+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0267 started at 11:57:11 on 24-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0267 in P2(1)/n CELL 0.71073 12.2480 9.1264 25.8185 90.000 96.561 90.000 ZERR 4.00 0.0003 0.0003 0.0007 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H O F P BR B UNIT 100 180 8 14.08 4 0.48 7.52 V = 2867.09 F(000) = 1085.1 Mu = 0.30 mm-1 Cell Wt = 2021.49 Rho = 1.171 MERG 2 OMIT -3.00 50.00 SHEL 7 0.84 FMAP 2 PLAN 10 SIZE 0.01 0.07 0.21 ACTA BOND $H WGHT 0.00000 7.53110 L.S. 1 TEMP -153.00 FVAR 0.37126 MOLE 1 C3 1 0.792195 0.065267 0.568973 11.00000 0.03069 0.04738 = 0.02502 0.00548 -0.00409 0.00660 C4 1 0.827089 -0.077695 0.543142 11.00000 0.03355 0.05981 = 0.02141 0.00739 0.00171 0.00883 C6 1 0.880926 0.181873 0.574787 11.00000 0.05400 0.05699 = 0.03380 0.00081 0.00051 -0.01312 AFIX 137 H6A 2 0.914689 0.189568 0.542264 11.00000 -1.50000 H6B 2 0.937114 0.155107 0.603328 11.00000 -1.50000 H6C 2 0.848328 0.276315 0.582527 11.00000 -1.50000 AFIX 0 C7 1 0.743442 0.045170 0.620389 11.00000 0.04054 0.06089 = 0.02700 -0.00005 0.00328 0.01057 AFIX 137 H7A 2 0.720774 0.140602 0.632900 11.00000 -1.50000 H7B 2 0.798804 0.001850 0.646314 11.00000 -1.50000 H7C 2 0.679473 -0.019834 0.614937 11.00000 -1.50000 AFIX 0 C8 1 0.752348 -0.207701 0.552439 11.00000 0.06061 0.05086 = 0.04121 0.01100 0.01165 0.00034 AFIX 137 H8A 2 0.675295 -0.178391 0.544423 11.00000 -1.50000 H8B 2 0.765822 -0.238315 0.588992 11.00000 -1.50000 H8C 2 0.768182 -0.289445 0.529841 11.00000 -1.50000 AFIX 0 C9 1 0.945668 -0.120473 0.556079 11.00000 0.05121 0.07934 = 0.02980 0.01073 0.00303 0.02664 AFIX 137 H9A 2 0.959147 -0.213627 0.539027 11.00000 -1.50000 H9B 2 0.962316 -0.131363 0.593918 11.00000 -1.50000 H9C 2 0.992800 -0.044300 0.543720 11.00000 -1.50000 AFIX 0 C10 1 0.664067 0.119743 0.431183 11.00000 0.02808 0.02858 = 0.02485 0.00024 -0.00005 -0.00733 C11 1 0.691871 0.079991 0.381867 11.00000 0.02382 0.02588 = 0.02790 -0.00020 0.00233 -0.00208 AFIX 43 H11 2 0.753138 0.017577 0.379402 11.00000 -1.20000 AFIX 0 C12 1 0.631085 0.130547 0.336370 11.00000 0.01941 0.02057 = 0.01832 -0.00069 0.00287 -0.00276 C13 1 0.541512 0.221795 0.340217 11.00000 0.02649 0.02446 = 0.02520 0.00349 -0.00026 -0.00267 AFIX 43 H13 2 0.499401 0.256519 0.309485 11.00000 -1.20000 AFIX 0 C14 1 0.513479 0.262177 0.388490 11.00000 0.02359 0.03367 = 0.03800 -0.00113 0.00736 0.00278 AFIX 43 H14 2 0.452040 0.324362 0.390850 11.00000 -1.20000 AFIX 0 C15 1 0.574294 0.212619 0.433306 11.00000 0.03322 0.03945 = 0.02391 -0.00369 0.00728 -0.00099 AFIX 43 H15 2 0.554648 0.242331 0.466268 11.00000 -1.20000 AFIX 0 C16 1 0.659339 0.084736 0.283351 11.00000 0.01966 0.02058 = 0.02674 0.00217 0.00233 -0.00015 AFIX 23 H16A 2 0.739107 0.064041 0.285792 11.00000 -1.20000 H16B 2 0.643697 0.167414 0.258799 11.00000 -1.20000 AFIX 0 C18 1 0.634391 -0.124345 0.196652 11.00000 0.02144 0.02901 = 0.02780 -0.00467 0.00099 0.00054 AFIX 23 H18A 2 0.715276 -0.135051 0.202738 11.00000 -1.20000 H18B 2 0.603458 -0.221274 0.185814 11.00000 -1.20000 AFIX 0 C19 1 0.606423 -0.015956 0.151594 11.00000 0.02729 0.02967 = 0.02708 0.00481 0.00146 0.00104 AFIX 23 H19A 2 0.525617 -0.006428 0.144270 11.00000 -1.20000 H19B 2 0.636859 0.081673 0.161830 11.00000 -1.20000 AFIX 0 C20 1 0.653413 -0.067432 0.102591 11.00000 0.03372 0.03840 = 0.02567 -0.00338 0.00589 -0.00743 AFIX 23 H20A 2 0.734557 -0.071229 0.109451 11.00000 -1.20000 H20B 2 0.626688 -0.167774 0.093811 11.00000 -1.20000 AFIX 0 C21 1 0.620910 0.033115 0.056504 11.00000 0.04832 0.06066 = 0.03000 0.00368 0.00056 -0.00118 AFIX 137 H21A 2 0.540885 0.031408 0.047919 11.00000 -1.50000 H21B 2 0.655987 -0.000500 0.026370 11.00000 -1.50000 H21C 2 0.644891 0.133295 0.065493 11.00000 -1.50000 AFIX 0 C22 1 0.439874 -0.035584 0.246618 11.00000 0.02153 