+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 18:01:14 on 02-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01src007 in P2(1)/c CELL 0.71073 10.579 17.772 10.1254 90 93.545 90 ZERR 2 0.002 0.004 0.0016 0 0.006 0 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 88 100 4 12 V = 1900.03 F(000) = 752.0 Mu = 0.08 mm-1 Cell Wt = 1405.72 Rho = 1.229 SHEL 7 0.9 TEMP -123 SIZE 0.2 0.1 0.05 FMAP 2 PLAN 20 L.S. 4 WGHT 0.036500 EXTI 0.003050 FVAR 0.38127 C1 1 0.485659 0.160987 1.407204 11.00000 0.09098 0.06839 = 0.03150 -0.00627 -0.00055 0.00641 C2 1 0.359102 0.132819 1.397803 11.00000 0.06259 0.08406 = 0.08354 0.00923 -0.00808 -0.01125 AFIX 43 H2 2 0.335729 0.093107 1.338411 11.00000 -1.20000 AFIX 0 C3 1 0.273279 0.163621 1.474803 11.00000 0.06808 0.11069 = 0.09700 0.00955 0.01677 0.00453 AFIX 43 H3 2 0.190777 0.142467 1.474224 11.00000 -1.20000 AFIX 0 C4 1 0.302650 0.226101 1.555760 11.00000 0.09438 0.10551 = 0.12542 -0.01073 0.00085 0.02506 AFIX 43 H4 2 0.237846 0.248911 1.602887 11.00000 -1.20000 AFIX 0 C5 1 0.420606 0.254261 1.567884 11.00000 0.09422 0.09620 = 0.10045 -0.01070 -0.00959 0.02083 AFIX 43 H5 2 0.440152 0.295089 1.626175 11.00000 -1.20000 AFIX 0 C6 1 0.516486 0.221929 1.491793 11.00000 0.08465 0.08488 = 0.04651 -0.00987 -0.00159 0.01451 C7 1 0.641162 0.252455 1.499152 11.00000 0.11366 0.06590 = 0.07682 -0.01149 -0.01631 -0.00338 AFIX 43 H7 2 0.659967 0.295532 1.552343 11.00000 -1.20000 AFIX 0 C8 1 0.734732 0.219802 1.429461 11.00000 0.09797 0.05292 = 0.06412 -0.00496 -0.01831 0.00351 C9 1 0.861708 0.247352 1.437351 11.00000 0.08268 0.08833 = 0.09852 -0.00945 -0.02835 -0.04020 AFIX 43 H9 2 0.884430 0.288568 1.493664 11.00000 -1.20000 AFIX 0 C10 1 0.949547 0.214770 1.364674 11.00000 0.06538 0.09479 = 0.13484 0.01921 0.00642 -0.00838 AFIX 43 H10 2 1.032115 0.235938 1.367018 11.00000 -1.20000 AFIX 0 C11 1 0.924178 0.151561 1.286596 11.00000 0.08314 0.08608 = 0.10167 0.00732 -0.00611 -0.00511 AFIX 43 H11 2 0.990049 0.128316 1.241658 11.00000 -1.20000 AFIX 0 C12 1 0.803715 0.122930 1.274742 11.00000 0.07178 0.09343 = 0.07556 0.01056 -0.01836 -0.00329 AFIX 43 H12 2 0.784554 0.080558 1.219906 11.00000 -1.20000 AFIX 0 C13 1 0.707389 0.158001 1.346423 11.00000 0.07164 0.07868 = 0.04609 0.00203 -0.00822 0.00128 C14 1 0.579760 0.130497 1.337100 11.00000 0.10392 0.05435 = 0.04189 -0.01390 -0.00707 0.00668 C15 1 0.553229 -0.001913 1.301447 11.00000 0.04572 0.11744 = 0.07004 -0.00771 -0.01164 0.00041 AFIX 23 H15A 2 0.512925 -0.002241 1.387120 11.00000 -1.20000 H15B 2 0.641691 -0.019524 1.316890 11.00000 -1.20000 AFIX 0 C16 1 0.482384 -0.053194 1.205339 11.00000 0.07108 0.11705 = 0.06904 -0.02190 -0.00516 -0.00203 AFIX 23 H16A 2 0.499452 -0.106235 1.230438 11.00000 -1.20000 H16B 2 0.511685 -0.045116 1.115443 11.00000 -1.20000 AFIX 0 C17 