+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src1029 started at 17:14:08 on 07-Aug-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src1029 in P2(1)/n CELL 0.71073 7.9160 9.9010 20.6610 90.000 99.445 90.000 ZERR 4.00 0.0050 0.0050 0.0050 0.005 0.005 0.005 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O F P UNIT 56 60 8 8 24 4 V = 1597.38 F(000) = 792.0 Mu = 0.25 mm-1 Cell Wt = 1553.00 Rho = 1.614 MERG 2 OMIT -3.00 55.00 OMIT 2 2 0 OMIT -2 2 3 OMIT -3 1 3 OMIT -1 3 1 OMIT -3 3 3 OMIT -2 2 4 OMIT 1 2 7 OMIT -1 2 5 FMAP 2 PLAN 10 WPDB SIZE 0.04 0.04 0.20 ACTA WGHT 0.18240 2.64000 L.S. 4 TEMP -153.00 FVAR 0.43805 C1 1 0.526125 0.085633 0.410955 11.00000 0.05077 0.04759 = 0.04460 -0.00449 0.00670 0.00164 AFIX 23 H1A 2 0.474498 0.101062 0.450844 11.00000 -1.20000 H1B 2 0.649963 0.105807 0.422194 11.00000 -1.20000 AFIX 0 C2 1 0.505040 -0.060834 0.392290 11.00000 0.04038 0.04947 = 0.04247 -0.00153 0.01172 -0.00093 C3 1 0.462340 -0.242687 0.309914 11.00000 0.05882 0.05632 = 0.04877 -0.00115 0.01171 0.00159 AFIX 33 H3A 2 0.438943 -0.254153 0.262167 11.00000 -1.50000 H3B 2 0.370077 -0.284270 0.329348 11.00000 -1.50000 H3C 2 0.571416 -0.286144 0.327573 11.00000 -1.50000 AFIX 0 C4 1 0.451541 -0.000122 0.275961 11.00000 0.03192 0.05803 = 0.04927 0.00308 0.01174 -0.00351 C5 1 0.480614 0.146183 0.294487 11.00000 0.05968 0.05443 = 0.03219 0.00130 0.00984 0.00326 AFIX 23 H5A 2 0.600209 0.170197 0.291029 11.00000 -1.20000 H5B 2 0.404315 0.202451 0.262535 11.00000 -1.20000 AFIX 0 C6 1 0.375357 0.289338 0.372370 11.00000 0.04736 0.03851 = 0.04085 -0.00182 0.00461 -0.00562 AFIX 43 H6 2 0.332947 0.343916 0.335451 11.00000 -1.20000 AFIX 0 C7 1 0.349054 0.338888 0.434740 11.00000 0.04298 0.05782 = 0.04367 -0.00016 0.01041 0.00056 AFIX 43 H7 2 0.388090 0.288724 0.473507 11.00000 -1.20000 AFIX 0 C8 1 0.266898 0.459568 0.438021 11.00000 0.04363 0.04744 = 0.04210 0.00407 0.00803 0.00044 AFIX 43 H8 2 0.230729 0.505790 0.397843 11.00000 -1.20000 AFIX 0 C9 1 0.230069 0.523257 0.497288 11.00000 0.04197 0.04621 = 0.04274 -0.00178 0.00740 -0.00018 C10 1 0.149176 0.647136 0.492043 11.00000 0.04775 0.05264 = 0.04288 -0.00007 0.01109 -0.00241 AFIX 43 H10 2 0.122532 0.689124 0.450269 11.00000 -1.20000 AFIX 0 C11 1 0.106113 0.711383 0.546674 11.00000 0.05349 0.04742 = 0.05670 -0.00287 0.01121 0.00224 AFIX 43 H11 2 0.052251 0.797399 0.542446 11.00000 -1.20000 AFIX 0 C12 1 0.142109 0.649381 0.607463 11.00000 0.05599 0.06343 = 0.05755 -0.01176 0.01483 -0.00601 AFIX 43 H12 2 0.111913 0.692156 0.645109 11.00000 -1.20000 AFIX 0 C13 1 0.220939 0.526897 0.612950 11.00000 0.05106 0.06901 = 0.04069 -0.00545 0.00936 0.00148 AFIX 43 H13 2 0.246311 0.485448 0.654890 11.00000 -1.20000 AFIX 0 C14 1 0.265442 0.460642 0.558746 