+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0256 started at 11:35:00 on 16-Mar-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0256 in P21/c CELL 0.71073 10.6006 9.5629 19.5682 90.0 91.038 90.0 ZERR 4.00 0.0006 0.0004 0.0011 0.00 0.002 0.00 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O P UNIT 72 96 20 8 12 V = 1983.35 F(000) = 912.0 Mu = 0.33 mm-1 Cell Wt = 1741.33 Rho = 1.458 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 10 SIZE 0.20 0.20 0.40 ACTA BOND $H WGHT 0.06150 8.56470 L.S. 5 TEMP -153.00 FVAR 0.51288 P1 5 0.934574 0.174594 0.082258 11.00000 0.01463 0.02958 = 0.01767 -0.00168 0.00193 0.00172 P2 5 0.851339 0.309440 -0.036321 11.00000 0.01940 0.02916 = 0.01655 -0.00027 0.00549 0.00054 P3 5 0.726983 0.351707 0.084963 11.00000 0.01623 0.02697 = 0.01659 0.00005 0.00352 0.00261 O1 4 1.068697 0.217047 0.115030 11.00000 0.01591 0.03752 = 0.02700 -0.00241 0.00021 -0.00057 O2 4 0.761634 0.217606 -0.085102 11.00000 0.02449 0.03035 = 0.02026 0.00156 0.00123 -0.00299 N1 3 0.943873 0.202240 0.002169 11.00000 0.02174 0.03714 = 0.02108 -0.00023 0.00385 0.00812 N2 3 0.769585 0.408941 0.011046 11.00000 0.02475 0.02824 = 0.01929 0.00285 0.00684 0.00346 N3 3 0.829095 0.255572 0.124033 11.00000 0.01765 0.03460 = 0.01626 -0.00047 0.00205 0.00726 N4 3 0.922423 0.005146 0.095322 11.00000 0.02162 0.03766 = 0.01581 -0.00025 -0.00214 -0.00137 AFIX 43 H4 2 0.897686 -0.052461 0.063048 11.00000 -1.20000 AFIX 0 N5 3 0.930862 0.400201 -0.092978 11.00000 0.02194 0.03761 = 0.02200 0.00162 0.00741 -0.00464 AFIX 43 H5 2 1.013634 0.406462 -0.090519 11.00000 -1.20000 AFIX 0 C1 1 0.956176 -0.043406 0.165403 11.00000 0.02586 0.03880 = 0.02003 0.00396 0.00285 0.00062 AFIX 23 H1A 2 0.958265 -0.146911 0.166593 11.00000 -1.20000 H1B 2 0.890370 -0.012528 0.197155 11.00000 -1.20000 AFIX 0 C2 1 1.085235 0.013043 0.189868 11.00000 0.02435 0.04894 = 0.02246 -0.00190 -0.00238 0.00687 AFIX 23 H2A 2 1.100784 -0.016636 0.237945 11.00000 -1.20000 H2B 2 1.152448 -0.027731 0.161831 11.00000 -1.20000 AFIX 0 C3 1 1.091570 0.170706 0.184750 11.00000 0.02394 0.04447 = 0.02530 -0.00364 -0.00639 0.00303 AFIX 23 H3A 2 1.027680 0.212107 0.214745 11.00000 -1.20000 H3B 2 1.175850 0.202893 0.200441 11.00000 -1.20000 AFIX 0 C4 1 0.857093 0.470894 -0.148287 11.00000 0.03674 0.03283 = 0.02219 0.00567 0.00990 -0.00325 AFIX 23 H4A 2 0.915242 0.516026 -0.180869 11.00000 -1.20000 H4B 2 0.803595 0.544572 -0.128654 11.00000 -1.20000 AFIX 0 C5 1 0.773760 0.365223 -0.186029 11.00000 0.03960 0.03856 = 0.02004 0.00288 0.00186 -0.00065 AFIX 23 H5A 2 0.722496 0.414561 -0.221613 11.00000 -1.20000 H5B 2 0.827802 0.296333 -0.208960 11.00000 -1.20000 AFIX 0 C6 1 0.687457 0.289681 -0.137311 11.00000 0.02539 0.03729 = 0.02437 0.00216 -0.00181 -0.00084 AFIX 23 H6A 2 0.630512 0.357701 -0.115827 11.00000 -1.20000 H6B 2 0.634985 0.221524 -0.162705 11.00000 -1.20000 AFIX 0 C7 1 0.690209 0.503311 0.135967 11.00000 0.01676 0.03814 = 0.01900 -0.00369 0.00048 0.00651 C8 1 0.721055 0.637388 0.114808 11.00000 0.02740 0.02611 = 0.02764 0.00136 -0.00204 0.00174 AFIX 43 H8 2 0.764925 0.651250 0.073363 11.00000 -1.20000 AFIX 0 C9 1 0.688252 0.752296 0.153842 11.00000 0.02808 0.03025 = 0.04433 -0.00392 -0.01168 0.00554 AFIX 43 H9 2 0.709446 0.843903 0.138616 