0.02456 = 0.02965 -0.00031 0.00203 0.00215 AFIX 23 H22A 2 0.412546 -0.017049 0.280654 11.00000 -1.20000 H22B 2 0.428120 0.054651 0.225430 11.00000 -1.20000 AFIX 0 C23 1 0.373199 -0.161049 0.218845 11.00000 0.02639 0.02535 = 0.03105 -0.00314 0.00025 -0.00248 AFIX 23 H23A 2 0.392170 -0.169275 0.182700 11.00000 -1.20000 H23B 2 0.393757 -0.254306 0.236984 11.00000 -1.20000 AFIX 0 C24 1 0.249836 -0.138239 0.217431 11.00000 0.02181 0.04323 = 0.04344 -0.00746 -0.00108 0.00241 AFIX 23 H24A 2 0.211695 -0.225120 0.201077 11.00000 -1.20000 H24B 2 0.231311 -0.131918 0.253697 11.00000 -1.20000 AFIX 0 C25 1 0.206517 -0.002945 0.188188 11.00000 0.03256 0.04044 = 0.07648 -0.00266 -0.01691 0.00168 AFIX 137 H25A 2 0.239641 0.084483 0.205542 11.00000 -1.50000 H25B 2 0.126466 0.001480 0.187728 11.00000 -1.50000 H25C 2 0.225355 -0.007077 0.152335 11.00000 -1.50000 AFIX 0 C26 1 0.610614 -0.223628 0.302198 11.00000 0.02442 0.02258 = 0.02933 -0.00161 0.00126 -0.00192 AFIX 23 H26A 2 0.599606 -0.316523 0.282490 11.00000 -1.20000 H26B 2 0.688706 -0.219767 0.317106 11.00000 -1.20000 AFIX 0 C27 1 0.539164 -0.227652 0.347427 11.00000 0.02287 0.02864 = 0.02964 0.00077 0.00309 -0.00332 AFIX 23 H27A 2 0.537138 -0.128759 0.363049 11.00000 -1.20000 H27B 2 0.463058 -0.255014 0.333799 11.00000 -1.20000 AFIX 0 C28 1 0.583050 -0.336240 0.389068 11.00000 0.04033 0.03279 = 0.03607 0.00638 0.00430 0.00456 AFIX 23 H28A 2 0.584477 -0.435021 0.373310 11.00000 -1.20000 H28B 2 0.659558 -0.309365 0.402159 11.00000 -1.20000 AFIX 0 C29 1 0.515490 -0.341675 0.434314 11.00000 0.06762 0.04768 = 0.03803 0.00825 0.01802 0.00727 AFIX 137 H29A 2 0.516051 -0.245131 0.450962 11.00000 -1.50000 H29B 2 0.546779 -0.414458 0.459704 11.00000 -1.50000 H29C 2 0.439721 -0.368968 0.421687 11.00000 -1.50000 AFIX 0 O2 3 0.705514 0.121045 0.530233 11.00000 0.03693 0.04517 = 0.02766 -0.00213 -0.00035 0.01048 O5 3 0.805345 -0.041975 0.487360 11.00000 0.03975 0.04303 = 0.02201 0.00121 0.00272 0.00975 P17 5 0.585072 -0.074440 0.257238 11.00000 0.01921 0.02108 = 0.02257 -0.00221 0.00136 0.00089 B1 7 0.726735 0.066529 0.483049 11.00000 0.02978 0.03405 = 0.02845 -0.00110 0.00305 -0.00446 MOLE 2 PART 1 B21 7 0.951159 -0.075029 0.291636 10.88000 0.06908 0.08332 = 0.07127 0.00776 -0.01565 -0.02117 F21 4 1.033645 -0.187320 0.289247 10.88000 0.02977 0.03549 = 0.03981 -0.00465 -0.00226 0.01367 F22 4 0.997885 0.046962 0.312356 10.88000 0.05157 0.02228 = 0.05132 -0.00042 -0.01288 -0.00460 F23 4 0.893324 -0.058793 0.244881 10.88000 0.04183 0.03665 = 0.03605 -0.00466 -0.01166 0.00521 F24 4 0.880330 -0.136217 0.326550 10.88000 0.03271 0.05133 = 0.06447 0.01712 0.01949 0.00293 PART 2 BR1 6 0.945099 -0.072637 0.290943 10.12000 0.01548 0.01843 = 0.01700 -0.00910 0.00445 -0.00087 HKLF 4 Covalent radii and connectivity table for 2009src0267 in P2(1)/n C 0.770 H 0.320 O 0.660 F 0.640 P 1.100 BR 1.140 B 0.820 C3 - O2 C6 C7 C4 C4 - O5 C9 C8 C3 C6 - C3 C7 - C3 C8 - C4 C9 - C4 C10 - C15 C11 B1 C11 - C12 C10 C12 - C13 C11 C16 C13 - C14 C12 C14 - C15 C13 C15 - C14 C10 C16 - C12 P17 C18 - C19 P17 C19 - C20 C18 C20 - C21 C19 C21 - C20 C22 - C23 P17 C23 - C24 C22 C24 - C25 C23 C25 - C24 C26 - C27 P17 C27 - C28 C26 C28 - C29 C27 C29 - C28 O2 - B1 C3 O5 - B1 C4 P17 - C26 C18 C22 C16 B1 - O2 O5 C10 B21_a - F22_a F23_a F24_a F21_a F21_a - B21_a F22_a - B21_a F23_a - B21_a F24_a - B21_a Br1_b - no bonds found 36613 Reflections read, of which 5993 rejected -14 =< h =< 14, -10 =< k =< 10, -30 =< l =< 30, Max. 2-theta = 50.00 0 Systematic absence violations 0 Inconsistent equivalents 5030 Unique reflections, of which 0 suppressed R(int) = 0.0867 R(sigma) = 0.0721 Friedel opposites merged Maximum memory for data reduction = 3780 / 49882 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 = 4793 / 409139 wR2 = 0.1603 before cycle 1 for 5030 data and 323 / 323 parameters GooF = S = 1.188; Restrained GooF = 1.188 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 7.