+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0031p21 started at 16:34:26 on 21-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0031p21 in P2(1) CELL 0.71073 7.6534 6.9693 10.5603 90.000 104.616 90.000 ZERR 2.00 0.0008 0.0007 0.0010 0.000 0.005 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O UNIT 18 28 4 12 V = 545.05 F(000) = 260.0 Mu = 0.13 mm-1 Cell Wt = 492.44 Rho = 1.500 MERG 4 OMIT -3.00 55.00 SHEL 7 0.77 HTAB N23 O3 HTAB N23 O2 HTAB N23 O4A EQIV_$1 x+1, y, z HTAB O1B O4A_$1 EQIV_$2 -x, y-1/2, -z HTAB O2 O4B_$2 EQIV_$3 -x, y+1/2, -z HTAB O3 O4B_$3 FMAP 2 PLAN 10 SIZE 0.02 0.10 0.22 ACTA BOND $H WGHT 0.05060 0.11930 L.S. 4 TEMP -153.00 FVAR 0.32501 MOLE 1 C1 1 0.516855 0.192156 0.154708 11.00000 0.01693 0.01845 = 0.02277 -0.00290 0.00574 0.00159 C2 1 0.314201 0.154512 0.114014 11.00000 0.01927 0.02094 = 0.01468 0.00247 0.00609 0.00006 AFIX 13 H2 2 0.285592 0.072354 0.033785 11.00000 -1.20000 AFIX 0 C3 1 0.211426 0.344264 0.083831 11.00000 0.01910 0.02405 = 0.01354 -0.00174 0.00234 0.00199 AFIX 13 H3 2 0.251177 0.411771 0.012329 11.00000 -1.20000 AFIX 0 C4 1 0.009181 0.304424 0.038317 11.00000 0.01884 0.01584 = 0.02228 0.00367 0.00111 0.00212 O1A 4 0.608950 0.168614 0.265394 11.00000 0.01729 0.04808 = 0.02312 0.00550 0.00006 -0.00124 O1B 4 0.577901 0.250742 0.054991 11.00000 0.01895 0.03363 = 0.02226 0.00148 0.00784 -0.00143 AFIX 147 H1 2 0.690787 0.261475 0.078782 11.00000 0.04694 AFIX 0 O2 4 0.264935 0.055235 0.217115 11.00000 0.02261 0.02268 = 0.02057 0.00230 0.00634 -0.00438 AFIX 147 H2O 2 0.187167 -0.028487 0.185575 11.00000 -1.50000 AFIX 0 O3 4 0.257727 0.459656 0.200011 11.00000 0.02386 0.01912 = 0.01963 -0.00165 0.00155 0.00136 AFIX 147 H3O 2 0.214528 0.570257 0.183079 11.00000 -1.50000 AFIX 0 O4A 4 -0.081567 0.309974 0.123086 11.00000 0.01784 0.03337 = 0.02696 0.00107 0.01060 -0.00053 O4B 4 -0.051434 0.266087 -0.082008 11.00000 0.02113 0.02414 = 0.02096 -0.00460 -0.00082 -0.00008 MOLE 2 C22 1 0.277041 0.253069 0.530685 11.00000 0.02670 0.02509 = 0.01943 -0.00516 0.00507 -0.00079 C24 1 -0.019802 0.263753 0.451859 11.00000 0.02770 0.03321 = 0.03119 -0.00038 0.00149 -0.00071 AFIX 43 H24 2 -0.135237 0.271974 0.391890 11.00000 -1.20000 AFIX 0 C25 1 0.013970 0.241089 0.581174 11.00000 0.02677 0.03746 = 0.03338 -0.00034 0.01144 0.00087 AFIX 43 H25 2 -0.073144 0.231896 0.630998 11.00000 -1.20000 AFIX 0 C26 1 0.294978 0.202583 0.766172 11.00000 0.04184 0.04293 = 0.01785 0.00367 0.00469 0.00132 AFIX 137 H26A 2 0.392122 0.109084 0.771155 11.00000 -1.50000 H26B 2 0.210234 0.153706 0.814232 11.00000 -1.50000 H26C 2 0.346454 0.324257 0.804927 11.00000 -1.50000 AFIX 0 C27 1 0.473457 0.254634 0.542505 11.00000 0.02963 0.03898 = 0.02762 -0.00255 0.00810 0.00002 AFIX 137 H27A 2 0.524852 0.376010 0.581844 11.00000 -1.50000 H27B 2 0.495610 0.241315 0.455489 11.00000 -1.50000 H27C 2 0.530254 0.147613 0.598026 11.00000 -1.50000 AFIX 0 N21 3 0.199710 0.233461 0.629258 11.00000 0.02401 0.02895 = 0.01654 