+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007may0001 started at 12:39:11 on 29-Sep-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007may0001 in P2(1)2(1)2(1) CELL 0.71073 6.5384 7.6439 18.4179 90.000 90.000 90.000 ZERR 4.00 0.0009 0.0010 0.0028 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O UNIT 44 48 8 4 V = 920.51 F(000) = 400.0 Mu = 0.09 mm-1 Cell Wt = 752.90 Rho = 1.358 MERG 4 OMIT -3.00 55.00 EQIV $1 x + 1/2, -y + 1/2, -z HTAB O1 N1_$1 FMAP 2 PLAN 5 SIZE 0.10 0.10 0.20 ACTA BOND $H L.S. 6 TEMP -153.00 WGHT 0.073900 0.125200 FVAR 0.93778 C1 1 0.460250 0.063056 0.067131 11.00000 0.02974 0.02489 = 0.02886 0.00234 -0.00236 -0.00082 C2 1 0.568864 -0.030738 0.016229 11.00000 0.03303 0.02724 = 0.03232 0.00158 0.00086 0.00349 AFIX 43 H2 2 0.708701 -0.063787 0.019061 11.00000 -1.20000 AFIX 0 C3 1 0.433383 -0.067816 -0.040374 11.00000 0.02709 0.02472 = 0.02956 0.00559 0.00153 0.00024 C4 1 0.472096 -0.158608 -0.109718 11.00000 0.02966 0.02252 = 0.02787 0.00568 -0.00002 -0.00206 C5 1 0.673353 -0.180888 -0.133343 11.00000 0.03013 0.02839 = 0.02967 0.00299 -0.00444 -0.00238 AFIX 43 H5 2 0.783181 -0.139778 -0.104201 11.00000 -1.20000 AFIX 0 C6 1 0.714430 -0.262986 -0.199361 11.00000 0.03264 0.03093 = 0.02897 0.00193 0.00507 0.00397 AFIX 43 H6 2 0.851805 -0.277369 -0.215062 11.00000 -1.20000 AFIX 0 C7 1 0.554561 -0.323781 -0.242204 11.00000 0.04470 0.02632 = 0.02634 -0.00017 0.00313 0.00218 AFIX 43 H7 2 0.582720 -0.379802 -0.287148 11.00000 -1.20000 AFIX 0 C8 1 0.354240 -0.302747 -0.219418 11.00000 0.04066 0.03273 = 0.02444 0.00009 -0.00480 -0.00255 AFIX 43 H8 2 0.245122 -0.345222 -0.248559 11.00000 -1.20000 AFIX 0 C9 1 0.312638 -0.219548 -0.153951 11.00000 0.03102 0.02763 = 0.02982 0.00659 -0.00032 -0.00046 AFIX 43 H9 2 0.174794 -0.203797 -0.139012 11.00000 -1.20000 AFIX 0 C10 1 0.521843 0.144839 0.137318 11.00000 0.03486 0.03177 = 0.02816 -0.00130 -0.00290 0.00187 AFIX 23 H10A 2 0.437590 0.094477 0.176788 11.00000 -1.20000 H10B 2 0.666416 0.114935 0.147375 11.00000 -1.20000 AFIX 0 C11 1 0.087144 0.145124 0.078207 11.00000 0.03619 0.03526 = 0.03275 0.00189 0.00427 0.00356 AFIX 137 H11A 2 0.038347 0.057230 0.112855 11.00000 -1.50000 H11B 2 -0.020862 0.170379 0.042834 11.00000 -1.50000 H11C 2 0.123037 0.252571 0.104289 11.00000 -1.50000 AFIX 0 N1 3 0.244976 -0.000686 -0.025575 11.00000 0.03321 0.02672 = 0.02575 -0.00166 -0.00001 -0.00157 N2 3 0.267791 0.078175 0.040322 11.00000 0.02927 0.02843 = 0.02722 -0.00148 0.00108 0.00194 O1 4 0.500073 0.329995 0.138157 11.00000 0.04000 0.02783 = 0.03190 -0.00336 0.00625 -0.00301 H1O 2 0.578117 0.370107 0.104204 11.00000 0.05594 HKLF 4 Covalent radii and connectivity table for 2007may0001 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - N2 C2 C10 C2 - C1 C3 C3 - N1 C2 C4 C4 - C5 C9 C3 C5 - C6 C4 C6 - C7 C5 C7 - C8 C6 C8 - C7 C9 C9 - C8 C4 C10 - O1 C1 C11 - N2 N1 - C3 N2 N2 - C1 N1 C11 O1 - C10 Operators for generating equivalent atoms: $1 x+1/2, -y+1/2, -z 9588 Reflections read, of which 58 rejected -7 =< h =< 8, -9 =< k =< 9, -18 =< l =< 23, Max. 2-theta = 54.95 0 Systematic absence violations 0 Inconsistent equivalents 1244 Unique reflections, of which 0 suppressed R(int) = 0.1335 R(sigma) = 0.0894 Friedel opposites merged Maximum memory for data reduction = 1514 / 12042 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 = 1886 / 166941 wR2 = 0.1423 before cycle 1 for 1244 data and 132 / 132 parameters GooF = S = 1.015; Restrained GooF = 1.015 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0739 * P )^2 + 0.