11.00000 0.03875 0.05933 = 0.05779 -0.00300 0.00847 0.00171 AFIX 43 H14 2 0.318860 0.374478 0.563395 11.00000 -1.20000 AFIX 0 N1 3 0.449985 0.179180 0.360646 11.00000 0.03970 0.05137 = 0.03666 0.00020 0.00781 -0.00518 N2 3 0.472323 -0.096331 0.326070 11.00000 0.04325 0.04907 = 0.03902 -0.00242 0.00822 -0.00741 O1 4 0.522834 -0.147420 0.434259 11.00000 0.05465 0.04905 = 0.04940 0.00700 0.01165 0.00649 O2 4 0.422071 -0.033009 0.218516 11.00000 0.04869 0.06188 = 0.03738 -0.00613 0.00781 -0.00463 F1 5 -0.114841 -0.056478 0.388481 11.00000 0.06323 0.11882 = 0.05880 -0.00737 0.02382 -0.00492 F2 5 -0.131512 0.077969 0.302141 11.00000 0.08381 0.06472 = 0.13394 0.01299 0.03976 0.02922 F3 5 -0.165937 -0.142083 0.286360 11.00000 0.04902 0.09909 = 0.08961 -0.03342 0.01961 -0.01029 F4 5 0.070771 -0.042308 0.262989 11.00000 0.07013 0.06637 = 0.06830 0.01091 0.02898 0.00530 F5 5 0.086941 -0.179936 0.347980 11.00000 0.09121 0.07389 = 0.07027 0.02100 0.02198 0.02688 F6 5 0.122240 0.042760 0.364797 11.00000 0.06010 0.14935 = 0.12358 -0.08415 0.03079 -0.04029 P1 6 -0.022208 -0.050134 0.326269 11.00000 0.04279 0.05360 = 0.05588 -0.00695 0.01598 0.00146 HKLF 4 Covalent radii and connectivity table for 2007src1029 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 P 1.100 C1 - N1 C2 C2 - O1 N2 C1 C3 - N2 C4 - O2 N2 C5 C5 - N1 C4 C6 - N1 C7 C7 - C8 C6 C8 - C7 C9 C9 - C10 C14 C8 C10 - C9 C11 C11 - C12 C10 C12 - C13 C11 C13 - C12 C14 C14 - C13 C9 N1 - C6 C1 C5 N2 - C2 C4 C3 O1 - C2 O2 - C4 F1 - P1 F2 - P1 F3 - P1 F4 - P1 F5 - P1 F6 - P1 P1 - F2 F5 F6 F3 F1 F4 h k l Fo^2 Sigma Why rejected 3 0 0 186.43 32.11 observed but should be systematically absent -6 0 1 66.76 15.97 observed but should be systematically absent -6 0 1 66.11 13.79 observed but should be systematically absent -2 0 1 17.99 4.09 observed but should be systematically absent -2 0 1 27.87 5.14 observed but should be systematically absent 1 0 2 16.01 2.99 observed but should be systematically absent 1 0 2 12.08 2.85 observed but should be systematically absent -8 0 3 134.63 27.78 observed but should be systematically absent -8 0 3 64.99 13.46 observed but should be systematically absent -1 0 4 42.95 9.36 observed but should be systematically absent 1 0 4 57.21 9.90 observed but should be systematically absent 1 0 4 82.09 17.96 observed but should be systematically absent 1 0 6 29.67 6.22 observed but should be systematically absent 1 0 6 27.35 6.64 observed but should be systematically absent -1 0 8 50.90 10.97 observed but should be systematically absent -1 0 10 48.63 12.09 observed but should be systematically absent 26743 Reflections read, of which 1190 rejected -9 =< h =< 10, -12 =< k =< 12, -26 =< l =< 26, Max. 2-theta = 55.00 16 