+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0217 started at 11:17:32 on 02-Mar-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0217 in P-1 CELL 0.71073 8.7992 9.0108 9.3873 73.957 78.099 63.845 ZERR 2.00 0.0003 0.0002 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H B N O UNIT 8 28 10 2 22 V = 638.99 F(000) = 316.0 Mu = 0.15 mm-1 Cell Wt = 612.42 Rho = 1.592 MERG 2 OMIT -3.00 55.00 OMIT -1 0 1 OMIT 1 1 1 SHEL 7 0.77 eqiv $1 -x+1, -y+2, -z+1 eqiv $2 x+1, y-1, z eqiv $3 -x+1, -y+2, -z eqiv $4 -x, -y+2, -z+1 eqiv $5 -x+1, -y+1, -z+1 HTAB O7 O1_$1 HTAB O8 O10_$2 HTAB O9 O4_$3 HTAB O10 O6_$4 HTAB N11 O3_$5 HTAB N11 O7 FMAP 2 PLAN 5 SIZE 0.04 0.17 0.22 ACTA BOND $H WGHT 0.01880 0.46660 L.S. 8 TEMP -153.00 FVAR 1.08753 MOLE 1 B1 3 0.341579 0.888488 0.305472 11.00000 0.01152 0.01122 = 0.01366 -0.00203 -0.00127 -0.00333 B2 3 0.585188 0.767296 0.457047 11.00000 0.01307 0.01352 = 0.01400 -0.00213 -0.00042 -0.00485 B3 3 0.544004 0.589601 0.336698 11.00000 0.01429 0.01422 = 0.01270 -0.00158 0.00115 -0.00637 B4 3 0.281236 1.145489 0.106967 11.00000 0.01459 0.01386 = 0.01563 -0.00414 -0.00148 -0.00545 B5 3 0.073600 1.140081 0.313709 11.00000 0.01269 0.01436 = 0.01358 -0.00374 -0.00253 -0.00385 O1 5 0.444650 0.900817 0.404650 11.00000 0.01529 0.01219 = 0.01856 -0.00401 -0.00592 -0.00271 O2 5 0.645290 0.614927 0.414255 11.00000 0.01316 0.01278 = 0.01900 -0.00455 -0.00389 -0.00164 O3 5 0.386449 0.711957 0.305205 11.00000 0.01331 0.01057 = 0.01578 -0.00280 -0.00189 -0.00345 O4 5 0.372512 0.976299 0.154089 11.00000 0.01421 0.01274 = 0.01418 -0.00187 0.00091 -0.00372 O5 5 0.137064 1.231719 0.194428 11.00000 0.01616 0.01163 = 0.01468 -0.00225 0.00104 -0.00365 O6 5 0.162174 0.969916 0.361796 11.00000 0.01145 0.01227 = 0.01366 -0.00148 -0.00032 -0.00279 O7 5 0.677081 0.777147 0.552368 11.00000 0.01853 0.01352 = 0.02305 -0.00554 -0.00790 -0.00251 AFIX 147 H7 2 0.633929 0.875633 0.568071 11.00000 -1.50000 AFIX 0 O8 5 0.596971 0.440328 0.295479 11.00000 0.01370 0.01234 = 0.02341 -0.00560 -0.00389 -0.00156 AFIX 147 H8 2 0.696818 0.378167 0.317540 11.00000 -1.50000 AFIX 0 O9 5 0.332049 1.234958 -0.019366 11.00000 0.01894 0.01372 = 0.01814 -0.00270 0.00478 -0.00381 AFIX 147 H9 2 0.424260 1.170785 -0.058067 11.00000 -1.50000 AFIX 0 O10 5 -0.082498 1.222759 0.382887 11.00000 0.01475 0.01502 = 0.01703 0.00086 0.00195 -0.00190 AFIX 147 H10 2 -0.101643 1.157347 0.460443 11.00000 -1.50000 AFIX 0 MOLE 2 C11 1 1.064221 0.184996 0.796292 11.00000 0.01835 0.01997 = 0.02472 -0.00476 -0.00363 -0.00465 AFIX 23 H11A 2 1.018752 0.120874 0.759881 11.00000 -1.20000 H11B 2 1.189533 0.135379 0.774694 11.00000 -1.20000 AFIX 0 C12 1 0.992819 0.368059 0.714310 11.00000 0.01530 0.02214 = 0.02410 -0.00152 -0.00090 -0.00665 AFIX 23 H12A 2 1.045212 0.431080 0.743611 11.00000 -1.20000 H12B 2 1.019305 0.374814 0.605567 11.00000 -1.20000 AFIX 0 C13 1 0.760778 0.421458 0.916843 11.00000 0.02432 0.01960 = 0.02329 -0.00707 0.00231 -0.00695 AFIX 23 H13A 2 0.635733 