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.93370 0.00425 -0.960 OSF Mean shift/esd = 0.058 Maximum = -0.960 for OSF Max. shift = 0.003 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 2 Maximum vector length = 511 Memory required = 1886 / 166941 wR2 = 0.1420 before cycle 2 for 1244 data and 132 / 132 parameters GooF = S = 1.012; Restrained GooF = 1.012 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0739 * P )^2 + 0.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.93278 0.00423 -0.219 OSF Mean shift/esd = 0.020 Maximum = -0.219 for OSF Max. shift = 0.001 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 3 Maximum vector length = 511 Memory required = 1886 / 166941 wR2 = 0.1420 before cycle 3 for 1244 data and 132 / 132 parameters GooF = S = 1.012; Restrained GooF = 1.012 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0739 * P )^2 + 0.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.93274 0.00423 -0.009 OSF Mean shift/esd = 0.002 Maximum = -0.009 for OSF Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 4 Maximum vector length = 511 Memory required = 1886 / 166941 wR2 = 0.1420 before cycle 4 for 1244 data and 132 / 132 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0739 * P )^2 + 0.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.93273 0.00423 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.002 for x H1O Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 5 Maximum vector length = 511 Memory required = 1886 / 166941 wR2 = 0.1420 before cycle 5 for 1244 data and 132 / 132 parameters GooF = S = 1.012; Restrained GooF = 1.012 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0739 * P )^2 + 0.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.93273 0.00423 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for x H1O Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 6 Maximum vector length = 511 Memory required = 1886 / 166941 wR2 = 0.1420 before cycle 6 for 1244 data and 132 / 132 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0739 * P )^2 + 0.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.93273 0.00423 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H1O Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.7087 -0.0638 0.0191 43 0.950 0.000 C2 C1 C3 H5 0.7832 -0.1398 -0.1042 43 0.950 0.000 C5 C6 C4 H6 0.8519 -0.2773 -0.2151 43 0.950 0.000 C6 C7 C5 H7 0.5827 -0.3798 -0.2872 43 0.950 0.000 C7 C8 C6 H8 0.2451 -0.3452 -0.2486 43 0.950 0.000 C8 C7 C9 H9 0.1748 -0.2038 -0.1390 43 0.950 0.000 C9 C8 C4 H10A 0.4377 0.0944 0.1768 23 0.990 0.000 C10 O1 C1 H10B 0.6665 0.1149 0.1474 23 0.990 0.000 C10 O1 C1 H11A 0.0384 0.0573 0.1129 137 0.980 0.000 C11 N2 H11A H11B -0.0209 0.1704 0.0429 137 0.980 0.000 C11 N2 H11A H11C 0.1231 0.2526 0.1043 137 0.980 0.000 C11 N2 H11A 2007may0001 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.46027 0.06304 0.06712 1.00000 0.02947 0.02461 0.02846 0.00225 -0.00237 -0.00082 0.02751 