+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 14:32:52 on 11-Apr-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0404 in P-1 CELL 0.71073 10.1145 10.9859 15.0878 72.775 72.933 73.224 ZERR 2.00 0.0004 0.0005 0.0006 0.003 0.003 0.003 LATT 1 SFAC C H N O P CL UNIT 24 48 12 8 12 16 V = 1492.97 F(000) = 792.0 Mu = 1.11 mm-1 Cell Wt = 1571.58 Rho = 1.748 MERG 2 OMIT -3.00 55.00 OMIT -1 0 1 OMIT 0 0 2 FMAP 2 PLAN 20 SIZE 0.02 0.09 0.26 ACTA BOND WGHT 0.04420 0.73970 L.S. 4 TEMP -153.00 FVAR 0.11684 C5 1 0.030289 0.257146 0.313152 11.00000 0.02331 0.02622 = 0.02993 -0.00386 -0.01235 -0.00397 AFIX 23 H5A 2 0.094570 0.264038 0.249037 11.00000 -1.20000 H5B 2 -0.067520 0.297129 0.304452 11.00000 -1.20000 AFIX 0 MOLE 1 C1 1 0.024005 0.171844 0.713893 11.00000 0.01958 0.02803 = 0.02630 -0.00933 0.00321 -0.01007 AFIX 23 H1A 2 -0.015483 0.267173 0.697820 11.00000 -1.20000 H1B 2 -0.011331 0.138546 0.783022 11.00000 -1.20000 AFIX 0 C2 1 -0.023794 0.105490 0.658253 11.00000 0.02405 0.02384 = 0.02039 -0.00329 -0.00454 -0.00705 AFIX 23 H2A 2 0.026302 0.126952 0.590475 11.00000 -1.20000 H2B 2 -0.126594 0.140378 0.661849 11.00000 -1.20000 AFIX 0 C3 1 0.003673 -0.042651 0.694301 11.00000 0.02657 0.02508 = 0.01744 -0.00200 -0.00592 -0.00921 AFIX 23 H3A 2 0.106104 -0.076694 0.692556 11.00000 -1.20000 H3B 2 -0.048362 -0.063558 0.761656 11.00000 -1.20000 AFIX 0 C4 1 -0.039486 -0.113131 0.638399 11.00000 0.02365 0.02644 = 0.01818 -0.00381 -0.00586 -0.00660 AFIX 23 H4A 2 0.023106 -0.105001 0.573693 11.00000 -1.20000 H4B 2 -0.137925 -0.071238 0.631734 11.00000 -1.20000 AFIX 0 C6 1 0.067492 0.334710 0.365815 11.00000 0.02095 0.03085 = 0.03759 -0.01299 -0.01378 -0.00286 AFIX 23 H6A 2 0.051191 0.428266 0.332632 11.00000 -1.20000 H6B 2 0.007060 0.326330 0.431202 11.00000 -1.20000 AFIX 0 C7 1 0.569488 0.126237 0.224372 11.00000 0.02288 0.02668 = 0.02489 -0.00403 -0.00232 -0.00990 AFIX 23 H7A 2 0.504919 0.213303 0.212496 11.00000 -1.20000 H7B 2 0.549148 0.087401 0.293761 11.00000 -1.20000 AFIX 0 C8 1 0.546129 0.039349 0.171643 11.00000 0.02513 0.02870 = 0.01567 -0.00865 -0.00132 -0.00894 AFIX 23 H8A 2 0.611151 -0.047286 0.184461 11.00000 -1.20000 H8B 2 0.570473 0.077774 0.102322 11.00000 -1.20000 AFIX 0 C9 1 0.394814 0.021083 0.199541 11.00000 0.02100 0.02982 = 0.03482 -0.00945 -0.00631 -0.00932 AFIX 23 H9A 2 0.329757 0.107346 0.185192 11.00000 -1.20000 H9B 2 0.369480 -0.015633 0.269069 11.00000 -1.20000 AFIX 0 C10 1 0.374333 -0.069219 0.147368 11.00000 0.01822 0.02810 = 0.02379 -0.00534 -0.00273 -0.00974 AFIX 23 H10A 2 0.271527 -0.063484 0.158297 11.00000 -1.20000 H10B 2 0.410821 -0.037954 0.078119 11.00000 -1.20000 AFIX 0 C11 1 0.447460 -0.211233 0.177685 11.00000 0.02692 0.02700 = 0.03246 -0.00222 -0.01527 -0.00752 AFIX 23 H11A 2 0.548567 -0.216198 0.172789 11.00000 -1.20000 H11B 2 0.404253 -0.245169 0.245397 11.00000 -1.20000 AFIX 0 C12 1 0.561427 0.298016 -0.119096 11.00000 0.02190 0.03580 = 0.04120 -0.01599 -0.01348 -0.00509 AFIX 23 H12A 2 0.512849 0.389342 -0.142489 11.00000 -1.20000 H12B 2 0.515152 0.268043 -0.051391 11.00000 -1.20000 AFIX 0 N1 3 0.423432 0.191828 0.606315 11.00000 0.01868 0.02680 = 0.01728 -0.00353 -0.00531 -0.00437 N2 3 0.445732 0.266837 0.415156 11.00000 0.02250 0.03148 = 0.01296 -0.00681 -0.00316 -0.00935 N3 3 0.191888 0.327974 0.534920 11.00000 0.01892 0.02981 = 0.01948 -0.00469 -0.00605 -0.00201 N4 3 0.925476 0.240949 0.096352 11.00000 0.01799 0.03403 = 0.01892 -0.00085 -0.00880 -0.00393 N5 3 0.926400 0.325060 -0.092639 