0.465030 0.940201 11.00000 -1.20000 H13B 2 0.803122 0.485150 0.957327 11.00000 -1.20000 AFIX 0 C14 1 0.842220 0.234580 0.986572 11.00000 0.02535 0.02106 = 0.01963 -0.00240 -0.00227 -0.00955 AFIX 23 H14A 2 0.814961 0.217663 1.096003 11.00000 -1.20000 H14B 2 0.795275 0.172456 0.949122 11.00000 -1.20000 AFIX 0 N11 4 0.804935 0.444294 0.752011 11.00000 0.01690 0.01371 = 0.02325 -0.00145 -0.00482 -0.00554 AFIX 23 H11C 2 0.755632 0.394138 0.713926 11.00000 -1.20000 H11D 2 0.762144 0.557839 0.708985 11.00000 -1.20000 AFIX 0 O11 5 1.022126 0.169009 0.951858 11.00000 0.02211 0.02194 = 0.02285 -0.00124 -0.00893 -0.00706 HKLF 4 Covalent radii and connectivity table for 2007src0217 in P-1 C 0.770 H 0.320 B 0.820 N 0.700 O 0.660 B1 - O4 O3 O6 O1 B2 - O1 O7 O2 B3 - O8 O3 O2 B4 - O9 O4 O5 B5 - O10 O6 O5 O1 - B2 B1 O2 - B2 B3 O3 - B3 B1 O4 - B4 B1 O5 - B5 B4 O6 - B5 B1 O7 - B2 O8 - B3 O9 - B4 O10 - B5 C11 - O11 C12 C12 - N11 C11 C13 - N11 C14 C14 - O11 C13 N11 - C12 C13 O11 - C11 C14 Operators for generating equivalent atoms: $1 -x+1, -y+2, -z+1 $2 x+1, y-1, z $3 -x+1, -y+2, -z $4 -x, -y+2, -z+1 $5 -x+1, -y+1, -z+1 11719 Reflections read, of which 26 rejected -11 =< h =< 11, -11 =< k =< 11, -12 =< l =< 12, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2921 Unique reflections, of which 0 suppressed R(int) = 0.0354 R(sigma) = 0.0326 Friedel opposites merged Maximum memory for data reduction = 2112 / 29520 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 = 2636 / 241588 wR2 = 0.0865 before cycle 1 for 2921 data and 194 / 194 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0188 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.08796 0.00171 0.250 OSF Mean shift/esd = 0.026 Maximum = 0.250 for OSF Max. shift = 0.001 A for H8 Max. dU = 0.000 for C11 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2636 / 241588 wR2 = 0.0865 before cycle 2 for 2921 data and 194 / 194 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0188 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.08801 0.00171 0.031 OSF Mean shift/esd = 0.009 Maximum = 0.039 for tors H8 Max. shift = 0.001 A for H8 Max. dU = 0.000 for C11 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2636 / 241588 wR2 = 0.0865 before cycle 3 for 2921 data and 194 / 194 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0188 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.08801 0.00171 0.002 OSF Mean shift/esd = 0.001 Maximum = 0.010 for tors H8 Max. shift = 0.000 A for H8 Max. dU = 0.000 for C11 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2636 / 241588 wR2 = 0.0865 before cycle 4 for 2921 data and 194 / 194 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0188 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.08802 0.00171 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.002 for tors H8 Max. shift = 0.000 A for H8 Max. dU = 0.000 for O8 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2636 / 241588 wR2 = 0.0865 before cycle 5 for 2921 data