+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 12:02:39 on 12-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src0078 in P-1 CELL 0.71073 8.6774 9.0176 10.0740 107.625 96.197 102.871 ZERR 2.00 0.0003 0.0003 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H B N F UNIT 26 38 2 4 8 V = 719.23 F(000) = 304.0 Mu = 0.11 mm-1 Cell Wt = 580.22 Rho = 1.340 MERG 2 OMIT -3.00 55.00 OMIT 0 -6 3 OMIT 0 -6 6 OMIT 9 -3 3 OMIT 0 -3 6 OMIT 3 -6 3 EXTI 0.08540 FMAP 2 PLAN 10 SIZE 0.10 0.40 0.50 ACTA BOND $H WGHT 0.04480 0.36840 L.S. 10 TEMP -153.00 FVAR 1.97912 MOLE 1 B1 3 0.274006 0.513059 0.806958 11.00000 0.02955 0.03100 = 0.03195 0.01341 0.00574 0.00547 F1 5 0.179127 0.438979 0.674480 11.00000 0.05513 0.07365 = 0.04212 0.01067 -0.01161 -0.00245 F2 5 0.357991 0.668867 0.821697 11.00000 0.04497 0.03390 = 0.05786 0.02329 0.01321 0.00442 F3 5 0.179274 0.517717 0.910038 11.00000 0.04656 0.03644 = 0.05416 0.02059 0.02575 0.01481 F4 5 0.385246 0.426593 0.825982 11.00000 0.04776 0.04473 = 0.05123 0.02760 0.02290 0.02253 MOLE 2 C1 1 0.207681 0.050571 0.079062 11.00000 0.02122 0.02313 = 0.02453 0.00643 -0.00216 0.00446 C2 1 0.165631 -0.111801 0.066194 11.00000 0.02673 0.02374 = 0.03542 0.00679 -0.00429 0.00606 AFIX 43 H2 2 0.194950 -0.190978 -0.005317 11.00000 -1.20000 AFIX 0 C3 1 0.078595 -0.151392 0.163595 11.00000 0.02769 0.02913 = 0.04866 0.01965 -0.00291 0.00210 AFIX 43 H3 2 0.046315 -0.261180 0.158264 11.00000 -1.20000 AFIX 0 C4 1 0.036690 -0.034740 0.269648 11.00000 0.02733 0.04425 = 0.04260 0.02619 0.00574 0.00688 AFIX 43 H4 2 -0.021934 -0.067441 0.335019 11.00000 -1.20000 AFIX 0 C5 1 0.077997 0.126889 0.282301 11.00000 0.02543 0.03817 = 0.03039 0.01378 0.00454 0.00955 AFIX 43 H5 2 0.049266 0.206109 0.354236 11.00000 -1.20000 AFIX 0 C6 1 0.163973 0.166464 0.183587 11.00000 0.02082 0.02464 = 0.02373 0.00759 -0.00075 0.00515 C7 1 0.296021 0.287340 0.054071 11.00000 0.02634 0.02341 = 0.02392 0.00646 0.00041 0.00392 AFIX 43 H7 2 0.346392 0.368854 0.019092 11.00000 -1.20000 AFIX 0 C8 1 0.362989 0.063067 -0.120193 11.00000 0.03640 0.03810 = 0.02551 0.00612 0.00720 0.01482 AFIX 137 H8A 2 0.356297 0.121857 -0.187101 11.00000 -1.50000 H8B 2 0.304684 -0.050979 -0.167646 11.00000 -1.50000 H8C 2 0.476107 0.071900 -0.086858 11.00000 -1.50000 AFIX 0 C9 1 0.207972 0.472828 0.247512 11.00000 0.03136 0.02237 = 0.02638 0.00192 -0.00057 0.01005 AFIX 23 H9A 2 0.101618 0.461167 0.276325 11.00000 -1.20000 H9B 2 0.215510 0.543563 0.188743 11.00000 -1.20000 AFIX 0 C10 1 0.340307 0.551189 0.379360 11.00000 0.02510 0.02247 = 0.02252 0.00531 0.00204 0.00633 AFIX 23 H10A 2 0.443186 0.532267 0.354322 11.00000 -1.20000 H10B 2 0.313618 0.500184 0.451247 11.00000 -1.20000 AFIX 0 C11 1 0.360662 0.732924 0.442502 11.00000 0.03243 0.02113 = 0.02145 0.00549 0.00257 0.00543 AFIX 13 H11 2 0.372577 0.780098 0.365011 11.00000 -1.20000 AFIX 0 C12 1 0.514023 0.811175 0.555961 11.00000 0.03425 0.02678 = 0.03449 0.00379 -0.00318 0.00217 AFIX 137 H12A 2 0.526875 0.927690 0.595921 11.00000 -1.50000 H12B 2 0.607177 0.792186 0.513207 11.00000 -1.50000 H12C 2 0.506263 0.763780 0.631440 11.00000 -1.50000 AFIX 0 C13 1 0.215547 0.769848 0.504030 11.00000 0.03977 0.03295 = 0.02639 0.00283 0.00271 0.01656 AFIX 137 H13A 2 0.203620 0.727232 0.582131 11.00000 -1.50000 H13B 2 0.118474 0.719073 0.430071 11.00000 -1.50000 H13C 2 0.230999 0.887044 0.539552 11.00000 -1.50000 AFIX 0 N1 4 0.291483 0.132050 0.000212 11.00000 0.02636 0.02355 = 0.02122 0.00377 0.00119 0.00585 N2 4 0.220979 0.312933 0.162841 11.00000 0.02607 0.02081 = 0.02210 0.00395 0.00072 0.00552 HKLF 4 Covalent radii and connectivity table for 04src0078 in P-1 C 0.770 H 0.320 B 0.820 N 0.700 F 0.640 B1 - F1 F2 F3 F4 F1 - B1 F2 - B1 F3 - B1 F4 - B1 C1 - C2 N1 C6 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C5 N2 C1 C7 - N2 N1 C8 - N1 C9 - N2 C10 C10 - C9 C11 C11 - C13 C10 C12 C12 - C11 C13 - C11 N1 - C7 C1 C8 N2 - C7 C6 C9 14188 Reflections read, of which 118 rejected -11 =< h =< 11, -11 =< k =< 11, -13 =< l =< 13, Max. 2-theta = 54.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 10 0 0 21.90 2.17 2 12.72 -9 1 0 125.09 0.98 5 29.99 -8 1 0 38.81 0.84 6 7.10 -5 1 0 162.09 0.99 7 22.91 -3 1 0 204.55 2.46 7 22.76 -1 1 0 2792.02 32.90 5 451.16 -5 2 0 446.26 6.53 6 45.35 -3 2 0 71.68 1.17 6 6.60 -2 2 0 4665.77 59.54 5 699.64 -4 3 0 405.39 6.23 6 33.81 -3 3 0 6155.82 52.95 5 1028.67 6 -8 1 41.24 0.68 6 6.63 2 -5 1 16.77 0.58 6 3.69 3 -2 1 7597.33 151.31 3 876.43 1 -1 1 277.99 3.61 7 29.28 8 -1 1 515.79 3.54 7 63.07 -1 0 1 1056.08 12.73 8 144.25 1 0 1 127.29 2.11 7 10.66 -2 1 1 53.49 1.08 6 6.21 -5 2 1 1106.19 14.85 6 165.20 -4 2 1 485.87 8.17 6 43.17 -3 2 1 1580.86 24.09 6 139.43 -2 2 1 619.21 11.16 5 57.71 -1 2 1 1813.02 30.41 5 161.89 -3 3 1 44.53 1.21 5 6.14 -6 6 1 396.86 5.35 6 43.48 3 -3 2 709.83 2.26 8 122.26 -2 -1 2 6380.73 111.37 4 585.49 0 -1 2 6720.72 127.77 3 932.16 1 -1 2 10381.62 207.00 3 1479.21 -2 0 2 7819.67 99.69 7 527.37 -1 0 2 5006.09 64.58 8 332.00 0 0 2 545.06 8.74 6 60.22 -3 1 2 705.85 10.64 7 59.94 -2 1 2 2833.47 41.19 6 258.79 -1 1 2 70.23 1.40 6 7.85 0 1 2 622.23 10.36 6 56.00 -8 2 2 117.19 1.74 6 18.35 -7 2 2 269.94 1.13 6 51.06 -4 2 2 1013.63 14.43 7 103.82 -2 2 2 110.45 2.64 5 15.61 -6 3 2 463.43 2.27 6 74.11 -5 3 2 849.13 12.75 7 69.44 -4 3 2 2178.48 35.14 5 220.15 -3 3 2 999.29 16.16 6 105.01 -4 4 2 1156.97 18.22 6 101.26 -3 5 2 133.91 2.62 6 13.27 4 -5 3 136.77 1.01 8 14.94 4 -4 3 475.94 5.16 7 44.80 4 -3 3 476.79 1.14 7 88.91 ** etc. ** 128 Inconsistent equivalents 3278 Unique reflections, of which 0 suppressed R(int) = 0.1318 R(sigma) = 0.0641 Friedel opposites merged Maximum memory for data reduction = 2020 / 33296 