6 Max. dU = 0.000 for C12 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3170 / 318294 wR2 = 0.1236 before cycle 4 for 2969 data and 257 / 257 parameters GooF = S = 1.044; Restrained GooF = 1.043 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0670 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27054 0.00073 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z O4 Max. shift = 0.000 A for H3O Max. dU = 0.000 for C15 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3170 / 318294 wR2 = 0.1236 before cycle 5 for 2969 data and 257 / 257 parameters GooF = S = 1.044; Restrained GooF = 1.043 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0670 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27054 0.00073 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H21B Max. dU = 0.000 for O4 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3170 / 318294 wR2 = 0.1236 before cycle 6 for 2969 data and 257 / 257 parameters GooF = S = 1.044; Restrained GooF = 1.043 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0670 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27054 0.00073 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H3O Max. dU = 0.000 for C13 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3170 / 318294 wR2 = 0.1236 before cycle 7 for 2969 data and 257 / 257 parameters GooF = S = 1.044; Restrained GooF = 1.043 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0670 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27054 0.00073 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z O4 Max. shift = 0.000 A for H6 Max. dU = 0.000 for C15 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3170 / 318294 wR2 = 0.1236 before cycle 8 for 2969 data and 257 / 257 parameters GooF = S = 1.044; Restrained GooF = 1.043 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0670 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27054 0.00073 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H3O Max. dU = 0.000 for O1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3170 / 318294 wR2 = 0.1236 before cycle 9 for 2969 data and 257 / 257 parameters GooF = S = 1.044; Restrained GooF = 1.043 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0670 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27054 0.00073 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C2 Max. shift = 0.000 A for H14 Max. dU = 0.000 for C6 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3170 / 318294 wR2 = 0.1236 before cycle 10 for 2969 data and 257 / 257 parameters GooF = S = 1.044; Restrained GooF = 1.043 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0670 