11.00000 -1.20000 AFIX 0 C10 1 0.624917 0.734040 0.214740 11.00000 0.02505 0.04590 = 0.04045 -0.01799 -0.01174 0.01203 AFIX 43 H10 2 0.602491 0.812849 0.240981 11.00000 -1.20000 AFIX 0 C11 1 0.594557 0.600651 0.237093 11.00000 0.02027 0.06527 = 0.02504 -0.01123 0.00131 0.00270 AFIX 43 H11 2 0.552007 0.587629 0.279008 11.00000 -1.20000 AFIX 0 C12 1 0.626597 0.484630 0.197871 11.00000 0.02286 0.04184 = 0.02249 -0.00283 0.00290 0.00037 AFIX 43 H12 2 0.605263 0.393112 0.213166 11.00000 -1.20000 AFIX 0 C13 1 0.579392 0.257206 0.078629 11.00000 0.01839 0.02995 = 0.01611 -0.00135 0.00247 0.00362 C14 1 0.465790 0.325245 0.062515 11.00000 0.02056 0.02872 = 0.02564 0.00033 0.00175 0.00174 AFIX 43 H14 2 0.464378 0.423980 0.056519 11.00000 -1.20000 AFIX 0 C15 1 0.354287 0.248665 0.055186 11.00000 0.01865 0.04854 = 0.02310 -0.00521 0.00163 0.00565 AFIX 43 H15 2 0.277079 0.295898 0.045344 11.00000 -1.20000 AFIX 0 C16 1 0.355527 0.105181 0.062130 11.00000 0.02125 0.03838 = 0.02435 -0.00474 0.00291 -0.00270 AFIX 43 H16 2 0.279565 0.053662 0.056377 11.00000 -1.20000 AFIX 0 C17 1 0.468091 0.035601 0.077581 11.00000 0.02953 0.02979 = 0.03186 -0.00004 0.00639 -0.00846 AFIX 43 H17 2 0.469573 -0.063398 0.082243 11.00000 -1.20000 AFIX 0 C18 1 0.579423 0.113442 0.086195 11.00000 0.01999 0.03469 = 0.02602 0.00290 0.00244 0.00058 AFIX 43 H18 2 0.656114 0.066347 0.097427 11.00000 -1.20000 AFIX 0 HKLF 4 1.0 0.00 1.00 0.00 -1.00 0.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for 2007src0256 in P21/c C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 P1 - N1 N3 O1 N4 P2 - N2 N1 O2 N5 P3 - N3 N2 C7 C13 O1 - C3 P1 O2 - C6 P2 N1 - P1 P2 N2 - P2 P3 N3 - P1 P3 N4 - C1 P1 N5 - C4 P2 C1 - N4 C2 C2 - C3 C1 C3 - O1 C2 C4 - N5 C5 C5 - C6 C4 C6 - O2 C5 C7 - C8 C12 P3 C8 - C9 C7 C9 - C8 C10 C10 - C11 C9 C11 - C10 C12 C12 - C11 C7 C13 - C18 C14 P3 C14 - C15 C13 C15 - C16 C14 C16 - C15 C17 C17 - C16 C18 C18 - C13 C17 h k l Fo^2 Sigma Why rejected 0 5 0 15.64 3.87 observed but should be systematically absent 0 5 0 8.34 1.78 observed but should be systematically absent 0 5 0 8.35 1.54 observed but should be systematically absent 32022 Reflections read, of which 1136 rejected -13 =< h =< 13, -12 =< k =< 12, -25 =< l =< 25, Max. 2-theta = 54.99 3 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 8 0 303.90 8.48 9 43.41 1 10 0 108.38 4.62 4 30.10 -4 7 1 139.21 3.63 11 18.83 -3 8 1 31.28 2.15 7 11.43 -4 9 1 23.93 1.40 7 8.26 3 10 1 47.46 4.41 2 24.11 6 11 1 49.88 7.73 2 42.28 -6 5 2 294.61 6.79 9 41.08 -5 5 2 301.38 6.49 9 38.76 5 7 2 90.16 2.29 15 12.20 2 8 2 110.27 2.49 11 18.40 -7 9 2 24.90 4.01 2 22.84 4 10 2 69.07 3.49 2 67.75 -1 11 2 67.39 5.63 2 51.13 3 8 3 65.44 1.35 14 16.57 6 8 3 57.24 4.56 4 24.96 -2 10 3 36.11 3.02 2 17.61 0 10 3 28.02 1.54 4 10.87 1 10 3 182.14 5.71 5 28.68 -4 7 4 59.16 1.84 10 15.02 3 8 4 18.99 2.34 12 14.66 -4 9 4 51.00 2.93 4 17.44 -2 9 4 350.84 12.74 4 86.47 -4 9 5 24.03 2.33 3 15.22 -5 10 5 22.33 4.05 2 22.37 -2 8 6 12.55 1.59 6 9.81 4 8 6 66.70 3.45 9 18.98 5 8 6 109.14 4.78 6 24.97 -2 9 6 63.90 5.63 2 32.71 0 9 6 88.31 3.53 6 22.89 -5 10 6 117.12 14.56 2 75.34 -3 10 6 39.19 4.40 2 23.31 -5 11 6 21.60 4.59 2 39.32 0 7 7 29.00 2.55 7 19.79 2 8 7 104.79 3.93 6 24.34 4 8 7 15.93 1.36 10 7.87 -7 9 7 26.00 