1 0.279689 -0.038864 1.070466 11.00000 0.07773 0.09491 = 0.04568 0.00559 0.00359 -0.01684 AFIX 23 H17A 2 0.204899 -0.072422 1.068439 11.00000 -1.20000 H17B 2 0.339028 -0.058456 1.006858 11.00000 -1.20000 AFIX 0 C18 1 0.239721 0.038369 1.032200 11.00000 0.08269 0.06637 = 0.06702 0.00261 -0.00155 0.01686 AFIX 23 H18A 2 0.180255 0.058534 1.095153 11.00000 -1.20000 H18B 2 0.314073 0.072176 1.031768 11.00000 -1.20000 AFIX 0 C19 1 0.139060 0.101417 0.853997 11.00000 0.07905 0.10825 = 0.07287 0.01326 -0.01648 0.01078 AFIX 23 H19A 2 0.213172 0.131970 0.832119 11.00000 -1.20000 H19B 2 0.093762 0.128759 0.921960 11.00000 -1.20000 AFIX 0 C20 1 0.051806 0.091040 0.731170 11.00000 0.08353 0.12670 = 0.08380 0.02097 -0.02022 0.01564 AFIX 23 H20A 2 0.043860 0.139212 0.682258 11.00000 -1.20000 H20B 2 0.088333 0.053283 0.672563 11.00000 -1.20000 AFIX 0 C21 1 -0.156626 0.058464 0.657508 11.00000 0.06641 0.15499 = 0.06564 0.01660 -0.01410 -0.01129 AFIX 23 H21A 2 -0.162877 0.004632 0.632823 11.00000 -1.20000 H21B 2 -0.131812 0.087166 0.579410 11.00000 -1.20000 AFIX 0 C22 1 0.284713 -0.086483 1.300297 11.00000 0.06050 0.09490 = 0.05689 0.00067 -0.01532 -0.00853 AFIX 23 H22A 2 0.343402 -0.091126 1.379902 11.00000 -1.20000 H22B 2 0.273434 -0.137290 1.261238 11.00000 -1.20000 AFIX 0 N1 3 0.342289 -0.037885 1.205088 11.00000 0.07995 0.07639 = 0.04323 0.02077 -0.00318 -0.02353 O1 4 0.551838 0.073334 1.247869 11.00000 0.07465 0.05595 = 0.06670 0.00703 -0.00487 -0.00424 O2 4 0.179574 0.032863 0.903589 11.00000 0.09193 0.09447 = 0.06900 0.01331 -0.01680 0.01340 O3 4 -0.063872 0.068003 0.763802 11.00000 0.06011 0.25879 = 0.08426 0.03626 0.00094 -0.01733 HKLF 4 Covalent radii and connectivity table for 01src007 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - C14 C6 C2 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C1 C7 C5 C7 - C8 C6 C8 - C7 C13 C9 C9 - C10 C8 C10 - C9 C11 C11 - C12 C10 C12 - C11 C13 C13 - C8 C12 C14 C14 - C1 O1 C13 C15 - O1 C16 C16 - C15 N1 C17 - N1 C18 C18 - O2 C17 C19 - O2 C20 C20 - O3 C19 C21 - O3 C22_$1 C22 - N1 C21_$1 N1 - C22 C17 C16 O1 - C14 C15 O2 - C19 C18 O3 - C20 C21 Operators for generating equivalent atoms: $1 -x, -y, -z+2 5854 Reflections read, of which 264 rejected -8 =< h =< 11, -17 =< k =< 19, -10 =< l =< 8, Max. 2-theta = 46.51 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 9 7 2 79.56 16.74 2 86.88 1 Inconsistent equivalents 2269 Unique reflections, of which 0 suppressed R(int) = 0.2052 R(sigma) = 0.3775 Friedel opposites merged Maximum memory for data reduction = 2100 / 22719 Default effective X-H distances for T = -123.0 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 = 2798 / 292625 wR2 = 0.1988 before cycle 1 for 2269 data and 236 / 236 parameters GooF = S = 0.869; Restrained GooF = 0.869 