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27054 0.00073 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H6 Max. dU = 0.000 for O3 Largest correlation matrix elements -0.597 U11 C15 / U11 C4 0.574 U12 C13 / U12 C2 0.515 U12 C18 / U12 C7 -0.588 U11 C17 / U11 C6 -0.532 U13 C15 / U13 C4 -0.515 U11 C19 / U11 C8 0.575 U12 C20 / U12 C9 0.519 U12 C12 / U12 C1 0.506 x C19 / x C8 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3O 0.6691 0.3887 0.9020 147 0.840 0.000 O3 C9 H3O H2 0.6262 0.0845 0.9003 43 0.950 0.000 C2 C3 C1 H3 0.3635 0.0096 0.8970 43 0.950 0.000 C3 C2 C4 H4 0.0371 0.0492 0.8912 43 0.950 0.000 C4 C5 C3 H5 -0.0238 0.1628 0.8869 43 0.950 0.000 C5 C4 C6 H7A 0.1409 0.2793 0.9331 23 0.990 0.000 C7 C6 C8 H7B 0.1476 0.2760 0.8124 23 0.990 0.000 C7 C6 C8 H10A 0.2235 0.4483 0.9327 137 0.980 0.000 C10 C9 H10A H10B 0.1049 0.3846 0.8853 137 0.980 0.000 C10 C9 H10A H10C 0.2014 0.4357 0.8122 137 0.980 0.000 C10 C9 H10A H6 0.2957 0.3483 0.6222 147 0.840 0.000 O6 C20 H6 H13 0.3261 0.0441 0.6143 43 0.950 0.000 C13 C12 C14 H14 0.5889 -0.0325 0.6227 43 0.950 0.000 C14 C15 C13 H15 0.9164 0.0058 0.6480 43 0.950 0.000 C15 C16 C14 H16 0.9823 0.1191 0.6594 43 0.950 0.000 C16 C15 C17 H18A 0.8240 0.2368 0.6026 23 0.990 0.000 C18 C17 C19 H18B 0.8094 0.2325 0.7226 23 0.990 0.000 C18 C17 C19 H21A 0.7991 0.3767 0.5908 137 0.980 0.000 C21 C20 H21A H21B 0.8464 0.3460 0.7028 137 0.980 0.000 C21 C20 H21A H21C 0.7249 0.4141 0.6865 137 0.980 0.000 C21 C20 H21A 02SRC410 in Cc ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O1 0.62004 0.20877 0.88935 1.00000 0.01703 0.02429 0.03659 0.00140 0.00604 0.00025 0.02574 0.00409 0.00034 0.00012 0.00017 0.00000 0.00140 0.00139 0.00147 0.00114 0.00100 0.00108 0.00062 O2 0.76307 0.30630 0.89954 1.00000 0.01870 0.03164 0.04066 0.00206 0.00557 -0.00310 0.03017 0.00413 0.00034 0.00011 0.00018 0.00000 0.00131 0.00154 0.00150 0.00105 0.00102 0.00107 0.00060 O3 0.56758 0.41279 0.90038 1.00000 0.02768 0.02587 0.05123 -0.00038 0.00603 -0.00358 0.03481 0.00446 0.00037 0.00012 0.00020 0.00000 0.00144 0.00142 0.00165 0.00119 0.00113 0.00121 0.00065 H3O 0.66906 0.38866 0.90199 1.00000 0.05222 0.00000 0.00000 C1 0.45354 0.16761 0.89173 1.00000 0.01688 0.02134 0.02222 0.00221 0.00341 -0.00254 0.02006 0.00583 0.00047 0.00017 0.00022 0.00000 0.00189 0.00202 0.00181 0.00141 0.00133 0.00155 0.00077 C2 0.49323 0.10017 0.89636 1.00000 0.02538 0.02717 0.02852 -0.00209 0.00352 0.00081 0.02699 0.00620 0.00057 0.00017 0.00025 0.00000 0.00221 0.00234 0.00207 0.00156 0.00150 0.00176 0.00096 H2 0.62617 0.08454 0.90027 1.00000 0.03239 0.00000 0.00000 C3 0.33842 0.05605 0.89523 1.00000 0.03718 0.02008 0.03369 -0.00043 0.00003 0.00168 0.03064 