4.84 2 24.65 -2 9 7 132.89 10.16 2 54.20 2 9 7 151.94 9.77 3 58.09 -4 11 7 58.44 10.70 3 62.04 -6 7 8 82.71 6.84 2 37.18 -5 7 8 247.60 8.92 6 45.18 -10 5 9 105.54 12.28 2 110.11 -2 10 9 81.23 4.33 4 28.42 -12 2 10 25.32 6.53 2 35.68 -3 9 10 99.94 8.01 2 45.27 -11 3 11 86.58 10.98 2 75.52 47 Inconsistent equivalents 4471 Unique reflections, of which 0 suppressed R(int) = 0.0807 R(sigma) = 0.0570 Friedel opposites merged Maximum memory for data reduction = 2637 / 44611 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 = 3370 / 315220 wR2 = 0.1927 before cycle 1 for 4471 data and 253 / 253 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0615 * P )^2 + 8.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.51200 0.00147 -0.599 OSF Mean shift/esd = 0.053 Maximum = -0.599 for OSF Max. shift = 0.001 A for N4 Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3370 / 315220 wR2 = 0.1925 before cycle 2 for 4471 data and 253 / 253 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0615 * P )^2 + 8.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.51198 0.00147 -0.012 OSF Mean shift/esd = 0.020 Maximum = -0.123 for U23 C4 Max. shift = 0.000 A for N4 Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3370 / 315220 wR2 = 0.1925 before cycle 3 for 4471 data and 253 / 253 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0615 * P )^2 + 8.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.51198 0.00147 0.001 OSF Mean shift/esd = 0.003 Maximum = 0.018 for U22 O2 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3370 / 315220 wR2 = 0.1925 before cycle 4 for 4471 data and 253 / 253 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0615 * P )^2 + 8.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.51198 0.00147 0.002 OSF Mean shift/esd = 0.001 Maximum = -0.005 for U22 C18 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C3 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3370 / 315220 wR2 = 0.1925 before cycle 5 for 4471 data and 253 / 253 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0615 * P )^2 + 8.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.51198 0.00147 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for U22 C2 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C2 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 6 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H4 0.8976 -0.0530 0.0629 43 0.880 0.000 N4 C1 P1 H5 1.0136 0.4066 -0.0905 43 0.880 0.000 N5 C4 P2 H1A 0.9580 -0.1469 0.1661 23 0.990 0.000 C1 N4 C2 H1B 0.8906 -0.0122 0.1974 23 0.990 0.000 C1 N4 C2 H2A 1.1008 -0.0156 0.2379 23 0.990 0.000 C2 C3 C1 H2B 1.1523 -0.0286 0.1617 23 0.990 0.000 C2 C3 C1 H3A 1.0278 0.2125 0.2149 23 0.990 0.000 C3 O1 C2 H3B 1.1759 0.2031 0.2006 23 0.990 0.000 C3 O1 C2 H4A 0.9154 0.5153 -0.1808 23 0.990 0.000 C4 N5 C5 H4B 0.8038 0.5451 -0.1285 23 0.990 0.000 C4 N5 C5 H5A 0.7222 0.4141 -0.2213 23 0.990 0.000 C5 C6 C4 H5B 0.8276 0.2961 -0.2094 23 0.990 0.000 C5 C6 C4 H6A 0.6306 0.3579 -0.1155 23 0.990 0.000 C6 O2 C5 H6B 0.6348 0.2213 -0.1630 23 0.990 0.000 C6 O2 C5 H8 0.7648 0.6505 0.0733 43 0.950 0.000 C8 C9 C7 H9 0.7091 0.8437 0.1389 43 0.950 0.000 C9 C8 C10 H10 0.6023 0.8132 0.2412 43 0.950 0.000 C10 C11 C9 H11 0.5520 0.5885 0.2790 43 0.950 0.000 C11 C10 C12 