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 4 0 0 1.66 0.33 5 2.14 4 9 1 -3.48 1.75 3 9.42 2 10 2 2.18 0.46 8 2.79 8 1 3 0.05 0.78 6 5.05 9 2 4 -0.02 0.38 5 4.87 -9 6 4 -13.77 5.53 2 39.63 -4 4 5 154.40 7.12 6 59.99 -3 8 5 43.40 3.26 5 17.36 -8 3 6 0.36 0.10 5 6.88 -6 1 8 9.57 0.94 9 5.12 -8 3 9 0.13 0.15 5 3.05 -7 1 10 0.18 0.06 9 3.96 -3 5 10 12.94 1.65 9 8.31 -5 10 11 -2.20 3.85 2 20.30 14 Inconsistent equivalents 3630 Unique reflections, of which 0 suppressed R(int) = 0.2237 R(sigma) = 0.1675 Friedel opposites merged Maximum memory for data reduction = 2025 / 36211 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 = 2617 / 282114 wR2 = 0.3784 before cycle 1 for 3630 data and 226 / 226 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1824 * P )^2 + 2.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43860 0.00329 0.168 OSF Mean shift/esd = 0.037 Maximum = 0.168 for OSF Max. shift = 0.001 A for C5 Max. dU = 0.000 for C9 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2617 / 282114 wR2 = 0.3783 before cycle 2 for 3630 data and 226 / 226 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1824 * P )^2 + 2.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43887 0.00329 0.081 OSF Mean shift/esd = 0.018 Maximum = 0.081 for OSF Max. shift = 0.001 A for C5 Max. dU = 0.000 for C3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2617 / 282114 wR2 = 0.3783 before cycle 3 for 3630 data and 226 / 226 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1824 * P )^2 + 2.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43892 0.00329 0.015 OSF Mean shift/esd = 0.005 Maximum = 0.021 for U22 N1 Max. shift = 0.000 A for C14 Max. dU = 0.000 for C11 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2617 / 282114 wR2 = 0.3783 before cycle 4 for 3630 data and 226 / 226 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1824 * P )^2 + 2.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43893 0.00330 0.003 OSF Mean shift/esd = 0.003 Maximum = -0.010 for y F1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for F6 Largest correlation matrix elements -0.522 U23 F6 / U22 F6 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.4744 0.1011 0.4508 23 0.990 0.000 C1 N1 C2 H1B 0.6499 0.1059 0.4222 23 0.990 0.000 C1 N1 C2 H3A 0.4390 -0.2543 0.2622 33 0.980 0.000 C3 N2 H3A H3B 0.3702 -0.2843 0.3294 33 0.980 0.000 C3 N2 H3A H3C 0.5715 -0.2862 0.3276 33 0.980 0.000 C3 N2 H3A H5A 0.6002 0.1700 0.2910 23 0.990 0.000 C5 N1 C4 H5B 0.4043 0.2023 0.2625 23 0.990 0.000 C5 N1 C4 H6 0.3328 0.3438 0.3355 43 0.950 0.000 C6 N1 C7 H7 0.3881 0.2886 0.4735 43 0.950 0.000 C7 C8 C6 H8 0.2310 0.5059 0.3978 43 0.950 0.000 C8 C7 C9 H10 0.1227 0.6891 0.4503 43 0.950 0.000 C10 C9 C11 H11 0.0521 0.7973 