and 194 / 194 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0188 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.08802 0.00171 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H8 Max. shift = 0.000 A for H8 Max. dU = 0.000 for N11 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2636 / 241588 wR2 = 0.0865 before cycle 6 for 2921 data and 194 / 194 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0188 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.08801 0.00171 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O10 Max. shift = 0.000 A for H8 Max. dU = 0.000 for N11 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2636 / 241588 wR2 = 0.0865 before cycle 7 for 2921 data and 194 / 194 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0188 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.08801 0.00171 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O10 Max. shift = 0.000 A for H7 Max. dU = 0.000 for C13 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2636 / 241588 wR2 = 0.0865 before cycle 8 for 2921 data and 194 / 194 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0188 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.08801 0.00171 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O10 Max. shift = 0.000 A for H8 Max. dU = 0.000 for B4 Largest correlation matrix elements -0.525 U12 B3 / U11 B3 -0.514 U12 C14 / U11 C14 -0.506 U12 C12 / U11 C12 -0.517 U12 B3 / U22 B3 -0.511 U12 B4 / U22 B4 -0.506 U12 B2 / U22 B2 -0.516 U12 B4 / U11 B4 -0.510 U12 B2 / U11 B2 -0.505 U12 B1 / U11 B1 -0.516 U12 C14 / U22 C14 -0.508 U12 N11 / U11 N11 -0.503 U12 O11 / U11 O11 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H7 0.6340 0.8756 0.5680 147 0.840 0.000 O7 B2 H7 H8 0.6967 0.3781 0.3178 147 0.840 0.000 O8 B3 H8 H9 0.4242 1.1708 -0.0581 147 0.840 0.000 O9 B4 H9 H10 -0.1016 1.1574 0.4605 147 0.840 0.000 O10 B5 H10 H11A 1.0187 0.1209 0.7599 23 0.990 0.000 C11 O11 C12 H11B 1.1895 0.1354 0.7747 23 0.990 0.000 C11 O11 C12 H12A 1.0452 0.4311 0.7436 23 0.990 0.000 C12 N11 C11 H12B 1.0193 0.3748 0.6056 23 0.990 0.000 C12 N11 C11 H13A 0.6357 0.4650 0.9402 23 0.990 0.000 C13 N11 C14 H13B 0.8031 0.4851 0.9573 23 0.990 0.000 C13 N11 C14 H14A 0.8149 0.2177 1.0960 23 0.990 0.000 C14 O11 C13 H14B 0.7953 0.1725 0.9491 23 0.990 0.000 C14 O11 C13 H11C 0.7556 0.3942 0.7139 23 0.920 0.000 N11 C12 C13 H11D 0.7622 0.5578 0.7090 23 0.920 0.000 N11 C12 C13 2007src0217 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq B1 0.34157 0.88849 0.30547 1.00000 0.01153 0.01127 0.01368 -0.00206 -0.00127 -0.00335 0.01277 0.00209 0.00019 0.00019 0.00017 0.00000 0.00069 0.00068 0.00071 0.00055 0.00055 0.00056 0.00029 B2 0.58518 0.76730 0.45705 1.00000 0.01310 0.01360 0.01399 -0.00212 -0.00041 -0.00491 0.01408 0.00213 0.00019 0.00019 0.00017 0.00000 0.00070 0.00072 0.00072 0.00057 0.00056 0.00059 0.00030 B3 0.54399 0.58961 0.33670 1.00000 0.01432 0.01424 0.01269 -0.00157 0.00116 -0.00639 0.01422 0.00216 