H12 0.6056 0.3932 0.2129 43 0.950 0.000 C12 C11 C7 H14 0.4646 0.4238 0.0566 43 0.950 0.000 C14 C15 C13 H15 0.2771 0.2956 0.0454 43 0.950 0.000 C15 C16 C14 H16 0.2795 0.0536 0.0564 43 0.950 0.000 C16 C15 C17 H17 0.4693 -0.0633 0.0822 43 0.950 0.000 C17 C16 C18 H18 0.6561 0.0665 0.0974 43 0.950 0.000 C18 C13 C17 2007src0256 in P21/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq P1 0.93457 0.17459 0.08226 1.00000 0.01449 0.02961 0.01770 -0.00176 0.00190 0.00169 0.02058 0.00174 0.00009 0.00012 0.00005 0.00000 0.00046 0.00060 0.00045 0.00040 0.00034 0.00040 0.00025 P2 0.85134 0.30942 -0.03632 1.00000 0.01929 0.02927 0.01659 -0.00026 0.00551 0.00047 0.02166 0.00180 0.00009 0.00012 0.00005 0.00000 0.00049 0.00060 0.00045 0.00040 0.00035 0.00042 0.00025 P3 0.72698 0.35172 0.08496 1.00000 0.01616 0.02702 0.01654 0.00004 0.00348 0.00259 0.01987 0.00176 0.00009 0.00012 0.00005 0.00000 0.00046 0.00058 0.00045 0.00038 0.00033 0.00040 0.00025 O1 1.06869 0.21703 0.11503 1.00000 0.01577 0.03776 0.02705 -0.00241 0.00029 -0.00063 0.02687 0.00490 0.00025 0.00033 0.00014 0.00000 0.00130 0.00185 0.00145 0.00126 0.00107 0.00121 0.00066 O2 0.76163 0.21762 -0.08511 1.00000 0.02430 0.03083 0.02033 0.00170 0.00128 -0.00310 0.02514 0.00484 0.00026 0.00032 0.00014 0.00000 0.00142 0.00172 0.00134 0.00115 0.00107 0.00122 0.00064 N1 0.94387 0.20219 0.00218 1.00000 0.02158 0.03730 0.02133 -0.00043 0.00384 0.00772 0.02669 0.00631 0.00031 0.00041 0.00017 0.00000 0.00164 0.00220 0.00164 0.00146 0.00127 0.00152 0.00079 N2 0.76957 0.40900 0.01104 1.00000 0.02463 0.02838 0.01923 0.00265 0.00677 0.00339 0.02400 0.00611 0.00031 0.00038 0.00016 0.00000 0.00167 0.00196 0.00156 0.00138 0.00124 0.00146 0.00073 N3 0.82907 0.25552 0.12403 1.00000 0.01754 0.03468 0.01637 -0.00055 0.00208 0.00714 0.02284 0.00588 0.00029 0.00039 0.00016 0.00000 0.00153 0.00206 0.00149 0.00136 0.00117 0.00143 0.00073 N4 0.92242 0.00506 0.09532 1.00000 0.02159 0.03765 0.01581 -0.00033 -0.00217 -0.00133 0.02505 0.00587 0.00030 0.00040 0.00016 0.00000 0.00162 0.00218 0.00154 0.00139 0.00122 0.00149 0.00076 H4 0.89756 -0.05302 0.06290 1.00000 0.03006 0.00000 0.00000 N5 0.93086 0.40025 -0.09298 1.00000 0.02175 0.03795 0.02210 0.00170 0.00742 -0.00463 0.02718 0.00618 0.00032 0.00040 0.00017 0.00000 0.00167 0.00223 0.00164 0.00150 0.00128 0.00153 0.00079 H5 1.01363 0.40657 -0.09052 1.00000 0.03262 0.00000 0.00000 C1 0.95618 -0.04344 0.16544 1.00000 0.02582 0.03896 0.02011 0.00332 0.00301 0.00043 0.02827 0.00759 0.00039 0.00052 0.00020 0.00000 0.00203 0.00263 0.00189 0.00174 0.00151 0.00186 0.00093 H1A 0.95804 -0.14694 0.16612 1.00000 0.03392 0.00000 0.00000 H1B 0.89056 -0.01219 0.19740 1.00000 0.03392 0.00000 0.00000 C2 1.08525 0.01297 0.18986 1.00000 0.02444 0.04860 0.02223 -0.00193 -0.00238 0.00691 0.03179 0.00768 0.00039 0.00053 0.00021 0.00000 0.00208 0.00301 0.00203 0.00188 0.00159 0.00198 0.00102 H2A 1.10081 -0.01556 0.23791 1.00000 0.03815 0.00000 0.00000 H2B 1.15232 -0.02857 0.16175 1.00000 0.03815 0.00000 0.00000 C3 1.09158 0.17066 0.18478 1.00000 0.02367 0.04486 0.02524 -0.00356 -0.00652 0.00309 0.03134 0.00746 0.00040 0.00052 0.00021 0.00000 0.00206 0.00291 0.00205 0.00191 0.00160 0.00191 0.00100 H3A 1.02780 0.21255 0.21493 1.00000 0.03761 0.00000 0.00000 