0.5424 43 0.950 0.000 C11 C12 C10 H12 0.1118 0.6919 0.6451 43 0.950 0.000 C12 C13 C11 H13 0.2464 0.4855 0.6549 43 0.950 0.000 C13 C12 C14 H14 0.3187 0.3743 0.5634 43 0.950 0.000 C14 C13 C9 2007src1029 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.52604 0.08566 0.41093 1.00000 0.05145 0.04738 0.04466 -0.00456 0.00680 0.00111 0.04795 0.01311 0.00095 0.00074 0.00034 0.00000 0.00430 0.00475 0.00407 0.00334 0.00322 0.00361 0.00181 H1A 0.47442 0.10106 0.45082 1.00000 0.05754 0.00000 0.00000 H1B 0.64987 0.10589 0.42217 1.00000 0.05754 0.00000 0.00000 C2 0.50512 -0.06085 0.39230 1.00000 0.04058 0.04971 0.04264 -0.00109 0.01184 -0.00099 0.04374 0.01279 0.00087 0.00077 0.00034 0.00000 0.00385 0.00482 0.00406 0.00359 0.00298 0.00330 0.00174 C3 0.46241 -0.24277 0.30993 1.00000 0.05902 0.05669 0.04895 -0.00104 0.01167 0.00181 0.05457 0.01428 0.00101 0.00081 0.00036 0.00000 0.00465 0.00532 0.00437 0.00368 0.00351 0.00401 0.00200 H3A 0.43901 -0.25428 0.26219 1.00000 0.08185 0.00000 0.00000 H3B 0.37016 -0.28435 0.32938 1.00000 0.08185 0.00000 0.00000 H3C 0.57150 -0.28619 0.32760 1.00000 0.08185 0.00000 0.00000 C4 0.45143 -0.00013 0.27590 1.00000 0.03171 0.05820 0.04971 0.00303 0.01187 -0.00369 0.04596 0.01365 0.00082 0.00082 0.00036 0.00000 0.00359 0.00496 0.00461 0.00375 0.00297 0.00333 0.00179 C5 0.48053 0.14601 0.29448 1.00000 0.05991 0.05491 0.03208 0.00121 0.00966 0.00311 0.04873 0.01353 0.00101 0.00078 0.00031 0.00000 0.00447 0.00498 0.00357 0.00325 0.00305 0.00381 0.00184 H5A 0.60015 0.16996 0.29104 1.00000 0.05847 0.00000 0.00000 H5B 0.40434 0.20230 0.26251 1.00000 0.05847 0.00000 0.00000 C6 0.37530 0.28926 0.37240 1.00000 0.04708 0.03821 0.04125 -0.00184 0.00468 -0.00534 0.04247 0.01186 0.00086 0.00072 0.00032 0.00000 0.00394 0.00429 0.00379 0.00312 0.00297 0.00343 0.00167 H6 0.33276 0.34382 0.33549 1.00000 0.05096 0.00000 0.00000 C7 0.34911 0.33880 0.43472 1.00000 0.04303 0.05850 0.04370 -0.00011 0.01043 0.00006 0.04804 0.01308 0.00088 0.00080 0.00034 0.00000 0.00389 0.00513 0.00399 0.00349 0.00305 0.00368 0.00185 H7 0.38815 0.28863 0.47349 1.00000 0.05764 0.00000 0.00000 C8 0.26700 0.45961 0.43802 1.00000 0.04393 0.04795 0.04205 0.00417 0.00797 0.00023 0.04454 0.01277 0.00087 0.00075 0.00033 0.00000 0.00392 0.00457 0.00396 0.00319 0.00302 0.00342 0.00173 H8 0.23097 0.50589 0.39785 1.00000 0.05345 0.00000 0.00000 C9 0.23008 0.52326 0.49725 1.00000 0.04239 0.04627 0.04300 -0.00168 0.00723 0.00000 0.04386 0.01271 0.00088 0.00074 0.00034 0.00000 0.00377 0.00465 0.00395 0.00325 0.00295 0.00341 0.00170 C10 0.14926 0.64707 0.49205 1.00000 0.04780 0.05312 0.04298 0.00005 0.01099 -0.00234 0.04757 0.01307 0.00090 0.00079 0.00034 0.00000 0.00407 0.00502 0.00396 0.00332 0.00311 0.00356 0.00184 H10 