+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0719 started at 19:45:57 on 14-Jun-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0719 in P2(1)/n CELL 0.71073 9.3182 15.1558 18.9653 90.000 99.587 90.000 ZERR 4.00 0.0001 0.0002 0.0002 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H B N O UNIT 128 124 4 8 8 V = 2640.96 F(000) = 1032.0 Mu = 0.08 mm-1 Cell Wt = 1945.59 Rho = 1.223 MERG 2 OMIT -3.00 55.00 OMIT 0 4 1 OMIT 2 1 0 OMIT 1 1 4 OMIT -1 1 4 OMIT 1 1 3 OMIT 1 1 1 FMAP 2 PLAN 20 SIZE 0.20 0.20 0.60 ACTA BOND WGHT 0.03940 1.02070 L.S. 4 TEMP -153.00 FVAR 0.81160 C1 1 0.664596 0.051543 0.215057 11.00000 0.01911 0.02932 = 0.02260 0.00444 0.00330 0.00364 C2 1 0.777884 0.173809 0.157005 11.00000 0.03007 0.03846 = 0.03917 0.01133 0.01295 -0.00248 AFIX 137 H2A 2 0.705159 0.210041 0.175353 11.00000 -1.50000 H2B 2 0.767354 0.181215 0.105064 11.00000 -1.50000 H2C 2 0.875650 0.192333 0.179415 11.00000 -1.50000 AFIX 0 C3 1 0.840183 0.015872 0.141026 11.00000 0.02831 0.04473 = 0.03835 0.00936 0.01550 0.01140 AFIX 137 H3A 2 0.810554 -0.043568 0.153017 11.00000 -1.50000 H3B 2 0.944108 0.023952 0.159200 11.00000 -1.50000 H3C 2 0.822146 0.023419 0.088979 11.00000 -1.50000 AFIX 0 C4 1 0.356372 0.062373 0.241772 11.00000 0.02134 0.03023 = 0.01997 -0.00186 0.00113 -0.00016 AFIX 43 H4 2 0.336460 0.061195 0.190998 11.00000 -1.20000 AFIX 0 C5 1 0.256446 0.031802 0.281813 11.00000 0.02111 0.03081 = 0.02861 -0.00475 0.00397 -0.00408 AFIX 43 H5 2 0.166052 0.008414 0.258861 11.00000 -1.20000 AFIX 0 C6 1 0.288368 0.035310 0.355818 11.00000 0.02677 0.02400 = 0.02810 0.00211 0.01162 0.00152 AFIX 43 H6 2 0.219612 0.014490 0.383700 11.00000 -1.20000 AFIX 0 C7 1 0.420639 0.069203 0.389150 11.00000 0.02973 0.02529 = 0.01885 -0.00035 0.00489 0.00535 AFIX 43 H7 2 0.442950 0.071785 0.439844 11.00000 -1.20000 AFIX 0 C8 1 0.519173 0.099031 0.348152 11.00000 0.02132 0.02338 = 0.02128 -0.00306 -0.00012 0.00310 AFIX 43 H8 2 0.610437 0.122620 0.369723 11.00000 -1.20000 AFIX 0 C9 1 0.187380 -0.208412 0.369883 11.00000 0.01972 0.01686 = 0.01929 0.00029 0.00251 -0.00223 C10 1 0.247176 -0.229299 0.308312 11.00000 0.02316 0.02336 = 0.02194 -0.00009 0.00485 0.00139 AFIX 43 H10 2 0.339524 -0.257406 0.314137 11.00000 -1.20000 AFIX 0 C11 1 0.176475 -0.210432 0.239394 11.00000 0.03823 0.02610 = 0.01929 -0.00149 0.00638 -0.00090 AFIX 43 H11 2 0.221329 -0.224982 0.199455 11.00000 -1.20000 AFIX 0 C12 1 0.040622 -0.170418 0.228876 11.00000 0.03764 0.02692 = 0.01889 0.00245 -0.00410 -0.00006 AFIX 43 H12 2 -0.008786 -0.158338 0.181903 11.00000 -1.20000 AFIX 0 C13 1 -0.022043 -0.148298 0.287942 11.00000 0.02277 0.02415 = 0.02864 0.00215 -0.00246 0.00231 AFIX 43 H13 2 -0.114494 -0.120269 0.281537 11.00000 -1.20000 AFIX 0 C14 1 0.050748 -0.167220 0.356910 11.00000 0.02119 0.02143 = 0.02168 -0.00036 0.00299 -0.00056 AFIX 43 H14 2 0.005791 -0.151528 0.396562 11.00000 -1.20000 AFIX 0 C15 1 0.200404 -0.201390 0.515929 11.00000 0.01415 0.02450 = 0.01790 -0.00095 0.00115 0.00033 C16 1 0.171402 -0.110668 0.520981 11.00000 0.01784 0.02456 = 0.02122 -0.00154 0.00088 0.00064 AFIX 43 H16 2 0.191467 -0.072699 0.483971 11.00000 -1.20000 AFIX 0 C17 1 0.114396 -0.073963 0.578030 11.00000 0.01795 0.02959 = 0.02912 -0.00926 -0.00027 0.00327 AFIX 43 H17 2 0.094428 -0.012525 0.578643 11.00000 -1.20000 AFIX 0 C18 1 0.086946 -0.127318 0.633819 11.00000 0.01913 0.04636 = 0.02383 -0.01167 0.00545 0.00022 AFIX 43 H18 2 0.047959 -0.102846 0.672700 11.00000 -1.20000 AFIX 0 C19 1 0.117212 -0.216784 0.632001 11.00000 0.02807 0.04250 = 0.02037 -0.00044 0.00717 -0.00310 AFIX 43 H19 2 0.100764 -0.253790 0.670292 11.00000 -1.20000 AFIX 0 C20 1 0.171858 -0.252632 0.573963 11.00000 0.02492 0.02745 = 0.02135 0.00032 0.00459 0.00074 AFIX 43 H20 2 