H3B 1.17587 0.20309 0.20058 1.00000 0.03761 0.00000 0.00000 C4 0.85706 0.47089 -0.14830 1.00000 0.03668 0.03322 0.02190 0.00492 0.00980 -0.00348 0.03049 0.00788 0.00042 0.00050 0.00021 0.00000 0.00234 0.00254 0.00197 0.00175 0.00168 0.00197 0.00097 H4A 0.91535 0.51527 -0.18078 1.00000 0.03659 0.00000 0.00000 H4B 0.80385 0.54506 -0.12845 1.00000 0.03659 0.00000 0.00000 C5 0.77374 0.36520 -0.18606 1.00000 0.03943 0.03871 0.02010 0.00301 0.00171 -0.00057 0.03273 0.00798 0.00044 0.00052 0.00021 0.00000 0.00244 0.00273 0.00197 0.00180 0.00171 0.00209 0.00101 H5A 0.72221 0.41414 -0.22134 1.00000 0.03928 0.00000 0.00000 H5B 0.82759 0.29614 -0.20940 1.00000 0.03928 0.00000 0.00000 C6 0.68743 0.28970 -0.13732 1.00000 0.02538 0.03739 0.02449 0.00171 -0.00183 -0.00111 0.02911 0.00757 0.00039 0.00051 0.00021 0.00000 0.00208 0.00268 0.00200 0.00177 0.00161 0.00184 0.00095 H6A 0.63055 0.35791 -0.11554 1.00000 0.03494 0.00000 0.00000 H6B 0.63483 0.22133 -0.16297 1.00000 0.03494 0.00000 0.00000 C7 0.69021 0.50331 0.13599 1.00000 0.01675 0.03799 0.01895 -0.00365 0.00045 0.00662 0.02457 0.00703 0.00035 0.00048 0.00019 0.00000 0.00177 0.00253 0.00182 0.00164 0.00139 0.00168 0.00087 C8 0.72103 0.63742 0.11480 1.00000 0.02704 0.02621 0.02780 0.00111 -0.00205 0.00166 0.02704 0.00728 0.00039 0.00047 0.00022 0.00000 0.00207 0.00229 0.00206 0.00168 0.00161 0.00173 0.00089 H8 0.76480 0.65049 0.07335 1.00000 0.03245 0.00000 0.00000 C9 0.68825 0.75224 0.15383 1.00000 0.02803 0.03013 0.04429 -0.00388 -0.01207 0.00525 0.03431 0.00778 0.00041 0.00053 0.00025 0.00000 0.00221 0.00250 0.00258 0.00205 0.00191 0.00194 0.00104 H9 0.70914 0.84374 0.13890 1.00000 0.04117 0.00000 0.00000 C10 0.62491 0.73405 0.21476 1.00000 0.02503 0.04593 0.04034 -0.01771 -0.01161 0.01215 0.03725 0.00784 0.00041 0.00057 0.00025 0.00000 0.00216 0.00310 0.00253 0.00226 0.00185 0.00208 0.00116 H10 0.60232 0.81317 0.24122 1.00000 0.04470 0.00000 0.00000 C11 0.59456 0.60070 0.23706 1.00000 0.02020 0.06535 0.02505 -0.01156 0.00130 0.00257 0.03686 0.00793 0.00039 0.00061 0.00022 0.00000 0.00202 0.00370 0.00212 0.00215 0.00160 0.00212 0.00118 H11 0.55203 0.58849 0.27896 1.00000 0.04423 0.00000 0.00000 C12 0.62661 0.48464 0.19789 1.00000 0.02266 0.04222 0.02272 -0.00291 0.00303 0.00034 0.02917 0.00748 0.00038 0.00053 0.00020 0.00000 0.00199 0.00277 0.00200 0.00179 0.00155 0.00185 0.00096 H12 0.60558 0.39324 0.21291 1.00000 0.03500 0.00000 0.00000 C13 0.57936 0.25717 0.07863 1.00000 0.01828 0.03012 0.01597 -0.00133 0.00238 0.00368 0.02143 0.00679 0.00035 0.00046 0.00018 0.00000 0.00178 0.00228 0.00170 0.00152 0.00135 0.00160 0.00081 C14 0.46578 0.32523 0.06252 1.00000 0.02048 0.02883 0.02579 0.00024 0.00187 0.00169 0.02502 0.00721 0.00036 0.00047 0.00020 0.00000 0.00189 0.00235 0.00194 0.00167 0.00149 0.00168 0.00086 H14 0.46457 0.42381 0.05656 1.00000 0.03002 0.00000 0.00000 C15 0.35430 0.24863 0.05520 1.00000 0.01841 0.04896 0.02297 -0.00509 0.00146 0.00564 0.03010 0.00757 0.00038 0.00054 0.00020 0.00000 0.00189 0.00294 0.00198 0.00191 0.00150 0.00192 0.00098 H15 0.27712 0.29563 0.04540 1.00000 0.03612 0.00000 0.00000 C16 0.35552 0.10519 0.06212 1.00000 0.02140 0.03786 0.02424 -0.00488 0.00283 -0.00257 0.02781 0.00727 0.00038 0.00049 0.00020 0.00000 0.00196 0.00267 