+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0258r started at 18:11:45 on 20-May-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0258r in P4(1) CELL 0.71073 11.4892 11.4892 16.7646 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0001 0.0003 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM - Y, X, 1/4 + Z SYMM Y, - X, 3/4 + Z SFAC C H N O P S UNIT 72 96 20 8 12 8 V = 2212.96 F(000) = 1040.0 Mu = 0.48 mm-1 Cell Wt = 1997.81 Rho = 1.499 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 20 SIZE 0.02 0.10 0.14 ACTA BOND WGHT 0.00760 1.43950 L.S. 4 TEMP -153.00 FVAR 0.68790 H5N 2 0.019630 0.272139 0.292750 11.00000 0.01638 H4N 2 0.408269 0.469024 0.150677 11.00000 0.03541 MOLE 1 C1 1 0.162861 0.291067 0.458787 11.00000 0.02934 0.02068 = 0.01648 0.00522 -0.00001 0.00033 C2 1 0.216852 0.193720 0.426910 11.00000 0.02528 0.02763 = 0.02877 0.00455 0.00209 0.00473 AFIX 43 H2 2 0.298532 0.193324 0.418102 11.00000 -1.20000 AFIX 0 C3 1 0.150120 0.096743 0.407993 11.00000 0.05023 0.02382 = 0.03020 0.00146 0.00138 0.00733 AFIX 43 H3 2 0.186464 0.029388 0.386546 11.00000 -1.20000 AFIX 0 C4 1 0.030770 0.097700 0.420236 11.00000 0.04431 0.02491 = 0.03450 0.00603 -0.00395 -0.00887 AFIX 43 H4 2 -0.014586 0.031640 0.406258 11.00000 -1.20000 AFIX 0 C5 1 -0.022107 0.194408 0.452667 11.00000 0.02917 0.03414 = 0.03617 0.01251 0.00271 -0.00195 AFIX 43 H5 2 -0.103769 0.194409 0.461558 11.00000 -1.20000 AFIX 0 C6 1 0.043168 0.291609 0.472370 11.00000 0.03053 0.02542 = 0.02523 0.00652 0.00317 0.00457 AFIX 43 H6 2 0.006667 0.358085 0.494951 11.00000 -1.20000 AFIX 0 C7 1 0.168861 0.709499 0.441144 11.00000 0.01843 0.01637 = 0.02135 -0.00324 0.00082 -0.00457 C8 1 0.083818 0.750876 0.389791 11.00000 0.03065 0.02136 = 0.02887 -0.00220 -0.00555 -0.00184 AFIX 43 H8 2 0.097141 0.751968 0.333870 11.00000 -1.20000 AFIX 0 C9 1 -0.020846 0.790660 0.420673 11.00000 0.02736 0.02605 = 0.05562 -0.00830 -0.01304 0.00440 AFIX 43 H9 2 -0.079767 0.818715 0.385875 11.00000 -1.20000 AFIX 0 C10 1 -0.039356 0.789453 0.502139 11.00000 0.02386 0.02728 = 0.06430 -0.01928 0.01019 -0.00395 AFIX 43 H10 2 -0.111064 0.817151 0.523013 11.00000 -1.20000 AFIX 0 C11 1 0.045034 0.748519 0.553478 11.00000 0.03872 0.02819 = 0.03205 -0.00649 0.01275 -0.00617 AFIX 43 H11 2 0.031529 0.747668 0.609381 11.00000 -1.20000 AFIX 0 C12 1 0.149880 0.708572 0.522757 11.00000 0.03197 0.02440 = 0.02394 -0.00210 0.00325 -0.00279 AFIX 43 H12 2 0.208644 0.680586 0.557707 11.00000 -1.20000 AFIX 0 C13 1 0.515415 0.217099 0.259702 11.00000 0.01952 0.02072 = 0.02546 0.00151 -0.00432 0.00671 AFIX 23 H13A 2 0.532030 0.132691 0.263075 11.00000 -1.20000 H13B 2 0.541183 0.253767 0.310139 11.00000 -1.20000 AFIX 0 C14 1 0.582678 0.269709 0.189991 11.00000 0.01578 0.02179 = 0.02698 -0.00166 -0.00115 0.00366 AFIX 23 H14A 2 0.667214 0.260552 0.199557 11.00000 -1.20000 H14B 2 0.562918 0.227162 0.140457 11.00000 -1.20000 AFIX 0 C15 1 0.554626 0.397799 0.179253 11.00000 0.01816 0.02503 = 0.02683 0.00178 -0.00124 -0.00063 AFIX 23 H15A 2 0.578911 0.441795 0.227224 11.00000 -1.20000 H15B 2 0.597658 0.429045 0.132788 11.00000 -1.20000 AFIX 0 C16 1 -0.060992 0.554201 0.208708 11.00000 0.01727 0.02581 = 0.02862 0.00425 -0.00652 0.00505 AFIX 23 H16A 2 -0.090477 