0.00605 0.00054 0.00046 0.00019 0.00000 0.00204 0.00183 0.00194 0.00166 0.00172 0.00172 0.00086 C2 0.56888 -0.03076 0.01624 1.00000 0.03266 0.02692 0.03200 0.00158 0.00082 0.00342 0.03053 0.00663 0.00062 0.00049 0.00020 0.00000 0.00220 0.00192 0.00203 0.00169 0.00170 0.00177 0.00092 H2 0.70871 -0.06383 0.01908 1.00000 0.03664 0.00000 0.00000 C3 0.43337 -0.06783 -0.04037 1.00000 0.02675 0.02444 0.02924 0.00552 0.00153 0.00021 0.02681 0.00631 0.00054 0.00046 0.00019 0.00000 0.00203 0.00181 0.00195 0.00164 0.00169 0.00165 0.00086 C4 0.47210 -0.15861 -0.10972 1.00000 0.02939 0.02227 0.02757 0.00555 0.00000 -0.00206 0.02641 0.00626 0.00055 0.00046 0.00020 0.00000 0.00205 0.00185 0.00192 0.00153 0.00162 0.00180 0.00085 C5 0.67339 -0.18087 -0.13333 1.00000 0.02985 0.02813 0.02936 0.00284 -0.00437 -0.00237 0.02911 0.00633 0.00054 0.00050 0.00020 0.00000 0.00221 0.00215 0.00202 0.00183 0.00160 0.00167 0.00091 H5 0.78320 -0.13976 -0.10418 1.00000 0.03493 0.00000 0.00000 C6 0.71449 -0.26297 -0.19936 1.00000 0.03239 0.03066 0.02872 0.00193 0.00507 0.00395 0.03059 0.00660 0.00061 0.00048 0.00019 0.00000 0.00210 0.00214 0.00199 0.00170 0.00179 0.00179 0.00092 H6 0.85186 -0.27734 -0.21507 1.00000 0.03671 0.00000 0.00000 C7 0.55455 -0.32379 -0.24221 1.00000 0.04435 0.02609 0.02608 -0.00020 0.00305 0.00219 0.03217 0.00691 0.00059 0.00051 0.00020 0.00000 0.00253 0.00206 0.00195 0.00159 0.00189 0.00208 0.00096 H7 0.58269 -0.37982 -0.28716 1.00000 0.03861 0.00000 0.00000 C8 0.35425 -0.30274 -0.21942 1.00000 0.04034 0.03239 0.02420 0.00012 -0.00474 -0.00255 0.03231 0.00669 0.00063 0.00050 0.00019 0.00000 0.00235 0.00231 0.00202 0.00185 0.00176 0.00190 0.00096 H8 0.24513 -0.34521 -0.24856 1.00000 0.03878 0.00000 0.00000 C9 0.31263 -0.21955 -0.15396 1.00000 0.03075 0.02734 0.02949 0.00652 -0.00038 -0.00046 0.02919 0.00652 0.00057 0.00048 0.00020 0.00000 0.00220 0.00214 0.00201 0.00169 0.00166 0.00164 0.00094 H9 0.17478 -0.20380 -0.13902 1.00000 0.03503 0.00000 0.00000 C10 0.52191 0.14480 0.13733 1.00000 0.03461 0.03144 0.02785 -0.00137 -0.00294 0.00189 0.03130 0.00631 0.00061 0.00049 0.00020 0.00000 0.00216 0.00211 0.00206 0.00167 0.00178 0.00177 0.00092 H10A 0.43769 0.09441 0.17681 1.00000 0.03756 0.00000 0.00000 H10B 0.66650 0.11492 0.14738 1.00000 0.03756 0.00000 0.00000 C11 0.08715 0.14516 0.07822 1.00000 0.03573 0.03497 0.03238 0.00183 0.00426 0.00356 0.03436 0.00703 0.00059 0.00053 0.00022 0.00000 0.00232 0.00219 0.00213 0.00185 0.00182 0.00195 0.00099 H11A 0.03837 0.05729 0.11288 1.00000 0.05155 0.00000 0.00000 H11B -0.02087 0.17040 0.04285 1.00000 0.05155 0.00000 0.00000 H11C 0.12307 0.25262 0.10429 1.00000 0.05155 0.00000 0.00000 N1 0.24495 -0.00067 -0.02558 1.00000 0.03289 0.02642 0.02542 -0.00166 -0.00001 -0.00152 0.02825 0.00516 0.00049 0.00039 0.00015 0.00000 0.00181 0.00163 0.00162 0.00133 0.00143 0.00146 0.00075 N2 0.26778 0.07819 0.04033 1.00000 0.02896 0.02805 0.02694 -0.00147 0.00107 0.00196 0.02798 0.00516 0.00046 0.00038 0.00016 0.00000 0.00175 0.00163 0.00160 0.00138 0.00146 0.00142 0.00074 O1 0.50005 0.33001 0.13817 1.00000 0.03966 0.02753 0.03156 -0.00328 0.00625 -0.00302 0.03292 0.00450 0.00043 0.00035 0.00015 0.00000 0.00165 0.00144 0.00154 0.00121 0.00129 0.00132 0.00069 H1O 0.57782 0.36988 0.10439 1.00000 0.05539 0.08225 0.00720 0.00625 0.00258 0.00000 0.01563 Final Structure Factor Calculation for 2007may0001 in P2(1)2(1)2(1) Total number of l.s. parameters = 132 Maximum vector length = 511 Memory required = 1756 / 25046 wR2 = 0.1420 before cycle 7 for 1244 data and 2 / 132 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0739 * P )^2 + 0.