11.00000 0.01715 0.03437 = 0.02017 -0.00816 -0.00036 -0.00694 N6 3 0.677575 0.323686 0.040340 11.00000 0.01341 0.03824 = 0.01878 -0.00285 -0.00401 -0.00420 O1 4 0.181130 0.145834 0.690552 11.00000 0.02154 0.02133 = 0.01996 -0.00324 -0.00317 -0.00952 O2 4 0.218425 0.284035 0.369602 11.00000 0.01800 0.02128 = 0.02564 -0.00690 -0.01142 -0.00299 O3 4 0.717345 0.139290 0.190641 11.00000 0.02189 0.02670 = 0.02604 -0.00281 -0.00585 -0.01060 O4 4 0.713106 0.290156 -0.128760 11.00000 0.02007 0.02524 = 0.02486 -0.00814 -0.00761 -0.00721 P1 5 0.258380 0.254714 0.624314 11.00000 0.01807 0.01885 = 0.01676 -0.00416 -0.00405 -0.00429 P2 5 0.518937 0.214291 0.501885 11.00000 0.01655 0.02469 = 0.01953 -0.00757 -0.00321 -0.00691 P3 5 0.282941 0.335822 0.429274 11.00000 0.02183 0.02043 = 0.01653 -0.00203 -0.00573 -0.00819 P4 5 0.758442 0.266711 0.124249 11.00000 0.01661 0.02442 = 0.01595 -0.00198 -0.00421 -0.00635 P5 5 1.009879 0.262196 -0.010646 11.00000 0.01637 0.02818 = 0.02256 -0.00766 -0.00352 -0.00672 P6 5 0.758283 0.356823 -0.067544 11.00000 0.01797 0.02497 = 0.01646 -0.00422 -0.00517 -0.00616 CL1 6 0.217734 0.383938 0.704989 11.00000 0.02992 0.02487 = 0.02789 -0.01188 -0.00528 -0.00708 CL2 6 0.660541 0.047956 0.486693 11.00000 0.02084 0.03106 = 0.03921 -0.01510 -0.00520 -0.00200 CL3 6 0.648519 0.329596 0.490100 11.00000 0.02967 0.03739 = 0.03739 -0.01230 -0.00728 -0.01738 CL4 6 0.266082 0.526480 0.363352 11.00000 0.05056 0.02325 = 0.02977 0.00130 -0.01827 -0.01544 CL5 6 0.686845 0.391697 0.210963 11.00000 0.02900 0.02537 = 0.02503 -0.00779 -0.00392 -0.00890 CL6 6 1.154334 0.364273 -0.028801 11.00000 0.02616 0.04677 = 0.03406 -0.01262 -0.00458 -0.01824 CL7 6 1.136887 0.092015 -0.034351 11.00000 0.03053 0.03659 = 0.05447 -0.02036 -0.00702 0.00401 CL8 6 0.689573 0.548465 -0.121758 11.00000 0.03890 0.02399 = 0.03204 -0.00323 -0.01579 -0.00780 HKLF 4 Covalent radii and connectivity table for 2009src0404 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C5 - C6 C4_$1 C1 - O1 C2 C2 - C1 C3 C3 - C4 C2 C4 - C3 C5_$1 C6 - O2 C5 C7 - O3 C8 C8 - C7 C9 C9 - C8 C10 C10 - C11 C9 C11 - C12_$2 C10 C12 - O4 C11_$2 N1 - P2 P1 N2 - P2 P3 N3 - P1 P3 N4 - P5 P4 N5 - P5 P6 N6 - P6 P4 O1 - C1 P1 O2 - C6 P3 O3 - C7 P4 O4 - C12 P6 P1 - O1 N3 N1 Cl1 P2 - N2 N1 Cl2 Cl3 P3 - O2 N3 N2 Cl4 P4 - O3 N4 N6 Cl5 P5 - N4 N5 Cl6 Cl7 P6 - O4 N6 N5 Cl8 Cl1 - P1 Cl2 - P2 Cl3 - P2 Cl4 - P3 Cl5 - P4 Cl6 - P5 Cl7 - P5 Cl8 - P6 Operators for generating equivalent atoms: $1 -x, -y, -z+1 $2 -x+1, -y, -z 34086 Reflections read, of which 37 rejected -13 =< h =< 13, -14 =< k =< 14, -19 =< l =< 19, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -8 -4 7 0.05 0.10 5 0.98 0 -3 15 0.06 0.05 4 0.82 2 Inconsistent equivalents 6837 Unique reflections, of which 0 suppressed R(int) = 0.1098 R(sigma) = 0.1023 Friedel opposites merged Maximum memory for data reduction = 2897 / 69066 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 = 3792 / 410814 wR2 = 0.1289 before cycle 1 for 6837 data and 325 / 325 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0442 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11676 0.00019 -0.419 OSF Mean shift/esd = 0.072 Maximum = -0.419 for OSF Max. shift = 0.001 A for C6 Max. dU = 0.000 for N2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3792 / 410814 wR2 = 0.1288 before cycle 2 for 6837 data and 325 / 325 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0442 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11673 0.00019 -0.146 