0.190559 -0.314237 0.573647 11.00000 -1.20000 AFIX 0 C21 1 0.243630 -0.350753 0.444106 11.00000 0.01967 0.02138 = 0.01383 0.00149 0.00223 0.00078 C22 1 0.100983 -0.384125 0.439887 11.00000 0.02082 0.02606 = 0.01853 0.00057 0.00449 -0.00038 AFIX 43 H22 2 0.023993 -0.343935 0.442882 11.00000 -1.20000 AFIX 0 C23 1 0.068769 -0.473307 0.431537 11.00000 0.02693 0.03077 = 0.01979 0.00302 0.00408 -0.00827 AFIX 43 H23 2 -0.028830 -0.492884 0.428907 11.00000 -1.20000 AFIX 0 C24 1 0.178415 -0.534109 0.427003 11.00000 0.03943 0.02026 = 0.02666 0.00217 0.00347 -0.00623 AFIX 43 H24 2 0.156625 -0.595212 0.421553 11.00000 -1.20000 AFIX 0 C25 1 0.320238 -0.504290 0.430550 11.00000 0.03168 0.02194 = 0.02601 0.00100 0.00265 0.00438 AFIX 43 H25 2 0.396360 -0.545061 0.427419 11.00000 -1.20000 AFIX 0 C26 1 0.351179 -0.413948 0.438759 11.00000 0.02096 0.02289 = 0.02012 0.00138 0.00265 0.00127 AFIX 43 H26 2 0.448865 -0.394819 0.440775 11.00000 -1.20000 AFIX 0 C27 1 0.444823 -0.217662 0.462450 11.00000 0.01870 0.01824 = 0.01933 -0.00410 0.00437 0.00183 C28 1 0.542075 -0.255796 0.519132 11.00000 0.02292 0.02235 = 0.01987 -0.00165 0.00303 0.00149 AFIX 43 H28 2 0.505426 -0.297228 0.549264 11.00000 -1.20000 AFIX 0 C29 1 0.689740 -0.235172 0.532737 11.00000 0.02129 0.02988 = 0.02374 -0.00605 -0.00127 0.00586 AFIX 43 H29 2 0.751438 -0.262946 0.571298 11.00000 -1.20000 AFIX 0 C30 1 0.747618 -0.174290 0.490369 11.00000 0.01764 0.03485 = 0.03040 -0.01184 0.00470 -0.00236 AFIX 43 H30 2 0.848438 -0.160420 0.499347 11.00000 -1.20000 AFIX 0 C31 1 0.655185 -0.134277 0.434785 11.00000 0.02443 0.02693 = 0.02953 -0.00347 0.00906 -0.00581 AFIX 43 H31 2 0.692389 -0.091925 0.405599 11.00000 -1.20000 AFIX 0 C32 1 0.507410 -0.155988 0.421491 11.00000 0.02157 0.02081 = 0.02330 -0.00042 0.00380 0.00061 AFIX 43 H32 2 0.446510 -0.127681 0.382938 11.00000 -1.20000 AFIX 0 B1 3 0.270441 -0.243173 0.448702 11.00000 0.01618 0.01989 = 0.01676 0.00068 0.00325 0.00063 N1 4 0.482753 0.093868 0.276865 11.00000 0.01795 0.02128 = 0.02027 0.00160 0.00589 0.00066 N2 4 0.756273 0.081219 0.173663 11.00000 0.02150 0.03408 = 0.02780 0.00791 0.00868 0.00373 O1 5 0.583192 0.124472 0.236332 11.00000 0.02216 0.02524 = 0.02790 0.00466 0.01069 -0.00042 O2 5 0.643697 -0.022328 0.233954 11.00000 0.03012 0.02847 = 0.03759 0.01037 0.01453 0.00724 HKLF 4 Covalent radii and connectivity table for 2007src0719 in P2(1)/n C 0.770 H 0.320 B 0.820 N 0.700 O 0.660 C1 - O2 N2 O1 C2 - N2 C3 - N2 C4 - N1 C5 C5 - C4 C6 C6 - C5 C7 C7 - C8 C6 C8 - N1 C7 C9 - C14 C10 B1 C10 - C11 C9 C11 - C12 C10 C12 - C11 C13 C13 - C12 C14 C14 - C13 C9 C15 - C16 C20 B1 C16 - C17 C15 C17 - C18 C16 C18 - C19 C17 C19 - C18 C20 C20 - C19 C15 C21 - C26 C22 B1 C22 - C23 C21 C23 - C22 C24 C24 - C25 C23 C25 - C24 C26 C26 - C21 C25 C27 - C32 C28 B1 C28 - C29 C27 C29 - C30 C28 C30 - C31 C29 C31 - C30 C32 C32 - C31 C27 B1 - C27 C21 C9 C15 N1 - C8 C4 O1 N2 - C1 C2 C3 O1 - N1 C1 O2 - C1 h k l Fo^2 Sigma Why rejected -3 0 4 16.99 2.53 observed but should be systematically absent 32693 Reflections read, of which 798 rejected -12 =< h =< 12, -19 =< k =< 19, -22 =< l =< 24, Max. 2-theta = 54.99 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 4 11 11 0.34 0.78 6 4.67 1 Inconsistent equivalents 6042 Unique reflections, of which 0 suppressed R(int) = 0.0372 R(sigma) = 0.0308 Friedel opposites merged Maximum memory for data reduction = 3097 / 59964 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 = 4045 / 424697 wR2 = 0.1010 before cycle 1 for 6042 data and 336 / 336 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0394 * P )^2 + 1.02 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80976 0.00110 -1.677 OSF Mean shift/esd = 0.220 Maximum = -1.677 for OSF Max. shift = 0.003 A for H3A Max. dU = 0.000 for O1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4045 / 424697 wR2 = 0.1008 before cycle 2 for 6042 data and 336 / 336 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0394 * P )^2 + 1.02 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80895 0.00109 -0.744 OSF Mean shift/esd = 0.077 Maximum = -0.744 for OSF Max. shift = 0.002 A for H2B Max. dU = 0.000 for O1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4045 / 424697 wR2 = 0.1008 before cycle 3 for 6042 data and 336 / 336 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0394 * P )^2 + 1.02 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80894 0.00109 -0.011 OSF Mean shift/esd = 0.003 Maximum = -0.098 for tors H2A Max. shift = 0.001 A for H2C Max. dU = 0.000 for C28 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4045 / 424697 wR2 = 0.1008 before cycle 4 for 6042 data and 336 / 336 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0394 * P )^2 + 1.02 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80894 0.00109 -0.002 OSF Mean shift/esd = 0.001 Maximum = -0.048 for tors H2A Max. shift = 0.001 A for H2C Max. dU = 0.000 for C17 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 H2A 0.7048 0.2101 0.1751 137 0.980 0.000 C2 N2 H2A H2B 0.7681 0.1812 0.1051 137 0.980 0.000 C2 N2 H2A H2C 0.8755 0.1925 0.1797 137 0.980 0.000 C2 N2 H2A H3A 0.8110 -0.0435 0.1532 137 0.980 0.000 C3 N2 H3A H3B 0.9442 0.0242 0.1591 137 0.980 0.000 C3 N2 H3A H3C 0.8219 0.0233 0.0890 137 0.980 0.000 C3 N2 H3A H4 0.3364 0.0613 0.1910 43 0.950 0.000 C4 N1 C5 H5 0.1661 0.0083 0.2589 43 0.950 0.000 C5 C4 C6 H6 0.2196 0.0146 0.3837 43 0.950 0.000 C6 C5 C7 H7 0.4430 0.0717 0.4398 43 0.950 0.000 C7 C8 C6 H8 0.6105 0.1226 0.3697 43 0.950 0.000 C8 N1 C7 H10 0.3395 -0.2574 0.3141 43 0.950 0.000 C10 C11 C9 H11 0.2213 -0.2250 0.1995 43 0.950 0.000 C11 C12 C10 H12 -0.0088 -0.1583 0.1819 43 0.950 0.000 C12 C11 C13 H13 -0.1145 -0.1203 0.2815 43 0.950 0.000 C13 C12 C14 H14 0.0057 -0.1515 0.3965 43 0.950 0.000 C14 C13 C9 H16 0.1914 -0.0727 0.4840 43 0.950 0.000 C16 C17 C15 H17 0.0945 -0.0126 0.5787 43 0.950 0.000 C17 C18 C16 H18 0.0479 -0.1029 0.6727 43 0.950 0.000 C18 C19 C17 H19 0.1007 -0.2538 0.6702 43 0.950 0.000 C19 C18 C20 H20 0.1906 -0.3142 0.5736 43 0.950 0.000 C20 C19 C15 H22 0.0240 -0.3439 0.4429 43 0.950 0.000 C22 C23 C21 H23 -0.0288 -0.4929 0.4290 43 0.950 0.000 C23 C22 C24 H24 0.1567 -0.5952 0.4215 43 0.950 0.000 C24 C25 C23 H25 0.3963 -0.5450 0.4274 43 0.950 0.000 C25 C24 C26 H26 0.4488 -0.3948 0.4408 43 0.950 0.000 C26 C21 C25 H28 0.5053 -0.2972 0.5493 43 0.950 0.000 C28 C29 C27 H29 0.7515 -0.2629 0.5713 43 0.950 0.000 C29 C30 C28 H30 0.8484 -0.1604 0.4994 43 0.950 0.000 C30 C31 C29 H31 0.6924 -0.0919 0.4056 43 0.950 0.000 C31 C30 C32 H32 0.4465 -0.1276 0.3830 43 0.950 0.000 C32 C31 C27 2007src0719 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.66469 0.05153 0.21507 1.00000 0.01879 0.02915 0.02248 0.00445 0.00325 0.00377 0.02350 0.00228 0.00013 0.00008 0.00006 0.00000 0.00056 0.00066 0.00057 0.00050 0.00044 0.00048 0.00025 C2 0.77794 0.17386 0.15700 1.00000 0.02995 0.03801 0.03909 0.01134 0.01293 -0.00258 0.03486 0.00281 0.00015 0.00010 0.00008 0.00000 0.00069 0.00079 0.00075 0.00063 0.00057 0.00059 0.00032 H2A 0.70482 0.21007 0.17506 1.00000 0.05230 0.00000 0.00000 H2B 0.76808 0.18119 0.10508 1.00000 0.05230 0.00000 0.00000 H2C 0.87547 0.19248 0.17968 1.00000 0.05230 0.00000 0.00000 C3 0.84027 0.01593 0.14105 1.00000 0.02821 0.04442 0.03829 0.00936 0.01570 0.01149 0.03581 0.00297 0.00015 0.00010 0.00008 0.00000 0.00068 0.00084 0.00075 0.00064 0.00057 0.00061 0.00033 H3A 0.81102 -0.04353 0.15320 1.00000 0.05372 0.00000 0.00000 H3B 0.94421 0.02423 0.15908 1.00000 0.05372 0.00000 0.00000 H3C 0.82191 