0.12271 0.68910 0.45029 1.00000 0.05708 0.00000 0.00000 C11 0.10604 0.71132 0.54665 1.00000 0.05375 0.04774 0.05690 -0.00301 0.01122 0.00228 0.05255 0.01390 0.00095 0.00081 0.00037 0.00000 0.00447 0.00481 0.00478 0.00376 0.00348 0.00369 0.00192 H11 0.05209 0.79731 0.54242 1.00000 0.06307 0.00000 0.00000 C12 0.14209 0.64922 0.60744 1.00000 0.05620 0.06296 0.05759 -0.01177 0.01504 -0.00563 0.05828 0.01433 0.00100 0.00089 0.00039 0.00000 0.00472 0.00571 0.00499 0.00408 0.00364 0.00428 0.00213 H12 0.11183 0.69195 0.64509 1.00000 0.06993 0.00000 0.00000 C13 0.22095 0.52688 0.61294 1.00000 0.05130 0.06875 0.04073 -0.00558 0.00940 0.00110 0.05339 0.01368 0.00096 0.00087 0.00035 0.00000 0.00437 0.00590 0.00406 0.00370 0.00324 0.00413 0.00200 H13 0.24644 0.48552 0.65490 1.00000 0.06406 0.00000 0.00000 C14 0.26541 0.46049 0.55875 1.00000 0.03826 0.05989 0.05827 -0.00289 0.00868 0.00163 0.05206 0.01354 0.00090 0.00085 0.00037 0.00000 0.00382 0.00512 0.00476 0.00386 0.00326 0.00353 0.00194 H14 0.31868 0.37427 0.56340 1.00000 0.06247 0.00000 0.00000 N1 0.44986 0.17928 0.36065 1.00000 0.03958 0.05211 0.03649 0.00021 0.00778 -0.00521 0.04255 0.01001 0.00069 0.00063 0.00025 0.00000 0.00306 0.00398 0.00307 0.00269 0.00234 0.00284 0.00144 N2 0.47235 -0.09632 0.32606 1.00000 0.04346 0.04898 0.03931 -0.00241 0.00835 -0.00747 0.04374 0.00996 0.00069 0.00063 0.00026 0.00000 0.00323 0.00385 0.00319 0.00271 0.00244 0.00278 0.00145 O1 0.52287 -0.14744 0.43425 1.00000 0.05452 0.04955 0.04970 0.00684 0.01170 0.00671 0.05090 0.00898 0.00061 0.00052 0.00023 0.00000 0.00306 0.00334 0.00296 0.00254 0.00230 0.00249 0.00134 O2 0.42210 -0.03299 0.21854 1.00000 0.04880 0.06223 0.03730 -0.00613 0.00776 -0.00476 0.04936 0.00867 0.00060 0.00053 0.00022 0.00000 0.00281 0.00366 0.00283 0.00232 0.00210 0.00248 0.00134 F1 -0.11483 -0.05653 0.38848 1.00000 0.06368 0.11860 0.05910 -0.00740 0.02384 -0.00491 0.07891 0.00918 0.00061 0.00059 0.00022 0.00000 0.00303 0.00462 0.00297 0.00270 0.00232 0.00282 0.00163 F2 -0.13155 0.07799 0.30214 1.00000 0.08371 0.06533 0.13406 0.01318 0.03972 0.02899 0.09191 0.01170 0.00071 0.00055 0.00031 0.00000 0.00368 0.00366 0.00493 0.00315 0.00337 0.00293 0.00184 F3 -0.16593 -0.14210 0.28639 1.00000 0.04912 0.09915 0.08979 -0.03352 0.01974 -0.01023 0.07842 0.00851 0.00056 0.00057 0.00025 0.00000 0.00265 0.00421 0.00354 0.00299 0.00239 0.00265 0.00162 F4 0.07077 -0.04229 0.26299 1.00000 0.07061 0.06604 0.06856 0.01099 0.02893 0.00517 0.06644 0.00908 0.00059 0.00047 0.00022 0.00000 0.00304 0.00329 0.00302 0.00230 0.00239 0.00236 0.00138 F5 0.08700 -0.17995 0.34799 1.00000 0.09148 0.07330 0.07057 0.02080 0.02199 0.02678 0.07747 0.01052 0.00068 0.00053 0.00023 0.00000 0.00359 0.00354 0.00311 0.00258 0.00257 