+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005slh1124 started at 16:42:36 on 20-Oct-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005slh112 in Pnnm CELL 0.71073 11.3361 11.3717 8.3386 90.000 90.000 90.000 ZERR 2.00 0.0002 0.0003 0.0002 0.000 0.000 0.000 LATT 1 SYMM - X, - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, 1/2 - Z SFAC C H N O P S CO UNIT 28 40 4 8 4 8 2 V = 1074.94 F(000) = 542.0 Mu = 1.36 mm-1 Cell Wt = 1058.86 Rho = 1.636 MERG 2 OMIT -3.00 55.00 OMIT 2 0 0 OMIT 1 0 1 OMIT 0 1 1 OMIT 0 0 6 OMIT 0 0 2 OMIT 0 3 1 OMIT 4 0 0 OMIT 1 3 2 OMIT 0 3 3 DFIX 0.98 0.01 C1 H1A DFIX 0.98 0.01 C1 H1B DFIX 0.98 0.01 C2 H2A DFIX 0.98 0.01 C2 H2B FMAP 2 PLAN 5 SIZE 0.06 0.08 0.20 ACTA BOND $H L.S. 6 TEMP -153.00 WGHT 0.031900 0.477500 FVAR 0.81946 C1 1 0.758912 0.207197 0.000000 10.50000 0.01524 0.02220 = 0.02739 0.00000 0.00000 0.00325 AFIX 2 H1A 2 0.770193 0.252747 0.096201 11.00000 -1.50000 H1B 2 0.815263 0.148511 0.000000 10.50000 -1.50000 AFIX 0 C2 1 0.313523 0.157728 0.000000 10.50000 0.01577 0.02198 = 0.02900 0.00000 0.00000 -0.00435 AFIX 2 H2A 2 0.293184 0.201752 0.094086 11.00000 -1.50000 H2B 2 0.271544 0.083971 0.000000 10.50000 -1.50000 AFIX 0 C3 1 0.250959 0.481185 0.137237 11.00000 0.01102 0.01989 = 0.01362 0.00192 -0.00122 -0.00030 AFIX 43 H3 2 0.293052 0.476909 0.235578 11.00000 -1.20000 AFIX 0 C4 1 0.129128 0.487997 0.142828 11.00000 0.01092 0.02186 = 0.01320 0.00247 0.00143 -0.00012 AFIX 43 H4 2 0.089371 0.488542 0.243117 11.00000 -1.20000 AFIX 0 C5 1 0.065023 0.494064 0.000000 10.50000 0.01077 0.01091 = 0.01487 0.00000 0.00000 -0.00138 N1 3 0.312530 0.480319 0.000000 10.50000 0.00788 0.01478 = 0.01497 0.00000 0.00000 -0.00049 O1 4 0.644089 0.152391 0.000000 10.50000 0.01641 0.01391 = 0.02092 0.00000 0.00000 0.00271 O2 4 0.438022 0.129938 0.000000 10.50000 0.01684 0.01390 = 0.02437 0.00000 0.00000 -0.00257 P1 5 0.530280 0.235242 0.000000 10.50000 0.01250 0.01154 = 0.01455 0.00000 0.00000 0.00019 S1 6 0.519293 0.331952 0.197486 11.00000 0.01457 0.01545 = 0.01248 0.00020 0.00046 0.00094 CO1 7 0.500000 0.500000 0.000000 10.25000 0.00666 0.01199 = 0.01244 0.00000 0.00000 0.00034 HKLF 4 Covalent radii and connectivity table for 2005slh112 in Pnnm C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 S 1.030 CO 1.250 C1 - O1 C2 - O2 C3 - N1 C4 C4 - C3 C5 C5 - C4 C4_$1 C5_$2 N1 - C3 C3_$1 Co1 O1 - C1 P1 O2 - C2 P1 P1 - O2 O1 S1 S1_$1 S1 - P1 Co1 Co1 - N1_$3 N1 S1_$1 S1 S1_$4 S1_$3 Operators for generating equivalent atoms: $1 x, y, -z $2 -x, -y+1, -z $3 -x+1, -y+1, -z $4 -x+1, -y+1, z h k l Fo^2 Sigma Why rejected 7 0 0 15.59 3.86 observed but should be systematically absent 13 0 0 9.42 2.32 observed but should be systematically absent 12762 Reflections read, of which 713 rejected -13 =< h =< 14, -14 =< k =< 14, -10 =< l =< 10, Max. 2-theta = 55.00 2 Systematic absence violations 0 Inconsistent equivalents 1309 Unique reflections, of which 0 suppressed R(int) = 0.0315 R(sigma) = 0.0205 Friedel opposites merged Maximum memory for data reduction = 1366 / 12800 Special position constraints for C1 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for H1B z = 0.0000 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C2 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for H2B z = 0.0000 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C5 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for N1 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O1 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O2 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for