0.02332 0.08899 1.00000 0.05372 0.00000 0.00000 C4 0.35637 0.06239 0.24179 1.00000 0.02108 0.03010 0.01953 -0.00191 0.00113 -0.00026 0.02383 0.00218 0.00013 0.00008 0.00006 0.00000 0.00057 0.00066 0.00055 0.00049 0.00044 0.00049 0.00025 H4 0.33643 0.06125 0.19101 1.00000 0.02859 0.00000 0.00000 C5 0.25648 0.03179 0.28185 1.00000 0.02087 0.03058 0.02839 -0.00478 0.00395 -0.00428 0.02663 0.00229 0.00013 0.00009 0.00007 0.00000 0.00059 0.00068 0.00063 0.00052 0.00047 0.00049 0.00027 H5 0.16612 0.00834 0.25891 1.00000 0.03196 0.00000 0.00000 C6 0.28837 0.03535 0.35580 1.00000 0.02646 0.02360 0.02777 0.00211 0.01159 0.00157 0.02514 0.00236 0.00014 0.00008 0.00007 0.00000 0.00062 0.00062 0.00062 0.00049 0.00049 0.00049 0.00026 H6 0.21957 0.01459 0.38368 1.00000 0.03017 0.00000 0.00000 C7 0.42065 0.06919 0.38914 1.00000 0.02944 0.02501 0.01845 -0.00032 0.00481 0.00548 0.02420 0.00230 0.00014 0.00008 0.00006 0.00000 0.00063 0.00062 0.00055 0.00047 0.00046 0.00050 0.00026 H7 0.44297 0.07174 0.43984 1.00000 0.02904 0.00000 0.00000 C8 0.51918 0.09902 0.34815 1.00000 0.02108 0.02314 0.02100 -0.00293 -0.00020 0.00299 0.02216 0.00216 0.00013 0.00008 0.00006 0.00000 0.00056 0.00060 0.00056 0.00046 0.00044 0.00046 0.00025 H8 0.61045 0.12261 0.36971 1.00000 0.02659 0.00000 0.00000 C9 0.18745 -0.20840 0.36989 1.00000 0.01934 0.01665 0.01914 0.00044 0.00262 -0.00207 0.01844 0.00202 0.00012 0.00007 0.00006 0.00000 0.00054 0.00053 0.00053 0.00043 0.00042 0.00042 0.00023 C10 0.24717 -0.22930 0.30831 1.00000 0.02300 0.02316 0.02168 -0.00032 0.00477 0.00134 0.02250 0.00219 0.00013 0.00008 0.00006 0.00000 0.00058 0.00060 0.00057 0.00047 0.00045 0.00046 0.00025 H10 0.33950 -0.25744 0.31413 1.00000 0.02699 0.00000 0.00000 C11 0.17649 -0.21044 0.23941 1.00000 0.03766 0.02592 0.01901 -0.00152 0.00628 -0.00086 0.02735 0.00235 0.00015 0.00009 0.00006 0.00000 0.00071 0.00064 0.00057 0.00049 0.00050 0.00054 0.00027 H11 0.22134 -0.22500 0.19946 1.00000 0.03282 0.00000 0.00000 C12 0.04060 -0.17041 0.22890 1.00000 0.03739 0.02639 0.01874 0.00251 -0.00428 0.00005 0.02853 0.00233 0.00015 0.00009 0.00007 0.00000 0.00071 0.00066 0.00056 0.00049 0.00049 0.00054 0.00028 H12 -0.00882 -0.15832 0.18194 1.00000 0.03423 0.00000 0.00000 C13 -0.02199 -0.14833 0.28792 1.00000 0.02256 0.02397 0.02841 0.00226 -0.00250 0.00243 0.02575 0.00227 0.00013 0.00008 0.00007 0.00000 0.00060 0.00062 0.00063 0.00050 0.00047 0.00047 0.00026 H13 -0.11446 -0.12032 0.28150 1.00000 0.03090 0.00000 0.00000 C14 0.05069 -0.16722 0.35690 1.00000 0.02071 0.02118 0.02154 -0.00011 0.00291 -0.00042 0.02121 0.00212 0.00012 0.00008 0.00006 0.00000 0.00056 0.00058 0.00055 0.00046 0.00043 0.00045 0.00024 H14 0.00568 -0.15154 0.39654 1.00000 0.02546 0.00000 0.00000 C15 0.20041 -0.20142 0.51593 1.00000 0.01383 0.02421 0.01777 -0.00085 0.00102 0.00030 0.01879 0.00203 0.00012 0.00008 0.00006 0.00000 0.00050 0.00059 0.00052 0.00044 0.00039 0.00043 0.00023 C16 0.17140 -0.11069 0.52099 1.00000 0.01762 0.02426 0.02099 -0.00151 0.00078 0.00068 0.02123 0.00206 0.00012 0.00008 0.00006 0.00000 0.00054 0.00061 0.00055 0.00046 0.00043 0.00045 0.00024 H16 0.19144 -0.07271 0.48398 1.00000 0.02548 0.00000 0.00000 C17 0.11443 -0.07403 0.57804 1.00000 0.01784 0.02931 0.02892 -0.00938 -0.00027 0.00317 0.02583 0.00217 0.00013 0.00009 0.00007 0.00000 0.00056 0.00066 0.00062 0.00052 0.00046 0.00048 0.00027 H17 0.09451 -0.01258 0.57867 1.00000 0.03100 0.00000 0.00000 C18 0.08694 -0.12734 0.63379 1.00000 0.01884 0.04596 0.02363 -0.01184 0.00531 0.00037 0.02928 0.00230 0.00013 0.00010 0.00007 0.00000 0.00057 0.00080 0.00060 0.00056 0.00046 0.00054 0.00029 H18 0.04793 -0.10287 0.67267 1.00000 0.03513 0.00000 0.00000 C19 0.11718 -0.21681 0.63197 1.00000 0.02792 0.04197 0.02003 -0.00040 0.00696 -0.00327 0.02963 0.00241 0.00014 0.00010 0.00007 0.00000 0.00065 0.00078 0.00058 0.00055 0.00048 0.00056 0.00029 H19 0.10068 -0.25384 0.67025 1.00000 0.03556 0.00000 0.00000 C20 0.17186 -0.25259 0.57395 1.00000 0.02460 0.02725 0.02127 0.00031 0.00455 0.00067 0.02429 0.00225 0.00013 0.00009 0.00006 0.00000 0.00060 0.00063 0.00057 0.00049 0.00046 0.00049 0.00026 H20 0.19061 -0.31419 0.57364 1.00000 0.02915 0.00000 0.00000 C21 0.24364 -0.35077 0.44411 1.00000 0.01934 0.02112 0.01362 0.00151 0.00223 0.00070 0.01809 0.00204 0.00012 0.00008 0.00006 0.00000 0.00053 0.00057 0.00048 0.00042 0.00039 0.00043 0.00023 C22 0.10099 -0.38412 0.43990 1.00000 0.02058 0.02576 0.01824 0.00057 0.00432 -0.00040 0.02141 0.00213 0.00013 0.00008 0.00006 0.00000 0.00056 0.00061 0.00053 0.00046 0.00043 0.00046 0.00024 H22 0.02400 -0.34393 0.44289 1.00000 0.02569 0.00000 0.00000 C23 0.06878 -0.47332 0.43155 1.00000 0.02659 0.03045 0.01937 0.00283 0.00395 -0.00840 0.02546 0.00223 0.00014 0.00009 0.00006 0.00000 0.00061 0.00067 0.00055 0.00049 0.00046 0.00051 0.00026 H23 -0.02880 -0.49292 0.42895 1.00000 0.03055 0.00000 0.00000 C24 0.17847 -0.53408 0.42698 1.00000 0.03922 0.01992 0.02616 0.00225 0.00322 -0.00607 0.02869 0.00236 0.00015 0.00008 0.00007 0.00000 0.00074 0.00061 0.00062 0.00049 0.00053 0.00052 0.00028 H24 0.15671 -0.59519 0.42150 1.00000 0.03443 0.00000 0.00000 C25 0.32021 -0.50425 0.43054 1.00000 0.03156 0.02128 0.02592 0.00088 0.00272 0.00447 0.02649 0.00233 0.00014 0.00008 0.00007 0.00000 0.00066 0.00061 0.00061 0.00049 0.00050 0.00050 0.00027 H25 0.39634 -0.54502 0.42741 1.00000 0.03179 0.00000 0.00000 C26 0.35115 -0.41395 0.43876 1.00000 0.02078 0.02264 0.01986 0.00133 0.00253 0.00115 0.02119 0.00216 0.00013 0.00008 0.00006 0.00000 0.00056 0.00059 0.00054 0.00046 0.00043 0.00046 0.00024 H26 0.44883 -0.39483 0.44078 1.00000 0.02543 0.00000 0.00000 C27 0.44479 -0.21768 0.46244 1.00000 0.01847 0.01794 0.01895 -0.00406 0.00422 0.00187 0.01833 0.00203 0.00012 0.00007 0.00006 0.00000 0.00053 0.00054 0.00052 0.00043 0.00041 0.00042 0.00023 C28 0.54199 -0.25581 0.51914 1.00000 0.02246 0.02202 0.01968 -0.00168 0.00296 0.00142 0.02145 0.00212 0.00013 0.00008 0.00006 0.00000 0.00057 0.00058 0.00055 0.00046 0.00044 0.00046 0.00024 H28 0.50534 -0.29721 0.54929 1.00000 0.02574 0.00000 0.00000 C29 0.68975 -0.23516 0.53272 1.00000 0.02098 0.02958 0.02343 -0.00601 -0.00139 0.00576 0.02524 0.00220 0.00013 0.00009 0.00006 0.00000 0.00059 0.00066 0.00059 0.00050 0.00046 0.00049 0.00027 H29 0.75148 -0.26294 0.57127 1.00000 0.03029 0.00000 0.00000 C30 0.74757 -0.17431 0.49038 1.00000 0.01724 0.03463 0.03016 -0.01176 0.00470 -0.00236 0.02726 0.00223 0.00013 0.00009 0.00007 0.00000 0.00056 0.00071 0.00064 0.00054 0.00047 0.00050 0.00028 H30 0.84839 -0.16043 0.49937 1.00000 0.03271 0.00000 0.00000 C31 0.65515 -0.13428 0.43478 1.00000 0.02428 0.02659 0.02910 -0.00338 0.00902 -0.00577 0.02614 0.00225 0.00013 0.00009 0.00007 0.00000 0.00061 0.00064 0.00063 0.00051 0.00049 0.00050 0.00027 H31 0.69236 -0.09193 0.40560 1.00000 0.03136 0.00000 0.00000 C32 0.50741 -0.15598 0.42150 1.00000 0.02139 0.02059 0.02291 -0.00043 0.00378 0.00054 0.02162 0.00215 0.00013 0.00008 0.00006 0.00000 0.00056 0.00057 0.00056 0.00046 0.00044 0.00045 0.00024 H32 0.44650 -0.12765 0.38296 1.00000 0.02594 0.00000 0.00000 B1 0.27039 -0.24321 0.44870 1.00000 0.01592 0.01975 0.01682 0.00061 0.00335 0.00072 0.01743 0.00232 0.00013 0.00009 0.00007 0.00000 0.00058 0.00062 0.00057 0.00047 0.00045 0.00047 0.00025 N1 0.48269 0.09385 0.27688 1.00000 0.01764 0.02093 0.02011 0.00149 0.00572 0.00049 0.01927 0.00176 0.00010 0.00006 0.00005 0.00000 0.00046 0.00050 0.00047 0.00038 0.00037 0.00037 0.00021 N2 0.75627 0.08121 0.17368 1.00000 0.02128 