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0365 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38127 0.00195 0.002 OSF 2 0.00305 0.00118 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for OSF Max. shift = 0.000 A for C13 Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2798 / 292625 wR2 = 0.1988 before cycle 2 for 2269 data and 236 / 236 parameters GooF = S = 0.869; Restrained GooF = 0.869 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0365 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38128 0.00195 0.000 OSF 2 0.00305 0.00118 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for U23 C8 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2798 / 292625 wR2 = 0.1988 before cycle 3 for 2269 data and 236 / 236 parameters GooF = S = 0.869; Restrained GooF = 0.869 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0365 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38128 0.00195 0.000 OSF 2 0.00305 0.00118 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U22 C8 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2798 / 292625 wR2 = 0.1988 before cycle 4 for 2269 data and 236 / 236 parameters GooF = S = 0.869; Restrained GooF = 0.869 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0365 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38128 0.00195 0.000 OSF 2 0.00305 0.00118 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C13 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C2 Largest correlation matrix elements 0.679 x C7 / x C6 -0.572 z C10 / x C9 0.544 U12 C12 / x C12 0.667 x O3 / x C20 0.571 x C9 / x C8 -0.542 y C10 / x C9 0.655 x C5 / x C4 0.569 EXTI / OSF -0.536 x C22 / x C21 0.637 x C12 / x C11 0.558 y C6 / z C1 0.533 x C14 / x C13 0.595 x C5 / U11 C4 0.556 x C5 / y C4 0.530 x C9 / U11 C8 0.594 y C4 / z C3 -0.555 x C2 / U11 C1 0.530 z C6 / y C1 0.591 y O1 / y C15 -0.546 z C3 / x C2 -0.529 y C11 / x C9 0.586 x C2 / x C1 0.545 y C11 / z C10 -0.527 U12 C5 / x C4 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.3357 0.0931 1.3384 43 0.950 0.000 C2 C3 C1 H3 0.1908 0.1425 1.4742 43 0.950 0.000 C3 C2 C4 H4 0.2378 0.2489 1.6029 43 0.950 0.000 C4 C5 C3 H5 0.4402 0.2951 1.6262 43 0.950 0.000 C5 C4 C6 H7 0.6600 0.2955 1.5523 43 0.950 0.000 C7 C8 C6 H9 0.8844 0.2886 1.4937 43 0.950 0.000 C9 C10 C8 H10 1.0321 0.2359 1.3670 43 0.950 0.000 C10 C9 C11 H11 0.9901 0.1283 1.2417 43 0.950 0.000 C11 C12 C10 H12 0.7846 0.0806 1.2199 43 0.950 0.000 C12 C11 C13 H15A 0.5129 -0.0022 1.3871 23 0.990 0.000 C15 O1 C16 H15B 0.6417 -0.0195 1.3169 23 0.990 0.000 C15 O1 C16 H16A 0.4995 -0.1062 1.2304 23 0.990 0.000 C16 C15 N1 H16B 0.5117 -0.0451 1.1154 23 0.990 0.000 C16 C15 N1 H17A 0.2049 -0.0724 1.0684 23 0.990 0.000 C17 N1 C18 H17B 0.3390 -0.0585 1.0069 23 0.990 0.000 C17 N1 C18 H18A 0.1803 0.0585 1.0952 23 0.990 0.000 C18 