0.00198 0.00180 0.00151 0.00181 0.00092 H16 0.27949 0.05359 0.05635 1.00000 0.03337 0.00000 0.00000 C17 0.46808 0.03562 0.07755 1.00000 0.02945 0.02967 0.03187 -0.00029 0.00636 -0.00874 0.03026 0.00758 0.00040 0.00051 0.00022 0.00000 0.00216 0.00246 0.00224 0.00183 0.00172 0.00187 0.00095 H17 0.46933 -0.06326 0.08217 1.00000 0.03631 0.00000 0.00000 C18 0.57943 0.11337 0.08618 1.00000 0.01982 0.03484 0.02608 0.00279 0.00235 0.00073 0.02689 0.00739 0.00038 0.00048 0.00021 0.00000 0.00188 0.00257 0.00201 0.00175 0.00150 0.00173 0.00090 H18 0.65608 0.06653 0.09738 1.00000 0.03227 0.00000 0.00000 Final Structure Factor Calculation for 2007src0256 in P21/c Total number of l.s. parameters = 253 Maximum vector length = 511 Memory required = 3117 / 24017 wR2 = 0.1925 before cycle 6 for 4471 data and 0 / 253 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0615 * P )^2 + 8.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0749 for 3616 Fo > 4sig(Fo) and 0.0947 for all 4471 data wR2 = 0.1925, GooF = S = 1.092, Restrained GooF = 1.092 for all data Occupancy sum of asymmetric unit = 28.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0300 0.0183 0.0135 P1 0.0293 0.0232 0.0125 P2 0.0277 0.0191 0.0128 P3 0.0383 0.0265 0.0158 O1 0.0322 0.0236 0.0196 O2 0.0405 0.0235 0.0161 N1 0.0328 0.0243 0.0149 N2 0.0373 0.0176 0.0136 N3 0.0378 0.0225 0.0149 N4 0.0392 0.0285 0.0139 N5 0.0396 0.0266 0.0186 C1 0.0507 0.0245 0.0201 C2 0.0464 0.0301 0.0176 C3 0.0412 0.0351 0.0153 C4 0.0398 0.0389 0.0195 C5 0.0378 0.0269 0.0226 C6 0.0405 0.0187 0.0145 C7 0.0301 0.0276 0.0235 C8 0.0531 0.0294 0.0204 C9 0.0682 0.0254 0.0181 C10 0.0686 0.0228 0.0192 C11 0.0426 0.0251 0.0198 C12 0.0312 0.0190 0.0141 C13 0.0292 0.0260 0.0198 C14 0.0508 0.0228 0.0167 C15 0.0399 0.0235 0.0200 C16 0.0405 0.0309 0.0194 C17 0.0357 0.0257 0.0192 C18 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.024 0.036 0.048 0.064 0.079 0.101 0.131 0.191 1.000 Number in group 455. 466. 448. 419. 461. 436. 456. 446. 435. 449. GooF 1.406 1.223 1.132 1.050 0.919 1.013 0.962 1.131 0.947 1.038 K 7.441 1.935 1.351 1.138 1.048 1.023 0.999 0.996 1.012 0.996 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 458. 444. 439. 452. 449. 441. 446. 450. 442. 450. GooF 1.293 1.130 1.166 1.273 1.027 0.963 0.850 1.004 0.917 1.197 K 1.033 1.041 1.082 1.041 1.053 1.010 1.004 1.010 1.041 0.976 R1 0.218 0.170 0.147 0.141 0.117 0.099 0.065 0.055 0.050 0.050 Recommended weighting scheme: WGHT 0.0532 8.4598 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) -10 5 6 84.23 1463.60 8.88 0.192 0.90 -9 6 9 3.17 445.11 7.33 0.106 0.87 -10 7 6 59.78 672.52 7.24 0.130 0.81 3 11 4 500.96 47.12 6.69 0.034 0.83 0 12 4 604.70 10.00 6.48 0.016 0.79 -6 3 12 392.52 1117.72 5.90 0.168 1.13 0 11 6 248.11 0.90 5.86 0.005 0.84 -3 10 8 201.24 679.90 5.53 0.131 0.86 -4 6 5 141.38 8.78 5.00 0.015 1.29 -8 6 11 -0.34 184.19 4.91 0.068 0.89 -1 10 3 627.70 64.53 4.82 0.040 0.94 0 8 3 170.62 7.30 4.81 0.014 1.18 -3 10 3 176.28 0.08 4.78 0.001 0.91 -11 4 4 107.09 521.53 4.64 0.115 0.88 4 5 2 95.73 5.19 4.61 0.011 1.53 -13 3 6 -54.25 359.21 4.60 0.095 0.77 8 8 3 219.47 25.07 4.59 0.025 0.88 1 11 8 245.82 2.16 4.54 0.007 0.82 -8 5 11 179.65 579.45 4.54 0.121 0.94 -1 9 3 117.12 2.18 4.49 0.007 1.04 7 8 5 280.22 