0.00020 0.00020 0.00017 0.00000 0.00072 0.00072 0.00071 0.00057 0.00056 0.00060 0.00030 B4 0.28124 1.14548 0.10697 1.00000 0.01462 0.01393 0.01564 -0.00415 -0.00150 -0.00550 0.01462 0.00210 0.00020 0.00020 0.00017 0.00000 0.00072 0.00073 0.00075 0.00058 0.00058 0.00060 0.00031 B5 0.07361 1.14006 0.31371 1.00000 0.01271 0.01444 0.01361 -0.00376 -0.00256 -0.00388 0.01383 0.00207 0.00019 0.00020 0.00017 0.00000 0.00070 0.00072 0.00071 0.00057 0.00056 0.00058 0.00030 O1 0.44465 0.90081 0.40466 1.00000 0.01529 0.01220 0.01856 -0.00399 -0.00592 -0.00273 0.01558 0.00130 0.00012 0.00012 0.00011 0.00000 0.00048 0.00046 0.00050 0.00038 0.00039 0.00039 0.00021 O2 0.64529 0.61493 0.41426 1.00000 0.01317 0.01279 0.01900 -0.00454 -0.00390 -0.00165 0.01572 0.00131 0.00012 0.00012 0.00011 0.00000 0.00047 0.00047 0.00051 0.00039 0.00038 0.00038 0.00021 O3 0.38646 0.71196 0.30520 1.00000 0.01331 0.01059 0.01580 -0.00281 -0.00188 -0.00346 0.01368 0.00128 0.00012 0.00011 0.00011 0.00000 0.00046 0.00046 0.00048 0.00037 0.00037 0.00037 0.00021 O4 0.37251 0.97630 0.15408 1.00000 0.01421 0.01276 0.01418 -0.00189 0.00093 -0.00374 0.01496 0.00133 0.00012 0.00012 0.00010 0.00000 0.00047 0.00047 0.00048 0.00037 0.00037 0.00038 0.00021 O5 0.13706 1.23173 0.19442 1.00000 0.01617 0.01164 0.01469 -0.00225 0.00106 -0.00367 0.01545 0.00135 0.00012 0.00012 0.00011 0.00000 0.00048 0.00046 0.00048 0.00037 0.00038 0.00039 0.00021 O6 0.16218 0.96992 0.36179 1.00000 0.01146 0.01227 0.01368 -0.00148 -0.00032 -0.00280 0.01366 0.00129 0.00012 0.00012 0.00010 0.00000 0.00045 0.00046 0.00047 0.00036 0.00036 0.00037 0.00020 O7 0.67708 0.77714 0.55237 1.00000 0.01854 0.01352 0.02307 -0.00555 -0.00792 -0.00250 0.01857 0.00134 0.00013 0.00012 0.00012 0.00000 0.00052 0.00049 0.00054 0.00041 0.00042 0.00041 0.00023 H7 0.63398 0.87564 0.56803 1.00000 0.02786 0.00000 0.00000 O8 0.59696 0.44033 0.29548 1.00000 0.01371 0.01235 0.02342 -0.00558 -0.00390 -0.00155 0.01717 0.00134 0.00012 0.00012 0.00011 0.00000 0.00048 0.00047 0.00054 0.00040 0.00040 0.00039 0.00022 H8 0.69671 0.37806 0.31775 1.00000 0.02576 0.00000 0.00000 O9 0.33204 1.23496 -0.01936 1.00000 0.01893 0.01374 0.01818 -0.00273 0.00480 -0.00383 0.01922 0.00149 0.00013 0.00012 0.00011 0.00000 0.00052 0.00049 0.00052 0.00040 0.00041 0.00041 0.00023 H9 0.42418 1.17077 -0.05814 1.00000 0.02883 0.00000 0.00000 O10 -0.08250 1.22276 0.38288 1.00000 0.01479 0.01505 0.01703 0.00086 0.00196 -0.00192 0.01869 0.00149 0.00012 0.00012 0.00011 0.00000 0.00049 0.00050 0.00052 0.00039 0.00039 0.00040 0.00023 H10 -0.10160 1.15740 0.46049 1.00000 0.02803 0.00000 0.00000 C11 1.06422 0.18499 0.79628 1.00000 0.01836 0.02004 0.02476 -0.00480 -0.00361 -0.00467 0.02198 0.00215 0.00019 0.00019 0.00017 0.00000 0.00072 0.00074 0.00079 0.00061 0.00060 0.00060 0.00032 H11A 1.01873 0.12089 0.75987 1.00000 0.02638 0.00000 0.00000 H11B 1.18953 0.13537 0.77468 1.00000 0.02638 0.00000 0.00000 C12 0.99283 0.36805 0.71432 1.00000 0.01529 0.02220 0.02414 -0.00156 -0.00089 -0.00666 0.02182 0.00222 0.00018 0.00019 0.00018 0.00000 0.00069 0.00075 0.00078 0.00061 0.00058 0.00060 0.00032 H12A 1.04523 0.43106 0.74363 1.00000 0.02618 0.00000 0.00000 H12B 1.01932 0.37481 0.60557 1.00000 0.02618 0.00000 0.00000 C13 0.76078 0.42146 0.91684 1.00000 0.02435 0.01962 0.02332 -0.00708 0.00234 -0.00698 0.02337 0.00225 0.00020 0.00019 0.00017 0.00000 0.00077 0.00074 0.00079 0.00061 0.00062 0.00063 0.00033 H13A 0.63574 0.46503 0.94020 1.00000 0.02805 0.00000 0.00000 H13B 0.80313 0.48515 0.95733 1.00000 0.02805 0.00000 0.00000 C14 0.84221 0.23459 0.98658 1.00000 0.02538 0.02110 0.01965 -0.00243 -0.00224 -0.00956 0.02242 0.00217 0.00020 0.00019 0.00017 0.00000 0.00079 0.00076 0.00075 0.00060 0.00061 0.00064 0.00032 H14A 0.81495 0.21768 1.09601 1.00000 0.02690 0.00000 0.00000 H14B 0.79526 0.17246 0.94913 1.00000 0.02690 0.00000 0.00000 N11 0.80494 0.44430 0.75201 1.00000 0.01690 0.01372 0.02329 -0.00146 -0.00483 -0.00555 0.01831 0.00168 0.00015 0.00015 0.00014 0.00000 0.00060 0.00057 0.00065 0.00048 0.00049 0.00048 0.00026 H11C 0.75563 0.39415 0.71392 1.00000 0.02197 0.00000 0.00000 H11D 0.76215 0.55785 0.70899 1.00000 0.02197 0.00000 0.00000 O11 1.02213 0.16900 0.95186 1.00000 0.02212 0.02196 0.02287 -0.00124 -0.00893 -0.00708 0.02272 0.00145 0.00014 0.00013 0.00012 0.00000 0.00056 0.00055 0.00056 0.00043 0.00044 0.00045 0.00024 Final Structure Factor Calculation for 2007src0217 in P-1 Total number of l.s. parameters = 194 Maximum vector length = 511 Memory required = 2442 / 24017 wR2 = 0.0865 before cycle 9 for 2921 data and 0 / 194 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0188 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0385 for 2573 Fo > 4sig(Fo) and 0.0457 for all 2921 data wR2 = 0.0865, GooF = S = 1.066, Restrained GooF = 1.066 for all data Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0148 0.0131 0.0105 B1 0.0165 0.0131 0.0126 B2 0.0177 0.0146 0.0103 B3 0.0160 0.0147 0.0131 B4 0.0168 0.0130 0.0117 B5 0.0223 0.0133 0.0112 O1 0.0210 0.0158 0.0104 O2 0.0159 0.0148 0.0104 O3 0.0205 0.0125 0.0119 O4 0.0218 0.0131 0.0114 O5 0.0182 0.0125 0.0104 O6 0.0285 0.0148 0.0124 O7 0.0242 0.0171 0.0102 O8 0.0314 0.0142 0.0121 O9 0.0313 0.0128 0.0120 O10 0.0252 0.0240 0.0168 C11 0.0299 0.0204 0.0152 C12 0.0306 0.0227 0.0169 C13 0.0258 0.0229 0.0186 C14 0.0247 0.0168 0.0134 N11 0.0287 0.0245 0.0150 O11 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.023 0.034 0.047 0.062 0.079 0.097 0.128 0.192 1.000 Number in group 295. 311. 271. 299. 287. 303. 283. 289. 289. 294. GooF 1.161 1.098 1.139 1.053 0.980 1.040 1.032 1.062 0.951 1.125 K 2.128 1.038 1.044 0.975 0.990 0.994 1.005 0.999 1.009 1.004 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.04 1.15 1.32 1.66 inf Number in group 300. 287. 295. 298. 285. 288. 290. 296. 289. 