O2 C17 H18B 0.3141 0.0722 1.0318 23 0.990 0.000 C18 O2 C17 H19A 0.2132 0.1320 0.8321 23 0.990 0.000 C19 O2 C20 H19B 0.0938 0.1288 0.9220 23 0.990 0.000 C19 O2 C20 H20A 0.0439 0.1392 0.6823 23 0.990 0.000 C20 O3 C19 H20B 0.0883 0.0533 0.6726 23 0.990 0.000 C20 O3 C19 H21A -0.1629 0.0046 0.6328 23 0.990 0.000 C21 O3 C22_$1 H21B -0.1318 0.0872 0.5794 23 0.990 0.000 C21 O3 C22_$1 H22A 0.3434 -0.0911 1.3799 23 0.990 0.000 C22 N1 C21_$1 H22B 0.2734 -0.1373 1.2612 23 0.990 0.000 C22 N1 C21_$1 01src007 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.48566 0.16099 1.40720 1.00000 0.09100 0.06837 0.03150 -0.00627 -0.00055 0.00643 0.06380 0.02461 0.00112 0.00075 0.00113 0.00000 0.01109 0.01045 0.00781 0.00695 0.00718 0.00810 0.00316 C2 0.35910 0.13282 1.39780 1.00000 0.06258 0.08408 0.08354 0.00923 -0.00808 -0.01127 0.07726 0.01777 0.00120 0.00054 0.00103 0.00000 0.00776 0.00999 0.01057 0.00719 0.00702 0.00822 0.00372 H2 0.33573 0.09311 1.33841 1.00000 0.09271 0.00000 0.00000 C3 0.27328 0.16362 1.47481 1.00000 0.06807 0.11070 0.09700 0.00956 0.01679 0.00453 0.09144 0.02499 0.00100 0.00082 0.00135 0.00000 0.00831 0.01298 0.01244 0.00923 0.00836 0.00905 0.00409 H3 0.19078 0.14247 1.47423 1.00000 0.10973 0.00000 0.00000 C4 0.30265 0.22610 1.55576 1.00000 0.09440 0.10549 0.12544 -0.01074 0.00084 0.02507 0.10869 0.03065 0.00133 0.00085 0.00131 0.00000 0.01173 0.01391 0.01356 0.00962 0.00868 0.01000 0.00471 H4 0.23785 0.24891 1.60289 1.00000 0.13042 0.00000 0.00000 C5 0.42061 0.25426 1.56788 1.00000 0.09421 0.09620 0.10045 -0.01069 -0.00960 0.02083 0.09760 0.02098 0.00141 0.00063 0.00114 0.00000 0.00969 0.01132 0.01136 0.00816 0.00985 0.00973 0.00439 H5 0.44016 0.29509 1.62617 1.00000 0.11712 0.00000 0.00000 C6 0.51649 0.22193 1.49179 1.00000 0.08464 0.08488 0.04652 -0.00987 -0.00159 0.01451 0.07225 0.02705 0.00125 0.00080 0.00120 0.00000 0.01054 0.01134 0.00909 0.00749 0.00808 0.00907 0.00339 C7 0.64116 0.25245 1.49915 1.00000 0.11364 0.06592 0.07682 -0.01149 -0.01631 -0.00340 0.08638 0.01890 0.00140 0.00058 0.00109 0.00000 0.01175 0.01046 0.01048 0.00690 0.00879 0.00919 0.00388 H7 0.65997 0.29553 1.55234 1.00000 0.10366 0.00000 0.00000 C8 0.73473 0.21980 1.42946 1.00000 0.09796 0.05294 0.06411 -0.00494 -0.01829 0.00350 0.07263 0.02450 0.00129 0.00072 0.00124 0.00000 0.01182 0.01024 0.01020 0.00724 0.00842 0.00895 0.00358 C9 0.86171 0.24735 1.43735 1.00000 0.08270 0.08831 0.09852 -0.00946 -0.02834 -0.04019 0.09125 0.01790 0.00129 0.00059 0.00111 0.00000 0.01007 0.01102 0.01198 0.00794 0.00828 0.00914 0.00433 H9 0.88443 0.28857 1.49366 1.00000 0.10950 0.00000 0.00000 C10 0.94955 0.21477 1.36468 1.00000 0.06539 0.09480 0.13482 0.01919 0.00641 -0.00838 0.09833 0.02497 0.00106 0.00079 0.00146 0.00000 0.00919 0.01292 0.01436 0.01004 0.00931 0.00906 0.00461 H10 