0.00071 0.00454 -0.00091 N23 3 0.145301 0.272933 0.422112 11.00000 0.02657 0.03364 = 0.01807 0.00032 0.00420 0.00149 AFIX 43 H23 2 0.161114 0.289456 0.343137 11.00000 0.04263 AFIX 0 HKLF 4 Covalent radii and connectivity table for 07skc0031p21 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - O2 C1 C3 C3 - O3 C4 C2 C4 - O4A O4B C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C22 - N21 N23 C27 C24 - C25 N23 C25 - C24 N21 C26 - N21 C27 - C22 N21 - C22 C25 C26 N23 - C22 C24 Operators for generating equivalent atoms: $1 x+1, y, z $2 -x, y-1/2, -z $3 -x, y+1/2, -z Floating origin restraints generated 7450 Reflections read, of which 22 rejected -9 =< h =< 9, -9 =< k =< 9, -13 =< l =< 13, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 1340 Unique reflections, of which 0 suppressed R(int) = 0.0875 R(sigma) = 0.0701 Friedel opposites merged Maximum memory for data reduction = 1848 / 13237 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 = 2297 / 200900 wR2 = 0.1177 before cycle 1 for 1340 data and 161 / 161 parameters GooF = S = 1.079; Restrained GooF = 1.079 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0506 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.32502 0.00112 0.010 OSF Mean shift/esd = 0.003 Maximum = 0.010 for OSF Max. shift = 0.000 A for H26A Max. dU = 0.000 for H23 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2297 / 200900 wR2 = 0.1177 before cycle 2 for 1340 data and 161 / 161 parameters GooF = S = 1.079; Restrained GooF = 1.079 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0506 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.32502 0.00112 0.003 OSF Mean shift/esd = 0.001 Maximum = -0.004 for tors H26A Max. shift = 0.000 A for H26A Max. dU = 0.000 for H1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2297 / 200900 wR2 = 0.1177 before cycle 3 for 1340 data and 161 / 161 parameters GooF = S = 1.079; Restrained GooF = 1.079 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0506 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.32502 0.00112 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for tors H26A Max. shift = 0.000 A for H26A Max. dU = 0.000 for H1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2297 / 200900 wR2 = 0.1177 before cycle 4 for 1340 data and 161 / 161 parameters GooF = S = 1.079; Restrained GooF = 1.079 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0506 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.32502 0.00112 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H26A Max. shift = 0.000 A for H26A Max. dU = 0.000 for H1 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 0.2856 0.0724 0.0338 13 1.000 0.000 C2 O2 C1 C3 H3 0.2512 0.4118 0.0123 13 1.000 0.000 C3 O3 C4 C2 H1 0.6908 0.2615 0.0788 147 0.840 0.000 O1B C1 H1 H2O 0.1872 -0.0285 0.1856 147 0.840 0.000 O2 C2 H2O H3O 0.2145 0.5702 0.1831 147 0.840 0.000 O3 C3 H3O H24 -0.1352 0.2720 0.3919 43 0.950 0.000 C24 C25 N23 H25 -0.0731 0.2319 0.6310 43 0.950 