0.03358 0.02768 0.00800 0.00882 0.00385 0.02698 0.00207 0.00011 0.00008 0.00006 0.00000 0.00051 0.00060 0.00053 0.00046 0.00041 0.00044 0.00024 O1 0.58316 0.12447 0.23635 1.00000 0.02191 0.02488 0.02747 0.00456 0.01069 -0.00035 0.02400 0.00159 0.00009 0.00006 0.00004 0.00000 0.00042 0.00045 0.00043 0.00035 0.00034 0.00034 0.00019 O2 0.64371 -0.02233 0.23395 1.00000 0.02968 0.02805 0.03751 0.01040 0.01445 0.00717 0.03073 0.00185 0.00010 0.00006 0.00005 0.00000 0.00048 0.00049 0.00051 0.00040 0.00039 0.00038 0.00022 Final Structure Factor Calculation for 2007src0719 in P2(1)/n Total number of l.s. parameters = 336 Maximum vector length = 511 Memory required = 3709 / 24017 wR2 = 0.1008 before cycle 5 for 6042 data and 0 / 336 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0394 * P )^2 + 1.02 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0406 for 5026 Fo > 4sig(Fo) and 0.0522 for all 6042 data wR2 = 0.1008, GooF = S = 1.031, Restrained GooF = 1.031 for all data Occupancy sum of asymmetric unit = 37.00 for non-hydrogen and 31.00 for hydrogen atoms Principal mean square atomic displacements U 0.0319 0.0213 0.0173 C1 0.0500 0.0350 0.0195 C2 0.0570 0.0317 0.0187 C3 0.0305 0.0230 0.0180 C4 0.0348 0.0260 0.0191 C5 0.0338 0.0230 0.0186 C6 0.0332 0.0216 0.0178 C7 0.0291 0.0196 0.0179 C8 0.0210 0.0189 0.0155 C9 0.0244 0.0226 0.0204 C10 0.0377 0.0261 0.0182 C11 0.0429 0.0268 0.0159 C12 0.0342 0.0254 0.0176 C13 0.0220 0.0213 0.0203 C14 0.0244 0.0185 0.0135 C15 0.0254 0.0216 0.0167 C16 0.0408 0.0198 0.0169 C17 0.0512 0.0206 0.0161 C18 0.0427 0.0278 0.0184 C19 0.0274 0.0245 0.0210 C20 0.0215 0.0194 0.0133 C21 0.0258 0.0208 0.0175 C22 0.0379 0.0216 0.0169 C23 0.0421 0.0264 0.0176 C24 0.0340 0.0260 0.0195 C25 0.0233 0.0214 0.0188 C26 0.0227 0.0193 0.0130 C27 0.0245 0.0212 0.0187 C28 0.0381 0.0201 0.0175 C29 0.0444 0.0205 0.0169 C30 0.0350 0.0247 0.0187 C31 0.0230 0.0217 0.0202 C32 0.0200 0.0168 0.0154 B1 0.0226 0.0197 0.0155 N1 0.0402 0.0230 0.0177 N2 0.0326 0.0243 0.0151 O1 0.0487 0.0221 0.0213 O2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.025 0.039 0.054 0.071 0.090 0.113 0.148 0.210 1.000 Number in group 617. 612. 625. 583. 600. 615. 581. 609. 596. 604. GooF 1.012 1.011 1.036 1.017 1.054 1.085 1.042 1.004 0.936 1.098 K 2.099 1.078 1.000 0.976 0.996 0.991 0.994 1.010 1.010 0.992 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 605. 614. 609. 601. 592. 601. 611. 602. 602. 605. GooF 0.935 0.952 0.997 1.004 0.869 0.871 0.904 0.945 1.230 1.449 K 1.025 1.025 1.002 0.985 1.000 1.000 1.008 1.011 1.024 0.978 R1 0.115 0.101 0.089 0.076 0.054 0.042 0.034 0.033 0.040 0.035 Recommended weighting scheme: WGHT 0.0360 1.0523 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) 4 6 1 491.32 357.71 4.89 0.150 1.67 0 1 3 35.73 100.04 4.84 0.079 5.76 -4 2 7 222.22 152.54 4.44 0.098 1.85 -5 2 6 19.84 4.58 4.36 0.017 1.67 1 1 2 1336.05 1652.09 4.16 0.322 5.63 -1 3 1 1442.06 1768.57 4.09 0.333 4.39 -3 0 5 1054.44 1307.35 3.90 0.287 2.59 5 2 1 7.60 0.13 3.83 0.003 1.75 -5 2 8 23.24 7.64 3.81 0.022 1.54 4 5 2 329.96 251.78 3.73 0.126 1.75 -6 1 4 97.08 61.85 3.71 0.062 1.52 3 0 3 284.43 371.71 3.69 0.153 2.58 0 4 11 102.85 64.75 3.59 0.064 1.55 -3 1 5 215.07 285.75 3.58 0.134 2.55 -2 2 12 54.42 30.75 3.54 0.044 1.52 9 3 9 122.05 182.14 3.48 0.107 0.85 -2 2 11 21.75 8.43 3.43 0.023 1.65 -10 4 8 263.44 192.48 3.43 0.110 0.88 2 2 0 8.03 1.23 3.35 0.009 3.93 -3 1 13 6.17 0.06 3.30 0.002 1.39 -3 2 3 32.57 15.84 3.28 0.032 2.75 5 4 4 29.46 13.70 3.28 0.029 1.49 -5 4 2 8.97 0.99 3.27 0.008 1.67 0 0 22 26.74 63.22 3.25 0.063 0.85 0 2 2 8297.65 9720.37 3.23 0.782 5.89 -2 3 11 158.23 116.37 3.19 0.086 1.60 -2 18 3 60.25 31.98 3.17 0.045 0.82 7 4 1 100.17 141.17 3.16 0.094 1.22 3 4 10 21.42 8.87 