0.00632 0.00054 0.00018 0.00026 0.00000 0.00232 0.00212 0.00205 0.00154 0.00164 0.00175 0.00091 H3 0.36351 0.00956 0.89699 1.00000 0.03677 0.00000 0.00000 C4 0.14456 0.07961 0.89149 1.00000 0.02988 0.02423 0.03569 0.00222 0.00122 -0.00587 0.03014 0.00646 0.00056 0.00018 0.00027 0.00000 0.00268 0.00220 0.00211 0.00164 0.00172 0.00172 0.00098 H4 0.03715 0.04923 0.89118 1.00000 0.03616 0.00000 0.00000 C5 0.10871 0.14719 0.88824 1.00000 0.01980 0.02589 0.03507 -0.00197 -0.00241 -0.00046 0.02736 0.00615 0.00052 0.00019 0.00026 0.00000 0.00189 0.00192 0.00205 0.00152 0.00134 0.00152 0.00082 H5 -0.02383 0.16282 0.88691 1.00000 0.03283 0.00000 0.00000 C6 0.26379 0.19330 0.88686 1.00000 0.02189 0.02630 0.01715 -0.00049 0.00091 0.00751 0.02189 0.00654 0.00055 0.00018 0.00024 0.00000 0.00225 0.00209 0.00180 0.00145 0.00138 0.00162 0.00089 C7 0.22390 0.26627 0.87939 1.00000 0.02183 0.02727 0.02041 0.00303 0.00388 0.00057 0.02306 0.00610 0.00048 0.00017 0.00025 0.00000 0.00182 0.00196 0.00173 0.00147 0.00124 0.00157 0.00076 H7A 0.14091 0.27925 0.93312 1.00000 0.02767 0.00000 0.00000 H7B 0.14762 0.27603 0.81245 1.00000 0.02767 0.00000 0.00000 C8 0.41125 0.30749 0.89073 1.00000 0.02280 0.01853 0.01838 -0.00043 0.00549 0.00041 0.01966 0.00628 0.00056 0.00016 0.00024 0.00000 0.00215 0.00189 0.00169 0.00138 0.00141 0.00155 0.00083 C9 0.40607 0.37478 0.89111 1.00000 0.02401 0.02781 0.02220 -0.00191 0.00363 -0.00110 0.02460 0.00598 0.00048 0.00016 0.00024 0.00000 0.00208 0.00220 0.00180 0.00167 0.00139 0.00176 0.00084 C10 0.21771 0.41427 0.87929 1.00000 0.03077 0.02840 0.03259 -0.00123 0.00577 0.00547 0.03042 0.00648 0.00054 0.00017 0.00028 0.00000 0.00208 0.00201 0.00202 0.00161 0.00149 0.00175 0.00086 H10A 0.22352 0.44831 0.93269 1.00000 0.04564 0.00000 0.00000 H10B 0.10487 0.38464 0.88527 1.00000 0.04564 0.00000 0.00000 H10C 0.20138 0.43572 0.81216 1.00000 0.04564 0.00000 0.00000 C11 0.60439 0.27650 0.89442 1.00000 0.02438 0.02329 0.02361 0.00061 0.00440 0.00311 0.02363 0.00628 0.00049 0.00018 0.00024 0.00000 0.00214 0.00192 0.00181 0.00157 0.00132 0.00166 0.00079 O4 0.33655 0.16793 0.62783 1.00000 0.02249 0.02165 0.03669 -0.00088 0.00442 -0.00482 0.02687 0.00375 0.00030 0.00011 0.00016 0.00000 0.00147 0.00136 0.00146 0.00113 0.00101 0.00109 0.00059 O5 0.19812 0.26613 0.61888 1.00000 0.01738 0.03317 0.03769 -0.00220 0.00276 0.00279 0.02945 0.00394 0.00031 0.00012 0.00017 0.00000 0.00126 0.00155 0.00154 0.00111 0.00101 0.00109 0.00060 O6 0.39881 0.37176 0.63030 1.00000 0.02594 0.02689 0.04444 -0.00224 0.00218 0.00497 0.03257 0.00458 0.00036 0.00011 0.00020 0.00000 0.00146 0.00146 0.00151 0.00122 0.00112 0.00115 0.00062 H6 0.29569 0.34828 