0.000 C25 C24 N21 H26A 0.3921 0.1090 0.7712 137 0.980 0.000 C26 N21 H26A H26B 0.2102 0.1537 0.8142 137 0.980 0.000 C26 N21 H26A H26C 0.3465 0.3242 0.8049 137 0.980 0.000 C26 N21 H26A H27A 0.5248 0.3760 0.5818 137 0.980 0.000 C27 C22 H27A H27B 0.4956 0.2413 0.4555 137 0.980 0.000 C27 C22 H27A H27C 0.5303 0.1476 0.5980 137 0.980 0.000 C27 C22 H27A H23 0.1611 0.2895 0.3431 43 0.880 0.000 N23 C22 C24 07skc0031p21 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.51685 0.19216 0.15471 1.00000 0.01695 0.01843 0.02278 -0.00291 0.00575 0.00159 0.01925 0.00694 0.00047 0.00055 0.00035 0.00000 0.00191 0.00201 0.00204 0.00152 0.00165 0.00164 0.00084 C2 0.31420 0.15451 0.11401 1.00000 0.01928 0.02095 0.01467 0.00248 0.00609 0.00006 0.01798 0.00731 0.00051 0.00054 0.00034 0.00000 0.00201 0.00208 0.00180 0.00156 0.00157 0.00170 0.00084 H2 0.28559 0.07236 0.03378 1.00000 0.02157 0.00000 0.00000 C3 0.21143 0.34426 0.08383 1.00000 0.01911 0.02406 0.01354 -0.00175 0.00235 0.00199 0.01922 0.00702 0.00050 0.00056 0.00034 0.00000 0.00201 0.00214 0.00176 0.00153 0.00157 0.00172 0.00087 H3 0.25118 0.41177 0.01233 1.00000 0.02306 0.00000 0.00000 C4 0.00918 0.30442 0.03832 1.00000 0.01886 0.01583 0.02230 0.00368 0.00112 0.00213 0.01973 0.00711 0.00050 0.00054 0.00034 0.00000 0.00183 0.00208 0.00196 0.00152 0.00156 0.00154 0.00085 O1A 0.60895 0.16861 0.26540 1.00000 0.01729 0.04809 0.02312 0.00550 0.00006 -0.00124 0.03041 0.00546 0.00035 0.00046 0.00026 0.00000 0.00145 0.00193 0.00151 0.00135 0.00119 0.00142 0.00073 O1B 0.57790 0.25074 0.05499 1.00000 0.01896 0.03364 0.02226 0.00148 0.00784 -0.00144 0.02448 0.00521 0.00034 0.00047 0.00022 0.00000 0.00133 0.00158 0.00126 0.00143 0.00103 0.00143 0.00061 H1 0.69079 0.26147 0.07878 1.00000 0.04690 0.00000 0.01416 O2 0.26494 0.05523 0.21711 1.00000 0.02262 0.02269 0.02057 0.00229 0.00634 -0.00439 0.02180 0.00523 0.00038 0.00039 0.00026 0.00000 0.00168 0.00157 0.00147 0.00115 0.00125 0.00122 0.00067 H2O 0.18715 -0.02847 0.18557 1.00000 0.03270 0.00000 0.00000 O3 0.25773 0.45965 0.20001 1.00000 0.02386 0.01911 0.01964 -0.00165 0.00155 0.00137 0.02158 0.00512 0.00040 0.00037 0.00026 0.00000 0.00171 0.00149 0.00149 0.00113 0.00126 0.00119 0.00068 H3O 0.21451 0.57025 0.18308 1.00000 0.03236 0.00000 0.00000 O4A -0.08157 0.30997 0.12309 1.00000 0.01784 0.03338 0.02696 0.00107 0.01060 -0.00053 0.02517 0.00491 0.00033 0.00040 0.00024 0.00000 0.00133 0.00188 0.00139 0.00125 0.00115 0.00127 0.00070 O4B -0.05143 0.26609 -0.08201 1.00000 0.02113 0.02415 0.02096 -0.00461 -0.00083 -0.00008 0.02318 0.00458 0.00031 0.00043 0.00021 0.00000 0.00134 0.00149 0.00130 0.00128 0.00100 0.00134 0.00060 C22 0.27704 0.25306 0.53069 1.00000 0.02671 0.02508 0.01943 -0.00516 0.00506 -0.00079 0.02387 0.00741 0.00049 0.00070 0.00032 0.00000 0.00201 0.00202 0.00180 0.00189 0.00159 0.00203 0.00082 C24 -0.01980 0.26375 0.45186 1.00000 0.02771 0.03321 0.03120 -0.00037 0.00149 -0.00070 0.03177 0.00819 0.00054 0.00075 0.00037 0.00000 