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37126 0.00075 -0.005 OSF Mean shift/su = 0.001 Maximum = 0.011 for U22 P17 Max. shift = 0.000 A for B21_a Max. dU = 0.000 for C8 Largest correlation matrix elements -0.916 U33 Br1_b / U33 B21_a -0.905 z Br1_b / z B21_a -0.885 x Br1_b / x B21_a -0.906 U23 Br1_b / U23 B21_a -0.904 y Br1_b / y B21_a -0.865 U11 Br1_b / U11 B21_a -0.905 U22 Br1_b / U22 B21_a -0.896 U12 Br1_b / U12 B21_a -0.862 U13 Br1_b / U13 B21_a Idealized hydrogen atom generation before cycle 2 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H6A 0.9147 0.1896 0.5423 137 0.980 0.000 C6 C3 H6A H6B 0.9371 0.1551 0.6033 137 0.980 0.000 C6 C3 H6A H6C 0.8483 0.2763 0.5825 137 0.980 0.000 C6 C3 H6A H7A 0.7208 0.1406 0.6329 137 0.980 0.000 C7 C3 H7A H7B 0.7988 0.0019 0.6463 137 0.980 0.000 C7 C3 H7A H7C 0.6795 -0.0198 0.6149 137 0.980 0.000 C7 C3 H7A H8A 0.6753 -0.1784 0.5444 137 0.980 0.000 C8 C4 H8A H8B 0.7658 -0.2383 0.5890 137 0.980 0.000 C8 C4 H8A H8C 0.7682 -0.2894 0.5298 137 0.980 0.000 C8 C4 H8A H9A 0.9591 -0.2136 0.5390 137 0.980 0.000 C9 C4 H9A H9B 0.9623 -0.1314 0.5939 137 0.980 0.000 C9 C4 H9A H9C 0.9928 -0.0443 0.5437 137 0.980 0.000 C9 C4 H9A H11 0.7531 0.0176 0.3794 43 0.950 0.000 C11 C12 C10 H13 0.4994 0.2565 0.3095 43 0.950 0.000 C13 C14 C12 H14 0.4520 0.3244 0.3908 43 0.950 0.000 C14 C15 C13 H15 0.5546 0.2423 0.4663 43 0.950 0.000 C15 C14 C10 H16A 0.7391 0.0640 0.2858 23 0.990 0.000 C16 C12 P17 H16B 0.6437 0.1674 0.2588 23 0.990 0.000 C16 C12 P17 H18A 0.7153 -0.1351 0.2027 23 0.990 0.000 C18 C19 P17 H18B 0.6035 -0.2213 0.1858 23 0.990 0.000 C18 C19 P17 H19A 0.5256 -0.0064 0.1443 23 0.990 0.000 C19 C20 C18 H19B 0.6369 0.0817 0.1618 23 0.990 0.000 C19 C20 C18 H20A 0.7346 -0.0712 0.1095 23 0.990 0.000 C20 C21 C19 H20B 0.6267 -0.1678 0.0938 23 0.990 0.000 C20 C21 C19 H21A 0.5409 0.0314 0.0479 137 0.980 0.000 C21 C20 H21A H21B 0.6560 -0.0005 0.0264 137 0.980 0.000 C21 C20 H21A H21C 0.6449 0.1333 0.0655 137 0.980 0.000 C21 C20 H21A H22A 0.4125 -0.0170 0.2807 23 0.990 0.000 C22 C23 P17 H22B 0.4281 0.0546 0.2254 23 0.990 0.000 C22 C23 P17 H23A 0.3922 -0.1693 0.1827 23 0.990 0.000 C23 C24 C22 H23B 0.3938 -0.2543 0.2370 23 0.990 0.000 C23 C24 C22 H24A 0.2117 -0.2251 0.2011 23 0.990 0.000 C24 C25 C23 H24B 0.2313 -0.1319 0.2537 23 0.990 0.000 C24 C25 C23 H25A 0.2396 0.0845 0.2055 137 0.980 0.000 C25 C24 H25A H25B 0.1265 0.0015 0.1877 137 0.980 0.000 C25 C24 H25A H25C 0.2254 -0.0071 0.1523 137 0.980 0.000 C25 C24 H25A H26A 0.5996 -0.3165 0.2825 23 0.990 0.000 C26 C27 P17 H26B 0.6887 -0.2198 0.3171 23 0.990 0.000 C26 C27 P17 H27A 0.5371 -0.1288 0.3631 23 0.990 0.000 C27 C28 C26 H27B 0.4631 -0.2550 0.3338 23 0.990 0.000 C27 C28 C26 H28A 0.5845 -0.4350 0.3733 23 0.990 0.000 C28 C29 C27 H28B 0.6596 -0.3094 0.4022 23 0.990 0.000 C28 C29 C27 H29A 0.5161 -0.2451 0.4510 137 0.980 0.000 C29 C28 H29A H29B 0.5468 -0.4145 0.4597 137 0.980 0.000 C29 C28 H29A H29C 0.4397 -0.3690 0.4217 137 0.980 0.000 C29 C28 H29A 2009src0267 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C3 0.79219 0.06527 0.56897 1.00000 0.03069 0.04739 0.02502 0.00548 -0.00409 0.00660 0.03493 0.00821 0.00035 0.00056 0.00016 0.00000 0.00243 0.00296 0.00232 0.00228 0.00192 0.00228 0.00110 C4 0.82709 -0.07769 0.54314 1.00000 0.03355 0.05982 0.02141 0.00739 0.00171 0.00883 0.03837 0.00867 0.00036 0.00059 0.00016 0.00000 0.00252 0.00334 0.00228 0.00241 0.00194 0.00248 0.00117 C6 0.88093 0.18187 0.57479 1.00000 0.05400 0.05700 0.03380 0.00081 0.00051 -0.01312 0.04861 0.00864 0.00042 0.00060 0.00019 0.00000 0.00326 0.00357 0.00277 0.00261 0.00240 0.00281 0.00136 H6A 0.91469 0.18957 0.54226 1.00000 0.07292 0.00000 