0.62219 1.00000 0.04886 0.00000 0.00000 C12 0.50302 0.12598 0.63232 1.00000 0.02146 0.02497 0.02213 -0.00059 0.00151 -0.00125 0.02293 0.00626 0.00053 0.00019 0.00024 0.00000 0.00205 0.00192 0.00179 0.00154 0.00146 0.00172 0.00082 C13 0.46002 0.05904 0.62367 1.00000 0.02911 0.02402 0.02969 0.00052 0.00405 -0.01018 0.02756 0.00592 0.00050 0.00016 0.00025 0.00000 0.00210 0.00190 0.00196 0.00158 0.00146 0.00177 0.00085 H13 0.32614 0.04414 0.61429 1.00000 0.03307 0.00000 0.00000 C14 0.61540 0.01384 0.62888 1.00000 0.03765 0.02125 0.03289 -0.00091 0.00195 -0.00250 0.03076 0.00679 0.00057 0.00018 0.00028 0.00000 0.00239 0.00211 0.00210 0.00157 0.00159 0.00169 0.00092 H14 0.58885 -0.03246 0.62269 1.00000 0.03692 0.00000 0.00000 C15 0.80960 0.03660 0.64315 1.00000 0.02714 0.02870 0.04081 0.00403 -0.00261 0.00383 0.03273 0.00651 0.00057 0.00017 0.00028 0.00000 0.00229 0.00219 0.00209 0.00182 0.00158 0.00169 0.00092 H15 0.91644 0.00575 0.64804 1.00000 0.03928 0.00000 0.00000 C16 0.84851 0.10408 0.65032 1.00000 0.02312 0.02467 0.02909 -0.00125 0.00060 0.00154 0.02582 0.00666 0.00056 0.00017 0.00028 0.00000 0.00193 0.00209 0.00194 0.00151 0.00141 0.00160 0.00082 H16 0.98231 0.11907 0.65936 1.00000 0.03098 0.00000 0.00000 C17 0.69460 0.15044 0.64451 1.00000 0.02320 0.01874 0.01821 -0.00199 0.00261 0.00049 0.02004 0.00582 0.00051 0.00017 0.00024 0.00000 0.00200 0.00194 0.00165 0.00132 0.00125 0.00153 0.00078 C18 0.73710 0.22352 0.65441 1.00000 0.01712 0.02105 0.02398 -0.00260 0.00058 -0.00234 0.02086 0.00603 0.00052 0.00018 0.00025 0.00000 0.00200 0.00193 0.00193 0.00148 0.00133 0.00149 0.00080 H18A 0.82405 0.23681 0.60260 1.00000 0.02503 0.00000 0.00000 H18B 0.80940 0.23252 0.72260 1.00000 0.02503 0.00000 0.00000 C19 0.55084 0.26467 0.64082 1.00000 0.01691 0.02425 0.02043 -0.00256 0.00123 0.00014 0.02060 0.00596 0.00050 0.00017 0.00026 0.00000 0.00191 0.00192 0.00164 0.00138 0.00127 0.00147 0.00075 C20 0.55861 0.33244 0.64189 1.00000 0.01906 0.02785 0.02189 -0.00091 0.00431 -0.00046 0.02278 0.00626 0.00050 0.00018 0.00026 0.00000 0.00215 0.00224 0.00164 0.00153 0.00146 0.00171 0.00087 C21 0.74855 0.37059 0.65678 1.00000 0.03142 0.02345 0.03665 -0.00305 0.00296 -0.00609 0.03059 0.00615 0.00052 0.00018 0.00028 0.00000 0.00225 0.00203 0.00215 0.00161 0.00153 0.00165 0.00085 H21A 0.79910 0.37674 0.59078 1.00000 0.04588 0.00000 0.00000 H21B 0.84641 0.34597 0.70281 1.00000 0.04588 0.00000 0.00000 H21C 0.72492 0.41411 0.68651 1.00000 0.04588 0.00000 0.00000 C22 0.35843 0.23488 0.62866 1.00000 0.02377 0.02830 0.02085 0.00131 0.00495 0.00235 0.02412 0.00663 0.00055 0.00018 0.00025 0.00000 0.00211 0.00211 0.00183 0.00159 0.00140 0.00171 