0.00288 0.00155 F6 0.12222 0.04275 0.36479 1.00000 0.06061 0.14968 0.12318 -0.08379 0.03083 -0.04049 0.10938 0.00892 0.00067 0.00071 0.00032 0.00000 0.00315 0.00608 0.00479 0.00435 0.00308 0.00354 0.00245 P1 -0.02224 -0.05010 0.32626 1.00000 0.04307 0.05374 0.05606 -0.00702 0.01598 0.00150 0.05007 0.00367 0.00024 0.00022 0.00010 0.00000 0.00114 0.00137 0.00127 0.00094 0.00088 0.00091 0.00068 Final Structure Factor Calculation for 2007src1029 in P2(1)/n Total number of l.s. parameters = 226 Maximum vector length = 511 Memory required = 2391 / 25039 wR2 = 0.3783 before cycle 5 for 3630 data and 0 / 226 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1824 * P )^2 + 2.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1137 for 1566 Fo > 4sig(Fo) and 0.2326 for all 3630 data wR2 = 0.3783, GooF = S = 1.042, Restrained GooF = 1.042 for all data Occupancy sum of asymmetric unit = 25.00 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0532 0.0494 0.0412 C1 0.0502 0.0456 0.0355 C2 0.0601 0.0562 0.0473 C3 0.0595 0.0499 0.0285 C4 0.0614 0.0534 0.0313 C5 0.0503 0.0421 0.0350 C6 0.0585 0.0462 0.0394 C7 0.0501 0.0440 0.0396 C8 0.0470 0.0426 0.0420 C9 0.0541 0.0484 0.0403 C10 0.0581 0.0542 0.0454 C11 0.0744 0.0530 0.0474 C12 0.0699 0.0514 0.0388 C13 0.0623 0.0561 0.0378 C14 0.0540 0.0386 0.0350 N1 0.0544 0.0388 0.0381 N2 0.0617 0.0485 0.0425 O1 0.0647 0.0476 0.0358 O2 0.1200 0.0721 0.0446 F1 0.1448 0.0879 0.0431 F2 0.1289 0.0607 0.0457 F3 0.0895 0.0627 0.0472 F4 0.1158 0.0683 0.0484 F5 0.2257 0.0605 0.0419 F6 may be split into 0.1129 0.0583 0.3588 and 0.1315 0.0272 0.3708 0.0626 0.0513 0.0363 P1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.005 0.009 0.014 0.019 0.026 0.033 0.044 0.062 0.103 1.000 Number in group 434. 326. 340. 358. 401. 321. 386. 346. 356. 362. GooF 0.952 1.058 0.921 0.954 1.186 1.057 1.108 1.048 1.115 0.986 K 5.230 2.364 0.991 1.046 1.091 0.970 1.036 1.070 1.067 0.986 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.64 inf Number in group 363. 374. 357. 359. 366. 363. 364. 360. 359. 365. GooF 0.874 0.780 0.906 0.958 0.985 1.030 1.016 1.038 1.189 1.484 K 1.332 1.082 1.081 0.724 0.970 1.080 1.139 1.071 1.017 0.971 R1 0.585 0.525 0.481 0.438 0.340 0.228 0.155 0.123 0.110 0.093 Recommended weighting scheme: WGHT 0.1851 2.1637 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) 2 4 0 682.05 185.65 6.39 0.064 2.09 1 1 0 240.14 46.96 6.26 0.032 6.13 -1 7 2 198.68 26.15 5.88 0.024 1.38 -2 4 3 337.02 55.10 5.81 0.035 2.05 2 1 8 184.28 3.59 5.29 0.009 1.95 7 4 2 197.04 13.08 5.26 0.017 1.00 -3 1 1 119.42 25.51 5.20 0.024 2.55 -1 4 1 120.23 17.81 5.04 0.020 2.36 1 2 0 554.97 214.32 4.86 0.069 4.18 -1 9 1 92.24 0.61 4.51 0.004 1.09 5 5 3 125.10 19.18 4.34 0.021 1.18 1 5 