0.00000 H6B 0.93711 0.15511 0.60333 1.00000 0.07292 0.00000 0.00000 H6C 0.84833 0.27631 0.58253 1.00000 0.07292 0.00000 0.00000 C7 0.74344 0.04517 0.62039 1.00000 0.04054 0.06090 0.02700 -0.00005 0.00328 0.01057 0.04286 0.00898 0.00039 0.00059 0.00017 0.00000 0.00282 0.00365 0.00248 0.00246 0.00214 0.00257 0.00129 H7A 0.72077 0.14060 0.63290 1.00000 0.06429 0.00000 0.00000 H7B 0.79880 0.00185 0.64631 1.00000 0.06429 0.00000 0.00000 H7C 0.67947 -0.01983 0.61494 1.00000 0.06429 0.00000 0.00000 C8 0.75235 -0.20770 0.55244 1.00000 0.06062 0.05087 0.04121 0.01100 0.01165 0.00034 0.05045 0.00971 0.00044 0.00059 0.00020 0.00000 0.00349 0.00346 0.00304 0.00263 0.00263 0.00283 0.00140 H8A 0.67529 -0.17839 0.54442 1.00000 0.07567 0.00000 0.00000 H8B 0.76582 -0.23831 0.58899 1.00000 0.07567 0.00000 0.00000 H8C 0.76818 -0.28944 0.52984 1.00000 0.07567 0.00000 0.00000 C9 0.94567 -0.12047 0.55608 1.00000 0.05121 0.07935 0.02980 0.01073 0.00303 0.02664 0.05358 0.01012 0.00040 0.00066 0.00018 0.00000 0.00324 0.00429 0.00273 0.00273 0.00239 0.00300 0.00154 H9A 0.95915 -0.21362 0.53903 1.00000 0.08037 0.00000 0.00000 H9B 0.96232 -0.13136 0.59392 1.00000 0.08037 0.00000 0.00000 H9C 0.99280 -0.04430 0.54372 1.00000 0.08037 0.00000 0.00000 C10 0.66407 0.11974 0.43118 1.00000 0.02808 0.02858 0.02485 0.00024 -0.00005 -0.00733 0.02741 0.00721 0.00034 0.00047 0.00016 0.00000 0.00231 0.00248 0.00229 0.00191 0.00185 0.00189 0.00099 C11 0.69187 0.07999 0.38187 1.00000 0.02382 0.02588 0.02790 -0.00020 0.00233 -0.00208 0.02591 0.00705 0.00032 0.00047 0.00015 0.00000 0.00213 0.00235 0.00229 0.00200 0.00179 0.00191 0.00095 H11 0.75314 0.01758 0.37940 1.00000 0.03110 0.00000 0.00000 C12 0.63109 0.13055 0.33637 1.00000 0.01941 0.02058 0.01832 -0.00069 0.00287 -0.00276 0.01938 0.00670 0.00030 0.00043 0.00014 0.00000 0.00203 0.00214 0.00204 0.00172 0.00165 0.00169 0.00087 C13 0.54151 0.22179 0.34022 1.00000 0.02649 0.02446 0.02519 0.00349 -0.00026 -0.00267 0.02563 0.00720 0.00033 0.00045 0.00016 0.00000 0.00224 0.00241 0.00228 0.00190 0.00183 0.00186 0.00097 H13 0.49940 0.25652 0.30948 1.00000 0.03075 0.00000 0.00000 C14 0.51348 0.26218 0.38849 1.00000 0.02359 0.03367 0.03799 -0.00113 0.00736 0.00278 0.03146 0.00770 0.00034 0.00049 0.00017 0.00000 0.00226 0.00268 0.00269 0.00219 0.00202 0.00198 0.00106 H14 0.45204 0.32436 0.39085 1.00000 0.03775 0.00000 0.00000 C15 0.57429 0.21262 0.43331 1.00000 0.03322 0.03945 0.02391 -0.00369 0.00728 -0.00099 0.03188 0.00772 0.00035 0.00050 0.00016 0.00000 0.00251 0.00287 0.00237 0.00207 0.00200 0.00214 0.00108 H15 0.55465 0.24233 0.46627 1.00000 0.03826 0.00000 0.00000 C16 0.65934 0.08474 0.28335 1.00000 0.01966 0.02058 0.02674 0.00217 0.00233 -0.00015 0.02235 0.00680 0.00031 0.00044 0.00015 0.00000 0.00202 0.00219 0.00219 0.00188 0.00168 0.00175 0.00089 H16A 0.73911 0.06404 0.28579 1.00000 0.02682 0.00000 0.00000 H16B 0.64369 0.16741 0.25880 1.00000 0.02682 0.00000 0.00000 C18 0.63439 -0.12434 0.19665 1.00000 0.02144 0.02901 0.02780 -0.00467 0.00099 0.00054 0.02622 0.00738 0.00033 0.00047 0.00015 0.00000 0.00212 0.00242 0.00231 0.00193 0.00180 0.00183 0.00097 H18A 0.71528 -0.13505 0.20274 1.00000 0.03147 0.00000 0.00000 H18B 0.60346 -0.22127 0.18581 1.00000 0.03147 0.00000 0.00000 C19 0.60642 -0.01596 0.15159 1.00000 0.02729 0.02967 0.02708 0.00481 0.00146 0.00104 0.02814 0.00776 0.00034 0.00048 0.00015 0.00000 0.00229 0.00248 0.00234 0.00199 0.00184 0.00194 0.00100 H19A 0.52562 -0.00643 0.14427 1.00000 0.03377 0.00000 0.00000 H19B 0.63686 0.08167 0.16183 1.00000 0.03377 0.00000 0.00000 C20 0.65341 -0.06743 0.10259 1.00000 0.03372 0.03840 0.02567 -0.00338 0.00589 -0.00743 0.03240 0.00780 0.00035 0.00052 0.00015 0.00000 0.00244 0.00269 0.00228 0.00218 0.00190 0.00219 0.00104 H20A 0.73456 -0.07123 0.10945 1.00000 0.03888 