1.03211 0.23594 1.36702 1.00000 0.11799 0.00000 0.00000 C11 0.92418 0.15156 1.28660 1.00000 0.08312 0.08610 0.10166 0.00732 -0.00610 -0.00512 0.09078 0.02576 0.00117 0.00072 0.00112 0.00000 0.01053 0.01173 0.01121 0.00816 0.00760 0.00865 0.00408 H11 0.99005 0.12832 1.24166 1.00000 0.10894 0.00000 0.00000 C12 0.80372 0.12293 1.27474 1.00000 0.07178 0.09343 0.07556 0.01056 -0.01835 -0.00327 0.08120 0.01825 0.00121 0.00058 0.00099 0.00000 0.00821 0.01027 0.00968 0.00714 0.00733 0.00848 0.00368 H12 0.78456 0.08056 1.21991 1.00000 0.09744 0.00000 0.00000 C13 0.70739 0.15800 1.34642 1.00000 0.07165 0.07867 0.04610 0.00203 -0.00824 0.00127 0.06596 0.02414 0.00111 0.00075 0.00110 0.00000 0.00957 0.01138 0.00883 0.00735 0.00739 0.00860 0.00329 C14 0.57976 0.13050 1.33710 1.00000 0.10393 0.05434 0.04189 -0.01391 -0.00708 0.00668 0.06720 0.02010 0.00125 0.00060 0.00104 0.00000 0.01046 0.00933 0.00869 0.00637 0.00782 0.00873 0.00327 C15 0.55323 -0.00191 1.30145 1.00000 0.04571 0.11745 0.07004 -0.00771 -0.01165 0.00040 0.07836 0.01661 0.00074 0.00064 0.00087 0.00000 0.00606 0.01105 0.00888 0.00810 0.00545 0.00686 0.00337 H15A 0.51293 -0.00224 1.38712 1.00000 0.09403 0.00000 0.00000 H15B 0.64169 -0.01952 1.31689 1.00000 0.09403 0.00000 0.00000 C16 0.48238 -0.05319 1.20534 1.00000 0.07108 0.11706 0.06904 -0.02190 -0.00516 -0.00203 0.08612 0.01541 0.00080 0.00051 0.00083 0.00000 0.00732 0.01044 0.00851 0.00712 0.00591 0.00723 0.00353 H16A 0.49945 -0.10623 1.23044 1.00000 0.10334 0.00000 0.00000 H16B 0.51169 -0.04512 1.11544 1.00000 0.10334 0.00000 0.00000 C17 0.27969 -0.03886 1.07047 1.00000 0.07773 0.09491 0.04568 0.00559 0.00360 -0.01684 0.07278 0.01426 0.00077 0.00055 0.00083 0.00000 0.00678 0.00947 0.00832 0.00666 0.00566 0.00681 0.00310 H17A 0.20490 -0.07242 1.06844 1.00000 0.08734 0.00000 0.00000 H17B 0.33903 -0.05846 1.00686 1.00000 0.08734 0.00000 0.00000 C18 0.23972 0.03837 1.03220 1.00000 0.08269 0.06637 0.06703 0.00261 -0.00156 0.01686 0.07229 0.01526 0.00079 0.00051 0.00092 0.00000 0.00672 0.00866 0.00889 0.00679 0.00626 0.00629 0.00316 H18A 0.18025 0.05853 1.09515 1.00000 0.08674 0.00000 0.00000 H18B 0.31407 0.07218 1.03177 1.00000 0.08674 0.00000 0.00000 C19 0.13906 0.10142 0.85400 1.00000 0.07905 0.10824 0.07288 0.01326 -0.01648 0.01078 0.08760 0.01609 0.00082 0.00057 0.00096 0.00000 0.00795 0.01120 0.00920 0.00756 0.00635 0.00694 0.00367 H19A 0.21317 0.13197 0.83212 1.00000 0.10512 0.00000 0.00000 H19B 0.09376 0.12876 0.92196 1.00000 0.10512 0.00000 0.00000 C20 0.05181 0.09104 0.73117 1.00000 0.08352 0.12671 0.08380 0.02097 -0.02022 0.01565 0.09906 0.01785 0.00097 0.00054 0.00094 0.00000 0.00857 0.01132 0.01063 0.00763 0.00791 0.00750 0.00390 H20A 0.04386 0.13921 0.68226 1.00000 0.11887 0.00000 0.00000 H20B 0.08833 0.05328 0.67256 1.00000 0.11887 