3.16 0.024 1.39 0 5 1 4.28 16.18 3.15 0.032 2.99 4 1 6 57.82 87.95 3.15 0.074 1.71 -3 5 9 1213.32 1033.72 3.15 0.255 1.59 -5 1 6 239.25 185.63 3.14 0.108 1.70 -1 7 5 138.86 186.66 3.14 0.108 1.87 -3 0 7 240.42 185.40 3.11 0.108 2.20 -1 1 14 193.55 147.74 3.08 0.096 1.35 -2 1 8 41.85 23.94 3.07 0.039 2.22 1 0 21 36.81 67.30 3.04 0.065 0.87 -2 4 13 56.23 34.93 3.04 0.047 1.35 5 9 16 31.53 62.70 3.03 0.063 0.81 6 12 7 12.12 38.19 3.02 0.049 0.89 8 4 1 22.90 9.82 2.99 0.025 1.09 -4 6 14 129.67 174.45 2.99 0.105 1.12 3 5 14 6.79 20.21 2.99 0.036 1.08 6 2 2 119.76 86.70 2.98 0.074 1.45 5 15 2 12.73 1.00 2.98 0.008 0.87 -7 12 14 407.40 312.10 2.98 0.140 0.80 -1 0 21 20.13 39.41 2.96 0.050 0.90 -1 0 11 21.56 8.03 2.95 0.022 1.72 -7 3 1 6.07 0.02 2.94 0.001 1.28 Bond lengths and angles C1 - Distance Angles O2 1.2012 (0.0015) N2 1.3303 (0.0016) 130.04 (0.12) O1 1.4368 (0.0015) 120.88 (0.10) 109.07 (0.10) C1 - O2 N2 C2 - Distance Angles N2 1.4608 (0.0018) C2 - C3 - Distance Angles N2 1.4614 (0.0017) C3 - C4 - Distance Angles N1 1.3397 (0.0015) C5 1.3764 (0.0017) 117.69 (0.11) C4 - N1 C5 - Distance Angles C4 1.3764 (0.0017) C6 1.3853 (0.0018) 119.66 (0.11) C5 - C4 C6 - Distance Angles C5 1.3853 (0.0017) C7 1.3866 (0.0018) 120.04 (0.11) C6 - C5 C7 - Distance Angles C8 1.3746 (0.0017) C6 1.3866 (0.0018) 119.37 (0.11) C7 - C8 C8 - Distance Angles N1 1.3400 (0.0015) C7 1.3746 (0.0017) 118.04 (0.11) C8 - N1 C9 - Distance Angles C14 1.4034 (0.0016) C10 1.4109 (0.0016) 115.23 (0.10) B1 1.6506 (0.0016) 125.15 (0.10) 119.21 (0.10) C9 - C14 C10 C10 - Distance Angles C11 1.3916 (0.0017) C9 1.4109 (0.0016) 122.75 (0.11) C10 - C11 C11 - Distance Angles C12 1.3883 (0.0019) C10 1.3916 (0.0017) 120.14 (0.11) C11 - C12 C12 - Distance Angles C11 1.3883 (0.0019) C13 1.3865 (0.0018) 119.08 (0.11) C12 - C11 C13 - Distance Angles C12 1.3865 (0.0018) C14 1.3989 (0.0016) 120.15 (0.11) C13 - C12 C14 - Distance Angles C13 1.3989 (0.0016) C9 1.4034 (0.0016) 122.63 (0.11) C14 - C13 C15 - Distance Angles C16 1.4077 (0.0017) C20 1.4073 (0.0016) 114.94 (0.11) B1 1.6521 (0.0016) 122.14 (0.10) 122.85 (0.10) C15 - C16 C20 C16 - Distance Angles C17 1.3974 (0.0016) C15 1.4077 (0.0017) 122.90 (0.12) C16 - C17 C17 - Distance Angles C18 1.3881 (0.0019) C16 1.3974 (0.0016) 120.03 (0.12) C17 - C18 C18 - Distance Angles C19 1.3866 (0.0020) C17 1.3881 (0.0019) 119.09 (0.11) C18 - C19 C19 - Distance Angles C18 1.3866 (0.0020) C20 1.3970 (0.0017) 120.10 (0.12) C19 - C18 C20 - Distance Angles C19 1.3970 (0.0017) C15 1.4073 (0.0016) 122.90 (0.12) C20 - C19 C21 - Distance Angles C26 1.4016 (0.0016) C22 1.4119 (0.0016) 115.39 (0.11) B1 1.6493 (0.0017) 125.14 (0.10) 119.30 (0.10) C21 - C26 C22 C22 - Distance Angles C23 1.3882 (0.0018) C21 1.4119 (0.0016) 122.60 (0.11) C22 - C23 C23 - Distance Angles C22 1.3882 (0.0018) C24 1.3891 (0.0019) 120.36 (0.11) C23 - C22 C24 - Distance Angles C25 1.3870 (0.0019) C23 1.3891 (0.0019) 119.04 (0.12) C24 - C25 C25 - Distance Angles C24 1.3870 (0.0019) C26 1.4019 (0.0017) 120.01 (0.12) C25 - C24 C26 - Distance Angles C21 1.4016 (0.0016) C25 1.4019 (0.0017) 122.60 (0.11) C26 - C21 C27 - Distance Angles C32 1.4030 (0.0016) C28 1.4094 (0.0016) 114.95 (0.10) B1 1.6485 (0.0016) 123.97 (0.10) 121.05 (0.10) C27 - C32 C28 C28 - Distance Angles C29 1.3935 (0.0017) C27 1.4094 (0.0016) 122.59 (0.11) C28 - C29 C29 - Distance Angles C30 1.3892 (0.0019) C28 1.3935 (0.0017) 120.57 (0.11) C29 - C30 C30 - Distance Angles C31 1.3853 (0.0018) C29 1.3892 (0.0019) 118.62 (0.11) C30 - C31 C31 - Distance Angles C30 1.3853 (0.0018) C32 1.3970 (0.0017) 120.21 (0.12) C31 - C30 C32 - Distance Angles C31 1.3970 (0.0017) C27 1.4030 (0.0016) 123.04 (0.11) C32 - C31 B1 - Distance Angles C27 1.6485 (0.0016) C21 1.6493 (0.0017) 112.13 (0.09) C9 1.6506 (0.0016) 111.64 (0.09) 102.96 (0.09) C15 1.6521 (0.0016) 107.06 (0.09) 110.12 (0.09) 113.01 (0.09) B1 - C27 C21 C9 N1 - Distance Angles C8 1.3400 (0.0015) C4 1.3397 (0.0015) 125.19 (0.10) O1 1.3865 (0.0012) 117.28 (0.09) 117.53 (0.09) N1 - C8 C4 N2 - Distance Angles C1 1.3303 (0.0015) C2 1.4608 (0.0018) 125.32 (0.11) C3 1.4614 (0.0017) 117.54 (0.11) 117.12 (0.11) N2 - C1 C2 O1 - Distance Angles N1 1.3865 (0.0012) C1 1.4368 (0.0015) 109.61 (0.08) O1 - N1 O2 - Distance Angles C1 1.2012 (0.0015) O2 - FMAP and GRID set by program FMAP 2 3 24 GRID -1.190 -2 -2 1.190 2 2 R1 = 0.0522 for 6042 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.2601 0.2806 0.0163 [ 0.81 A from C15 ] Deepest hole -0.21 at 0.9434 0.5992 0.1976 [ 0.78 A from N1 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 3601 / 26775 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2399 -0.2194 0.4837 1.00000 0.05 0.24 0.81 C15 0.85 B1 1.94 C16 1.99 C20 Q2 1 0.3650 -0.2349 0.4508 1.00000 0.05 0.24 0.78 C27 0.88 B1 1.94 C32 1.95 C28 Q3 1 0.2341 -0.2212 0.4100 1.00000 0.05 0.21 0.83 B1 0.83 C9 1.96 C10 2.01 C14 Q4 1 0.2498 -0.2995 0.4409 1.00000 0.05 0.21 0.78 C21 0.88 B1 1.89 C22 1.95 C9 Q5 1 0.5864 -0.1521 0.4267 1.00000 0.05 0.20 0.69 C31 0.73 C32 1.45 H31 1.47 H32 Q6 1 0.0186 -0.1649 0.3221 1.00000 0.05 0.19 0.68 C14 0.74 C13 1.45 H14 1.51 H13 Q7 1 0.1257 -0.1850 0.3547 1.00000 0.05 0.19 0.70 C9 0.76 C14 1.56 H14 1.68 C10 Q8 1 0.2173 -0.2036 0.2759 1.00000 0.05 0.17 0.74 C11 0.74 C10 1.49 H10 1.49 H11 Q9 1 0.2139 -0.2105 0.3399 1.00000 0.05 0.16 0.66 C9 0.77 C10 1.52 H10 1.74 C14 Q10 1 0.3280 -0.4582 0.4184 1.00000 0.05 0.16 0.74 C25 0.79 C26 1.46 H25 1.49 H26 Q11 1 0.0897 -0.4253 0.4188 1.00000 0.05 0.16 0.74 C22 0.80 C23 1.48 H22 1.54 H23 Q12 1 0.8608 0.1789 0.1275 1.00000 0.05 0.16 0.90 H2B 1.00 H2C 1.03 C2 1.89 H2A Q13 1 0.1751 -0.0923 0.5586 1.00000 0.05 0.16 0.76 C16 0.78 C17 1.48 H16 1.50 H17 Q14 1 0.2086 -0.2223 0.5470 1.00000 0.05 0.16 0.66 C15 0.80 C20 1.50 H20 1.78 C16 Q15 1 0.1239 -0.1009 0.5469 1.00000 0.05 0.15 0.73 C16 0.73 C17 1.50 H16 1.51 H17 Q16 1 0.4568 0.0981 0.3685 1.00000 0.05 0.15 0.71 C7 0.75 C8 1.44 H7 1.48 H8 Q17 1 0.0404 -0.1434 0.2625 1.00000 0.05 0.15 0.76 C12 0.82 C13 1.54 H12 1.58 H13 Q18 1 0.2055 -0.1600 0.5275 1.00000 0.05 0.15 0.66 C15 0.81 C16 1.55 H16 1.71 C20 Q19 1 0.1349 -0.5003 0.4441 1.00000 0.05 0.15 0.74 C23 0.76 C24 1.51 H23 1.52 H24 Q20 1 0.1820 -0.3694 0.4537 1.00000 0.05 0.15 0.69 C21 0.79 C22 1.50 H22 1.78 C26 Shortest distances between peaks (including symmetry equivalents) 13 15 0.51 7 9 0.99 14 18 1.01 6 7 1.13 6 17 1.22 8 9 1.22 13 18 1.24 15 18 1.27 4 20 1.28 11 19 1.28 1 14 1.28 1 18 1.30 11 20 1.31 3 9 1.32 3 4 1.32 2 3 1.35 1 3 1.39 1 2 1.43 3 7 1.44 2 4 1.44 1 4 1.47 7 8 1.86 8 17 1.86 7 17 1.90 6 9 1.92 14 15 2.00 13 14 2.01 19 20 2.03 10 19 2.04 10 20 2.10 9 17 2.24 6 8 2.25 10 11 2.28 4 9 2.32 2 9 2.36 1 20 2.38 4 11 2.41 4 14 2.41 3 18 2.47 3 20 2.47 1 15 2.50 2 18 2.52 2 5 2.52 2 14 2.53 1 13 2.53 4 7 2.53 3 6 2.53 3 8 2.54 1 7 2.55 4 10 2.57 3 14 2.65 2 20 2.66 1 9 2.70 2 7 2.74 4 18 2.75 14 20 2.83 5 12 2.83 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 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.01: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.01: Analyse other restraints etc. 8.29: 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 4.02: Structure factors and derivatives 6.74: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.96: Solve l.s. equations 0.00: Generate HTAB table 0.04: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.08: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0719 finished at 19:46:21 Total CPU time: 20.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++