0.00000 0.00000 H20B 0.62669 -0.16777 0.09381 1.00000 0.03888 0.00000 0.00000 C21 0.62091 0.03311 0.05650 1.00000 0.04832 0.06067 0.03000 0.00368 0.00056 -0.00118 0.04663 0.00901 0.00041 0.00059 0.00017 0.00000 0.00309 0.00373 0.00262 0.00250 0.00229 0.00267 0.00135 H21A 0.54088 0.03141 0.04792 1.00000 0.06995 0.00000 0.00000 H21B 0.65599 -0.00050 0.02637 1.00000 0.06995 0.00000 0.00000 H21C 0.64489 0.13329 0.06549 1.00000 0.06995 0.00000 0.00000 C22 0.43987 -0.03558 0.24662 1.00000 0.02153 0.02457 0.02965 -0.00031 0.00203 0.00215 0.02532 0.00695 0.00030 0.00045 0.00016 0.00000 0.00212 0.00239 0.00231 0.00192 0.00181 0.00175 0.00096 H22A 0.41255 -0.01705 0.28065 1.00000 0.03038 0.00000 0.00000 H22B 0.42812 0.05465 0.22543 1.00000 0.03038 0.00000 0.00000 C23 0.37320 -0.16105 0.21885 1.00000 0.02639 0.02535 0.03105 -0.00314 0.00025 -0.00248 0.02783 0.00700 0.00032 0.00046 0.00017 0.00000 0.00228 0.00248 0.00239 0.00199 0.00190 0.00187 0.00100 H23A 0.39217 -0.16928 0.18270 1.00000 0.03340 0.00000 0.00000 H23B 0.39376 -0.25430 0.23699 1.00000 0.03340 0.00000 0.00000 C24 0.24984 -0.13824 0.21743 1.00000 0.02181 0.04324 0.04343 -0.00746 -0.00108 0.00240 0.03653 0.00805 0.00033 0.00053 0.00018 0.00000 0.00234 0.00294 0.00287 0.00238 0.00207 0.00211 0.00116 H24A 0.21169 -0.22511 0.20108 1.00000 0.04384 0.00000 0.00000 H24B 0.23131 -0.13192 0.25370 1.00000 0.04384 0.00000 0.00000 C25 0.20652 -0.00294 0.18819 1.00000 0.03256 0.04044 0.07647 -0.00266 -0.01690 0.00168 0.05161 0.00888 0.00039 0.00055 0.00022 0.00000 0.00274 0.00312 0.00398 0.00291 0.00264 0.00238 0.00146 H25A 0.23964 0.08448 0.20554 1.00000 0.07742 0.00000 0.00000 H25B 0.12647 0.00148 0.18773 1.00000 0.07742 0.00000 0.00000 H25C 0.22535 -0.00708 0.15233 1.00000 0.07742 0.00000 0.00000 C26 0.61061 -0.22363 0.30220 1.00000 0.02442 0.02258 0.02932 -0.00161 0.00126 -0.00192 0.02558 0.00734 0.00032 0.00045 0.00016 0.00000 0.00222 0.00235 0.00233 0.00190 0.00184 0.00180 0.00096 H26A 0.59961 -0.31652 0.28249 1.00000 0.03070 0.00000 0.00000 H26B 0.68871 -0.21977 0.31711 1.00000 0.03070 0.00000 0.00000 C27 0.53916 -0.22765 0.34743 1.00000 0.02287 0.02864 0.02964 0.00077 0.00309 -0.00332 0.02704 0.00756 0.00033 0.00047 0.00016 0.00000 0.00218 0.00249 0.00236 0.00196 0.00184 0.00187 0.00099 H27A 0.53714 -0.12876 0.36305 1.00000 0.03245 0.00000 0.00000 H27B 0.46306 -0.25501 0.33380 1.00000 0.03245 0.00000 0.00000 C28 0.58305 -0.33624 0.38907 1.00000 0.04033 0.03279 0.03606 0.00638 0.00430 0.00456 0.03640 0.00865 0.00038 0.00051 0.00017 0.00000 0.00271 0.00279 0.00268 0.00223 0.00219 0.00219 0.00114 H28A 0.58448 -0.43502 0.37331 1.00000 0.04368 0.00000 0.00000 H28B 0.65956 -0.30937 0.40216 1.00000 0.04368 0.00000 0.00000 C29 0.51549 -0.34167 0.43431 1.00000 0.06762 0.04768 0.03803 0.00825 0.01802 0.00727 0.05019 0.01007 0.00044 0.00059 0.00019 0.00000 0.00368 0.00341 0.00288 0.00258 0.00264 0.00284 0.00141 H29A 0.51605 -0.24514 0.45096 1.00000 0.07528 0.00000 0.00000 H29B 0.54678 -0.41446 0.45970 1.00000 0.07528 0.00000 0.00000 H29C 0.43972 -0.36897 0.42169 1.00000 0.07528 0.00000 0.00000 O2 0.70551 0.12105 0.53023 1.00000 0.03693 0.04518 0.02766 -0.00213 -0.00035 0.01048 0.03690 0.00540 0.00024 0.00035 0.00011 0.00000 0.00179 0.00202 0.00168 0.00148 0.00139 0.00152 0.00079 O5 0.80534 -0.04197 0.48736 1.00000 0.03975 0.04304 0.02201 0.00121 0.00272 0.00975 0.03500 0.00533 0.00024 0.00034 0.00010 0.00000 0.00181 0.00206 0.00155 0.00144 0.00134 0.00155 0.00078 P17 0.58507 -0.07444 0.25724 1.00000 0.01921 0.02109 0.02257 -0.00221 0.00136 0.00089 0.02103 0.00186 0.00008 0.00012 0.00004 0.00000 0.00052 0.00057 0.00055 0.00049 0.00042 0.00046 0.00026 B1 0.72674 0.06653 0.48305 1.00000 0.02978 0.03405 0.02845 -0.00110 0.00305 -0.00446 0.03078 0.00903 0.00040 0.00061 0.00019 0.00000 0.00274 