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0608 for 828 Fo > 4sig(Fo) and 0.1113 for all 1244 data wR2 = 0.1420, GooF = S = 1.011, Restrained GooF = 1.011 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0320 0.0270 0.0236 C1 0.0350 0.0315 0.0251 C2 0.0332 0.0265 0.0207 C3 0.0317 0.0291 0.0185 C4 0.0358 0.0265 0.0251 C5 0.0384 0.0283 0.0250 C6 0.0451 0.0263 0.0252 C7 0.0423 0.0318 0.0229 C8 0.0351 0.0307 0.0218 C9 0.0367 0.0306 0.0267 C10 0.0412 0.0325 0.0294 C11 0.0332 0.0274 0.0241 N1 0.0305 0.0285 0.0249 N2 0.0441 0.0289 0.0257 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.025 0.034 0.043 0.053 0.066 0.083 0.105 0.146 1.000 Number in group 135. 117. 127. 128. 115. 127. 125. 126. 121. 123. GooF 0.907 0.956 0.964 1.061 1.010 1.098 1.089 1.024 0.999 0.994 K 0.807 0.881 1.128 0.968 1.026 1.004 1.001 1.005 1.016 0.993 Resolution(A) 0.77 0.80 0.83 0.88 0.92 0.99 1.07 1.18 1.37 1.75 inf Number in group 125. 124. 127. 122. 127. 123. 124. 123. 124. 125. GooF 1.020 0.984 1.048 0.972 1.082 1.062 1.063 0.861 0.999 1.001 K 1.082 1.073 1.109 1.036 1.005 1.013 1.009 1.004 1.050 0.969 R1 0.377 0.335 0.225 0.155 0.126 0.088 0.062 0.042 0.044 0.035 Recommended weighting scheme: WGHT 0.0739 0.1256 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) 7 5 1 99.56 19.24 3.46 0.040 0.80 1 6 8 66.47 92.00 3.22 0.088 1.10 7 1 2 7.26 28.01 2.97 0.049 0.92 0 1 21 30.70 1.39 2.87 0.011 0.87 0 4 19 78.05 34.21 2.85 0.054 0.86 0 0 4 150.27 195.00 2.80 0.128 4.60 7 2 1 21.88 41.05 2.79 0.059 0.91 3 8 3 140.41 101.44 2.77 0.092 0.87 6 2 8 26.01 48.46 2.77 0.064 0.95 4 0 7 49.92 33.56 2.74 0.053 1.39 4 0 2 323.76 258.05 2.72 0.147 1.61 5 1 8 48.90 69.62 2.72 0.077 1.12 0 7 5 25.35 6.99 2.68 0.024 1.05 1 4 19 58.34 32.44 2.67 0.052 0.86 5 4 8 98.17 73.00 2.64 0.078 0.98 7 1 10 28.55 9.13 2.64 0.028 0.83 2 0 22 39.00 4.68 2.60 0.020 0.81 5 1 5 45.12 60.87 2.57 0.072 1.22 7 4 3 41.42 13.07 2.54 0.033 0.83 0 9 3 88.49 44.61 2.54 0.061 0.84 6 0 4 749.21 609.38 2.52 0.227 1.06 2 5 10 152.62 191.35 2.52 0.127 1.11 2 0 19 238.03 180.01 2.47 0.123 0.93 1 5 7 70.32 88.95 2.45 0.087 1.30 1 2 14 7.80 16.80 2.45 0.038 1.22 0 8 9 203.82 147.10 2.41 0.111 0.87 4 1 16 53.18 31.98 2.41 0.052 0.93 3 1 1 88.75 71.15 2.37 0.077 2.08 5 6 4 95.85 69.33 2.36 0.076 0.90 4 0 14 12.84 40.69 2.33 0.059 1.02 6 5 10 52.70 20.01 2.25 0.041 0.80 1 7 8 13.64 27.87 2.24 0.048 0.98 0 7 6 171.88 119.57 2.23 0.100 1.03 4 3 17 45.51 24.28 2.22 0.045 0.85 1 5 20 -17.85 8.47 2.22 0.027 0.78 4 7 1 69.18 46.70 2.21 0.063 0.91 3 1 3 295.94 250.12 2.20 0.145 1.98 0 3 22 83.90 43.46 2.20 0.061 0.80 2 0 20 22.29 1.33 2.20 0.011 0.89 0 5 13 15.56 26.83 2.19 0.048 1.04 6 6 3 52.66 16.82 2.18 0.038 0.82 0 6 11 40.04 71.04 2.16 0.077 1.01 6 2 16 88.69 57.08 2.14 0.069 0.77 3 4 0 6.66 14.70 2.12 0.035 1.44 5 8 0 34.33 0.38 2.11 0.006 0.77 0 3 14 106.27 130.33 2.10 0.105 