0.00209 0.00246 0.00211 0.00219 0.00170 0.00228 0.00095 H24 -0.13523 0.27196 0.39189 1.00000 0.03813 0.00000 0.00000 C25 0.01397 0.24109 0.58117 1.00000 0.02677 0.03747 0.03338 -0.00034 0.01144 0.00086 0.03185 0.00818 0.00053 0.00074 0.00036 0.00000 0.00211 0.00266 0.00223 0.00221 0.00176 0.00222 0.00100 H25 -0.07314 0.23191 0.63100 1.00000 0.03822 0.00000 0.00000 C26 0.29498 0.20258 0.76617 1.00000 0.04184 0.04293 0.01786 0.00367 0.00470 0.00132 0.03472 0.00859 0.00062 0.00071 0.00036 0.00000 0.00264 0.00305 0.00197 0.00182 0.00183 0.00227 0.00114 H26A 0.39209 0.10904 0.77116 1.00000 0.05208 0.00000 0.00000 H26B 0.21022 0.15375 0.81424 1.00000 0.05208 0.00000 0.00000 H26C 0.34649 0.32424 0.80492 1.00000 0.05208 0.00000 0.00000 C27 0.47346 0.25463 0.54251 1.00000 0.02964 0.03897 0.02761 -0.00255 0.00811 0.00003 0.03192 0.00834 0.00051 0.00080 0.00036 0.00000 0.00220 0.00250 0.00199 0.00222 0.00166 0.00239 0.00094 H27A 0.52485 0.37601 0.58184 1.00000 0.04788 0.00000 0.00000 H27B 0.49561 0.24131 0.45549 1.00000 0.04788 0.00000 0.00000 H27C 0.53026 0.14762 0.59803 1.00000 0.04788 0.00000 0.00000 N21 0.19971 0.23346 0.62926 1.00000 0.02401 0.02896 0.01654 0.00071 0.00454 -0.00092 0.02327 0.00602 0.00041 0.00051 0.00026 0.00000 0.00163 0.00196 0.00148 0.00150 0.00127 0.00158 0.00074 N23 0.14530 0.27294 0.42211 1.00000 0.02657 0.03365 0.01807 0.00031 0.00419 0.00149 0.02636 0.00624 0.00040 0.00058 0.00028 0.00000 0.00173 0.00210 0.00156 0.00159 0.00134 0.00180 0.00077 H23 0.16111 0.28946 0.34314 1.00000 0.04259 0.00000 0.01294 Final Structure Factor Calculation for 07skc0031p21 in P2(1) Total number of l.s. parameters = 161 Maximum vector length = 511 Memory required = 2138 / 25046 wR2 = 0.1177 before cycle 5 for 1340 data and 2 / 161 parameters GooF = S = 1.079; Restrained GooF = 1.079 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0506 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0518 for 1009 Fo > 4sig(Fo) and 0.0826 for all 1340 data wR2 = 0.1177, GooF = S = 1.079, Restrained GooF = 1.079 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0244 0.0188 0.0145 C1 0.0218 0.0194 0.0127 C2 0.0256 0.0189 0.0132 C3 0.0268 0.0196 0.0128 C4 0.0498 0.0261 0.0153 O1A 0.0340 0.0232 0.0163 O1B 0.0277 0.0218 0.0160 O2 0.0282 0.0190 0.0175 O3 0.0336 0.0280 0.0139 O4A 0.0313 0.0232 0.0150 O4B 0.0283 0.0270 0.0164 C22 0.0377 0.0333 0.0244 C24 0.0376 0.0344 0.0236 C25 0.0438 0.0430 0.0173 C26 0.0395 0.0298 0.0264 C27 0.0292 0.0241 0.0165 N21 0.0340 0.0270 0.0181 N23 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.018 0.027 0.036 0.045 0.054 0.067 0.082 0.104 0.144 1.000 Number in group 141. 128. 135. 133. 144. 130. 133. 130. 132. 134. GooF 1.079 1.015 1.016 1.236 1.098 1.047 0.991 1.041 0.944 1.270 K 1.441 1.071 0.965 0.969 0.959 0.982 0.990 0.996 1.022 0.980 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.06 1.17 1.34 1.70 inf Number in group 134. 137. 134. 134. 135. 134. 131. 134. 132. 