P1 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Co1 x = 0.5000 y = 0.5000 z = 0.0000 U23 = 0 U13 = 0 sof = 0.25000 Input constraints retained (at least in part) for sof 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 = 1591 / 115647 wR2 = 0.0583 before cycle 1 for 1309 data and 84 / 84 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.9238 0.9800 -0.0562 0.0100 DFIX C1 H1B Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.077; Restrained GooF = 1.092 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0319 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.81960 0.00156 0.088 OSF Mean shift/esd = 0.104 Maximum = 1.346 for x H1B Max. shift = 0.036 A for H1B Max. dU = 0.000 for O1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1591 / 115647 wR2 = 0.0584 before cycle 2 for 1309 data and 84 / 84 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.078; Restrained GooF = 1.079 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0319 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.81962 0.00154 0.016 OSF Mean shift/esd = 0.034 Maximum = 0.475 for x H1B Max. shift = 0.012 A for H1B Max. dU = 0.000 for O1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1591 / 115647 wR2 = 0.0585 before cycle 3 for 1309 data and 84 / 84 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0319 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.81962 0.00154 -0.002 OSF Mean shift/esd = 0.002 Maximum = -0.012 for y C5 Max. shift = 0.000 A for H1B Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1591 / 115647 wR2 = 0.0584 before cycle 4 for 1309 data and 84 / 84 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0319 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.81962 0.00154 -0.002 OSF Mean shift/esd = 0.001 Maximum = 0.007 for y H1B Max. shift = 0.000 A for H1B Max. dU = 0.000 for C1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1591 / 115647 wR2 = 0.0584 before cycle 5 for 1309 data and 84 / 84 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0319 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.81962 0.00154 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y H2B Max. shift = 0.000 A for H2B Max. dU = 0.000 for C1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1591 / 115647 wR2 = 0.0584 before cycle 6 for 1309 data and 84 / 84 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0319 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.81962 0.00154 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for x S1 Max. shift = 0.000 A for H2B Max. dU = 0.000 for C3 Largest correlation matrix elements 0.726 y H1B / x H1B 0.521 U11 Co1 / OSF -0.686 y H2B / x H2B 0.503 U11 S1 / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.2931 0.4769 0.2356 43 0.950 0.000 C3 N1 C4 H4 0.0894 0.4886 0.2431 43 0.950 0.000 C4 C3 C5 2005slh112 in Pnnm ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.75895 0.20718 0.00000 0.50000 0.01521 0.02227 0.02732 0.00000 0.00000 0.00297 0.02160 0.00280 0.00017 0.00017 0.00000 0.00000 0.00087 0.00091 0.00095 0.00000 0.00000 0.00072 0.00038 H1A 0.77027 0.25337 0.09716 1.00000 0.03240 0.02074 0.00161 0.00130 0.00141 0.00000 0.00000 H1B 0.81841 0.14569 0.00000 0.50000 0.03240 0.03504 0.00169 0.00163 0.00000 0.00000 0.00000 C2 0.31352 0.15773 0.00000 0.50000 0.01562 0.02197 0.02919 0.00000 0.00000 -0.00429 0.02226 0.00271 0.00017 0.00018 0.00000 0.00000 0.00091 0.00089 0.00103 0.00000 0.00000 0.00069 0.00040 H2A 0.29270 0.20306 0.09507 1.00000 0.03339 0.02574 0.00155 0.00134 0.00145 0.00000 