0.605096 0.165553 11.00000 -1.20000 H16B 2 -0.047014 0.603092 0.256382 11.00000 -1.20000 AFIX 0 C17 1 -0.151335 0.462100 0.228057 11.00000 0.01489 0.02930 = 0.02918 -0.00071 -0.00529 0.00385 AFIX 23 H17A 2 -0.170857 0.418750 0.178806 11.00000 -1.20000 H17B 2 -0.223159 0.500647 0.247200 11.00000 -1.20000 AFIX 0 C18 1 -0.109279 0.376656 0.291216 11.00000 0.01554 0.02464 = 0.02986 -0.00049 0.00122 -0.00218 AFIX 23 H18A 2 -0.094270 0.418229 0.341908 11.00000 -1.20000 H18B 2 -0.169592 0.316800 0.301017 11.00000 -1.20000 AFIX 0 N1 3 0.360384 0.434424 0.320016 11.00000 0.01633 0.02231 = 0.02263 -0.00308 -0.00503 0.00106 N2 3 0.213139 0.353580 0.205552 11.00000 0.01715 0.02316 = 0.01891 -0.00241 -0.00220 0.00000 N3 3 0.130866 0.488868 0.326244 11.00000 0.01679 0.01927 = 0.02020 -0.00255 -0.00197 0.00060 N4 3 0.428225 0.411658 0.166590 11.00000 0.01834 0.01813 = 0.02312 0.00422 -0.00282 0.00219 N5 3 -0.000304 0.320462 0.262403 11.00000 0.01666 0.01722 = 0.02256 0.00125 -0.00220 -0.00156 O1 4 0.390441 0.234993 0.249496 11.00000 0.01818 0.01760 = 0.02213 0.00223 -0.00033 0.00012 O2 4 0.047521 0.500535 0.183764 11.00000 0.01941 0.02440 = 0.02196 0.00398 -0.00387 0.00126 P1 5 0.254317 0.489473 0.368018 11.00000 0.01686 0.01702 = 0.01636 -0.00077 -0.00298 -0.00049 P2 5 0.342894 0.363650 0.237730 11.00000 0.01521 0.01666 = 0.01740 -0.00100 -0.00215 0.00087 P3 5 0.106427 0.415470 0.247068 11.00000 0.01462 0.01683 = 0.01683 0.00026 -0.00253 -0.00028 S1 6 0.244885 0.418467 0.482826 11.00000 0.03186 0.02642 = 0.01771 0.00310 -0.00511 -0.00199 S2 6 0.303828 0.658814 0.401501 11.00000 0.01945 0.02120 = 0.02234 -0.00498 0.00197 -0.00399 HKLF 4 Covalent radii and connectivity table for 2007src0258r in P4(1) C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 S 1.030 C1 - C2 C6 S1 C2 - C1 C3 C3 - C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - C12 C8 S2 C8 - C7 C9 C9 - C10 C8 C10 - C11 C9 C11 - C10 C12 C12 - C7 C11 C13 - O1 C14 C14 - C15 C13 C15 - N4 C14 C16 - O2 C17 C17 - C16 C18 C18 - N5 C17 N1 - P1 P2 N2 - P3 P2 N3 - P1 P3 N4 - C15 P2 N5 - C18 P3 O1 - C13 P2 O2 - C16 P3 P1 - N3 N1 S1 S2 P2 - O1 N2 N1 N4 P3 - N2 O2 N3 N5 S1 - C1 P1 S2 - C7 P1 Floating origin restraints generated 19890 Reflections read, of which 42 rejected -14 =< h =< 14, -14 =< k =< 14, -19 =< l =< 21, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 6 8 1 39.47 1.11 4 5.84 1 Inconsistent equivalents 4720 Unique reflections, of which 0 suppressed R(int) = 0.0337 R(sigma) = 0.0333 Friedel opposites not merged Maximum memory for data reduction = 2583 / 50436 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 = 3366 / 349795 wR2 = 0.0584 before cycle 1 for 4720 data and 279 / 279 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0076 * P )^2 + 1.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68795 0.00059 0.084 OSF Mean shift/esd = 0.024 Maximum = -0.104 for U11 O1 Max. shift = 0.002 A for H4N Max. dU = 0.000 for H4N Least-squares cycle 2 Maximum vector length = 511 Memory required = 3366 / 349795 wR2 = 0.0584 before cycle 2 for 4720 data and 279 / 279 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0076 * P )^2 + 1.