OSF Mean shift/esd = 0.023 Maximum = -0.146 for OSF Max. shift = 0.000 A for H3A Max. dU = 0.000 for N2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3792 / 410814 wR2 = 0.1288 before cycle 3 for 6837 data and 325 / 325 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0442 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11673 0.00019 0.002 OSF Mean shift/esd = 0.001 Maximum = 0.005 for U11 C8 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3792 / 410814 wR2 = 0.1288 before cycle 4 for 6837 data and 325 / 325 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0442 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11673 0.00019 0.004 OSF Mean shift/esd = 0.000 Maximum = 0.004 for OSF Max. shift = 0.000 A for C6 Max. dU = 0.000 for C3 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H5A 0.0947 0.2640 0.2491 23 0.990 0.000 C5 C6 C4_$1 H5B -0.0674 0.2971 0.3044 23 0.990 0.000 C5 C6 C4_$1 H1A -0.0155 0.2672 0.6978 23 0.990 0.000 C1 O1 C2 H1B -0.0114 0.1387 0.7830 23 0.990 0.000 C1 O1 C2 H2A 0.0264 0.1269 0.5905 23 0.990 0.000 C2 C1 C3 H2B -0.1265 0.1404 0.6618 23 0.990 0.000 C2 C1 C3 H3A 0.1060 -0.0767 0.6925 23 0.990 0.000 C3 C4 C2 H3B -0.0484 -0.0635 0.7616 23 0.990 0.000 C3 C4 C2 H4A 0.0232 -0.1051 0.5737 23 0.990 0.000 C4 C3 C5_$1 H4B -0.1379 -0.0713 0.6317 23 0.990 0.000 C4 C3 C5_$1 H6A 0.0512 0.4283 0.3325 23 0.990 0.000 C6 O2 C5 H6B 0.0070 0.3265 0.4311 23 0.990 0.000 C6 O2 C5 H7A 0.5050 0.2133 0.2124 23 0.990 0.000 C7 O3 C8 H7B 0.5492 0.0875 0.2937 23 0.990 0.000 C7 O3 C8 H8A 0.6111 -0.0473 0.1845 23 0.990 0.000 C8 C7 C9 H8B 0.5705 0.0777 0.1023 23 0.990 0.000 C8 C7 C9 H9A 0.3299 0.1074 0.1852 23 0.990 0.000 C9 C8 C10 H9B 0.3695 -0.0155 0.2691 23 0.990 0.000 C9 C8 C10 H10A 0.2716 -0.0634 0.1582 23 0.990 0.000 C10 C11 C9 H10B 0.4109 -0.0379 0.0781 23 0.990 0.000 C10 C11 C9 H11A 0.5486 -0.2162 0.1727 23 0.990 0.000 C11 C12_$2 C10 H11B 0.4042 -0.2451 0.2453 23 0.990 0.000 C11 C12_$2 C10 H12A 0.5129 0.3893 -0.1426 23 0.990 0.000 C12 O4 C11_$2 H12B 0.5151 0.2681 -0.0514 23 0.990 0.000 C12 O4 C11_$2 2009src0404 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C5 0.03034 0.25713 0.31316 1.00000 0.02319 0.02616 0.02977 -0.00380 -0.01238 -0.00393 0.02588 0.00620 0.00046 0.00042 0.00031 0.00000 0.00234 0.00248 0.00249 0.00198 0.00197 0.00193 0.00102 H5A 0.09468 0.26398 0.24906 1.00000 0.03105 0.00000 0.00000 H5B -0.06743 0.29712 0.30440 1.00000 0.03105 0.00000 0.00000 C1 0.02400 0.17189 0.71387 1.00000 0.01943 0.02813 0.02621 -0.00928 0.00348 -0.00991 0.02483 0.00607 0.00043 0.00044 0.00030 0.00000 0.00221 0.00253 0.00239 0.00196 0.00187 0.00191 0.00102 H1A -0.01546 0.26723 0.69775 1.00000 0.02979 0.00000 0.00000 H1B -0.01138 0.13865 0.78301 1.00000 0.02979 0.00000 0.00000 C2 -0.02376 0.10548 0.65826 1.00000 0.02345 0.02416 0.02025 -0.00371 -0.00435 -0.00686 0.02273 0.00603 0.00045 0.00040 0.00029 0.00000 0.00228 0.00240 0.00222 0.00182 0.00181 0.00188 0.00097 H2A 0.02636 0.12694 0.59049 1.00000 0.02727 0.00000 0.00000 H2B -0.12655 0.14040 0.66183 1.00000 0.02727 0.00000 0.00000 C3 0.00361 -0.04259 0.69423 1.00000 0.02614 0.02491 0.01711 -0.00207 -0.00570 -0.00887 0.02246 0.00599 0.00046 0.00041 0.00028 0.00000 0.00234 0.00241 0.00214 0.00178 0.00181 0.00190 0.00097 H3A 0.10603 -0.07665 0.69252 1.00000 0.02695 0.00000 0.00000 H3B -0.04844 -0.06348 0.76159 1.00000 0.02695 0.00000 0.00000 C4 -0.03945 -0.11316 0.63844 1.00000 0.02341 0.02636 0.01776 -0.00357 -0.00574 -0.00653 0.02239 0.00594 0.00045 0.00041 