45.53 4.25 0.034 0.91 -7 6 10 100.10 385.66 4.23 0.099 0.96 -13 0 8 -18.04 198.74 4.20 0.071 0.78 1 12 6 549.62 190.24 4.08 0.069 0.77 1 11 4 396.95 85.68 3.90 0.046 0.85 -3 9 11 191.50 4.32 3.88 0.010 0.89 -4 11 9 625.66 216.66 3.87 0.074 0.77 1 10 4 762.88 311.56 3.87 0.089 0.93 -8 10 3 363.26 46.64 3.87 0.034 0.77 6 9 11 247.40 31.23 3.82 0.028 0.81 4 10 7 120.26 5.35 3.82 0.012 0.85 -12 4 2 42.99 233.58 3.65 0.077 0.83 -4 11 8 923.36 518.49 3.63 0.114 0.78 2 10 7 123.86 11.35 3.60 0.017 0.89 4 9 15 107.48 0.48 3.60 0.003 0.78 0 1 2 2857.57 4335.39 3.57 0.330 6.84 4 10 9 140.68 22.98 3.55 0.024 0.83 0 11 3 414.69 183.12 3.54 0.068 0.86 2 11 4 122.59 0.07 3.47 0.001 0.84 8 9 8 96.52 3.87 3.47 0.010 0.78 -5 7 9 66.63 1.41 3.45 0.006 1.02 0 4 5 143.97 38.61 3.44 0.031 2.04 3 10 10 159.52 25.11 3.41 0.025 0.83 4 10 12 106.51 2.81 3.40 0.008 0.79 2 2 8 1581.02 1104.94 3.37 0.167 2.00 4 1 4 169.06 63.03 3.34 0.040 2.25 -7 10 6 -47.82 205.04 3.30 0.072 0.79 -3 10 7 349.41 122.99 3.30 0.056 0.88 -5 11 7 302.62 676.67 3.29 0.131 0.77 1 3 0 57.76 5.23 3.28 0.011 3.05 Bond lengths and angles P1 - Distance Angles N1 1.5939 (0.0034) N3 1.5973 (0.0033) 118.63 (0.18) O1 1.6013 (0.0028) 106.35 (0.17) 107.28 (0.17) N4 1.6467 (0.0039) 108.79 (0.19) 109.89 (0.19) 105.00 (0.17) P1 - N1 N3 O1 P2 - Distance Angles N2 1.5957 (0.0034) N1 1.5982 (0.0036) 116.38 (0.18) O2 1.5980 (0.0029) 110.56 (0.17) 106.42 (0.18) N5 1.6517 (0.0035) 111.42 (0.19) 109.73 (0.18) 101.14 (0.16) P2 - N2 N1 O2 P3 - Distance Angles N3 1.6037 (0.0033) N2 1.6188 (0.0033) 115.05 (0.17) C7 1.8068 (0.0043) 110.32 (0.18) 106.79 (0.20) C13 1.8096 (0.0041) 108.74 (0.19) 111.27 (0.17) 104.11 (0.18) P3 - N3 N2 C7 O1 - Distance Angles C3 1.4513 (0.0050) P1 1.6013 (0.0028) 115.55 (0.26) O1 - C3 O2 - Distance Angles C6 1.4521 (0.0048) P2 1.5980 (0.0029) 117.94 (0.27) O2 - C6 N1 - Distance Angles P1 1.5939 (0.0034) P2 1.5982 (0.0036) 121.42 (0.21) N1 - P1 N2 - Distance Angles P2 1.5957 (0.0035) P3 1.6188 (0.0033) 118.70 (0.22) N2 - P2 N3 - Distance Angles P1 1.5973 (0.0033) P3 1.6037 (0.0033) 120.44 (0.20) N3 - P1 N4 - Distance Angles C1 1.4859 (0.0049) P1 1.6467 (0.0039) 115.63 (0.29) H4 0.8800 122.19 122.19 N4 - C1 P1 N5 - Distance Angles C4 1.4864 (0.0054) P2 1.6517 (0.0035) 117.36 (0.27) H5 0.8800 121.32 121.32 N5 - C4 P2 C1 - Distance Angles N4 1.4859 (0.0049) C2 1.5387 (0.0057) 112.04 (0.35) H1A 0.9900 109.20 109.20 H1B 0.9900 109.20 109.20 107.90 C1 - N4 C2 H1A C2 - Distance Angles C3 1.5129 (0.0069) C1 1.5387 (0.0057) 111.67 (0.36) H2A 0.9900 109.29 109.29 H2B 0.9900 109.29 109.29 107.95 C2 - C3 C1 H2A C3 - Distance Angles O1 1.4513 (0.0050) C2 1.5129 (0.0069) 111.07 (0.35) H3A 0.9900 109.42 109.42 H3B 0.9900 109.42 109.42 108.03 C3 - O1 C2 H3A C4 - Distance Angles N5 1.4864 (0.0054) C5 1.5244 (0.0063) 110.14 (0.37) H4A 0.9900 109.63 109.63 H4B 0.9900 109.63 109.63 108.15 C4 - N5 C5 H4A C5 - Distance Angles C6 1.5165 (0.0061) C4 1.5244 (0.0063) 111.20 (0.35) H5A 0.9900 109.39 109.39 H5B 0.9900 109.39 109.39 108.01 C5 - C6 C4 H5A C6 - Distance Angles O2 1.4521 (0.0048) C5 1.5165 (0.0060) 110.08 (0.33) H6A 0.9900 109.64 109.64 H6B 0.9900 109.64 109.64 108.16 C6 - O2 C5 H6A C7 - Distance Angles C8 1.3887 (0.0063) C12 1.4082 (0.0056) 119.52 (0.40) P3 