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68794 0.00059 -0.019 OSF Mean shift/esd = 0.008 Maximum = -0.034 for U11 O1 Max. shift = 0.000 A for H4N Max. dU = 0.000 for H5N Least-squares cycle 3 Maximum vector length = 511 Memory required = 3366 / 349795 wR2 = 0.0583 before cycle 3 for 4720 data and 279 / 279 parameters GooF = S = 1.046; Restrained GooF = 1.045 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0076 * P )^2 + 1.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68794 0.00059 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.003 for U11 H4N Max. shift = 0.000 A for H5N Max. dU = 0.000 for H4N Least-squares cycle 4 Maximum vector length = 511 Memory required = 3366 / 349795 wR2 = 0.0583 before cycle 4 for 4720 data and 279 / 279 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0076 * P )^2 + 1.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68794 0.00059 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z H5N Max. shift = 0.000 A for H5N Max. dU = 0.000 for H4N 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 H2 0.2985 0.1933 0.4181 43 0.950 0.000 C2 C1 C3 H3 0.1865 0.0294 0.3866 43 0.950 0.000 C3 C4 C2 H4 -0.0146 0.0317 0.4063 43 0.950 0.000 C4 C5 C3 H5 -0.1037 0.1944 0.4616 43 0.950 0.000 C5 C4 C6 H6 0.0067 0.3581 0.4950 43 0.950 0.000 C6 C5 C1 H8 0.0972 0.7520 0.3339 43 0.950 0.000 C8 C7 C9 H9 -0.0798 0.8187 0.3859 43 0.950 0.000 C9 C10 C8 H10 -0.1111 0.8171 0.5230 43 0.950 0.000 C10 C11 C9 H11 0.0315 0.7477 0.6094 43 0.950 0.000 C11 C10 C12 H12 0.2086 0.6806 0.5577 43 0.950 0.000 C12 C7 C11 H13A 0.5320 0.1327 0.2631 23 0.990 0.000 C13 O1 C14 H13B 0.5412 0.2538 0.3101 23 0.990 0.000 C13 O1 C14 H14A 0.6672 0.2606 0.1996 23 0.990 0.000 C14 C15 C13 H14B 0.5629 0.2272 0.1405 23 0.990 0.000 C14 C15 C13 H15A 0.5789 0.4418 0.2272 23 0.990 0.000 C15 N4 C14 H15B 0.5976 0.4290 0.1328 23 0.990 0.000 C15 N4 C14 H16A -0.0905 0.6051 0.1656 23 0.990 0.000 C16 O2 C17 H16B -0.0470 0.6031 0.2564 23 0.990 0.000 C16 O2 C17 H17A -0.1709 0.4188 0.1788 23 0.990 0.000 C17 C16 C18 H17B -0.2232 0.5007 0.2472 23 0.990 0.000 C17 C16 C18 H18A -0.0943 0.4182 0.3419 23 0.990 0.000 C18 N5 C17 H18B -0.1696 0.3168 0.3010 23 0.990 0.000 C18 N5 C17 2007src0258r in P4(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq H5N 0.01957 0.27222 0.29281 1.00000 0.01631 0.04085 0.00207 0.00216 0.00146 0.00000 0.00629 H4N 0.40811 0.46900 0.15078 1.00000 0.03540 0.04809 0.00247 0.00247 0.00171 0.00000 0.00843 C1 0.16286 0.29107 0.45878 1.00000 0.02934 0.02062 0.01647 0.00521 -0.00001 0.00030 0.02214 0.00381 0.00020 0.00019 0.00013 0.00000 0.00116 0.00110 0.00103 0.00085 0.00089 0.00091 0.00046 C2 0.21686 0.19373 0.42690 1.00000 0.02528 0.02758 0.02875 0.00462 0.00207 0.00469 0.02720 0.00431 0.00021 0.00021 0.00014 0.00000 0.00119 0.00126 0.00126 0.00099 0.00096 0.00099 0.00052 H2 0.29854 0.19334 0.41808 1.00000 0.03264 0.00000 0.00000 C3 0.15013 0.09675 0.40800 1.00000 0.05022 0.02379 0.03022 0.00141 0.00136 0.00733 0.03474 0.00474 0.00024 0.00022 0.00015 0.00000 0.00162 0.00121 0.00132 0.00105 0.00121 0.00115 0.00058 H3 0.18647 0.02938 0.38656 1.00000 0.04169 0.00000 0.00000 C4 0.03076 0.09772 0.42024 1.00000 0.04421 0.02491 0.03446 0.00603 -0.00388 -0.00886 0.03453 0.00462 0.00024 0.00022 0.00016 0.00000 0.00153 0.00127 0.00141 0.00106 0.00118 0.00117 0.00058 H4 -0.01461 0.03167 0.40626 1.00000 0.04143 0.00000 0.00000 C5 -0.02209 0.19441 0.45268 1.00000 0.02915 0.03417 0.03610 0.01254 0.00271 -0.00200 0.03314 0.00469 0.00022 0.00023 0.00016 0.00000 0.00129 0.00144 0.00140 0.00113 0.00110 0.00110 0.00057 H5 -0.10375 0.19441 0.46158 1.00000 0.03977 0.00000 0.00000 C6 0.04318 0.29159 0.47237 1.00000 0.03056 0.02548 0.02515 0.00649 0.00312 0.00462 0.02706 0.00423 0.00020 0.00021 0.00014 0.00000 0.00125 0.00117 0.00118 0.00096 0.00099 0.00096 0.00050 H6 0.00667 0.35806 0.49496 1.00000 0.03247 0.00000 0.00000 C7 0.16886 0.70950 0.44114 1.00000 0.01841 0.01634 0.02131 -0.00324 0.00086 -0.00456 0.01869 0.00356 0.00018 0.00019 0.00013 0.00000 0.00102 0.00103 0.00104 0.00083 0.00083 0.00083 0.00043 C8 0.08383 0.75087 0.38980 1.00000 0.03060 0.02135 0.02882 -0.00223 -0.00549 -0.00182 0.02692 0.00391 0.00021 0.00019 0.00015 0.00000 0.00125 0.00112 0.00127 0.00095 0.00098 0.00095 0.00051 H8 0.09716 0.75196 0.33388 1.00000 0.03231 0.00000 0.00000 C9 -0.02086 0.79066 0.42068 1.00000 0.02735 0.02606 0.05561 -0.00834 -0.01299 0.00438 0.03634 0.00442 0.00022 0.00022 0.00018 0.00000 0.00129 0.00128 0.00179 0.00121 0.00120 0.00103 0.00063 H9 -0.07979 0.81872 0.38589 1.00000 0.04361 0.00000 0.00000 C10 -0.03934 0.78944 0.50215 1.00000 0.02382 0.02725 0.06435 -0.01926 0.01028 -0.00396 0.03847 0.00445 0.00022 0.00022 0.00019 0.00000 0.00122 0.00129 0.00192 0.00129 0.00127 0.00099 0.00066 H10 -0.11105 0.81713 0.52303 1.00000 0.04617 0.00000 0.00000 C11 0.04502 0.74853 0.55347 1.00000 0.03870 0.02819 0.03199 -0.00650 0.01274 -0.00615 0.03296 0.00440 0.00023 0.00021 0.00016 0.00000 0.00147 0.00129 0.00134 0.00107 0.00114 0.00112 0.00057 H11 0.03151 0.74770 0.60937 1.00000 0.03955 0.00000 0.00000 C12 0.14988 0.70856 0.52276 1.00000 0.03194 0.02438 0.02395 -0.00207 0.00318 -0.00275 0.02676 0.00408 0.00022 0.00020 0.00014 0.00000 0.00129 0.00119 0.00116 0.00092 0.00097 0.00099 0.00051 H12 0.20863 0.68056 0.55771 1.00000 0.03211 0.00000 0.00000 C13 0.51543 0.21711 0.25969 1.00000 0.01949 0.02074 0.02549 0.00155 -0.00431 0.00671 0.02191 0.00388 0.00018 0.00019 0.00013 0.00000 0.00105 0.00106 0.00114 0.00090 0.00087 0.00086 0.00046 H13A 0.53205 0.13271 0.26307 1.00000 0.02629 0.00000 0.00000 H13B 0.54120 0.25378 0.31013 1.00000 0.02629 0.00000 0.00000 C14 0.58267 0.26972 0.18999 1.00000 0.01572 0.02184 0.02699 -0.00166 -0.00115 0.00367 0.02152 0.00382 0.00018 0.00019 0.00014 0.00000 0.00103 0.00106 0.00116 0.00090 0.00087 0.00089 0.00046 H14A 0.66721 0.26057 0.19955 1.00000 0.02582 0.00000 0.00000 H14B 0.56291 0.22716 0.14045 1.00000 0.02582 0.00000 0.00000 C15 0.55461 0.39778 0.17925 1.00000 0.01815 0.02503 0.02679 0.00175 -0.00123 -0.00068 0.02332 0.00394 0.00019 0.00020 0.00014 0.00000 0.00108 0.00114 0.00118 0.00092 0.00089 0.00092 0.00047 H15A 0.57890 0.44178 0.22721 1.00000 0.02799 0.00000 0.00000 H15B 0.59763 0.42903 0.13278 1.00000 0.02799 0.00000 0.00000 C16 -0.06099 0.55420 0.20871 1.00000 0.01727 0.02583 0.02859 0.00423 -0.00655 0.00509 0.02390 0.00392 0.00018 0.00020 0.00014 0.00000 0.00106 0.00114 0.00119 0.00096 0.00091 0.00090 0.00048 H16A -0.09048 0.60510 0.16556 1.00000 0.02868 0.00000 0.00000 H16B -0.04701 0.60309 0.25639 1.00000 0.02868 0.00000 0.00000 C17 -0.15133 0.46210 0.22806 1.00000 0.01487 0.02932 0.02909 -0.00070 -0.00523 0.00386 0.02443 0.00382 0.00018 0.00020 0.00014 0.00000 0.00098 0.00119 0.00121 0.00100 0.00093 0.00088 0.00048 H17A -0.17086 0.41876 0.17881 1.00000 0.02931 0.00000 0.00000 H17B -0.22316 0.50066 0.24721 1.00000 0.02931 0.00000 0.00000 C18 -0.10928 0.37664 0.29122 1.00000 0.01555 0.02461 0.02982 -0.00053 0.00124 -0.00218 0.02333 0.00396 0.00018 0.00020 0.00014 0.00000 0.00103 0.00115 0.00124 0.00098 0.00090 0.00088 0.00047 H18A -0.09428 0.41820 0.34192 1.00000 0.02799 0.00000 0.00000 H18B -0.16959 0.31678 0.30101 1.00000 0.02799 0.00000 0.00000 N1 0.36039 0.43443 0.32002 1.00000 0.01633 0.02225 0.02260 -0.00309 -0.00506 0.00105 0.02039 0.00308 0.00015 0.00016 0.00011 0.00000 0.00086 0.00091 0.00095 0.00073 0.00074 0.00071 0.00039 N2 0.21315 0.35359 0.20555 1.00000 0.01711 0.02307 0.01889 -0.00242 -0.00219 0.00003 0.01969 0.00299 0.00015 0.00016 0.00011 0.00000 0.00089 0.00092 0.00089 0.00073 0.00071 0.00073 0.00038 N3 0.13087 0.48886 0.32625 1.00000 0.01677 0.01926 0.02017 -0.00255 -0.00198 0.00061 0.01873 0.00297 0.00015 0.00015 0.00010 0.00000 0.00085 0.00088 0.00091 0.00072 0.00072 0.00070 0.00037 N4 0.42823 0.41165 0.16659 1.00000 0.01832 0.01809 0.02313 0.00423 -0.00282 0.00218 0.01985 0.00315 0.00016 0.00017 0.00011 0.00000 0.00092 0.00095 0.00098 0.00078 0.00075 0.00076 0.00039 N5 -0.00030 0.32047 0.26240 1.00000 0.01659 0.01721 0.02257 0.00127 -0.00220 -0.00156 0.01879 0.00304 0.00015 0.00016 0.00011 0.00000 0.00091 0.00090 0.00096 0.00079 0.00074 0.00071 0.00038 O1 0.39044 0.23500 0.24949 1.00000 0.01808 0.01760 0.02219 0.00223 -0.00038 0.00016 0.01929 0.00245 0.00012 0.00012 0.00009 0.00000 0.00072 0.00072 0.00078 0.00062 0.00061 0.00058 0.00031 O2 0.04752 0.50053 0.18376 1.00000 0.01942 0.02438 0.02194 0.00398 -0.00387 0.00126 0.02191 0.00257 0.00013 0.00013 0.00009 0.00000 0.00077 0.00078 0.00077 0.00062 0.00062 0.00064 0.00033 P1 0.25431 0.48947 0.36802 1.00000 0.01687 0.01701 0.01636 -0.00077 -0.00298 -0.00050 0.01675 0.00091 0.00005 0.00005 0.00003 0.00000 0.00026 0.00026 0.00024 0.00021 0.00021 0.00021 0.00011 P2 0.34289 0.36365 0.23773 1.00000 0.01521 0.01667 0.01739 -0.00100 -0.00214 0.00087 0.01642 0.00087 0.00004 0.00005 0.00003 0.00000 0.00025 0.00025 0.00026 0.00021 0.00021 0.00020 0.00011 P3 0.10643 0.41547 0.24707 1.00000 0.01462 0.01683 0.01683 0.00026 -0.00253 -0.00029 0.01609 0.00087 0.00004 0.00004 0.00003 0.00000 0.00025 0.00026 0.00026 0.00021 0.00020 0.00020 0.00011 S1 0.24489 0.41847 0.48283 1.00000 0.03186 0.02641 0.01771 0.00311 -0.00511 -0.00200 0.02533 0.00098 0.00005 0.00005 0.00003 0.00000 0.00031 0.00029 0.00025 0.00023 0.00023 0.00024 0.00012 S2 0.30383 0.65882 0.40150 1.00000 0.01945 0.02118 0.02235 -0.00499 0.00197 -0.00400 0.02099 0.00091 0.00005 0.00005 0.00003 0.00000 0.00026 0.00026 0.00026 0.00021 0.00021 0.00021 0.00012 Final Structure Factor Calculation for 2007src0258r in P4(1) Total number of l.s. parameters = 279 Maximum vector length = 511 Memory required = 3089 / 27090 wR2 = 0.0583 before cycle 5 for 4720 data and 2 / 279 parameters GooF = S = 1.046; Restrained GooF = 1.045 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0076 * P )^2 + 1.