0.00084 Final Structure Factor Calculation for 02SRC410 in Cc Total number of l.s. parameters = 257 Maximum vector length = 511 Memory required = 2915 / 24024 wR2 = 0.1236 before cycle 11 for 2969 data and 2 / 257 parameters GooF = S = 1.044; Restrained GooF = 1.043 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0670 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0503 for 2319 Fo > 4sig(Fo) and 0.0731 for all 2969 data wR2 = 0.1236, GooF = S = 1.044, Restrained GooF = 1.043 for all data Flack x parameter = 1.9553 with su 1.2772 Expected values are 0 (within 3 su's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 28.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0369 0.0241 0.0162 O1 0.0411 0.0321 0.0173 O2 0.0512 0.0302 0.0230 O3 0.0242 0.0210 0.0149 C1 0.0301 0.0264 0.0244 C2 0.0406 0.0314 0.0199 C3 0.0387 0.0312 0.0204 C4 0.0379 0.0258 0.0184 C5 0.0322 0.0174 0.0161 C6 0.0285 0.0221 0.0186 C7 0.0241 0.0187 0.0162 C8 0.0287 0.0238 0.0214 C9 0.0353 0.0329 0.0231 C10 0.0274 0.0230 0.0204 C11 0.0368 0.0267 0.0172 O4 0.0389 0.0326 0.0168 O5 0.0455 0.0309 0.0214 O6 0.0254 0.0230 0.0205 C12 0.0371 0.0297 0.0158 C13 0.0390 0.0325 0.0208 C14 0.0446 0.0318 0.0218 C15 0.0308 0.0246 0.0220 C16 0.0233 0.0205 0.0164 C17 0.0256 0.0215 0.0154 C18 0.0256 0.0194 0.0168 C19 0.0280 0.0225 0.0178 C20 0.0373 0.0346 0.0198 C21 0.0297 0.0235 0.0192 C22 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.018 0.027 0.036 0.046 0.057 0.069 0.088 0.113 0.176 1.000 Number in group 300. 303. 291. 306. 294. 286. 303. 295. 292. 299. GooF 0.942 0.968 1.029 0.971 1.093 1.026 1.131 1.074 0.951 1.218 K 1.141 1.018 1.018 0.977 0.984 1.004 0.999 0.974 1.018 1.028 Resolution(A) 0.84 0.87 0.91 0.95 1.01 1.07 1.15 1.27 1.45 1.81 inf Number in group 306. 304. 290. 299. 285. 304. 301. 287. 294. 299. GooF 0.957 1.074 1.025 1.011 1.008 1.052 0.959 1.012 1.074 1.237 K 1.048 1.020 0.994 1.009 1.019 1.052 1.045 1.038 1.046 0.986 R1 0.171 0.147 0.123 0.095 0.064 0.059 0.050 0.048 0.042 0.042 Recommended weighting scheme: WGHT 0.0670 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)/su Fc/Fc(max) Resolution(A) 6 12 2 54.52 0.95 3.91 0.004 0.91 7 1 -9 180.44 307.95 3.89 0.078 0.85 -1 5 -5 316.61 425.27 3.71 0.092 2.03 -2 10 -1 170.16 114.68 3.45 0.048 1.70 -6 14 0 306.19 196.69 3.44 0.062 0.88 5 11 5 283.78 406.29 3.37 0.090 0.97 5 13 4 206.72 316.59 3.30 0.079 0.95 5 11 -3 465.14 603.07 3.18 0.109 1.08 5 7 0 33.98 3.40 3.18 0.008 1.22 -1 3 10 -14.07 29.81 3.11 0.024 1.29 3 17 -2 69.82 160.89 3.11 0.056 1.04 3 11 -8 24.70 54.39 3.10 0.033 1.11 0 20 5 297.04 451.63 3.08 0.094 0.94 2 2 -2 206.75 261.00 3.08 0.072 3.00 3 7 6 436.26 571.48 3.04 