0.00299 0.00272 0.00247 0.00220 0.00243 0.00117 B21_a 0.95116 -0.07503 0.29164 0.88000 0.06904 0.08325 0.07136 0.00773 -0.01565 -0.02123 0.07638 0.04580 0.00198 0.00296 0.00093 0.00000 0.01507 0.01731 0.01575 0.01339 0.01149 0.01381 0.00764 F21_a 1.03365 -0.18732 0.28925 0.88000 0.02977 0.03549 0.03980 -0.00465 -0.00226 0.01367 0.03550 0.00494 0.00023 0.00032 0.00011 0.00000 0.00159 0.00175 0.00175 0.00141 0.00131 0.00145 0.00072 F22_a 0.99788 0.04696 0.31236 0.88000 0.05157 0.02228 0.05132 -0.00042 -0.01288 -0.00460 0.04317 0.00543 0.00025 0.00032 0.00012 0.00000 0.00194 0.00169 0.00196 0.00147 0.00157 0.00148 0.00081 F23_a 0.89332 -0.05879 0.24488 0.88000 0.04183 0.03665 0.03605 -0.00466 -0.01166 0.00521 0.03942 0.00498 0.00023 0.00032 0.00011 0.00000 0.00175 0.00176 0.00175 0.00147 0.00140 0.00143 0.00075 F24_a 0.88033 -0.13622 0.32655 0.88000 0.03271 0.05134 0.06447 0.01712 0.01949 0.00293 0.04843 0.00604 0.00024 0.00036 0.00013 0.00000 0.00171 0.00206 0.00220 0.00177 0.00159 0.00154 0.00086 Br1_b 0.94510 -0.07264 0.29094 0.12000 0.01549 0.01845 0.01697 -0.00909 0.00445 -0.00085 0.01677 0.01628 0.00071 0.00096 0.00031 0.00000 0.00381 0.00419 0.00438 0.00367 0.00333 0.00364 0.00196 Final Structure Factor Calculation for 2009src0267 in P2(1)/n Total number of l.s. parameters = 323 Maximum vector length = 511 Memory required = 4470 / 26061 wR2 = 0.1603 before cycle 2 for 5030 data and 0 / 323 parameters GooF = S = 1.188; Restrained GooF = 1.188 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 7.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0856 for 3524 Fo > 4sig(Fo) and 0.1320 for all 5030 data wR2 = 0.1603, GooF = S = 1.188, Restrained GooF = 1.188 for all data Occupancy sum of asymmetric unit = 33.52 for non-hydrogen and 45.00 for hydrogen atoms Principal mean square atomic displacements U 0.0499 0.0362 0.0187 C3 0.0633 0.0322 0.0197 C4 0.0696 0.0431 0.0332 C6 0.0655 0.0361 0.0270 C7 0.0627 0.0562 0.0325 C8 0.0958 0.0394 0.0255 C9 0.0365 0.0253 0.0204 C10 0.0281 0.0271 0.0225 C11 0.0229 0.0181 0.0171 C12 0.0322 0.0233 0.0213 C13 0.0386 0.0344 0.0213 C14 0.0406 0.0337 0.0213 C15 0.0275 0.0200 0.0196 C16 0.0336 0.0240 0.0211 C18 0.0334 0.0281 0.0229 C19 0.0444 0.0283 0.0245 C20 0.0614 0.0493 0.0292 C21 0.0300 0.0256 0.0204 C22 0.0334 0.0284 0.0218 C23 0.0523 0.0361 0.0212 C24 0.0896 0.0402 0.0250 C25 0.0303 0.0256 0.0209 C26 0.0308 0.0291 0.0213 C27 0.0435 0.0386 0.0272 C28 0.0739 0.0462 0.0305 C29 0.0535 0.0308 0.0264 O2 0.0513 0.0317 0.0219 O5 0.0247 0.0196 0.0189 P17 0.0369 0.0287 0.0268 B1 0.1132 0.0702 0.0457 B21_a 0.0528 0.0351 0.0187 F21_a 0.0728 0.0355 0.0212 F22_a 0.0598 0.0343 0.0242 F23_a 0.0786 0.0419 0.0248 F24_a 0.0270 0.0153 0.0080 Br1_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.016 0.025 0.034 0.045 0.057 0.071 0.092 0.133 1.000 Number in group 507. 507. 532. 497. 519. 480. 482. 514. 486. 506. GooF 1.241 1.356 1.341 1.233 1.275 1.170 1.139 1.137 0.980 0.909 K 12.065 2.897 1.554 1.180 1.115 1.069 1.019 1.001 0.984 1.006 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.26 1.44 1.81 inf Number in group 525. 480. 512. 497. 507. 506. 495. 498. 507. 503. GooF 1.310 1.359 1.315 1.312 1.259 1.136 1.076 1.016 0.934 1.080 K 1.212 1.163 1.110 1.083 1.050 1.005 0.977 0.994 0.997 1.010 R1 0.310 0.283 0.247 0.199 0.165 0.119 0.098 0.073 0.053 0.035 Recommended weighting scheme: WGHT 0.0000 7.5837 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) -12 5 7 168.43 10.29 3.71 0.012 0.88 -11 2 12 257.36 42.08 3.69 0.025 1.01 -6 4 10 109.78 1.45 3.42 0.005 1.36 3 6 16 195.99 10.32 3.33 0.012 1.04 4 2 26 827.30 410.85 3.30 0.077 0.89 -6 9 11 272.07 41.00 3.26 0.024 0.86 10 4 12 201.74 9.08 3.23 0.011 0.92 7 6 16 276.96 29.09 3.20 0.020 0.90 -2 8 17 252.49 30.80 3.20 0.021 0.91 -10 7 8 273.37 14.92 