0.00000 0.00000 C21 -0.15663 0.05846 0.65751 1.00000 0.06641 0.15500 0.06564 0.01659 -0.01411 -0.01130 0.09644 0.01622 0.00084 0.00055 0.00086 0.00000 0.00780 0.01124 0.00873 0.00742 0.00708 0.00747 0.00377 H21A -0.16288 0.00463 0.63282 1.00000 0.11572 0.00000 0.00000 H21B -0.13181 0.08717 0.57941 1.00000 0.11572 0.00000 0.00000 C22 0.28471 -0.08648 1.30030 1.00000 0.06050 0.09491 0.05689 0.00067 -0.01531 -0.00853 0.07155 0.01391 0.00081 0.00051 0.00086 0.00000 0.00708 0.00963 0.00840 0.00687 0.00558 0.00642 0.00312 H22A 0.34340 -0.09113 1.37990 1.00000 0.08586 0.00000 0.00000 H22B 0.27344 -0.13729 1.26124 1.00000 0.08586 0.00000 0.00000 N1 0.34229 -0.03789 1.20509 1.00000 0.07995 0.07639 0.04323 0.02077 -0.00318 -0.02353 0.06681 0.01245 0.00070 0.00041 0.00077 0.00000 0.00603 0.00721 0.00626 0.00477 0.00493 0.00511 0.00244 O1 0.55184 0.07333 1.24787 1.00000 0.07465 0.05595 0.06670 0.00703 -0.00486 -0.00424 0.06615 0.01159 0.00048 0.00042 0.00061 0.00000 0.00433 0.00566 0.00548 0.00472 0.00359 0.00429 0.00202 O2 0.17957 0.03286 0.90359 1.00000 0.09193 0.09447 0.06900 0.01330 -0.01679 0.01340 0.08603 0.01108 0.00055 0.00037 0.00070 0.00000 0.00481 0.00689 0.00565 0.00457 0.00405 0.00436 0.00238 O3 -0.06387 0.06800 0.76380 1.00000 0.06011 0.25880 0.08427 0.03626 0.00094 -0.01732 0.13454 0.01463 0.00071 0.00047 0.00068 0.00000 0.00521 0.01016 0.00665 0.00605 0.00497 0.00576 0.00337 Final Structure Factor Calculation for 01src007 in P2(1)/c Total number of l.s. parameters = 236 Maximum vector length = 511 Memory required = 2562 / 22995 wR2 = 0.1988 before cycle 5 for 2269 data and 0 / 236 parameters GooF = S = 0.869; Restrained GooF = 0.869 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0365 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0788 for 581 Fo > 4sig(Fo) and 0.3258 for all 2269 data wR2 = 0.1988, GooF = S = 0.869, Restrained GooF = 0.869 for all data Occupancy sum of asymmetric unit = 26.00 for non-hydrogen and 25.00 for hydrogen atoms Principal mean square atomic displacements U 0.0937 0.0673 0.0304 C1 0.1015 0.0746 0.0556 C2 0.1171 0.0941 0.0632 C3 0.1388 0.1133 0.0740 C4 0.1298 0.0891 0.0739 C5 0.1021 0.0705 0.0441 C6 0.1256 0.0784 0.0551 C7 0.1119 0.0559 0.0501 C8 0.1379 0.1034 0.0324 C9 0.1429 0.0898 0.0623 C10 0.1114 0.0833 0.0776 C11 0.1065 0.0856 0.0515 C12 0.0789 0.0770 0.0420 C13 0.1086 0.0604 0.0326 C14 0.1188 0.0771 0.0392 C15 0.1257 0.0771 0.0556 C16 0.1059 0.0677 0.0448 C17 0.0942 0.0687 0.0540 C18 0.1131 0.0987 0.0510 C19 0.1356 0.1102 0.0513 C20 0.1606 0.0799 0.0487 C21 0.0979 0.0764 0.0403 C22 0.1089 0.0591 0.0324 N1 0.0835 0.0625 0.0525 O1 0.1089 0.0992 0.0500 O2 0.2680 0.0770 0.0586 O3 may be split into -0.0654 0.0800 0.7681 and -0.0624 0.0560 0.7595 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.006 0.012 0.018 0.025 0.032 0.043 0.057 0.080 0.125 1.000 Number in group 249. 