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 = 2544 / 230662 wR2 = 0.1340 before cycle 1 for 3278 data and 185 / 185 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.97731 0.00619 -0.293 OSF 2 0.08411 0.01016 -0.127 EXTI Mean shift/su = 0.100 Maximum = -0.399 for y N1 Max. shift = 0.002 A for H8C Max. dU = 0.000 for C12 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2544 / 230662 wR2 = 0.1338 before cycle 2 for 3278 data and 185 / 185 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.97705 0.00618 -0.042 OSF 2 0.08376 0.01008 -0.034 EXTI Mean shift/su = 0.037 Maximum = 0.175 for tors H8A Max. shift = 0.002 A for H8C Max. dU = 0.000 for C12 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2544 / 230662 wR2 = 0.1338 before cycle 3 for 3278 data and 185 / 185 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.97704 0.00618 -0.001 OSF 2 0.08377 0.01006 0.001 EXTI Mean shift/su = 0.004 Maximum = 0.108 for tors H8A Max. shift = 0.001 A for H8C Max. dU = 0.000 for C13 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2544 / 230662 wR2 = 0.1338 before cycle 4 for 3278 data and 185 / 185 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.97704 0.00618 -0.001 OSF 2 0.08376 0.01006 0.000 EXTI Mean shift/su = 0.001 Maximum = 0.067 for tors H8A Max. shift = 0.001 A for H8C Max. dU = 0.000 for C12 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2544 / 230662 wR2 = 0.1338 before cycle 5 for 3278 data and 185 / 185 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.97703 0.00617 -0.001 OSF 2 0.08376 0.01006 -0.001 EXTI Mean shift/su = 0.001 Maximum = 0.042 for tors H8A Max. shift = 0.001 A for H8C Max. dU = 0.000 for C11 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2544 / 230662 wR2 = 0.1338 before cycle 6 for 3278 data and 185 / 185 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.97703 0.00617 0.000 OSF 2 0.08376 0.01006 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.026 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for C11 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2544 / 230662 wR2 = 0.1338 before cycle 7 for 3278 data and 185 / 185 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.97703 0.00617 0.000 OSF 2 0.08375 0.01006 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.016 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for C11 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2544 / 230662 wR2 = 0.1338 before cycle 8 for 3278 data and 185 / 185 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.97702 0.00618 -0.001 OSF 2 0.08375 0.01006 -0.001 EXTI Mean shift/su = 0.000 Maximum = 0.010 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for C11 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2544 / 230662 wR2 = 0.1338 before cycle 9 for 3278 data and 185 / 185 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.97702 