0.106 1.32 4 18 0 -13.94 27.89 3.00 0.023 0.93 1 3 7 50.29 83.22 2.98 0.041 1.70 -5 13 2 65.64 98.87 2.95 0.044 1.02 -3 7 11 248.12 164.02 2.87 0.057 1.03 7 9 -2 84.16 129.81 2.85 0.051 0.89 -7 9 4 42.36 2.57 2.83 0.007 0.88 0 2 -6 163.37 208.71 2.78 0.064 2.13 -1 11 6 20.80 48.29 2.71 0.031 1.39 -4 6 -1 414.95 316.82 2.71 0.079 1.48 6 8 4 424.97 538.32 2.70 0.103 0.95 -4 10 -4 45.28 20.14 2.69 0.020 1.17 4 8 -2 153.55 111.72 2.68 0.047 1.40 -1 9 -12 52.37 108.95 2.65 0.046 0.96 6 8 5 279.14 364.52 2.64 0.085 0.92 0 2 -13 145.08 64.69 2.64 0.036 1.00 -1 9 -11 0.00 42.99 2.63 0.029 1.02 0 6 5 597.90 740.83 2.63 0.121 2.06 4 2 -6 13.70 34.91 2.62 0.026 1.40 -5 11 -1 450.28 558.49 2.59 0.105 1.07 -1 3 -6 92.44 124.80 2.58 0.050 1.93 3 17 7 70.64 146.29 2.58 0.054 0.89 5 11 6 283.65 405.33 2.58 0.090 0.94 6 4 0 -13.39 20.97 2.57 0.020 1.10 3 9 -2 111.76 73.29 2.56 0.038 1.57 -6 10 -3 27.65 52.27 2.55 0.032 0.94 -4 14 -3 939.47 771.17 2.54 0.123 1.04 -6 12 5 -13.80 20.84 2.51 0.020 0.91 0 10 -1 407.60 330.46 2.51 0.081 1.99 1 5 5 315.48 426.17 2.49 0.092 2.03 2 0 -6 512.78 634.70 2.49 0.112 1.94 3 17 1 25.10 83.39 2.48 0.041 1.04 -5 13 -1 82.58 110.68 2.47 0.047 1.01 0 4 4 1592.84 1959.59 2.45 0.197 2.75 -4 8 -11 69.35 12.98 2.44 0.016 0.87 -1 17 -10 483.40 335.75 2.42 0.081 0.86 Bond lengths and angles O1 - Distance Angles C11 1.3685 (0.0041) C1 1.4028 (0.0040) 121.27 (0.26) O1 - C11 O2 - Distance Angles C11 1.2262 (0.0042) O2 - O3 - Distance Angles C9 1.3291 (0.0041) H3O 0.8400 109.47 O3 - C9 C1 - Distance Angles C6 1.3804 (0.0048) C2 1.3827 (0.0045) 123.00 (0.33) O1 1.4028 (0.0040) 121.72 (0.30) 115.27 (0.28) C1 - C6 C2 C2 - Distance Angles C3 1.3730 (0.0049) C1 1.3827 (0.0045) 119.27 (0.35) H2 0.9500 120.36 120.36 C2 - C3 C1 C3 - Distance Angles C2 1.3730 (0.0049) C4 1.3922 (0.0051) 119.83 (0.34) H3 0.9500 120.09 120.09 C3 - C2 C4 C4 - Distance Angles C5 1.3804 (0.0053) C3 1.3922 (0.0051) 119.88 (0.34) H4 0.9500 120.06 120.06 C4 - C5 C3 C5 - Distance Angles C4 1.3804 (0.0053) C6 1.4035 (0.0049) 121.44 (0.32) H5 0.9500 119.28 119.28 C5 - C4 C6 C6 - Distance Angles C1 1.3804 (0.0048) C5 1.4035 (0.0049) 116.57 (0.30) C7 1.4933 (0.0043) 122.10 (0.35) 121.33 (0.31) C6 - C1 C5 C7 - Distance Angles C6 1.4933 (0.0043) C8 1.5093 (0.0048) 112.92 (0.30) H7A 0.9900 109.00 109.00 H7B 0.9900 109.00 109.00 107.79 C7 - C6 C8 H7A C8 - Distance Angles C9 1.3538 (0.0042) C11 1.4455 (0.0049) 117.04 (0.32) C7 1.5093 (0.0048) 121.84 (0.34) 120.97 (0.31) C8 - C9 C11 C9 - Distance Angles O3 1.3291 (0.0040) C8 1.3538 (0.0042) 123.62 (0.30) C10 1.4961 (0.0047) 112.84 (0.30) 123.53 (0.33) C9 - O3 C8 C10 - Distance Angles C9 1.4961 (0.0047) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B C11 - Distance Angles O2 1.2262 (0.0041) O1 1.3685 (0.0041) 114.63 (0.29) C8 1.4455 (0.0049) 125.18 (0.34) 120.17 (0.30) C11 - O2 O1 O4 - Distance Angles C22 1.3544 (0.0042) C12 1.4046 (0.0042) 120.67 (0.25) O4 - C22 O5 - Distance Angles C22 1.2489 (0.0042) O5 - O6 - Distance Angles C20 1.3355 (0.0041) H6 0.8400 109.47 O6 - C20 C12 - Distance Angles C13 1.3794 (0.0046) C17 1.3803 (0.0051) 122.98 (0.35) O4 1.4046 (0.0042) 114.95 (0.30) 122.07 (0.32) C12 - C13 C17 C13 - Distance Angles C12 1.3794 (0.0046) C14 1.3868 (0.0049) 118.93 (0.32) H13 0.9500 120.54 120.54 C13 - C12 C14 C14 - Distance Angles C15 1.3856 (0.0053) C13 1.3868 (0.0049) 119.61 (0.33) H14 0.9500 120.20 120.20 C14 - C15 C13 C15 - Distance Angles C16 1.3835 (0.0046) C14 1.3856 (0.0053) 120.26 (0.36) H15 0.9500 119.87 119.87 C15 - C16 C14 C16 - Distance Angles C15 1.3835 (0.0046) C17 1.3947 (0.0047) 121.10 (0.34) H16 0.9500 119.45 119.45 C16 - C15 C17 C17 - Distance Angles C12 1.3803 (0.0051) C16 1.3947 (0.0047) 117.10 (0.31) C18 1.5003 (0.0045) 121.85 (0.33) 121.02 (0.31) C17 - C12 C16 C18 - Distance Angles C17 1.5003 (0.0045) C19 1.5028 (0.0048) 112.27 (0.29) H18A 0.9900 109.15 109.15 H18B 0.9900 109.15 109.15 107.87 C18 - C17 C19 H18A C19 - Distance Angles C20 1.3638 (0.0044) C22 1.4271 (0.0049) 117.02 (0.30) C18 1.5028 (0.0048) 121.21 (0.28) 121.75 (0.31) C19 - C20 C22 C20 - Distance Angles O6 1.3355 (0.0041) C19 1.3638 (0.0044) 124.11 (0.29) C21 1.4919 (0.0049) 112.73 (0.31) 123.15 (0.31) C20 - O6 C19 C21 - Distance Angles C20 1.4919 (0.0049) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - C20 H21A H21B C22 - Distance Angles O5 1.2489 (0.0042) O4 1.3544 (0.0042) 113.97 (0.31) C19 1.4271 (0.0049) 124.96 (0.33) 121.07 (0.30) C22 - O5 O4 Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) ** No suitable H-bond found for O3...O3 = 0.000(7) A ** 0.84 1.78 2.518(3) 145.8 O6-H6...O5 FMAP and GRID set by program FMAP 2 1 17 GRID -3.571 -1 -2 3.571 1 2 R1 = 0.0614 for 1570 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.25 at 0.4270 0.3021 0.8878 [ 0.16 A from C8 ] Deepest hole -0.29 at 0.0674 0.3427 0.3948 [ 0.80 A from C1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3220 / 28393 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.2059 0.1682 0.9012 1.00000 0.05 0.20 1.27 H5 1.43 O1 2.03 H2 2.20 C5 Q2 1 -0.0712 0.3554 0.8950 1.00000 0.05 0.20 1.35 H10B 1.50 O2 1.90 H3O 2.12 H7A Q3 1 0.8670 0.4109 0.9002 1.00000 0.05 0.20 1.42 H3O 1.73 H10B 1.99 H3 2.03 O3 Q4 1 1.0730 0.1487 0.6391 1.00000 0.05 0.19 0.92 H16 1.79 C16 1.85 O4 2.46 H18A Q5 1 0.5655 0.4145 0.8213 1.00000 0.05 0.18 1.04 O3 1.31 