0.00028 0.00000 0.00229 0.00245 0.00217 0.00181 0.00180 0.00189 0.00097 H4A 0.02318 -0.10507 0.57374 1.00000 0.02687 0.00000 0.00000 H4B -0.13786 -0.07126 0.63172 1.00000 0.02687 0.00000 0.00000 C6 0.06745 0.33479 0.36575 1.00000 0.02085 0.03072 0.03726 -0.01275 -0.01366 -0.00306 0.02749 0.00608 0.00045 0.00045 0.00033 0.00000 0.00227 0.00261 0.00267 0.00212 0.00199 0.00194 0.00104 H6A 0.05119 0.42831 0.33249 1.00000 0.03298 0.00000 0.00000 H6B 0.00695 0.32650 0.43111 1.00000 0.03298 0.00000 0.00000 C7 0.56952 0.12627 0.22433 1.00000 0.02296 0.02686 0.02423 -0.00400 -0.00204 -0.01024 0.02482 0.00610 0.00044 0.00043 0.00030 0.00000 0.00231 0.00248 0.00233 0.00192 0.00187 0.00194 0.00101 H7A 0.50497 0.21334 0.21242 1.00000 0.02978 0.00000 0.00000 H7B 0.54916 0.08748 0.29373 1.00000 0.02978 0.00000 0.00000 C8 0.54613 0.03933 0.17164 1.00000 0.02558 0.02847 0.01531 -0.00828 -0.00107 -0.00913 0.02250 0.00584 0.00044 0.00043 0.00028 0.00000 0.00232 0.00248 0.00212 0.00183 0.00178 0.00194 0.00097 H8A 0.61111 -0.04732 0.18450 1.00000 0.02700 0.00000 0.00000 H8B 0.57051 0.07770 0.10231 1.00000 0.02700 0.00000 0.00000 C9 0.39488 0.02115 0.19953 1.00000 0.02098 0.03016 0.03457 -0.00949 -0.00612 -0.00954 0.02729 0.00616 0.00044 0.00045 0.00033 0.00000 0.00229 0.00259 0.00261 0.00207 0.00197 0.00197 0.00104 H9A 0.32985 0.10743 0.18516 1.00000 0.03275 0.00000 0.00000 H9B 0.36952 -0.01555 0.26906 1.00000 0.03275 0.00000 0.00000 C10 0.37440 -0.06916 0.14734 1.00000 0.01818 0.02809 0.02372 -0.00532 -0.00251 -0.00999 0.02291 0.00593 0.00043 0.00041 0.00029 0.00000 0.00217 0.00249 0.00229 0.00189 0.00180 0.00186 0.00098 H10A 0.27159 -0.06338 0.15825 1.00000 0.02750 0.00000 0.00000 H10B 0.41092 -0.03789 0.07810 1.00000 0.02750 0.00000 0.00000 C11 0.44744 -0.21119 0.17763 1.00000 0.02632 0.02717 0.03227 -0.00232 -0.01508 -0.00754 0.02736 0.00625 0.00047 0.00042 0.00032 0.00000 0.00240 0.00255 0.00254 0.00200 0.00201 0.00199 0.00104 H11A 0.54855 -0.21619 0.17275 1.00000 0.03283 0.00000 0.00000 H11B 0.40422 -0.24510 0.24535 1.00000 0.03283 0.00000 0.00000 C12 0.56144 0.29800 -0.11911 1.00000 0.02149 0.03612 0.04077 -0.01572 -0.01324 -0.00512 0.03012 0.00621 0.00045 0.00047 0.00034 0.00000 0.00234 0.00282 0.00278 0.00226 0.00207 0.00206 0.00109 H12A 0.51289 0.38932 -0.14255 1.00000 0.03614 0.00000 0.00000 H12B 0.51513 0.26809 -0.05141 1.00000 0.03614 0.00000 0.00000 N1 0.42347 0.19180 0.60627 1.00000 0.01855 0.02654 0.01692 -0.00344 -0.00516 -0.00442 0.02090 0.00486 0.00034 0.00033 0.00023 0.00000 0.00181 0.00203 0.00176 0.00150 0.00146 0.00153 0.00080 N2 0.44572 0.26684 0.41514 1.00000 0.02210 0.03144 0.01257 -0.00673 -0.00312 -0.00929 0.02110 0.00478 0.00035 0.00035 0.00022 0.00000 0.00187 0.00210 0.00172 0.00149 0.00144 0.00159 0.00079 N3 0.19189 0.32792 0.53494 1.00000 0.01859 0.02991 0.01909 -0.00480 -0.00584 -0.00206 0.02311 0.00499 0.00035 0.00034 0.00023 0.00000 0.00183 0.00212 0.00183 0.00157 0.00149 0.00157 0.00083 N4 0.92550 0.24089 0.09638 1.00000 0.01775 0.03376 0.01870 -0.00082 -0.00871 -0.00400 0.02394 0.00506 0.00035 0.00035 0.00023 0.00000 0.00184 0.00219 0.00185 0.00160 0.00150 0.00161 0.00084 N5 0.92637 0.32508 -0.09266 1.00000 0.01687 0.03428 0.01974 -0.00795 -0.00029 -0.00683 0.02385 0.00504 0.00035 0.00035 0.00023 0.00000 0.00181 0.00221 0.00187 0.00161 0.00148 0.00160 0.00084 N6 0.67755 0.32369 0.04036 1.00000 0.01344 0.03796 0.01844 -0.00261 -0.00398 -0.00430 0.02439 0.00508 0.00034 0.00036 0.00023 0.00000 0.00174 0.00226 