0.00617 0.000 OSF 2 0.08375 0.01006 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.006 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for C2 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2544 / 230662 wR2 = 0.1338 before cycle 10 for 3278 data and 185 / 185 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.97702 0.00618 0.000 OSF 2 0.08375 0.01006 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.004 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for C11 Largest correlation matrix elements 0.553 EXTI / OSF 0.542 U23 C4 / U22 C4 0.506 U23 C3 / U33 C3 0.553 U23 F4 / U33 F4 0.536 U23 F4 / U22 F4 0.548 U23 C4 / U33 C4 0.510 U23 F2 / U33 F2 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.1950 -0.1910 -0.0052 43 0.950 0.000 C2 C3 C1 H3 0.0463 -0.2611 0.1582 43 0.950 0.000 C3 C2 C4 H4 -0.0219 -0.0674 0.3350 43 0.950 0.000 C4 C5 C3 H5 0.0492 0.2061 0.3541 43 0.950 0.000 C5 C4 C6 H7 0.3464 0.3688 0.0191 43 0.950 0.000 C7 N2 N1 H8A 0.3572 0.1225 -0.1867 137 0.980 0.000 C8 N1 H8A H8B 0.3041 -0.0507 -0.1682 137 0.980 0.000 C8 N1 H8A H8C 0.4759 0.0710 -0.0868 137 0.980 0.000 C8 N1 H8A H9A 0.1016 0.4613 0.2762 23 0.990 0.000 C9 N2 C10 H9B 0.2156 0.5436 0.1887 23 0.990 0.000 C9 N2 C10 H10A 0.4432 0.5323 0.3543 23 0.990 0.000 C10 C9 C11 H10B 0.3136 0.5002 0.4512 23 0.990 0.000 C10 C9 C11 H11 0.3726 0.7801 0.3650 13 1.000 0.000 C11 C13 C10 C12 H12A 0.5269 0.9276 0.5961 137 0.980 0.000 C12 C11 H12A H12B 0.6072 0.7922 0.5132 137 0.980 0.000 C12 C11 H12A H12C 0.5064 0.7636 0.6314 137 0.980 0.000 C12 C11 H12A H13A 0.2037 0.7273 0.5822 137 0.980 0.000 C13 C11 H13A H13B 0.1184 0.7190 0.4301 137 0.980 0.000 C13 C11 H13A H13C 0.2309 0.8870 0.5395 137 0.980 0.000 C13 C11 H13A 04src0078 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq B1 0.27400 0.51302 0.80689 1.00000 0.02963 0.03091 0.03192 0.01335 0.00577 0.00542 0.03064 0.00413 0.00021 0.00022 0.00020 0.00000 0.00085 0.00087 0.00088 0.00071 0.00068 0.00067 0.00038 F1 0.17909 0.43893 0.67454 1.00000 0.05517 0.07351 0.04208 0.01071 -0.01158 -0.00257 0.06402 0.00271 0.00016 0.00018 0.00014 0.00000 0.00074 0.00091 0.00069 0.00062 0.00056 0.00063 0.00040 F2 0.35800 0.66887 0.82170 1.00000 0.04502 0.03371 0.05782 0.02331 0.01324 0.00447 0.04442 0.00255 0.00013 0.00012 0.00013 0.00000 0.00060 0.00055 0.00070 0.00050 0.00050 0.00044 0.00030 F3 0.17931 0.51770 0.91009 1.00000 0.04662 0.03644 0.05400 0.02070 0.02577 0.01481 0.04249 0.00261 0.00013 0.00012 0.00012 0.00000 0.00060 0.00055 0.00067 0.00048 0.00051 0.00044 0.00029 F4 0.38526 0.42657 0.82603 1.00000 0.04775 0.04490 0.05119 0.02764 0.02299 0.02253 0.04247 0.00272 0.00013 0.00013 0.00012 0.00000 0.00061 0.00060 0.00065 0.00051 0.00050 0.00048 0.00029 C1 0.20769 0.05058 0.07907 1.00000 0.02097 0.02327 0.02451 0.00636 -0.00226 0.00453 