238. 212. 236. 213. 225. 214. 237. 218. 227. GooF 0.774 0.747 0.748 0.794 0.804 0.800 0.945 0.928 0.952 1.131 K 44.899 1.864 1.301 1.656 1.110 1.041 0.894 1.000 1.035 1.035 Resolution(A) 0.90 0.97 1.02 1.08 1.13 1.20 1.30 1.43 1.63 2.04 inf Number in group 232. 231. 222. 222. 233. 225. 229. 220. 230. 225. GooF 0.867 0.785 0.816 0.797 0.811 0.850 0.841 0.854 0.992 1.040 K 1.541 1.270 1.233 1.051 0.974 1.089 1.044 1.052 1.098 1.013 R1 0.731 0.640 0.576 0.451 0.360 0.342 0.293 0.224 0.117 0.047 Recommended weighting scheme: WGHT 0.0323 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) 5 1 1 2010.53 1288.21 5.66 0.238 2.03 4 1 1 4164.37 2636.25 5.55 0.341 2.49 5 0 2 4859.73 3249.16 4.61 0.378 1.91 9 4 2 866.90 307.00 3.99 0.116 1.09 3 3 9 417.03 96.99 3.87 0.065 1.03 3 1 0 808.86 636.95 3.59 0.168 3.45 -3 1 6 792.29 472.94 3.50 0.144 1.55 6 0 2 715.42 315.57 3.46 0.118 1.63 -1 13 8 277.29 3.06 3.39 0.012 0.93 5 3 0 1210.14 970.36 3.37 0.207 1.99 8 0 2 1312.77 725.55 3.20 0.179 1.26 2 1 1 229.79 297.11 3.16 0.114 4.42 -2 5 2 32.52 90.64 3.07 0.063 2.59 1 10 0 454.32 279.32 3.06 0.111 1.75 3 8 5 240.96 93.87 3.00 0.064 1.35 1 7 3 3807.48 2715.39 2.98 0.346 1.98 2 5 8 -69.38 97.11 2.92 0.065 1.15 -2 17 2 283.69 0.78 2.91 0.006 1.01 4 11 1 207.83 54.66 2.89 0.049 1.36 4 7 1 129.29 66.90 2.85 0.054 1.79 5 8 2 37.98 119.41 2.81 0.073 1.45 -9 2 1 83.08 157.87 2.81 0.083 1.16 11 6 0 557.13 16.86 2.78 0.027 0.91 -2 13 3 172.81 0.67 2.76 0.005 1.24 -2 0 2 24686.95 21607.51 2.70 0.976 3.77 6 10 0 139.86 13.30 2.70 0.024 1.25 3 16 0 184.08 11.31 2.69 0.022 1.06 3 2 0 2341.53 2033.39 2.67 0.299 3.27 4 0 0 998.06 855.40 2.67 0.194 2.64 -4 10 3 -40.78 101.05 2.66 0.067 1.37 9 11 2 576.59 4.11 2.64 0.013 0.92 3 4 9 -57.37 86.18 2.61 0.062 1.02 2 2 0 109.66 144.39 2.54 0.080 4.54 10 8 3 205.83 5.65 2.54 0.016 0.90 -2 16 6 356.05 0.18 2.53 0.003 0.92 1 1 7 -51.73 54.37 2.49 0.049 1.41 -3 7 2 164.36 255.69 2.48 0.106 1.93 -3 12 6 531.73 370.75 2.47 0.128 1.07 2 7 1 10.75 60.15 2.47 0.051 2.22 -8 4 7 205.35 0.58 2.45 0.005 0.98 -6 8 4 -24.94 62.25 2.44 0.052 1.24 5 8 4 -54.38 54.74 2.44 0.049 1.28 -3 13 2 555.52 399.27 2.43 0.133 1.24 0 11 2 -17.91 64.03 2.42 0.053 1.54 -2 6 2 -12.82 37.80 2.41 0.041 2.33 2 9 1 54.56 154.17 2.39 0.082 1.81 10 5 4 177.46 0.66 2.38 0.005 0.92 -1 10 7 -61.11 58.03 2.37 0.051 1.12 -1 8 1 503.47 404.71 2.37 0.134 2.13 0 6 2 9.27 55.32 2.36 0.049 2.56 FMAP and GRID set by program FMAP 2 3 13 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.3257 for 2269 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.16 at 0.9285 0.1831 0.1282 [ 1.50 A from H9 ] Deepest hole -0.18 at 0.6781 0.0982 0.2262 [ 1.17 A from H12 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 