0.00184 0.00161 0.00146 0.00158 0.00085 O1 0.18115 0.14582 0.69055 1.00000 0.02137 0.02124 0.02004 -0.00326 -0.00316 -0.00952 0.02051 0.00391 0.00028 0.00026 0.00019 0.00000 0.00150 0.00156 0.00149 0.00121 0.00121 0.00124 0.00064 O2 0.21841 0.28407 0.36961 1.00000 0.01793 0.02109 0.02538 -0.00685 -0.01141 -0.00300 0.01996 0.00380 0.00028 0.00026 0.00019 0.00000 0.00145 0.00156 0.00154 0.00123 0.00121 0.00121 0.00063 O3 0.71734 0.13929 0.19061 1.00000 0.02167 0.02643 0.02580 -0.00243 -0.00584 -0.01066 0.02417 0.00404 0.00029 0.00028 0.00020 0.00000 0.00156 0.00169 0.00161 0.00131 0.00128 0.00131 0.00069 O4 0.71311 0.29011 -0.12876 1.00000 0.01996 0.02504 0.02447 -0.00815 -0.00757 -0.00703 0.02158 0.00387 0.00028 0.00027 0.00019 0.00000 0.00149 0.00164 0.00155 0.00127 0.00123 0.00126 0.00065 P1 0.25840 0.25473 0.62430 1.00000 0.01799 0.01871 0.01668 -0.00416 -0.00397 -0.00424 0.01773 0.00153 0.00011 0.00010 0.00007 0.00000 0.00054 0.00058 0.00054 0.00044 0.00043 0.00044 0.00025 P2 0.51893 0.21427 0.50188 1.00000 0.01652 0.02465 0.01955 -0.00763 -0.00322 -0.00696 0.01933 0.00153 0.00011 0.00011 0.00007 0.00000 0.00055 0.00061 0.00057 0.00046 0.00044 0.00046 0.00025 P3 0.28294 0.33583 0.42926 1.00000 0.02184 0.02037 0.01638 -0.00202 -0.00570 -0.00819 0.01895 0.00154 0.00011 0.00011 0.00007 0.00000 0.00057 0.00059 0.00054 0.00044 0.00045 0.00046 0.00025 P4 0.75844 0.26673 0.12425 1.00000 0.01655 0.02440 0.01588 -0.00197 -0.00419 -0.00637 0.01903 0.00157 0.00011 0.00011 0.00007 0.00000 0.00054 0.00061 0.00054 0.00045 0.00044 0.00046 0.00025 P5 1.00988 0.26219 -0.01064 1.00000 0.01639 0.02809 0.02249 -0.00772 -0.00348 -0.00667 0.02172 0.00159 0.00011 0.00011 0.00008 0.00000 0.00055 0.00064 0.00059 0.00048 0.00046 0.00048 0.00026 P6 0.75828 0.35682 -0.06755 1.00000 0.01792 0.02492 0.01642 -0.00423 -0.00517 -0.00617 0.01927 0.00155 0.00011 0.00011 0.00007 0.00000 0.00055 0.00061 0.00055 0.00045 0.00044 0.00046 0.00025 Cl1 0.21773 0.38392 0.70500 1.00000 0.02980 0.02482 0.02775 -0.01185 -0.00525 -0.00707 0.02620 0.00153 0.00011 0.00010 0.00007 0.00000 0.00059 0.00058 0.00058 0.00046 0.00047 0.00047 0.00026 Cl2 0.66054 0.04795 0.48669 1.00000 0.02075 0.03106 0.03914 -0.01512 -0.00514 -0.00204 0.02991 0.00162 0.00011 0.00011 0.00008 0.00000 0.00055 0.00064 0.00066 0.00051 0.00048 0.00047 0.00027 Cl3 0.64850 0.32961 0.49010 1.00000 0.02943 0.03727 0.03734 -0.01228 -0.00723 -0.01731 0.03172 0.00157 0.00012 0.00011 0.00008 0.00000 0.00061 0.00069 0.00066 0.00053 0.00051 0.00052 0.00028 Cl4 0.26608 0.52647 0.36336 1.00000 0.05050 0.02315 0.02977 0.00130 -0.01826 -0.01542 0.03248 0.00162 0.00013 0.00011 0.00008 0.00000 0.00075 0.00060 0.00061 0.00047 0.00055 0.00054 0.00029 Cl5 0.68685 0.39170 0.21097 1.00000 0.02896 0.02533 0.02494 -0.00777 -0.00391 -0.00894 0.02581 0.00153 0.00011 0.00010 0.00007 0.00000 0.00058 0.00058 0.00057 0.00045 0.00046 0.00046 0.00026 Cl6 1.15432 0.36426 -0.02879 1.00000 0.02603 0.04685 0.03391 -0.01263 -0.00449 -0.01830 0.03310 0.00160 0.00012 0.00012 0.00008 0.00000 0.00059 0.00075 0.00064 0.00054 0.00049 0.00054 0.00029 Cl7 1.13687 0.09203 -0.03435 1.00000 0.03048 0.03663 0.05437 -0.02051 -0.00703 0.00407 0.04135 0.00193 0.00013 0.00012 0.00010 0.00000 0.00065 0.00072 0.00080 0.00061 0.00058 0.00054 0.00033 Cl8 0.68960 0.54844 -0.12176 1.00000 0.03877 0.02397 0.03195 -0.00318 -0.01570 -0.00786 0.03037 0.00161 0.00012 0.00011 0.00008 0.00000 0.00066 0.00060 0.00061 0.00047 0.00051 0.00050 0.00028 Final Structure Factor Calculation for 2009src0404 in P-1 Total number of l.s. parameters = 325 Maximum vector length = 511 Memory required = 3467 / 25039 wR2 = 0.1288 before cycle 5 for 6837 data and 0 / 325 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0442 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0592 for 4332 Fo > 4sig(Fo) and 0.1117 for all 6837 data wR2 = 0.1288, GooF = S = 1.033, Restrained GooF = 1.033 for all data Occupancy sum of asymmetric unit = 36.