1.8068 (0.0043) 121.44 (0.31) 119.02 (0.35) C7 - C8 C12 C8 - Distance Angles C9 1.3855 (0.0064) C7 1.3887 (0.0063) 120.31 (0.42) H8 0.9500 119.85 119.85 C8 - C9 C7 C9 - Distance Angles C8 1.3855 (0.0064) C10 1.3897 (0.0071) 120.24 (0.47) H9 0.9500 119.88 119.88 C9 - C8 C10 C10 - Distance Angles C11 1.3875 (0.0079) C9 1.3897 (0.0072) 120.22 (0.44) H10 0.9500 119.89 119.89 C10 - C11 C9 C11 - Distance Angles C10 1.3875 (0.0079) C12 1.3943 (0.0066) 119.90 (0.43) H11 0.9500 120.05 120.05 C11 - C10 C12 C12 - Distance Angles C11 1.3943 (0.0066) C7 1.4082 (0.0056) 119.81 (0.46) H12 0.9500 120.09 120.09 C12 - C11 C7 C13 - Distance Angles C18 1.3830 (0.0063) C14 1.3995 (0.0053) 119.03 (0.38) P3 1.8096 (0.0041) 119.38 (0.29) 121.49 (0.33) C13 - C18 C14 C14 - Distance Angles C15 1.3955 (0.0059) C13 1.3995 (0.0053) 120.16 (0.42) H14 0.9500 119.92 119.92 C14 - C15 C13 C15 - Distance Angles C16 1.3785 (0.0068) C14 1.3955 (0.0059) 120.39 (0.40) H15 0.9500 119.81 119.81 C15 - C16 C14 C16 - Distance Angles C15 1.3785 (0.0068) C17 1.3944 (0.0061) 120.16 (0.39) H16 0.9500 119.92 119.92 C16 - C15 C17 C17 - Distance Angles C16 1.3944 (0.0061) C18 1.4026 (0.0058) 119.22 (0.43) H17 0.9500 120.39 120.39 C17 - C16 C18 C18 - Distance Angles C13 1.3830 (0.0063) C17 1.4026 (0.0058) 121.02 (0.39) H18 0.9500 119.49 119.49 C18 - C13 C17 FMAP and GRID set by program FMAP 2 3 24 GRID -1.190 -2 -2 1.190 2 2 R1 = 0.0944 for 4471 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.75 at 0.9314 0.0863 0.0846 [ 0.81 A from N4 ] Deepest hole -0.76 at 0.7408 0.2932 0.0563 [ 0.81 A from P3 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 3009 / 21639 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9314 0.0863 0.0846 1.00000 0.05 0.75 0.81 N4 0.85 P1 1.44 H4 1.96 N1 Q2 1 0.7228 0.2625 0.0851 1.00000 0.05 0.63 0.85 P3 1.35 N3 1.52 C13 2.02 H18 Q3 1 0.9702 -0.0228 0.0627 1.00000 0.05 0.57 0.82 H4 0.86 N4 1.96 P1 2.03 C1 Q4 1 0.9199 0.2673 0.0849 1.00000 0.05 0.55 0.90 P1 1.25 N3 1.74 O1 1.76 N1 Q5 1 0.9821 0.4718 -0.0718 1.00000 0.05 0.50 0.80 H5 0.96 N5 1.98 C4 2.20 P2 Q6 1 0.6533 0.2725 -0.0214 1.00000 0.05 0.43 1.79 O2 1.90 N2 2.03 H6A 2.13 C13 Q7 1 0.8115 0.2783 -0.2897 1.00000 0.05 0.42 1.59 H5B 1.73 N3 2.10 H5A 2.23 C5 Q8 1 0.8839 0.1790 -0.2249 1.00000 0.05 0.39 1.31 H5B 1.59 H2A 1.94 H2B 1.98 C2 Q9 1 0.6085 0.8548 0.2146 1.00000 0.05 0.39 0.66 H10 1.17 C10 1.77 C9 1.84 H9 Q10 1 0.7471 0.4942 -0.0457 1.00000 0.05 0.39 1.39 N2 1.80 H4B 2.03 H15 2.09 P2 Shortest distances between peaks (including symmetry equivalents) 1 3 1.20 1 4 1.73 7 8 1.75 2 4 2.09 2 6 2.20 6 10 2.39 5 10 2.56 3 3 2.58 2 7 2.64 4 5 2.72 4 7 2.76 1 2 2.78 3 4 2.86 5 5 2.88 Time profile in seconds ----------------------- 0.04: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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 0.01: Analyse other restraints etc. 4.96: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.01: Generate idealized H-atoms 2.48: Structure factors and derivatives 3.69: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.39: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.19: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0256 finished at 11:36:25 Total CPU time: 12.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++