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0279 for 4559 Fo > 4sig(Fo) and 0.0299 for all 4720 data wR2 = 0.0583, GooF = S = 1.046, Restrained GooF = 1.045 for all data Flack x parameter = 0.0442 with esd 0.0523 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 30.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0294 0.0241 0.0129 C1 0.0351 0.0252 0.0213 C2 0.0522 0.0302 0.0218 C3 0.0499 0.0335 0.0201 C4 0.0477 0.0305 0.0212 C5 0.0367 0.0257 0.0187 C6 0.0245 0.0193 0.0122 C7 0.0353 0.0260 0.0195 C8 0.0630 0.0242 0.0218 C9 0.0749 0.0215 0.0190 C10 0.0518 0.0254 0.0216 C11 0.0342 0.0241 0.0220 C12 0.0285 0.0252 0.0120 C13 0.0279 0.0226 0.0140 C14 0.0281 0.0239 0.0180 C15 0.0323 0.0280 0.0114 C16 0.0323 0.0286 0.0124 C17 0.0300 0.0250 0.0150 C18 0.0274 0.0203 0.0135 N1 0.0243 0.0194 0.0154 N2 0.0229 0.0175 0.0157 N3 0.0258 0.0203 0.0134 N4 0.0237 0.0175 0.0152 N5 0.0231 0.0181 0.0166 O1 0.0276 0.0229 0.0153 O2 0.0196 0.0172 0.0134 P1 0.0193 0.0160 0.0139 P2 0.0186 0.0167 0.0130 P3 0.0346 0.0259 0.0155 S1 0.0287 0.0187 0.0156 S2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.050 0.075 0.096 0.120 0.141 0.164 0.194 0.238 0.318 1.000 Number in group 481. 474. 461. 489. 466. 461. 474. 474. 466. 474. GooF 1.092 1.096 1.056 0.986 1.071 1.073 0.996 1.010 0.972 1.097 K 1.014 0.983 0.972 0.997 1.003 0.996 1.001 1.009 1.005 1.005 Resolution(A) 0.77 0.81 0.85 0.89 0.93 1.00 1.07 1.17 1.35 1.68 inf Number in group 492. 461. 481. 456. 471. 478. 464. 479. 464. 474. GooF 1.144 1.187 0.973 0.915 0.918 0.916 0.912 0.836 1.020 1.473 K 1.012 1.016 1.017 1.010 1.007 1.002 0.996 0.997 1.002 1.004 R1 0.080 0.055 0.043 0.037 0.031 0.026 0.023 0.016 0.017 0.020 Recommended weighting scheme: WGHT 0.0059 1.4595 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 10 0 170.16 531.79 11.70 0.161 0.81 -1 5 -4 1209.94 1003.06 4.67 0.221 1.98 3 5 2 7196.12 6483.48 4.09 0.561 1.92 1 3 3 1696.24 1946.70 4.03 0.307 3.05 4 4 0 868.93 1034.47 4.02 0.224 2.03 1 3 -3 1748.85 1996.17 3.99 0.311 3.05 1 5 -5 1555.51 1776.31 3.94 0.294 1.87 4 5 -3 176.62 116.47 3.92 0.075 1.71 3 5 -2 7052.82 6415.45 3.85 0.558 1.92 -1 5 0 235.36 319.37 3.76 0.125 2.25 2 7 0 572.01 699.15 3.70 0.184 1.58 -1 5 4 1154.31 992.08 3.61 0.220 1.98 1 1 -5 4354.33 3980.40 3.55 0.440 3.10 0 0 -8 2716.17 3067.34 3.51 0.386 2.10 3 5 -6 503.53 618.05 3.44 0.173 1.61 0 2 4 480.37 390.09 3.42 0.138 3.39 4 5 3 168.61 118.34 3.35 0.076 1.71 -7 10 -3 -1.50 22.41 3.34 0.033 0.93 6 10 10 786.57 614.26 3.31 0.173 0.85 3 8 -16 189.98 276.15 3.22 0.116 0.83 -4 9 16 61.66 140.87 3.16 0.083 0.78 1 6 0 6105.36 5586.28 3.14 0.521 1.89 0 3 -9 801.03 928.37 3.10 0.212 1.68 9 10 6 75.46 24.70 3.08 0.035 0.82 4 10 -1 540.25 649.23 3.05 0.178 1.06 0 2 -4 448.85 371.49 2.98 0.134 3.39 3 5 0 475.41 393.72 2.97 0.138 1.97 0 5 0 395.75 317.31 2.96 0.124 2.30 -6 10 4 239.90 311.04 2.94 0.123 0.96 3 3 3 2157.73 1952.95 2.94 0.308 2.44 3 8 16 208.20 286.75 2.91 0.118 0.83 8 12 5 124.53 65.37 2.90 0.056 0.78 -4 14 0 71.63 134.07 2.89 0.081 0.79 2 10 2 315.68 395.36 2.89 0.139 1.12 4 13 7 572.84 410.55 2.87 0.141 0.80 3 3 -8 4441.22 4122.04 2.85 0.447 1.66 2 3 21 17.77 50.17 2.83 0.049 0.77 2 8 0 3284.79 3026.90 2.83 0.383 1.39 1 10 15 3.29 34.23 2.80 0.041 0.80 2 4 -1 