135. GooF 1.010 1.107 1.066 1.000 1.091 1.017 1.071 0.936 1.058 1.375 K 1.010 0.967 1.020 1.011 0.984 1.001 1.023 1.030 1.043 0.954 R1 0.219 0.239 0.182 0.106 0.103 0.054 0.048 0.036 0.033 0.036 Recommended weighting scheme: WGHT 0.0507 0.1194 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) -1 0 1 4.61 20.86 4.54 0.044 6.88 -7 0 2 80.84 113.52 3.45 0.103 1.09 1 1 0 1362.67 1671.97 3.32 0.395 5.08 -8 2 7 32.67 67.25 3.30 0.079 0.86 2 2 7 32.95 21.40 3.21 0.045 1.18 1 0 1 81.71 103.94 3.20 0.098 5.39 0 0 2 317.82 388.93 3.15 0.190 5.11 2 1 1 32.86 23.54 3.13 0.047 2.93 3 8 0 46.71 18.70 3.05 0.042 0.82 -4 4 12 17.20 49.15 3.04 0.068 0.77 2 8 0 10.28 26.53 2.95 0.050 0.85 7 3 0 17.40 28.69 2.89 0.052 0.96 0 1 2 1924.66 2262.25 2.88 0.459 4.12 -1 0 13 27.80 6.71 2.78 0.025 0.80 -8 1 1 17.09 31.96 2.71 0.055 0.94 7 0 3 25.12 7.71 2.71 0.027 0.95 7 1 5 40.85 14.91 2.71 0.037 0.85 4 1 2 46.11 35.12 2.61 0.057 1.57 2 0 8 69.24 92.36 2.59 0.093 1.12 -6 1 10 10.54 2.06 2.54 0.014 0.90 -4 4 11 14.93 1.42 2.48 0.012 0.82 1 0 4 217.71 185.20 2.45 0.131 2.25 0 2 0 9347.60 10717.29 2.43 1.000 3.48 -3 2 10 21.56 13.09 2.39 0.035 1.00 3 3 3 68.42 55.83 2.39 0.072 1.42 -6 7 3 6.09 35.01 2.39 0.057 0.78 0 3 1 346.04 301.29 2.37 0.168 2.27 -5 1 2 53.93 42.76 2.37 0.063 1.49 -6 6 3 2.88 16.58 2.36 0.039 0.86 1 0 3 15.10 21.77 2.34 0.045 2.83 -1 6 10 17.68 36.18 2.26 0.058 0.78 -8 3 1 -0.53 6.90 2.25 0.025 0.87 6 5 3 59.84 37.17 2.25 0.059 0.85 -3 0 10 3.16 11.20 2.24 0.032 1.04 6 1 3 77.18 96.34 2.24 0.095 1.06 4 2 0 13.20 8.15 2.24 0.028 1.63 -2 1 5 263.01 230.84 2.20 0.147 1.94 -3 3 4 253.28 220.25 2.18 0.143 1.54 1 3 9 7.34 15.95 2.18 0.039 0.98 -8 3 9 17.78 5.03 2.15 0.022 0.78 -3 7 7 -13.85 8.62 2.14 0.028 0.82 4 0 10 2.39 22.56 2.14 0.046 0.81 -4 3 8 78.31 94.04 2.14 0.094 1.07 -1 5 11 22.27 3.57 2.13 0.018 0.79 2 2 8 191.01 221.95 2.09 0.144 1.07 -9 1 8 19.41 2.94 2.08 0.017 0.78 1 7 0 31.45 23.05 2.08 0.046 0.99 -7 5 4 40.25 18.19 2.07 0.041 0.85 2 3 4 82.22 69.80 2.07 0.081 1.47 -3 2 13 -10.27 3.98 2.05 0.019 0.79 Bond lengths and angles C1 - Distance Angles O1A 1.2142 (0.0043) O1B 1.3199 (0.0042) 124.99 (0.32) C2 1.5240 (0.0051) 123.40 (0.31) 111.61 (0.28) C1 - O1A O1B C2 - Distance Angles O2 1.4190 (0.0043) C1 1.5240 (0.0051) 108.43 (0.29) C3 1.5305 (0.0050) 111.04 (0.29) 110.06 (0.30) H2 1.0000 109.10 109.10 109.10 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4346 (0.0045) C4 1.5260 (0.0053) 112.54 (0.29) C2 1.5305 (0.0050) 107.65 (0.28) 109.60 (0.29) H3 1.0000 108.99 108.99 108.99 C3 - O3 C4 C2 C4 - Distance Angles O4A 1.2645 (0.0044) O4B 1.2664 (0.0040) 126.10 (0.34) C3 1.5260 (0.0053) 117.78 (0.31) 116.11 (0.29) C4 - O4A O4B O1A - Distance Angles C1 1.2142 (0.0043) O1A - O1B - Distance Angles C1 1.3199 (0.0042) H1 0.8400 109.47 O1B - C1 O2 - Distance Angles C2 1.4190 (0.0043) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4346 (0.0045) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2645 (0.0044) O4A - O4B - Distance