293. GooF 1.081 1.217 1.028 0.988 1.006 0.968 0.922 0.820 1.085 1.428 K 1.048 1.040 1.033 1.012 0.998 0.994 0.992 0.989 1.015 1.003 R1 0.092 0.099 0.081 0.066 0.051 0.041 0.029 0.027 0.029 0.028 Recommended weighting scheme: WGHT 0.0179 0.4692 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) 3 6 0 7.77 0.06 5.04 0.002 1.44 -3 0 3 110.96 67.32 4.14 0.083 1.88 7 7 7 24.83 9.50 4.08 0.031 0.95 -3 1 0 17.86 7.95 3.98 0.028 2.23 0 -1 1 409.16 478.38 3.51 0.221 5.40 0 1 3 120.75 152.86 3.49 0.125 3.02 -1 -2 3 163.15 131.30 3.45 0.116 2.18 2 6 1 51.04 71.21 3.43 0.085 1.48 0 0 9 5.43 0.12 3.24 0.004 1.00 -4 -1 4 9.52 3.68 3.23 0.019 1.43 0 0 2 120.46 150.07 3.13 0.124 4.49 -1 9 6 1.43 10.68 3.12 0.033 0.80 3 1 3 73.81 55.77 3.07 0.075 2.29 1 1 2 1256.29 1382.97 2.96 0.376 4.42 5 5 7 2.44 8.26 2.94 0.029 1.13 6 -3 2 6.22 1.48 2.94 0.012 0.99 2 4 1 228.50 194.64 2.89 0.141 2.24 -7 1 4 4.31 11.59 2.88 0.034 0.93 8 5 8 13.21 4.78 2.85 0.022 0.88 -1 0 11 1.82 7.05 2.85 0.027 0.80 2 2 2 8445.96 9802.50 2.83 1.000 3.32 0 3 0 960.52 1058.00 2.82 0.329 2.64 0 8 0 51.99 69.02 2.79 0.084 0.99 3 3 5 186.04 157.28 2.74 0.127 1.69 2 1 0 588.75 653.01 2.71 0.258 4.28 2 0 4 188.39 219.69 2.69 0.150 2.04 0 -9 3 5.87 1.00 2.67 0.010 0.80 -5 2 6 4.34 0.11 2.66 0.003 0.97 0 -2 1 13.02 21.12 2.63 0.046 3.37 4 -7 1 7.04 1.36 2.63 0.012 0.83 0 6 7 8.26 15.22 2.61 0.039 1.03 1 2 0 1960.97 2119.80 2.59 0.465 4.31 0 -1 11 8.27 1.17 2.58 0.011 0.79 1 5 2 2697.31 2495.83 2.56 0.505 1.73 -3 -3 9 6.67 0.03 2.55 0.002 0.84 -6 2 5 37.37 50.66 2.55 0.072 0.94 2 -5 3 43.11 58.90 2.54 0.078 1.13 -4 -1 10 107.07 77.33 2.52 0.089 0.78 2 1 1 2629.81 2843.33 2.51 0.539 4.25 9 5 1 38.57 52.02 2.51 0.073 0.96 -2 -1 3 32.31 43.88 2.51 0.067 2.23 -4 -1 1 849.17 774.44 2.50 0.281 1.99 -2 9 1 7.65 2.44 2.46 0.016 0.80 4 11 2 -1.07 1.54 2.45 0.013 0.81 3 5 2 114.44 94.36 2.45 0.098 1.76 11 3 3 -1.76 1.70 2.44 0.013 0.78 -1 2 0 117.62 98.36 2.41 0.100 3.06 11 7 1 8.51 2.41 2.39 0.016 0.77 -3 -3 3 1104.59 1017.85 2.38 0.322 1.66 4 -5 6 47.96 68.26 2.37 0.083 0.82 Bond lengths and angles B1 - Distance Angles O4 1.4590 (0.0018) O3 1.4609 (0.0017) 108.96 (0.11) O6 1.4693 (0.0017) 110.29 (0.11) 110.35 (0.11) O1 1.4820 (0.0018) 109.24 (0.11) 110.87 (0.11) 107.12 (0.11) B1 - O4 O3 O6 B2 - Distance Angles O1 1.3530 (0.0018) O7 1.3667 (0.0018) 121.92 (0.13) O2 1.3796 (0.0018) 121.58 (0.13) 116.49 (0.12) B2 - O1 O7 B3 - Distance Angles O8 1.3553 (0.0018) O3 1.3660 (0.0018) 118.80 (0.13) O2 1.3840 (0.0018) 120.47 (0.13) 120.69 (0.12) B3 - O8 O3 B4 - Distance Angles O9 1.3517 (0.0018) O4 1.3635 (0.0018) 121.65 (0.13) O5 1.3933 (0.0018) 118.47 (0.13) 119.78 (0.13) B4 - O9 O4 B5 - Distance Angles O10 1.3641 (0.0018) O6 1.3678 (0.0018) 120.30 (0.13) O5 1.3731 (0.0018) 118.22 (0.13) 121.48 (0.13) B5 - O10 O6 O1 - Distance Angles B2 1.3530 (0.0018) B1 1.4820 (0.0018) 121.93 (0.11) O1 - B2 O2 - Distance Angles B2 1.3796 (0.0018) B3 1.3840 (0.0018) 118.69 (0.11) O2 - B2 O3 - Distance Angles B3 1.3660 (0.0018) B1 1.4609 (0.0017) 121.09 (0.11) O3 - B3 O4 - Distance Angles B4 1.3635 (0.0018) B1 1.4590 (0.0018) 121.32 (0.11) O4 - B4 O5 - Distance