1.17 0 7 3 29.77 46.24 2.09 0.062 1.08 6 2 5 68.60 89.11 2.08 0.087 1.01 5 3 13 -5.72 6.77 2.06 0.024 0.90 4 7 4 279.34 230.89 2.05 0.139 0.89 Bond lengths and angles C1 - Distance Angles N2 1.3568 (0.0045) C2 1.3771 (0.0052) 105.98 (0.33) C10 1.4918 (0.0051) 122.02 (0.32) 131.97 (0.35) C1 - N2 C2 C2 - Distance Angles C1 1.3771 (0.0052) C3 1.3973 (0.0051) 106.64 (0.35) H2 0.9500 126.68 126.68 C2 - C1 C3 C3 - Distance Angles N1 1.3621 (0.0045) C2 1.3973 (0.0051) 110.36 (0.32) C4 1.4755 (0.0052) 120.37 (0.31) 129.23 (0.33) C3 - N1 C2 C4 - Distance Angles C5 1.3965 (0.0050) C9 1.4029 (0.0050) 118.62 (0.34) C3 1.4755 (0.0052) 119.26 (0.32) 122.10 (0.32) C4 - C5 C9 C5 - Distance Angles C6 1.3947 (0.0050) C4 1.3965 (0.0050) 120.53 (0.33) H5 0.9500 119.73 119.73 C5 - C6 C4 C6 - Distance Angles C7 1.3901 (0.0054) C5 1.3947 (0.0050) 120.04 (0.35) H6 0.9500 119.98 119.98 C6 - C7 C5 C7 - Distance Angles C8 1.3847 (0.0055) C6 1.3901 (0.0054) 120.03 (0.34) H7 0.9500 119.98 119.98 C7 - C8 C6 C8 - Distance Angles C7 1.3847 (0.0055) C9 1.3900 (0.0051) 120.09 (0.35) H8 0.9500 119.96 119.96 C8 - C7 C9 C9 - Distance Angles C8 1.3900 (0.0051) C4 1.4029 (0.0050) 120.67 (0.35) H9 0.9500 119.66 119.66 C9 - C8 C4 C10 - Distance Angles O1 1.4230 (0.0047) C1 1.4918 (0.0051) 113.52 (0.30) H10A 0.9900 108.86 108.86 H10B 0.9900 108.86 108.86 107.71 C10 - O1 C1 H10A C11 - Distance Angles N2 1.4643 (0.0047) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - N2 H11A H11B N1 - Distance Angles C3 1.3621 (0.0045) N2 1.3635 (0.0040) 104.22 (0.29) N1 - C3 N2 - Distance Angles C1 1.3568 (0.0045) N1 1.3635 (0.0040) 112.81 (0.29) C11 1.4643 (0.0047) 127.20 (0.30) 119.38 (0.30) N2 - C1 N1 O1 - Distance Angles C10 1.4230 (0.0047) H1O 0.8593 (0.0483) 106.60 (3.13) O1 - C10 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.86(5) 2.07(5) 2.927(4) 172(4) O1-H1O...N1_$1 FMAP and GRID set by program FMAP 2 3 23 GRID -1.250 -2 -2 1.250 2 2 R1 = 0.1113 for 1244 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.22 at 0.4052 0.4833 0.0326 [ 1.71 A from H2 ] Deepest hole -0.24 at 0.0479 0.7606 0.1520 [ 1.08 A from C5 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 1710 / 14669 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9052 0.0167 -0.0326 1.00000 0.05 0.22 1.71 H2 1.88 H11B 1.94 H1O 1.95 H5 Q2 1 0.7526 0.1356 -0.0214 1.00000 0.05 0.22 1.72 H2 1.88 C2 1.91 H11B 1.94 H11C Q3 1 0.1306 -0.1574 -0.1893 1.00000 0.05 0.20 1.03 H9 1.44 C9 1.92 C8 1.95 H8 Q4 1 0.7360 -0.5037 -0.2776 1.00000 0.05 0.19 1.39 H7 1.93 C7 2.10 C9 2.21 H6 Q5 1 0.1753 -0.5415 -0.2455 1.00000 0.05 0.19 1.57 H8 1.89 H10B 1.95 H6 2.04 H10A Shortest distances between peaks (including symmetry equivalents) 1 2 1.36 3 4 1.59 3 5 2.49 4 5 2.95 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: 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. 0.69: 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 0.58: Structure factors and derivatives 0.46: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.02: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.01: Fourier summations 0.01: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007may0001 finished at 12:39:24 Total CPU time: 2.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++