Angles C4 1.2664 (0.0040) O4B - C22 - Distance Angles N21 1.3279 (0.0043) N23 1.3293 (0.0046) 107.20 (0.31) C27 1.4767 (0.0051) 125.45 (0.31) 127.34 (0.31) C22 - N21 N23 C24 - Distance Angles C25 1.3336 (0.0051) N23 1.3783 (0.0051) 106.68 (0.33) H24 0.9500 126.66 126.66 C24 - C25 N23 C25 - Distance Angles C24 1.3336 (0.0051) N21 1.3846 (0.0048) 107.21 (0.32) H25 0.9500 126.40 126.40 C25 - C24 N21 C26 - Distance Angles N21 1.4616 (0.0047) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - N21 H26A H26B C27 - Distance Angles C22 1.4767 (0.0051) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C22 H27A H27B N21 - Distance Angles C22 1.3279 (0.0043) C25 1.3846 (0.0048) 109.15 (0.29) C26 1.4616 (0.0047) 125.51 (0.32) 125.32 (0.30) N21 - C22 C25 N23 - Distance Angles C22 1.3293 (0.0046) C24 1.3783 (0.0051) 109.76 (0.30) H23 0.8800 125.12 125.12 N23 - C22 C24 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.19 2.992(4) 151.1 N23-H23...O3 0.88 2.37 2.971(4) 126.1 N23-H23...O2 0.88 2.59 3.207(4) 128.3 N23-H23...O4A 0.84 1.72 2.556(3) 173.6 O1B-H1...O4A_$1 0.84 1.94 2.755(4) 164.3 O2-H2O...O4B_$2 0.84 1.97 2.759(4) 155.8 O3-H3O...O4B_$3 FMAP and GRID set by program FMAP 2 2 19 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0826 for 1340 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.7710 0.2477 0.9334 [ 1.41 A from O4B ] Deepest hole -0.27 at 0.1320 0.3736 0.1343 [ 0.93 A from C3 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2139 / 16272 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.2290 0.2477 -0.0666 1.00000 0.05 0.27 1.41 O4B 1.77 H3O 1.79 H1 1.92 C4 Q2 1 0.5177 0.1959 -0.0606 1.00000 0.05 0.24 1.25 O1B 1.77 H1 1.89 H26A 1.90 H26C Q3 1 0.2863 0.5307 -0.0574 1.00000 0.05 0.23 1.18 H3 1.64 H1 1.85 O1B 2.16 C3 Q4 1 0.5796 0.4426 0.0757 1.00000 0.05 0.23 1.35 O1B 1.52 H1 1.95 H2 1.96 H26A Q5 1 -0.0942 -0.0013 0.4626 1.00000 0.05 0.22 1.94 C24 1.96 C24 1.99 C25 2.04 H24 Q6 1 0.2065 0.3261 0.8337 1.00000 0.05 0.21 1.19 H26C 1.22 H26B 1.40 C26 1.92 H3 Q7 1 0.6834 0.2582 0.4348 1.00000 0.05 0.21 1.51 H27B 1.57 H24 1.84 O1A 2.19 C27 Q8 1 -0.0047 0.0338 0.2829 1.00000 0.05 0.20 2.04 H2O 2.19 H23 2.31 H25 2.32 N23 Q9 1 0.1934 0.4471 -0.0569 1.00000 0.05 0.20 0.79 H3 1.62 C3 2.17 C4 2.22 O4B Q10 1 -0.1845 0.1144 0.6438 1.00000 0.05 0.20 1.21 H25 1.92 H3O 2.01 C25 2.13 H27C Shortest distances between peaks (including symmetry equivalents) 3 9 0.92 6 9 1.45 3 6 1.84 2 4 1.91 1 2 1.99 2 3 2.04 1 3 2.12 5 8 2.19 2 4 2.21 6 8 2.24 5 10 2.34 7 10 2.40 3 4 2.41 1 9 2.45 5 7 2.45 2 6 2.53 8 9 2.53 1 4 2.71 3 8 2.78 2 9 2.84 4 9 2.93 2 3 2.93 Time profile in seconds ----------------------- 0.09: 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. 0.36: 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 0.23: Structure factors and derivatives 0.25: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0031p21 finished at 16:34:27 Total CPU time: 1.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++