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0330 0.0272 0.0174 C5 0.0355 0.0245 0.0145 C1 0.0254 0.0230 0.0199 C2 0.0287 0.0221 0.0166 C3 0.0272 0.0228 0.0172 C4 0.0408 0.0269 0.0148 C6 0.0292 0.0274 0.0179 C7 0.0309 0.0230 0.0135 C8 0.0353 0.0296 0.0170 C9 0.0292 0.0247 0.0148 C10 0.0387 0.0260 0.0174 C11 0.0453 0.0301 0.0150 C12 0.0278 0.0189 0.0160 N1 0.0319 0.0201 0.0113 N2 0.0326 0.0199 0.0168 N3 0.0380 0.0216 0.0123 N4 0.0343 0.0224 0.0149 N5 0.0417 0.0183 0.0132 N6 0.0252 0.0212 0.0151 O1 0.0283 0.0203 0.0112 O2 0.0313 0.0246 0.0166 O3 0.0267 0.0240 0.0140 O4 0.0187 0.0179 0.0166 P1 0.0256 0.0179 0.0144 P2 0.0247 0.0165 0.0156 P3 0.0260 0.0157 0.0154 P4 0.0284 0.0214 0.0153 P5 0.0252 0.0180 0.0146 P6 0.0322 0.0290 0.0175 Cl1 0.0419 0.0279 0.0200 Cl2 0.0437 0.0356 0.0159 Cl3 0.0540 0.0244 0.0190 Cl4 0.0314 0.0246 0.0214 Cl5 0.0498 0.0322 0.0173 Cl6 0.0570 0.0452 0.0219 Cl7 0.0425 0.0252 0.0234 Cl8 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.020 0.031 0.043 0.056 0.070 0.089 0.113 0.159 1.000 Number in group 714. 661. 675. 703. 700. 654. 706. 659. 681. 684. GooF 0.930 0.958 0.931 1.081 1.139 1.104 1.112 1.063 1.005 0.978 K 7.865 2.067 1.181 1.028 0.993 0.977 0.991 1.005 1.010 1.003 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 707. 666. 683. 689. 693. 667. 688. 680. 677. 687. GooF 0.962 0.953 1.000 0.962 1.025 1.013 1.109 0.984 1.015 1.267 K 1.073 1.039 1.038 1.018 1.029 1.028 1.008 1.025 1.016 0.978 R1 0.285 0.226 0.189 0.153 0.130 0.103 0.083 0.052 0.044 0.040 Recommended weighting scheme: WGHT 0.0428 0.8039 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 0 1 391.86 201.74 6.50 0.051 1.93 -1 3 17 11.01 113.51 6.01 0.039 0.82 -2 1 6 473.04 307.09 4.37 0.063 1.93 4 2 14 353.32 760.74 3.73 0.100 1.06 -1 -2 3 1075.00 858.77 3.69 0.106 2.94 4 -1 2 119.73 30.93 3.67 0.020 2.20 6 6 2 489.00 300.18 3.64 0.063 1.38 7 11 8 205.45 520.92 3.62 0.083 0.91 0 0 4 364.12 266.09 3.59 0.059 3.51 0 5 0 2717.86 2249.36 3.51 0.172 2.05 -5 -5 6 94.33 10.18 3.49 0.012 1.13 7 4 12 284.94 5.32 3.44 0.008 1.08 -8 -2 4 117.84 6.69 3.38 0.009 1.05 10 10 0 450.54 862.56 3.35 0.106 0.79 0 -6 12 125.18 396.79 3.34 0.072 0.87 0 2 6 549.63 423.79 3.32 0.074 2.34 0 -1 6 595.12 461.50 3.31 0.078 2.17 10 0 12 272.84 9.12 3.30 0.011 0.83 2 2 6 377.48 269.67 3.30 0.059 2.44 7 -3 6 128.63 350.77 3.30 0.068 1.10 1 6 17 215.61 454.85 3.24 0.077 0.84 2 0 6 295.29 160.03 3.24 0.046 2.32 -6 1 2 286.03 177.64 3.20 0.048 1.42 -2 -2 10 865.07 572.79 3.19 0.087 1.19 0 3 1 112.99 51.82 3.17 0.026 3.51 -5 -11 3 911.43 300.56 3.15 0.063 0.85 -1 -2 5 1500.09 1819.34 3.11 0.154 2.15 3 2 5 2270.16 2744.14 3.10 0.189 2.54 -10 5 0 1200.87 698.76 3.08 0.096 0.79 7 6 10 231.51 433.67 3.07 0.075 1.13 -3 -4 1 669.53 527.11 3.04 0.083 2.10 0 -3 6 78.73 21.73 3.04 0.017 1.75 0 -2 1 48.41 4.57 3.02 0.008 4.49 -3 0 16 394.69 115.17 2.97 0.039 0.80 -6 -1 13 805.45 316.37 2.97 0.064 0.80 -7 2 10 411.51 172.83 2.96 0.048 0.86 -2 -9 3 14.34 112.56 2.95 0.038 1.06 2 5 9 197.83 73.26 2.95 0.031 