0 102.56 26.44 4.28 0.024 1.92 -1 6 3 85.32 15.04 4.24 0.018 1.58 6 3 2 68.29 3.78 4.15 0.009 1.18 -1 4 2 657.57 301.91 4.06 0.082 2.32 1 0 7 612.07 2663.89 3.86 0.244 2.59 3 2 0 109.93 36.78 3.86 0.029 2.30 -1 4 7 96.88 19.29 3.82 0.021 1.88 4 4 2 190.61 57.18 3.75 0.036 1.49 6 5 3 71.46 2.45 3.71 0.007 1.05 1 9 1 91.47 1.49 3.66 0.006 1.09 2 3 1 309.30 143.79 3.62 0.057 2.47 -1 7 3 70.45 12.97 3.54 0.017 1.37 -3 4 3 92.70 16.66 3.47 0.019 1.78 2 0 6 243.48 83.09 3.42 0.043 2.38 -6 1 4 169.37 56.65 3.35 0.036 1.30 -5 4 8 502.80 1167.74 3.32 0.161 1.25 -1 1 3 286.40 128.20 3.28 0.054 4.87 0 6 2 107.30 272.61 3.22 0.078 1.63 0 6 1 873.66 1771.91 3.18 0.199 1.64 3 2 1 28.86 2.62 3.15 0.008 2.25 0 10 0 897.98 436.00 3.14 0.099 0.99 -1 2 11 153.17 31.37 3.14 0.026 1.75 -2 0 4 4989.11 2349.51 3.12 0.229 3.38 -4 5 3 107.08 28.24 3.01 0.025 1.39 -3 7 3 88.62 29.60 2.99 0.026 1.24 -2 5 6 357.86 115.23 2.96 0.051 1.62 -5 1 1 77.47 26.95 2.94 0.025 1.56 -8 1 1 527.60 256.28 2.93 0.076 0.98 -8 2 7 99.92 6.47 2.92 0.012 0.96 1 1 13 65.64 17.79 2.89 0.020 1.47 -2 7 1 50.41 2.36 2.89 0.007 1.33 -4 5 1 126.16 21.89 2.86 0.022 1.40 -10 1 4 139.02 12.67 2.82 0.017 0.79 -9 2 7 342.43 130.32 2.81 0.054 0.86 1 8 1 179.50 78.32 2.81 0.042 1.22 2 0 10 152.99 49.18 2.78 0.033 1.70 1 9 6 62.53 1.71 2.77 0.006 1.03 1 10 6 52.14 159.09 2.76 0.060 0.94 4 5 5 64.05 0.77 2.76 0.004 1.27 Bond lengths and angles C1 - Distance Angles N1 1.4479 (0.0089) C2 1.5030 (0.0102) 114.75 (0.58) C1 - N1 C2 - Distance Angles O1 1.2108 (0.0081) N2 1.3955 (0.0086) 120.33 (0.67) C1 1.5030 (0.0102) 120.34 (0.63) 119.27 (0.63) C2 - O1 N2 C3 - Distance Angles N2 1.4869 (0.0097) C3 - C4 - Distance Angles O2 1.2142 (0.0081) N2 1.3972 (0.0094) 121.45 (0.72) C5 1.5049 (0.0110) 120.22 (0.66) 118.14 (0.62) C4 - O2 N2 C5 - Distance Angles N1 1.4647 (0.0084) C4 1.5049 (0.0110) 114.36 (0.58) C5 - N1 C6 - Distance Angles N1 1.2807 (0.0088) C7 1.4244 (0.0094) 127.17 (0.66) C6 - N1 C7 - Distance Angles C8 1.3683 (0.0102) C6 1.4244 (0.0094) 119.13 (0.66) C7 - C8 C8 - Distance Angles C7 1.3683 (0.0102) C9 1.4483 (0.0097) 125.86 (0.65) C8 - C7 C9 - Distance Angles C10 1.3788 (0.0104) C14 1.4008 (0.0105) 119.09 (0.66) C8 1.4483 (0.0097) 118.45 (0.64) 122.38 (0.70) C9 - C10 C14 C10 - Distance Angles C9 1.3788 (0.0104) C11 1.3860 (0.0099) 121.20 (0.68) C10 - C9 C11 - Distance Angles C12 1.3854 (0.0108) C10 1.3860 (0.0099) 119.50 (0.74) C11 - C12 C12 - Distance Angles C13 1.3589 (0.0115) C11 1.3854 (0.0109) 119.66 (0.73) C12 - C13 C13 - Distance Angles C12 1.3589 (0.0115) C14 1.3924 (0.0101) 121.79 (0.74) C13 - C12 C14 - Distance Angles C13 1.3924 (0.0101) C9 1.4008 (0.0105) 118.74 (0.75) C14 - C13 N1 - Distance Angles C6 1.2807 (0.0088) C1 1.4479 (0.0089) 