2662.92 2444.46 2.79 0.345 2.54 0 5 20 48.22 101.08 2.79 0.070 0.79 3 6 6 1307.97 1147.18 2.78 0.236 1.46 1 1 -7 1316.56 1456.92 2.78 0.266 2.30 8 8 3 427.46 344.81 2.76 0.129 1.00 -5 12 2 135.80 202.51 2.71 0.099 0.88 4 9 -2 12.34 33.35 2.70 0.040 1.16 -2 6 4 155.51 112.35 2.70 0.074 1.67 -3 12 11 347.76 197.47 2.70 0.098 0.79 1 1 7 1308.49 1444.76 2.69 0.265 2.30 -1 5 7 536.71 621.86 2.68 0.174 1.64 Bond lengths and angles C1 - Distance Angles C2 1.3862 (0.0032) C6 1.3938 (0.0032) 120.53 (0.22) S1 1.7869 (0.0022) 120.79 (0.18) 118.68 (0.18) C1 - C2 C6 C2 - Distance Angles C1 1.3862 (0.0032) C3 1.3891 (0.0036) 119.22 (0.23) C2 - C1 C3 - Distance Angles C4 1.3868 (0.0038) C2 1.3891 (0.0036) 120.37 (0.24) C3 - C4 C4 - Distance Angles C5 1.3778 (0.0037) C3 1.3868 (0.0038) 120.05 (0.24) C4 - C5 C5 - Distance Angles C4 1.3778 (0.0037) C6 1.3849 (0.0035) 120.37 (0.24) C5 - C4 C6 - Distance Angles C5 1.3849 (0.0035) C1 1.3938 (0.0032) 119.45 (0.22) C6 - C5 C7 - Distance Angles C12 1.3856 (0.0031) C8 1.3861 (0.0032) 120.33 (0.22) S2 1.7848 (0.0022) 120.13 (0.18) 119.54 (0.18) C7 - C12 C8 C8 - Distance Angles C7 1.3861 (0.0032) C9 1.3870 (0.0036) 119.50 (0.23) C8 - C7 C9 - Distance Angles C10 1.3823 (0.0042) C8 1.3870 (0.0036) 119.92 (0.25) C9 - C10 C10 - Distance Angles C11 1.3786 (0.0040) C9 1.3823 (0.0042) 120.80 (0.24) C10 - C11 C11 - Distance Angles C10 1.3786 (0.0040) C12 1.3883 (0.0034) 119.44 (0.24) C11 - C10 C12 - Distance Angles C7 1.3856 (0.0031) C11 1.3883 (0.0034) 120.01 (0.24) C12 - C7 C13 - Distance Angles O1 1.4607 (0.0024) C14 1.5257 (0.0032) 110.64 (0.17) C13 - O1 C14 - Distance Angles C15 1.5170 (0.0030) C13 1.5257 (0.0032) 111.56 (0.18) C14 - C15 C15 - Distance Angles N4 1.4760 (0.0028) C14 1.5170 (0.0030) 109.32 (0.18) C15 - N4 C16 - Distance Angles O2 1.4524 (0.0026) C17 1.5173 (0.0031) 110.65 (0.17) C16 - O2 C17 - Distance Angles C16 1.5173 (0.0031) C18 1.5227 (0.0031) 112.41 (0.17) C17 - C16 C18 - Distance Angles N5 1.4892 (0.0027) C17 1.5227 (0.0031) 108.70 (0.18) C18 - N5 N1 - Distance Angles P1 1.5914 (0.0019) P2 1.6139 (0.0019) 122.48 (0.11) N1 - P1 N2 - Distance Angles P3 1.5790 (0.0019) P2 1.5895 (0.0018) 123.08 (0.11) N2 - P3 N3 - Distance Angles P1 1.5817 (0.0018) P3 1.5975 (0.0018) 121.86 (0.11) N3 - P1 N4 - Distance Angles C15 1.4760 (0.0028) P2 1.6395 (0.0019) 116.58 (0.15) N4 - C15 N5 - Distance Angles C18 1.4892 (0.0027) P3 1.6616 (0.0018) 112.71 (0.14) N5 - C18 O1 - Distance Angles C13 1.4607 (0.0024) P2 1.5881 (0.0014) 118.93 (0.12) O1 - C13 O2 - Distance Angles C16 1.4524 (0.0026) P3 1.5935 (0.0015) 115.67 (0.13) O2 - C16 P1 - Distance Angles N3 1.5817 (0.0018) N1 1.5914 (0.0019) 117.46 (0.10) S1 2.0933 (0.0008) 111.04 (0.07) 110.47 (0.07) S2 2.1034 (0.0007) 111.39 (0.07) 107.18 (0.07) 97.41 (0.03) P1 - N3 N1 S1 P2 - Distance Angles O1 1.5881 (0.0014) N2 1.5895 (0.0018) 107.28 (0.09) N1 1.6139 (0.0019) 108.66 (0.09) 116.33 (0.09) N4 1.6395 (0.0019) 101.40 (0.09) 109.78 (0.10) 112.20 (0.10) P2 - O1 N2 N1 P3 - Distance Angles N2 1.5790 (0.0019) O2 1.5935 (0.0015) 108.20 (0.09) N3 1.5975 (0.0018) 117.87 (0.09) 107.72 (0.09) N5 1.6616 (0.0018) 110.21 (0.10) 101.09 (0.09) 110.36 (0.09) P3 - N2 O2 N3 S1 - Distance Angles C1 1.7869 (0.0022) P1 2.0933 (0.0008) 