Angles B5 1.3731 (0.0018) B4 1.3933 (0.0018) 118.81 (0.11) O5 - B5 O6 - Distance Angles B5 1.3678 (0.0018) B1 1.4693 (0.0017) 119.58 (0.11) O6 - B5 O7 - Distance Angles B2 1.3667 (0.0018) H7 0.8400 109.47 O7 - B2 O8 - Distance Angles B3 1.3553 (0.0018) H8 0.8400 109.47 O8 - B3 O9 - Distance Angles B4 1.3517 (0.0018) H9 0.8400 109.47 O9 - B4 O10 - Distance Angles B5 1.3641 (0.0018) H10 0.8400 109.47 O10 - B5 C11 - Distance Angles O11 1.4137 (0.0019) C12 1.5139 (0.0021) 111.73 (0.12) H11A 0.9900 109.27 109.27 H11B 0.9900 109.27 109.27 107.94 C11 - O11 C12 H11A C12 - Distance Angles N11 1.4908 (0.0018) C11 1.5139 (0.0021) 109.11 (0.12) H12A 0.9900 109.86 109.86 H12B 0.9900 109.86 109.86 108.28 C12 - N11 C11 H12A C13 - Distance Angles N11 1.4946 (0.0019) C14 1.5159 (0.0021) 108.62 (0.12) H13A 0.9900 109.97 109.97 H13B 0.9900 109.97 109.97 108.35 C13 - N11 C14 H13A C14 - Distance Angles O11 1.4250 (0.0018) C13 1.5159 (0.0021) 110.73 (0.12) H14A 0.9900 109.50 109.50 H14B 0.9900 109.50 109.50 108.07 C14 - O11 C13 H14A N11 - Distance Angles C12 1.4908 (0.0018) C13 1.4946 (0.0019) 111.00 (0.12) H11C 0.9200 109.44 109.44 H11D 0.9200 109.44 109.44 108.04 N11 - C12 C13 H11C O11 - Distance Angles C11 1.4137 (0.0019) C14 1.4250 (0.0018) 110.48 (0.11) O11 - C11 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.89 2.7313(14) 174.9 O7-H7...O1_$1 0.84 1.93 2.7681(14) 174.9 O8-H8...O10_$2 0.84 1.92 2.7556(14) 176.9 O9-H9...O4_$3 0.84 1.87 2.7076(14) 174.5 O10-H10...O6_$4 0.92 1.94 2.8264(15) 162.1 N11-H11C...O3_$5 0.92 2.04 2.9259(16) 160.6 N11-H11D...O7 FMAP and GRID set by program FMAP 2 1 26 GRID -2.174 -2 -2 2.174 2 2 R1 = 0.0457 for 2921 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.0408 0.2770 0.7566 [ 0.76 A from C11 ] Deepest hole -0.23 at -0.0099 0.8731 0.7321 [ 0.84 A from B5 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2428 / 19764 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.0408 0.2770 0.7566 1.00000 0.05 0.28 0.76 C11 0.77 C12 1.37 H11B 1.38 H12A Q2 1 0.6034 0.6836 0.4388 1.00000 0.05 0.21 0.64 O2 0.76 B2 1.72 B3 1.82 O1 Q3 1 0.4486 0.6532 0.3580 1.00000 0.05 0.21 0.73 O3 0.80 B3 1.77 O2 1.87 B1 Q4 1 0.2467 0.9281 0.3401 1.00000 0.05 0.20 0.69 O6 0.79 B1 1.83 B5 1.85 O1 Q5 1 0.8094 0.3360 0.9475 1.00000 0.05 0.20 0.70 C13 0.82 C14 1.35 H13B 1.46 H13A Shortest distances between peaks (including symmetry equivalents) 2 3 1.84 3 4 2.31 1 5 2.39 Time profile in seconds ----------------------- 0.07: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.01: 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. 1.34: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.01: Generate idealized H-atoms 0.92: Structure factors and derivatives 1.64: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.36: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.01: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0217 finished at 11:18:10 Total CPU time: 4.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++