0.02409 0.00309 0.00016 0.00017 0.00015 0.00000 0.00063 0.00067 0.00068 0.00053 0.00051 0.00051 0.00031 C2 0.16563 -0.11182 0.06627 1.00000 0.02642 0.02388 0.03545 0.00664 -0.00444 0.00610 0.03031 0.00336 0.00018 0.00018 0.00018 0.00000 0.00072 0.00070 0.00082 0.00061 0.00060 0.00056 0.00035 H2 0.19499 -0.19102 -0.00519 1.00000 0.03638 0.00000 0.00000 C3 0.07861 -0.15134 0.16356 1.00000 0.02759 0.02893 0.04890 0.01951 -0.00300 0.00213 0.03539 0.00376 0.00019 0.00020 0.00020 0.00000 0.00077 0.00077 0.00101 0.00073 0.00068 0.00061 0.00039 H3 0.04628 -0.26114 0.15819 1.00000 0.04246 0.00000 0.00000 C4 0.03669 -0.03473 0.26966 1.00000 0.02723 0.04449 0.04242 0.02605 0.00568 0.00682 0.03593 0.00409 0.00019 0.00022 0.00020 0.00000 0.00077 0.00095 0.00093 0.00078 0.00066 0.00066 0.00039 H4 -0.02190 -0.06743 0.33505 1.00000 0.04311 0.00000 0.00000 C5 0.07800 0.12686 0.28224 1.00000 0.02523 0.03834 0.03034 0.01361 0.00444 0.00964 0.03071 0.00366 0.00018 0.00020 0.00017 0.00000 0.00071 0.00084 0.00078 0.00065 0.00059 0.00061 0.00035 H5 0.04922 0.20609 0.35414 1.00000 0.03685 0.00000 0.00000 C6 0.16398 0.16643 0.18363 1.00000 0.02081 0.02459 0.02376 0.00741 -0.00080 0.00504 0.02381 0.00309 0.00016 0.00017 0.00015 0.00000 0.00064 0.00067 0.00067 0.00054 0.00051 0.00051 0.00031 C7 0.29605 0.28732 0.05407 1.00000 0.02618 0.02318 0.02404 0.00653 0.00035 0.00390 0.02562 0.00318 0.00017 0.00017 0.00016 0.00000 0.00070 0.00067 0.00068 0.00054 0.00054 0.00053 0.00032 H7 0.34642 0.36882 0.01908 1.00000 0.03074 0.00000 0.00000 C8 0.36300 0.06304 -0.12020 1.00000 0.03635 0.03811 0.02542 0.00616 0.00720 0.01488 0.03343 0.00384 0.00021 0.00021 0.00017 0.00000 0.00083 0.00086 0.00075 0.00064 0.00062 0.00067 0.00037 H8A 0.35718 0.12250 -0.18666 1.00000 0.05015 0.00000 0.00000 H8B 0.30410 -0.05074 -0.16820 1.00000 0.05015 0.00000 0.00000 H8C 0.47585 0.07099 -0.08678 1.00000 0.05015 0.00000 0.00000 C9 0.20796 0.47289 0.24746 1.00000 0.03130 0.02230 0.02628 0.00206 -0.00053 0.01012 0.02806 0.00327 0.00019 0.00017 0.00016 0.00000 0.00075 0.00068 0.00072 0.00056 0.00058 0.00056 0.00033 H9A 0.10159 0.46127 0.27624 1.00000 0.03367 0.00000 0.00000 H9B 0.21556 0.54359 0.18866 1.00000 0.03367 0.00000 0.00000 C10 0.34031 0.55123 0.37936 1.00000 0.02503 0.02259 0.02252 0.00513 0.00205 0.00632 0.02418 0.00309 0.00017 0.00017 0.00015 0.00000 0.00067 0.00067 0.00066 0.00053 0.00052 0.00052 0.00031 H10A 0.44320 0.53233 0.35433 1.00000 0.02901 0.00000 0.00000 H10B 0.31360 0.50020 0.45123 1.00000 0.02901 0.00000 0.00000 C11 0.36064 0.73292 0.44252 1.00000 0.03240 0.02120 0.02146 0.00536 0.00259 0.00537 0.02597 0.00319 0.00018 0.00017 0.00015 0.00000 0.00076 0.00067 0.00067 0.00053 0.00056 0.00055 0.00032 H11 0.37256 0.78012 0.36504 1.00000 0.03116 0.00000 0.00000 C12 0.51407 0.81115 0.55600 1.00000 0.03424 0.02669 0.03431 0.00400 -0.00320 0.00223 0.03501 0.00347 0.00020 0.00019 0.00018 0.00000 0.00083 0.00076 0.00085 0.00063 0.00066 0.00062 0.00038 H12A 0.52688 0.92764 0.59606 1.00000 0.05252 0.00000 0.00000 H12B 0.60722 0.79225 0.51321 1.00000 0.05252 0.00000 0.00000 H12C 0.50635 0.76364 0.63141 1.00000 0.05252 0.00000 0.00000 C13 0.21553 0.76983 0.50406 1.00000 0.03962 0.03283 0.02639 0.00299 0.00273 0.01658 0.03372 0.00371 0.00020 0.00020 0.00017 0.00000 0.00087 0.00081 0.00075 0.00062 0.00064 0.00067 0.00037 H13A 0.20368 0.72729 0.58222 1.00000 0.05058 0.00000 0.00000 H13B 0.11844 0.71896 0.43013 1.00000 0.05058 0.00000 0.00000 H13C 0.23093 0.88702 0.53951 1.00000 0.05058 0.00000 0.00000 N1 0.29146 0.13197 0.00025 1.00000 0.02625 0.02360 0.02120 0.00361 0.00115 0.00580 0.02503 0.00267 0.00015 0.00015 0.00013 0.00000 0.00060 0.00059 0.00058 0.00046 0.00046 0.00046 0.00028 N2 0.22100 0.31290 0.16286 1.00000 0.02617 0.02072 0.02200 0.00391 0.00074 0.00553 0.02418 0.00264 0.00015 0.00014 0.00013 0.00000 0.00059 0.00057 0.00058 0.00045 0.00046 0.00045 0.00028 Final Structure Factor Calculation for 04src0078 in P-1 Total number of l.s. parameters = 185 Maximum vector length = 511 Memory required = 2359 / 24017 wR2 = 0.1338 before cycle 11 for 3278 data and 0 / 185 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0517 for 2899 Fo > 4sig(Fo) and 0.0575 for all 3278 data wR2 = 0.1338, GooF = S = 1.031, Restrained GooF = 1.031 for all data Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 19.00 for hydrogen atoms Principal mean square atomic displacements U 0.0352 0.0307 0.0259 B1 0.0936 0.0689 0.0296 F1 0.0584 0.0500 0.0249 F2 0.0646 0.0339 0.0289 F3 0.0639 0.0331 0.0304 F4 0.0312 0.0241 0.0170 C1 0.0454 0.0242 0.0213 C2 0.0572 0.0256 0.0233 C3 0.0542 0.0278 0.0257 C4 0.0385 0.0295 0.0241 C5 0.0287 0.0250 0.0177 C6 0.0309 0.0253 0.0207 C7 0.0439 0.0330 0.0234 C8 0.0402 0.0249 0.0190 C9 0.0279 0.0240 0.0206 C10 0.0339 0.0240 0.0199 C11 0.0463 0.0369 0.0218 C12 0.0486 0.0300 0.0226 C13 0.0297 0.0265 0.0190 N1 0.0297 0.0242 0.0186 N2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.019 0.027 0.037 0.049 0.064 0.082 0.112 0.164 1.000 Number in group 333. 354. 313. 325. 327. 324. 320. 333. 321. 328. GooF 1.211 0.962 1.010 1.143 0.973 0.977 0.995 0.982 1.007 1.022 K 3.013 1.108 1.052 1.065 1.018 1.022 1.016 1.017 0.995 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 330. 335. 319. 331. 325. 331. 323. 327. 330. 