97.99 (0.07) S1 - C1 S2 - Distance Angles C7 1.7848 (0.0022) P1 2.1034 (0.0007) 99.57 (0.07) S2 - C7 FMAP and GRID set by program FMAP 2 3 21 GRID -1.389 -2 -2 1.389 2 2 R1 = 0.0288 for 2609 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.21 at 0.1843 0.4003 0.2110 [ 0.64 A from N2 ] Deepest hole -0.23 at 0.4150 0.3606 0.2366 [ 0.83 A from P2 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2922 / 20559 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1843 0.4003 0.2110 1.00000 0.05 0.21 0.64 N2 1.09 P3 1.92 P2 2.00 O2 Q2 1 0.0403 0.3565 0.2567 1.00000 0.05 0.21 0.63 N5 1.03 P3 1.17 H5N 1.83 C18 Q3 1 0.1985 0.2199 0.4707 1.00000 0.05 0.19 0.82 C2 0.94 C1 1.48 H2 1.85 C3 Q4 1 0.2608 0.3559 0.2203 1.00000 0.05 0.19 0.60 N2 0.99 P2 1.95 P3 2.09 O1 Q5 1 -0.0859 0.9062 0.4036 1.00000 0.05 0.19 1.05 H9 1.55 C9 1.66 H4 2.17 H11 Q6 1 0.2345 0.3644 0.1615 1.00000 0.05 0.18 0.79 N2 1.78 P2 2.03 H13B 2.14 P3 Q7 1 0.5437 0.4487 0.1358 1.00000 0.05 0.18 0.66 H15B 0.94 C15 1.49 N4 1.59 H15A Q8 1 0.2537 0.4452 0.4234 1.00000 0.05 0.17 1.05 S1 1.06 P1 2.13 N1 2.14 C1 Q9 1 0.4610 0.3790 0.2099 1.00000 0.05 0.17 0.90 N4 1.21 C15 1.45 P2 1.56 H4N Q10 1 0.6631 0.2479 0.2468 1.00000 0.05 0.17 0.81 H14A 1.35 C14 1.75 C13 1.76 H13B Q11 1 0.0596 0.2425 0.2925 1.00000 0.05 0.17 0.57 H5N 1.24 N5 2.20 P3 2.48 C18 Q12 1 0.3992 0.5235 0.3556 1.00000 0.05 0.16 1.27 N1 1.72 P1 2.05 S2 2.15 H4N Q13 1 0.4447 0.2415 0.2482 1.00000 0.05 0.16 0.63 O1 0.88 C13 1.53 H13B 1.62 H13A Q14 1 0.0707 0.4754 0.2231 1.00000 0.05 0.16 0.77 O2 0.90 P3 1.78 C16 1.87 N3 Q15 1 0.3757 0.3823 0.1847 1.00000 0.05 0.16 0.75 N4 0.99 P2 1.21 H4N 1.93 N2 Q16 1 0.3812 0.4024 0.3486 1.00000 0.05 0.16 0.65 N1 1.80 P1 1.93 H4N 1.96 P2 Q17 1 -0.0428 0.3444 0.2631 1.00000 0.05 0.16 0.56 N5 0.97 C18 1.20 H5N 1.62 H18B Q18 1 0.3018 0.4255 0.3354 1.00000 0.05 0.16 0.73 N1 1.07 P1 1.85 P2 2.10 N3 Q19 1 0.0234 0.2204 0.4787 1.00000 0.05 0.16 0.74 C5 0.86 C6 1.52 H5 1.62 H6 Q20 1 -0.1987 0.0849 0.4619 1.00000 0.05 0.16 1.67 H5 1.77 H5N 1.91 N5 2.26 H11 Shortest distances between peaks (including symmetry equivalents) 2 17 0.97 16 18 0.97 1 4 1.03 4 6 1.04 9 15 1.07 1 6 1.09 12 16 1.41 2 11 1.46 11 20 1.47 4 15 1.48 2 14 1.52 1 14 1.58 8 18 1.59 12 18 1.62 6 15 1.68 9 13 1.72 11 17 1.73 7 9 1.76 7 12 1.83 1 2 1.89 8 16 1.99 3 19 2.02 2 20 2.03 13 15 2.09 14 17 2.10 4 18 2.14 8 12 2.21 7 15 2.23 1 15 2.25 4 9 2.32 17 20 2.39 6 14 2.50 1 18 2.50 10 13 2.51 9 16 2.51 4 13 2.53 4 14 2.58 1 20 2.58 13 16 2.60 2 4 2.60 4 16 2.61 7 16 2.62 5 20 2.62 1 11 2.68 6 20 2.70 15 18 2.71 4 20 2.71 6 9 2.73 2 6 2.74 15 16 2.76 3 8 2.78 6 10 2.78 1 17 2.82 9 10 2.83 9 18 2.84 4 11 2.92 11 14 2.92 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: Generate connectivity array 0.01: 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. 4.63: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.93: Structure factors and derivatives 3.89: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.07: Apply other restraints 0.71: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.17: Analysis of variance 0.08: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0258r finished at 18:12:01 Total CPU time: 13.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++