1.50 -9 4 5 396.21 757.54 2.93 0.100 0.83 5 -1 3 1424.96 1138.96 2.93 0.122 1.78 5 -6 5 249.46 370.35 2.89 0.070 1.05 -7 3 4 226.75 105.70 2.87 0.037 1.07 -1 2 5 4262.23 4963.40 2.85 0.255 2.42 3 5 14 11.34 118.67 2.85 0.039 1.06 10 6 0 135.92 24.09 2.84 0.018 0.92 4 -1 6 2100.01 2512.44 2.83 0.181 1.75 5 -6 2 79.03 171.49 2.83 0.047 1.13 -2 3 0 80.64 25.12 2.83 0.018 2.51 8 10 16 2127.86 1479.47 2.83 0.139 0.78 3 -3 4 1453.26 1760.85 2.82 0.152 1.80 Bond lengths and angles C5 - Distance Angles C6 1.5029 (0.0062) C4_$1 1.5214 (0.0058) 115.08 (0.37) C5 - C6 C1 - Distance Angles O1 1.4836 (0.0047) C2 1.5078 (0.0060) 109.66 (0.33) C1 - O1 C2 - Distance Angles C1 1.5078 (0.0060) C3 1.5241 (0.0057) 113.28 (0.36) C2 - C1 C3 - Distance Angles C4 1.5152 (0.0060) C2 1.5241 (0.0057) 114.82 (0.35) C3 - C4 C4 - Distance Angles C3 1.5152 (0.0060) C5_$1 1.5214 (0.0058) 111.90 (0.35) C4 - C3 C6 - Distance Angles O2 1.4789 (0.0049) C5 1.5029 (0.0062) 108.50 (0.34) C6 - O2 C7 - Distance Angles O3 1.4658 (0.0048) C8 1.5135 (0.0059) 108.70 (0.32) C7 - O3 C8 - Distance Angles C7 1.5135 (0.0059) C9 1.5186 (0.0056) 113.31 (0.33) C8 - C7 C9 - Distance Angles C8 1.5186 (0.0056) C10 1.5245 (0.0060) 112.47 (0.35) C9 - C8 C10 - Distance Angles C11 1.5164 (0.0059) C9 1.5245 (0.0060) 114.21 (0.37) C10 - C11 C11 - Distance Angles C12_$2 1.5139 (0.0062) C10 1.5164 (0.0059) 113.92 (0.37) C11 - C12_$2 C12 - Distance Angles O4 1.4771 (0.0049) C11_$2 1.5139 (0.0062) 107.61 (0.34) C12 - O4 N1 - Distance Angles P2 1.5775 (0.0033) P1 1.5868 (0.0034) 119.95 (0.22) N1 - P2 N2 - Distance Angles P2 1.5714 (0.0035) P3 1.5811 (0.0035) 120.75 (0.20) N2 - P2 N3 - Distance Angles P1 1.5795 (0.0035) P3 1.5813 (0.0033) 122.26 (0.22) N3 - P1 N4 - Distance Angles P5 1.5725 (0.0034) P4 1.5778 (0.0034) 121.58 (0.22) N4 - P5 N5 - Distance Angles P5 1.5788 (0.0037) P6 1.5854 (0.0034) 120.15 (0.21) N5 - P5 N6 - Distance Angles P6 1.5780 (0.0033) P4 1.5832 (0.0036) 122.20 (0.21) N6 - P6 O1 - Distance Angles C1 1.4836 (0.0047) P1 1.5537 (0.0027) 119.88 (0.25) O1 - C1 O2 - Distance Angles C6 1.4789 (0.0049) P3 1.5561 (0.0030) 120.09 (0.25) O2 - C6 O3 - Distance Angles C7 1.4658 (0.0048) P4 1.5482 (0.0029) 121.86 (0.26) O3 - C7 O4 - Distance Angles C12 1.4771 (0.0049) P6 1.5622 (0.0030) 120.10 (0.26) O4 - C12 P1 - Distance Angles O1 1.5537 (0.0027) N3 1.5795 (0.0035) 111.65 (0.18) N1 1.5868 (0.0034) 107.13 (0.17) 118.25 (0.18) Cl1 2.0145 (0.0015) 103.85 (0.12) 107.35 (0.14) 107.61 (0.14) P1 - O1 N3 N1 P2 - Distance Angles N2 1.5714 (0.0035) N1 1.5775 (0.0033) 119.04 (0.18) Cl2 1.9968 (0.0015) 108.93 (0.14) 108.40 (0.14) Cl3 2.0107 (0.0015) 109.31 (0.14) 109.23 (0.15) 100.29 (0.07) P2 - N2 N1 Cl2 P3 - Distance Angles O2 1.5561 (0.0030) N3 1.5813 (0.0033) 112.07 (0.17) N2 1.5811 (0.0035) 107.39 (0.17) 117.49 (0.18) Cl4 2.0160 (0.0015) 103.02 (0.12) 107.51 (0.14) 108.33 (0.14) P3 - O2 N3 N2 P4 - Distance Angles O3 1.5482 (0.0029) N4 1.5778 (0.0034) 107.56 (0.18) N6 1.5832 (0.0036) 112.14 (0.18) 117.51 (0.18) Cl5 2.0137 (0.0015) 102.81 (0.12) 107.91 (0.15) 107.84 (0.15) P4 - O3 N4 N6 P5 - Distance Angles N4 1.5725 (0.0034) N5 1.5788 (0.0037) 119.60 (0.18) Cl6 1.9989 (0.0016) 108.75 (0.15) 109.09 (0.14) Cl7 2.0031 (0.0017) 109.15 (0.15) 108.20 (0.15) 100.33 (0.07) P5 - N4 N5 Cl6 P6 - Distance Angles O4 1.5622 (0.0030) N6 1.5780 (0.0033) 111.26 (0.18) N5 1.5854 (0.0034) 106.84 (0.18) 118.63 (0.19) Cl8 2.0131 (0.0015) 102.88 (0.12) 108.09 (0.15) 107.97 (0.14) P6 - O4 N6 N5 Cl1 - Distance Angles