H3O 1.70 C9 2.19 H21C Q6 1 -0.1595 0.1097 0.8955 1.00000 0.05 0.18 1.42 H5 1.55 H2 1.81 H4 1.98 C5 Q7 1 0.0111 0.3135 0.6188 1.00000 0.05 0.17 1.59 O5 1.79 H21B 1.92 H21A 1.99 H18A Q8 1 1.0770 -0.0224 0.6407 1.00000 0.05 0.17 1.24 H15 1.69 H21C 2.17 C15 2.21 H13 Q9 1 -0.0853 0.0171 0.8917 1.00000 0.05 0.17 1.05 H4 2.00 C4 2.01 H10A 2.34 O3 Q10 1 0.6029 0.1409 0.6266 1.00000 0.05 0.16 0.67 C17 0.75 C12 1.82 C16 1.89 O4 Q11 1 -0.0340 0.2397 0.9026 1.00000 0.05 0.16 1.45 H7A 1.56 H5 1.89 C7 1.92 O2 Q12 1 -0.0437 0.1818 0.9045 1.00000 0.05 0.16 0.47 H5 1.28 C5 2.14 C6 2.33 O1 Q13 1 0.1833 0.0615 0.6227 1.00000 0.05 0.16 1.05 H13 1.87 C13 1.89 H16 2.19 H15 Q14 1 0.8649 0.2468 0.6535 1.00000 0.05 0.16 0.72 H18A 0.99 C18 1.07 H18B 2.11 H21B Q15 1 0.6114 0.0853 0.8417 1.00000 0.05 0.15 0.77 H2 1.18 C2 2.12 C1 2.14 C3 Q16 1 0.2023 0.0687 0.6431 1.00000 0.05 0.15 1.08 H13 1.81 C13 1.84 H16 2.21 O4 Q17 1 0.2023 0.3380 0.6241 1.00000 0.05 0.14 0.67 H6 1.45 O5 1.49 O6 2.33 C22 Q18 1 0.3813 0.4502 0.8893 1.00000 0.05 0.14 1.27 H10A 1.32 C10 1.46 O3 1.52 H10C Q19 1 0.7571 0.4478 0.6341 1.00000 0.05 0.14 1.01 H21C 1.58 H21A 1.58 C21 2.02 H13 Q20 1 0.0348 0.3077 0.8829 1.00000 0.05 0.13 1.08 H7A 1.42 H7B 1.53 C7 1.62 H10B Q21 1 0.9966 0.1922 0.6237 1.00000 0.05 0.13 1.47 H18A 1.55 H16 1.95 C18 2.03 O5 Q22 1 1.0259 0.1988 0.6439 1.00000 0.05 0.13 1.61 H18A 1.65 H16 1.84 O5 2.01 H18B Q23 1 0.4548 0.0110 0.9380 1.00000 0.05 0.13 0.77 H3 1.29 C3 1.90 C2 1.98 H2 Q24 1 0.6448 -0.0523 0.6411 1.00000 0.05 0.13 0.58 H14 1.35 C14 2.11 C15 2.17 H15 Q25 1 0.0611 0.2150 0.6608 1.00000 0.05 0.13 1.53 O5 1.75 H18A 2.00 H16 2.01 H18B Shortest distances between peaks (including symmetry equivalents) 13 16 0.32 21 22 0.34 22 25 0.45 21 25 0.77 4 21 1.02 4 22 1.06 1 12 1.13 11 12 1.16 2 3 1.20 2 20 1.22 1 6 1.22 9 18 1.36 4 25 1.37 8 19 1.37 7 17 1.38 14 25 1.47 14 22 1.47 11 20 1.48 14 21 1.50 6 12 1.65 6 15 1.70 7 14 1.76 5 18 1.77 4 16 1.83 1 11 1.85 8 13 1.86 4 13 1.93 6 9 1.93 8 16 2.02 7 25 2.07 3 23 2.14 1 15 2.17 3 5 2.18 17 24 2.26 15 23 2.30 7 22 2.33 13 19 2.34 2 11 2.34 3 20 2.39 7 21 2.44 4 14 2.45 16 19 2.47 9 15 2.50 5 9 2.53 12 20 2.61 19 24 2.62 5 8 2.71 17 25 2.72 6 11 2.75 10 14 2.77 2 5 2.80 16 21 2.84 7 24 2.85 10 21 2.86 16 22 2.88 13 21 2.92 23 24 2.95 13 22 2.98 8 24 2.99 14 17 2.99 5 19 3.00 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.33: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.31: Structure factors and derivatives 2.59: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.42: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:45:53 Total CPU time: 4.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++