3.17 0.015 0.88 3 9 5 -4.40 136.00 3.16 0.044 0.96 -2 5 23 159.97 9.91 3.15 0.012 0.95 7 2 24 -60.05 107.08 3.14 0.039 0.85 8 6 7 246.03 86.26 3.14 0.035 1.01 3 3 24 151.19 0.24 3.13 0.002 0.95 -9 1 21 247.12 18.42 3.11 0.016 0.96 -6 5 2 118.62 2.65 3.10 0.006 1.36 2 1 26 204.50 36.23 3.08 0.023 0.95 9 5 9 142.35 7.85 3.04 0.011 0.99 -12 0 10 111.44 397.07 3.00 0.076 0.98 5 0 25 215.48 524.41 2.96 0.087 0.91 10 2 19 431.89 198.13 2.95 0.053 0.84 12 4 2 219.50 57.85 2.95 0.029 0.92 -10 1 19 931.94 559.97 2.95 0.090 0.95 -11 3 15 160.82 26.10 2.93 0.019 0.93 -12 4 8 146.09 20.61 2.92 0.017 0.92 2 4 18 257.23 93.52 2.91 0.037 1.16 3 9 15 371.11 58.64 2.90 0.029 0.84 -3 1 25 129.53 16.34 2.88 0.015 1.02 1 3 10 83.98 16.95 2.88 0.016 1.91 -6 9 1 198.41 3.54 2.88 0.007 0.91 2 3 21 139.22 1.40 2.86 0.004 1.09 -3 6 23 521.45 260.17 2.85 0.061 0.90 -2 4 5 61.72 0.08 2.84 0.001 2.00 8 5 18 741.80 334.00 2.84 0.069 0.87 -2 9 8 223.96 9.22 2.84 0.012 0.96 7 5 14 127.29 16.59 2.83 0.015 1.00 6 0 2 12480.59 11171.00 2.83 0.401 1.97 -7 2 18 64.83 207.39 2.83 0.055 1.13 -11 1 8 173.54 44.06 2.81 0.025 1.08 4 4 24 197.91 16.35 2.81 0.015 0.90 9 6 8 143.04 2.90 2.80 0.006 0.94 -2 7 5 -9.16 129.63 2.79 0.043 1.24 5 6 19 192.92 36.66 2.78 0.023 0.91 2 4 15 266.27 452.13 2.78 0.081 1.31 -5 2 27 130.01 17.34 2.77 0.016 0.90 8 4 0 78.36 4.76 2.76 0.008 1.27 1 7 15 249.81 75.21 2.75 0.033 1.03 -6 8 5 254.39 110.73 2.75 0.040 0.99 -8 3 23 -57.66 86.84 2.74 0.035 0.91 Bond lengths and angles C3 - Distance Angles O2 1.4642 (0.0048) C6 1.5162 (0.0065) 106.21 (0.38) C7 1.5276 (0.0059) 108.09 (0.35) 110.19 (0.40) C4 1.5475 (0.0067) 102.30 (0.33) 113.85 (0.39) 115.33 (0.41) C3 - O2 C6 C7 C4 - Distance Angles O5 1.4710 (0.0048) C9 1.5042 (0.0062) 109.70 (0.35) C8 1.5341 (0.0068) 106.26 (0.37) 110.05 (0.44) C3 1.5475 (0.0067) 101.95 (0.35) 115.49 (0.42) 112.67 (0.37) C4 - O5 C9 C8 C6 - Distance Angles C3 1.5162 (0.0065) H6A 0.9800 109.47 H6B 0.9800 109.47 109.47 H6C 0.9800 109.47 109.47 109.47 C6 - C3 H6A H6B C7 - Distance Angles C3 1.5276 (0.0059) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C3 H7A H7B C8 - Distance Angles C4 1.5341 (0.0068) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C4 H8A H8B C9 - Distance Angles C4 1.5042 (0.0062) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - C4 H9A H9B C10 - Distance Angles C15 1.3944 (0.0058) C11 1.4028 (0.0055) 117.85 (0.38) B1 1.5438 (0.0064) 118.25 (0.38) 123.90 (0.40) C10 - C15 C11 C11 - Distance Angles C12 1.3954 (0.0053) C10 1.4028 (0.0055) 121.13 (0.39) H11 0.9500 119.43 119.43 C11 - C12 C10 C12 - Distance Angles C13 1.3899 (0.0054) C11 1.3954 (0.0053) 119.18 (0.36) C16 1.5088 (0.0051) 119.71 (0.35) 121.10 (0.35) C12 - C13 C11 C13 - Distance Angles C14 1.3802 (0.0057) C12 1.3899 (0.0054) 120.29 (0.39) H13 0.9500 119.86 119.86 C13 - C14 C12 C14 - Distance Angles C15 1.3789 (0.0058) C13 1.3802 (0.0057) 120.26 (0.41) H14 0.9500 119.87 119.87 C14 - C15 C13 C15 - Distance Angles C14 1.3789 (0.0058) C10 1.3944 (0.0058) 121.28 (0.40) H15 0.9500 119.36 119.36 C15 - C14 C10 C16 - Distance Angles C12 1.5088 (0.0051) P17 1.8034 (0.0040) 113.84 (0.27) H16A 0.9900 108.79 108.79 H16B 0.9900 108.79 108.79 107.67 C16 - C12 P17 H16A C18 - Distance Angles C19 1.5356 (0.0056) P17 1.7986 (0.0040) 115.32 (0.29) H18A 0.9900 108.44 108.44 H18B 0.9900 108.44 108.44 107.48 C18 - C19 P17 H18A C19 - Distance Angles C20 1.5228 (0.0055) C18 1.5356 (0.0056) 110.97 (0.35) H19A 0.9900 109.44 109.44 H19B 0.9900 109.44 109.44 108.04 C19 - C20 C18 H19A C20 - Distance Angles C21 1.5193 (0.0061) C19 1.5228 (0.0055) 111.98 (0.39) H20A 0.9900 109.22 109.22 H20B 0.9900 109.22 109.22 107.91 C20 - C21 C19 H20A C21 - Distance Angles C20 1.5193 (0.0061) 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 C23 1.5357 (0.0054) P17 