P1 2.0145 (0.0015) Cl1 - Cl2 - Distance Angles P2 1.9968 (0.0015) Cl2 - Cl3 - Distance Angles P2 2.0107 (0.0015) Cl3 - Cl4 - Distance Angles P3 2.0160 (0.0015) Cl4 - Cl5 - Distance Angles P4 2.0137 (0.0015) Cl5 - Cl6 - Distance Angles P5 1.9989 (0.0016) Cl6 - Cl7 - Distance Angles P5 2.0031 (0.0017) Cl7 - Cl8 - Distance Angles P6 2.0131 (0.0015) Cl8 - FMAP and GRID set by program FMAP 2 3 38 GRID -1.429 -2 -2 1.429 2 2 R1 = 0.1111 for 6837 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.55 at 0.4614 0.2346 0.2566 [ 0.74 A from H7A ] Deepest hole -0.51 at 0.2017 0.6972 0.0961 [ 0.78 A from P6 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 3317 / 30267 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4614 0.2346 0.2566 1.00000 0.05 0.55 0.74 H7A 1.46 C7 1.62 H7B 2.47 N2 Q2 1 0.3382 0.1360 0.4309 1.00000 0.05 0.52 1.90 O2 1.96 N2 2.03 CL2 2.10 P3 Q3 1 0.4778 0.3565 0.1354 1.00000 0.05 0.45 1.66 H7A 1.75 CL8 2.11 N6 2.53 C7 Q4 1 0.7409 0.3368 0.0037 1.00000 0.05 0.45 0.73 N6 1.00 P6 1.79 P4 2.01 N5 Q5 1 0.0230 0.2394 0.7311 1.00000 0.05 0.44 0.67 H1A 0.85 C1 1.23 H1B 1.68 O1 Q6 1 0.3489 0.4556 0.4468 1.00000 0.05 0.44 1.60 CL4 1.75 P3 2.15 N2 2.28 N3 Q7 1 0.6033 0.0348 0.3128 1.00000 0.05 0.43 0.73 H7B 1.48 C7 2.08 O3 2.26 H7A Q8 1 -0.1580 -0.0781 0.6204 1.00000 0.05 0.43 0.34 H4B 1.23 C4 1.73 H4A 2.16 C5 Q9 1 1.2776 -0.0478 0.0026 1.00000 0.05 0.42 1.84 CL7 1.89 H8B 2.05 H10B 2.29 H10A Q10 1 0.9365 0.3988 0.0887 1.00000 0.05 0.42 1.74 N4 2.26 P5 2.40 CL6 2.47 P4 Q11 1 1.1430 0.2997 0.0190 1.00000 0.05 0.42 0.86 CL6 1.72 P5 2.34 N4 2.66 CL7 Q12 1 0.2870 -0.2966 0.3166 1.00000 0.05 0.41 1.47 H11B 1.91 CL4 2.02 H2B 2.37 C11 Q13 1 0.5942 0.0553 0.3958 1.00000 0.05 0.41 1.64 H7B 1.67 CL2 2.42 N2 2.52 P2 Q14 1 1.2392 0.2454 0.0127 1.00000 0.05 0.41 1.42 CL6 2.39 P5 2.56 CL7 2.73 H12B Q15 1 0.7877 0.2481 0.5036 1.00000 0.05 0.41 1.47 CL3 2.35 H4A 2.44 H6B 2.61 H2B Q16 1 0.4639 0.0638 0.0673 1.00000 0.05 0.41 1.32 H10B 1.39 H8B 1.87 C10 1.87 C9 Q17 1 0.1933 0.1410 0.5458 1.00000 0.05 0.40 1.66 H2A 2.01 N3 2.17 O1 2.27 CL2 Q18 1 0.9906 0.3859 -0.0732 1.00000 0.05 0.40 1.20 N5 1.40 P5 1.89 CL6 2.43 P6 Q19 1 0.4001 0.2036 -0.0550 1.00000 0.05 0.40 1.55 H12B 1.67 H11A 2.03 C11 2.03 C12 Q20 1 0.1759 0.4731 0.2366 1.00000 0.05 0.40 1.67 H6A 1.89 CL8 2.29 C6 2.46 O2 Shortest distances between peaks (including symmetry equivalents) 11 14 0.98 7 13 1.31 14 19 1.67 1 3 1.91 2 17 1.92 16 19 2.15 10 11 2.17 11 18 2.20 1 7 2.32 10 18 2.38 2 13 2.43 2 8 2.47 9 16 2.49 11 19 2.56 4 18 2.59 10 18 2.60 1 2 2.61 16 16 2.62 14 16 2.71 13 17 2.71 12 15 2.76 1 13 2.79 3 4 2.81 6 12 2.87 2 7 2.87 16 19 2.90 8 17 2.93 2 13 2.95 4 10 2.97 14 18 2.98 Time profile in seconds ----------------------- 0.25: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.06: Generate connectivity array 0.05: 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 0.02: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.06: Analyse other restraints etc. 47.36: 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 0.00: Generate idealized H-atoms 6.55: Structure factors and derivatives 7.63: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.28: Apply other restraints 3.64: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.17: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.81: Fourier summations 0.08: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxl finished at 14:33:59 Total CPU time: 67.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++