327. GooF 0.906 0.871 1.003 0.918 0.886 0.944 1.039 1.022 1.223 1.383 K 1.034 1.070 1.048 1.027 1.023 0.983 0.988 0.985 1.014 1.010 R1 0.112 0.100 0.094 0.076 0.060 0.053 0.044 0.043 0.048 0.046 Recommended weighting scheme: WGHT 0.0446 0.3505 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/su Fc/Fc(max) Resolution(A) -3 6 0 9.87 0.77 5.77 0.010 1.39 3 3 3 62.24 21.36 5.41 0.054 1.34 -3 9 3 6.42 0.18 5.26 0.005 0.85 -6 -3 6 18.35 5.01 4.92 0.026 1.07 0 -9 3 4.46 0.11 4.86 0.004 0.98 -6 6 0 22.57 6.70 4.79 0.030 1.14 -3 0 6 30.84 9.10 4.46 0.035 1.49 -6 3 6 6.41 0.35 4.45 0.007 1.05 9 -6 3 22.76 7.53 4.26 0.032 0.86 6 0 3 175.71 123.12 4.04 0.129 1.19 -1 5 0 41.36 25.69 4.02 0.059 1.71 3 0 3 2.84 0.08 3.82 0.003 1.91 -3 -6 6 9.93 3.06 3.78 0.020 1.12 0 9 0 7.46 0.43 3.78 0.008 0.92 0 0 10 7.32 0.15 3.67 0.004 0.94 -1 -5 1 34.45 21.61 3.62 0.054 1.62 -1 -1 1 23.90 38.17 3.59 0.072 5.37 -1 1 0 844.54 1368.91 3.54 0.429 6.86 -1 2 4 14.12 5.55 3.52 0.027 1.87 -1 1 4 223.93 164.83 3.40 0.149 2.15 5 -1 1 4.03 9.95 3.27 0.037 1.66 3 -3 6 109.01 63.09 3.27 0.092 1.38 3 9 0 13.86 6.29 3.26 0.029 0.81 3 3 6 8.02 1.37 3.26 0.014 1.01 -1 0 1 286.71 430.16 3.23 0.241 6.91 2 -5 1 4.29 0.33 3.23 0.007 1.76 1 -3 3 70.21 47.76 3.22 0.080 2.50 9 1 0 9.93 4.54 3.22 0.025 0.89 -7 0 7 6.94 0.45 3.20 0.008 0.99 2 -5 2 62.81 43.06 3.12 0.076 1.76 -3 -6 3 46.84 33.11 3.09 0.067 1.20 6 -3 6 66.94 36.05 3.09 0.070 1.03 -3 -3 3 70.59 52.07 3.05 0.084 1.79 -3 -1 4 9.80 4.80 3.00 0.025 1.98 0 -5 3 87.36 65.02 2.99 0.094 1.72 0 6 0 74.90 56.54 2.97 0.087 1.38 -1 -3 1 36.32 25.50 2.87 0.059 2.58 -8 8 0 6.89 1.98 2.85 0.016 0.86 1 3 2 31.44 43.61 2.84 0.077 1.90 -5 6 6 25.33 16.58 2.82 0.047 0.90 6 0 6 32.70 8.84 2.82 0.035 0.95 -5 1 0 41.57 63.63 2.81 0.093 1.72 -6 3 1 23.98 15.62 2.80 0.046 1.39 0 10 0 25.22 14.55 2.80 0.044 0.83 3 -5 5 5.14 10.28 2.77 0.037 1.39 0 -3 3 330.07 266.08 2.77 0.189 2.54 1 -4 4 15.08 23.36 2.76 0.056 1.90 -1 3 3 327.36 255.64 2.74 0.186 1.87 0 6 2 1.69 0.21 2.73 0.005 1.22 -2 8 1 1.29 4.78 2.73 0.025 1.03 Bond lengths and angles B1 - Distance Angles F1 1.3714 (0.0022) F2 1.3863 (0.0020) 110.19 (0.15) F3 1.3896 (0.0021) 109.96 (0.14) 109.63 (0.14) F4 1.4011 (0.0021) 109.78 (0.16) 108.50 (0.13) 108.75 (0.14) B1 - F1 F2 F3 F1 - Distance Angles B1 1.3714 (0.0022) F1 - F2 - Distance Angles B1 1.3863 (0.0020) F2 - F3 - Distance Angles B1 1.3896 (0.0021) F3 - F4 - Distance Angles B1 1.4011 (0.0021) F4 - C1 - Distance Angles C2 1.3899 (0.0020) N1 1.3919 (0.0020) 131.64 (0.14) C6 1.3932 (0.0020) 121.86 (0.14) 106.49 (0.12) C1 - C2 N1 C2 - Distance Angles C3 1.3817 (0.0025) C1 1.3899 (0.0020) 116.09 (0.15) H2 0.9500 121.96 121.96 C2 - C3 C1 C3 - Distance Angles C2 1.3817 (0.0025) C4 1.3979 (0.0027) 122.03 (0.15) H3 0.9500 118.98 118.98 C3 - C2 C4 C4 - Distance Angles C5 1.3833 (0.0024) C3 1.3979 (0.0027) 121.94 (0.16) H4 0.9500 119.03 119.03 C4 - C5 C3 C5 - Distance Angles C4 1.3833 (0.0024) C6 1.3882 (0.0022) 116.06 (0.16) H5 0.9500 121.97 121.97 C5 - C4 C6 C6 - Distance Angles C5 1.3882 (0.0022) N2 1.3898 (0.0019) 131.53 (0.14) C1 1.3932 (0.0020) 122.01 (0.14) 106.45 (0.13) C6 - C5 N2 C7 - Distance Angles N2 1.3214 (0.0020) N1 1.3299 (0.0019) 110.77 (0.13) H7 0.9500 124.61 124.61 C7 - N2 N1 C8 - Distance Angles N1 1.4567 (0.0020) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - N1 H8A H8B C9 - Distance Angles N2 1.4730 (0.0018) C10 1.5246 (0.0020) 111.37 (0.12) H9A 0.9900 109.35 109.35 H9B 0.9900 109.35 109.35 107.99 C9 - N2 C10 H9A C10 - Distance Angles C9 1.5246 (0.0020) C11 1.5284 (0.0019) 111.64 (0.12) H10A 0.9900 109.29 109.29 H10B 0.9900 109.29 109.29 107.95 C10 - C9 C11 H10A C11 - Distance Angles C13 1.5202 (0.0022) C10 1.5284 (0.0019) 111.91 (0.13) C12 1.5302 (0.0021) 110.51 (0.13) 109.69 (0.12) H11 1.0000 108.21 108.21 108.21 C11 - C13 C10 C12 C12 - Distance Angles C11 1.5302 (0.0021) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C11 H12A H12B C13 - Distance Angles C11 1.5202 (0.0022) H13A 0.9800 109.47 H13B 0.9800 109.47 109.47 H13C 0.9800 109.47 109.47 109.47 C13 - C11 H13A H13B N1 - Distance Angles C7 1.3299 (0.0019) C1 1.3919 (0.0020) 107.95 (0.13) C8 1.4567 (0.0020) 124.84 (0.13) 127.22 (0.13) N1 - C7 C1 N2 - Distance Angles C7 1.3214 (0.0020) C6 1.3898 (0.0019) 108.33 (0.12) C9 1.4730 (0.0018) 124.08 (0.13) 127.56 (0.13) N2 - C7 C6 FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.0574 for 3278 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.31 at 0.3077 0.3601 0.7687 [ 0.82 A from F4 ] Deepest hole -0.27 at 0.4519 0.4691 0.8733 [ 0.66 A from F4 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2350 / 19078 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3077 0.3601 0.7687 1.00000 0.05 0.31 0.82 F4 1.42 B1 1.78 F1 2.26 F3 Q2 1 0.2822 0.0007 -0.1983 1.00000 0.05 0.28 0.67 H8B 0.93 C8 1.11 H8A 1.78 H8C Q3 1 0.2733 0.6732 0.7861 1.00000 0.05 0.27 0.80 F2 1.52 B1 2.00 F1 2.23 F3 Q4 1 0.3986 -0.0206 -0.1027 1.00000 0.05 0.26 0.90 H8C 0.93 H8B 0.93 C8 1.82 H8A Q5 1 0.2666 0.5689 0.9578 1.00000 0.05 0.24 0.81 F3 1.46 B1 2.00 F2 2.08 F4 Q6 1 0.1461 -0.0333 0.0385 1.00000 0.05 0.24 0.78 C1 0.88 C2 1.53 H2 1.89 N1 Q7 1 0.4699 0.1414 -0.1147 1.00000 0.05 0.24 0.78 H8C 1.02 C8 1.10 H8A 1.88 H8B Q8 1 0.1699 0.1570 0.2596 1.00000 0.05 0.22 0.79 C6 0.86 C5 1.54 H5 1.88 C1 Q9 1 0.4246 0.7639 0.5034 1.00000 0.05 0.22 0.72 C11 0.83 C12 1.40 H12C 1.48 H11 Q10 1 0.2757 0.5166 0.3164 1.00000 0.05 0.22 0.73 C10 0.79 C9 1.42 H10B 1.43 H10A Shortest distances between peaks (including symmetry equivalents) 2 4 1.40 4 7 1.50 2 7 1.76 3 5 2.21 6 8 2.32 1 5 2.36 9 10 2.42 4 4 2.44 3 4 2.57 4 6 2.74 6 6 2.82 2 6 2.84 1 3 2.86 2 3 2.89 5 7 2.93 4 7 2.96 Time profile in seconds ----------------------- 0.02: 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. 0.61: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.81: Structure factors and derivatives 1.67: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.27: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 12:02:42 Total CPU time: 3.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++