123.98 (0.58) C5 1.4647 (0.0084) 121.36 (0.59) 114.36 (0.58) N1 - C6 C1 N2 - Distance Angles C2 1.3955 (0.0086) C4 1.3972 (0.0094) 122.43 (0.64) C3 1.4869 (0.0098) 117.37 (0.58) 120.20 (0.58) N2 - C2 C4 O1 - Distance Angles C2 1.2108 (0.0082) O1 - O2 - Distance Angles C4 1.2142 (0.0082) O2 - F1 - Distance Angles P1 1.5820 (0.0047) F1 - F2 - Distance Angles P1 1.5698 (0.0055) F2 - F3 - Distance Angles P1 1.5794 (0.0051) F3 - F4 - Distance Angles P1 1.6040 (0.0046) F4 - F5 - Distance Angles P1 1.5731 (0.0052) F5 - F6 - Distance Angles P1 1.5773 (0.0053) F6 - P1 - Distance Angles F2 1.5698 (0.0055) F5 1.5731 (0.0052) 178.09 (0.32) F6 1.5773 (0.0053) 90.32 (0.37) 90.76 (0.36) F3 1.5794 (0.0051) 89.31 (0.32) 89.58 (0.31) 178.89 (0.35) F1 1.5820 (0.0047) 89.18 (0.31) 92.38 (0.29) 90.43 (0.31) 90.61 (0.27) F4 1.6040 (0.0046) 90.29 (0.29) 88.15 (0.26) 89.51 (0.30) 89.44 (0.27) 179.47 (0.31) P1 - F2 F5 F6 F3 F1 FMAP and GRID set by program FMAP 2 3 26 GRID -1.087 -2 -2 1.087 2 2 R1 = 0.2319 for 3630 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.72 at 0.6724 0.4570 0.2160 [ 0.98 A from F3 ] Deepest hole -0.45 at 0.5797 0.5085 0.1852 [ 0.75 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 2298 / 19519 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.1724 -0.0430 0.2840 1.00000 0.05 0.72 0.98 F3 1.28 F2 1.36 P1 2.04 F4 Q2 1 -0.0585 -0.1789 0.3238 1.00000 0.05 0.53 1.11 F3 1.18 F5 1.31 P1 1.91 F1 Q3 1 0.1204 -0.0567 0.3782 1.00000 0.05 0.50 1.02 F6 1.38 F5 1.43 P1 1.91 F1 Q4 1 0.4758 -0.2993 0.2146 1.00000 0.05 0.45 1.16 H3A 1.80 F2 2.07 C3 2.20 H12 Q5 1 0.4538 0.0378 0.3357 1.00000 0.05 0.41 1.29 C4 1.35 N2 1.41 C5 1.49 N1 Q6 1 0.2558 0.2305 0.2848 1.00000 0.05 0.40 1.36 H5B 1.59 H6 1.69 H3A 1.95 C5 Q7 1 0.3809 -0.0445 0.1584 1.00000 0.05 0.40 1.24 O2 1.43 H8 2.04 H6 2.14 C8 Q8 1 0.1430 0.0357 0.4393 1.00000 0.05 0.39 1.52 F6 2.32 F1 2.34 H11 2.62 P1 Q9 1 -0.0915 0.9424 0.4986 1.00000 0.05 0.39 1.96 H11 2.25 F1 2.75 H11 2.85 F1 Q10 1 0.0194 0.6704 0.6609 1.00000 0.05 0.38 0.88 H12 1.60 C12 2.04 O2 2.43 H3A Shortest distances between peaks (including symmetry equivalents) 8 9 1.42 3 8 1.55 7 10 1.65 1 2 1.75 4 10 1.76 9 9 1.84 4 6 1.86 2 3 2.05 8 9 2.56 5 6 2.58 1 3 2.77 6 10 2.79 6 7 2.82 4 7 2.83 3 9 2.83 1 4 2.87 Time profile in seconds ----------------------- 0.07: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.79: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.46: Structure factors and derivatives 1.88: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.34: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.12: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src1029 finished at 17:14:25 Total CPU time: 5.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++