2583 / 17602 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9285 0.3169 1.6282 1.00000 0.05 0.16 1.50 H9 1.61 H11 1.70 C11 2.31 C12 Q2 1 -0.1411 0.1295 0.5945 1.00000 0.05 0.16 0.78 H21B 1.43 C21 2.06 C22 2.09 H22B Q3 1 0.5801 0.0371 1.2256 1.00000 0.05 0.14 0.75 O1 1.09 C15 1.49 H15B 1.91 C16 Q4 1 0.5636 -0.0192 1.2731 1.00000 0.05 0.13 0.44 C15 0.91 H15B 1.22 C16 1.34 H15A Q5 1 0.8002 0.0247 1.2112 1.00000 0.05 0.13 1.01 H12 1.57 O2 1.86 C12 2.13 H20B Q6 1 0.7147 -0.0396 1.4891 1.00000 0.05 0.13 1.90 H15B 2.04 H21A 2.09 H2 2.11 H3 Q7 1 0.8479 0.3026 1.5372 1.00000 0.05 0.12 0.65 H9 1.42 C9 2.01 H7 2.15 C8 Q8 1 0.4863 -0.0617 1.4774 1.00000 0.05 0.12 1.44 H15A 1.78 H15A 1.83 H22A 2.13 C1 Q9 1 0.1292 0.1761 0.9139 1.00000 0.05 0.12 0.93 H19B 1.47 C19 1.48 H19A 1.91 H10 Q10 1 0.5205 0.0667 1.4168 1.00000 0.05 0.12 1.26 H15A 1.55 C14 1.72 C1 1.74 C15 Q11 1 0.3438 0.2556 1.7034 1.00000 0.05 0.12 1.47 H4 1.50 H5 1.62 C4 1.64 C5 Q12 1 0.3650 -0.1564 1.2965 1.00000 0.05 0.12 1.07 H22B 1.46 H22A 1.51 C22 1.84 H16A Q13 1 0.2331 0.0628 1.5663 1.00000 0.05 0.12 1.74 H3 1.88 H15B 1.93 H20B 2.07 C3 Q14 1 0.5650 -0.0412 1.2124 1.00000 0.05 0.12 0.90 C16 1.10 H16B 1.15 C15 1.35 H15B Q15 1 0.2779 -0.0600 1.5423 1.00000 0.05 0.12 1.91 H22A 1.98 H21B 2.07 C13 2.15 H15B Q16 1 0.9257 0.2591 1.5496 1.00000 0.05 0.12 0.87 H9 1.30 C9 2.06 C10 2.26 H10 Q17 1 0.1037 0.0757 0.5933 1.00000 0.05 0.12 0.92 H20B 1.56 C20 1.60 H20A 1.96 H3 Q18 1 0.5038 -0.1404 1.3089 1.00000 0.05 0.11 1.00 H16A 1.88 C16 2.08 H22A 2.46 H22B Q19 1 0.8213 0.0609 1.0865 1.00000 0.05 0.11 1.47 H12 1.59 H17A 1.67 O2 1.89 H17B Q20 1 1.0418 0.0765 1.2759 1.00000 0.05 0.11 1.12 H11 1.83 C11 2.10 H21A 2.43 H18A Shortest distances between peaks (including symmetry equivalents) 4 14 0.73 6 13 0.91 8 10 1.08 3 4 1.13 7 16 1.13 1 7 1.24 1 16 1.30 3 14 1.41 13 17 1.43 5 19 1.45 12 18 1.49 6 15 1.80 14 18 2.13 3 10 2.14 10 15 2.15 4 10 2.18 8 18 2.22 6 17 2.24 13 15 2.25 8 8 2.25 4 18 2.28 2 15 2.30 8 15 2.34 3 5 2.35 4 8 2.39 8 10 2.40 6 8 2.44 2 16 2.46 1 19 2.47 7 19 2.49 11 18 2.61 4 6 2.65 1 20 2.65 2 12 2.72 4 13 2.73 4 5 2.73 3 15 2.74 8 12 2.75 5 15 2.75 5 14 2.75 5 20 2.76 6 10 2.76 2 17 2.76 5 13 2.78 5 17 2.81 4 15 2.81 6 8 2.82 6 10 2.85 9 16 2.87 8 14 2.88 10 14 2.88 19 20 2.94 10 10 2.95 4 8 2.98 Time profile in seconds ----------------------- 0.20: 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 0.02: Analyse other restraints etc. 0.83: 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 1.02: Structure factors and derivatives 1.14: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.34: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.03: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 18:01:18 Total CPU time: 3.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++