1.8034 (0.0038) 112.76 (0.28) H22A 0.9900 109.04 109.04 H22B 0.9900 109.04 109.04 107.81 C22 - C23 P17 H22A C23 - Distance Angles C24 1.5215 (0.0054) C22 1.5357 (0.0054) 112.51 (0.35) H23A 0.9900 109.10 109.10 H23B 0.9900 109.10 109.10 107.84 C23 - C24 C22 H23A C24 - Distance Angles C25 1.5115 (0.0065) C23 1.5215 (0.0054) 114.50 (0.40) H24A 0.9900 108.64 108.64 H24B 0.9900 108.64 108.64 107.58 C24 - C25 C23 H24A C25 - Distance Angles C24 1.5115 (0.0065) H25A 0.9800 109.47 H25B 0.9800 109.47 109.47 H25C 0.9800 109.47 109.47 109.47 C25 - C24 H25A H25B C26 - Distance Angles C27 1.5376 (0.0054) P17 1.7934 (0.0041) 115.94 (0.29) H26A 0.9900 108.30 108.30 H26B 0.9900 108.30 108.30 107.40 C26 - C27 P17 H26A C27 - Distance Angles C28 1.5149 (0.0057) C26 1.5376 (0.0054) 111.59 (0.35) H27A 0.9900 109.30 109.30 H27B 0.9900 109.30 109.30 107.96 C27 - C28 C26 H27A C28 - Distance Angles C29 1.5076 (0.0060) C27 1.5149 (0.0057) 112.94 (0.39) H28A 0.9900 109.00 109.00 H28B 0.9900 109.00 109.00 107.78 C28 - C29 C27 H28A C29 - Distance Angles C28 1.5076 (0.0060) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - C28 H29A H29B O2 - Distance Angles B1 1.3681 (0.0056) C3 1.4642 (0.0048) 106.57 (0.34) O2 - B1 O5 - Distance Angles B1 1.3768 (0.0059) C4 1.4710 (0.0048) 106.57 (0.33) O5 - B1 P17 - Distance Angles C26 1.7934 (0.0041) C18 1.7986 (0.0040) 108.64 (0.20) C22 1.8034 (0.0038) 110.11 (0.19) 109.93 (0.19) C16 1.8034 (0.0040) 109.05 (0.19) 108.90 (0.19) 110.18 (0.19) P17 - C26 C18 C22 B1 - Distance Angles O2 1.3681 (0.0056) O5 1.3768 (0.0059) 113.07 (0.39) C10 1.5438 (0.0064) 122.13 (0.43) 124.76 (0.41) B1 - O2 O5 B21_a - Distance Angles F22_a 1.3354 (0.0256) F23_a 1.3363 (0.0240) 115.34 (1.99) F24_a 1.4337 (0.0246) 109.59 (1.58) 108.35 (1.71) F21_a 1.4453 (0.0235) 109.79 (1.67) 109.94 (1.57) 103.11 (1.72) B21_a - F22_a F23_a F24_a F21_a - Distance Angles B21_a 1.4453 (0.0235) F21_a - F22_a - Distance Angles B21_a 1.3354 (0.0257) F22_a - F23_a - Distance Angles B21_a 1.3363 (0.0240) F23_a - F24_a - Distance Angles B21_a 1.4337 (0.0247) F24_a - FMAP and GRID set by program FMAP 2 3 28 GRID -1.000 -2 -2 1.000 2 2 R1 = 0.1296 for 5030 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.4620 0.3035 0.1765 [ 0.88 A from F21 ] Deepest hole -0.28 at 0.7071 0.0790 0.1496 [ 0.95 A from H19B ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 4119 / 22499 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.0380 -0.1965 0.3235 1.00000 0.05 0.28 0.88 F21 1.68 B21 1.75 BR1 1.92 H6B Q2 1 0.8405 0.0072 0.4403 1.00000 0.05 0.28 1.41 O5 1.80 H11 1.95 B1 2.06 H9C Q3 1 0.6285 -0.0719 0.1271 1.00000 0.05 0.28 0.73 C20 0.88 C19 1.22 H20B 1.42 H20A Q4 1 0.7551 -0.0011 0.2914 1.00000 0.05 0.27 0.64 H16A 1.41 C16 2.09 F24 2.16 H16B Q5 1 0.5002 -0.0581 0.2588 1.00000 0.05 0.26 0.80 C22 1.06 P17 1.32 H22A 1.55 H22B Q6 1 0.4387 -0.0807 0.0714 1.00000 0.05 0.26 1.78 H21A 2.08 H9A 2.16 H19A 2.44 H20B Q7 1 0.6157 -0.1764 0.2697 1.00000 0.05 0.26 0.95 C26 1.04 P17 1.34 H26A 1.49 H26B Q8 1 0.6741 -0.1681 0.1022 1.00000 0.05 0.26 0.60 H20B 0.95 C20 1.15 H20A 2.12 C19 Q9 1 0.0784 -0.0271 0.2516 1.00000 0.05 0.25 1.83 H25B 1.87 F21 2.01 B21 2.06 F22 Q10 1 0.7722 -0.1548 0.4009 1.00000 0.05 0.25 1.68 H11 1.98 H28B 2.31 H21C 2.36 H26B Shortest distances between peaks (including symmetry equivalents) 3 8 1.25 5 7 1.78 2 10 1.93 4 7 2.36 1 9 2.51 3 6 2.59 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 1.70: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.80: Structure factors and derivatives 0.81: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.08: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.16: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0267 finished at 11:57:14 Total CPU time: 3.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++