0.00000 H2B 0.27027 0.08339 0.00000 0.50000 0.03339 0.01656 0.00201 0.00134 0.00000 0.00000 0.00000 C3 0.25096 0.48119 0.13723 1.00000 0.01101 0.01993 0.01359 0.00191 -0.00122 -0.00028 0.01484 0.00211 0.00011 0.00011 0.00015 0.00000 0.00055 0.00057 0.00059 0.00046 0.00047 0.00044 0.00025 H3 0.29306 0.47691 0.23556 1.00000 0.01781 0.00000 0.00000 C4 0.12913 0.48801 0.14284 1.00000 0.01092 0.02189 0.01321 0.00245 0.00141 -0.00012 0.01534 0.00216 0.00011 0.00010 0.00015 0.00000 0.00059 0.00060 0.00059 0.00045 0.00047 0.00043 0.00026 H4 0.08937 0.48856 0.24313 1.00000 0.01841 0.00000 0.00000 C5 0.06502 0.49406 0.00000 0.50000 0.01083 0.01090 0.01486 0.00000 0.00000 -0.00137 0.01219 0.00224 0.00015 0.00013 0.00000 0.00000 0.00085 0.00074 0.00080 0.00000 0.00000 0.00056 0.00033 N1 0.31252 0.48033 0.00000 0.50000 0.00788 0.01476 0.01499 0.00000 0.00000 -0.00047 0.01254 0.00201 0.00013 0.00013 0.00000 0.00000 0.00065 0.00063 0.00069 0.00000 0.00000 0.00051 0.00029 O1 0.64409 0.15238 0.00000 0.50000 0.01644 0.01391 0.02095 0.00000 0.00000 0.00269 0.01710 0.00180 0.00011 0.00011 0.00000 0.00000 0.00063 0.00055 0.00065 0.00000 0.00000 0.00047 0.00027 O2 0.43802 0.12994 0.00000 0.50000 0.01684 0.01394 0.02438 0.00000 0.00000 -0.00259 0.01839 0.00173 0.00012 0.00010 0.00000 0.00000 0.00066 0.00058 0.00065 0.00000 0.00000 0.00049 0.00027 P1 0.53028 0.23524 0.00000 0.50000 0.01251 0.01155 0.01455 0.00000 0.00000 0.00019 0.01287 0.00062 0.00004 0.00004 0.00000 0.00000 0.00023 0.00022 0.00022 0.00000 0.00000 0.00015 0.00012 S1 0.51929 0.33195 0.19749 1.00000 0.01459 0.01546 0.01249 0.00020 0.00046 0.00093 0.01418 0.00053 0.00003 0.00003 0.00004 0.00000 0.00018 0.00018 0.00017 0.00011 0.00010 0.00010 0.00011 Co1 0.50000 0.50000 0.00000 0.25000 0.00667 0.01199 0.01245 0.00000 0.00000 0.00035 0.01037 0.00000 0.00000 0.00000 0.00000 0.00000 0.00017 0.00018 0.00018 0.00000 0.00000 0.00010 0.00011 Final Structure Factor Calculation for 2005slh112 in Pnnm Total number of l.s. parameters = 84 Maximum vector length = 511 Memory required = 1507 / 26061 wR2 = 0.0584 before cycle 7 for 1309 data and 0 / 84 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0319 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0197 for 1264 Fo > 4sig(Fo) and 0.0206 for all 1309 data wR2 = 0.0584, GooF = S = 1.079, Restrained GooF = 1.078 for all data Occupancy sum of asymmetric unit = 6.75 for non-hydrogen and 5.00 for hydrogen atoms Principal mean square atomic displacements U 0.0273 0.0234 0.0141 C1 0.0292 0.0241 0.0135 C2 0.0205 0.0135 0.0105 C3 0.0225 0.0134 0.0101 C4 0.0149 0.0122 0.0095 C5 0.0150 0.0148 0.0079 N1 0.0209 0.0181 0.0122 O1 0.0244 0.0184 0.0124 O2 0.0146 0.0125 0.0115 P1 0.0161 0.0140 0.0124 S1 0.0124 0.0120 0.0066 Co1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.032 0.061 0.090 0.121 0.151 0.190 0.236 0.295 0.400 1.000 Number in group 131. 134. 131. 131. 129. 130. 130. 131. 130. 132. GooF 1.064 1.111 1.171 1.229 1.242 1.276 0.902 0.724 1.049 0.890 K 1.145 0.995 0.966 0.990 0.996 0.994 1.003 1.006 1.012 0.999 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.33 1.66 inf Number in group 138. 129. 128. 130. 133. 127. 133. 129. 130. 132. GooF 0.941 0.942 0.934 0.824 0.763 0.896 1.117 0.888 1.213 1.844 K 0.996 1.006 1.011 1.016 1.011 1.007 1.018 1.004 0.996 0.989 R1 0.027 0.028 0.023 0.021 0.017 0.017 0.019 0.014 0.017 0.025 Recommended weighting scheme: WGHT 0.0184 0.6708 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) 3 1 4 239.68 344.69 6.33 0.158 1.80 1 4 1 129.90 191.48 5.50 0.118 2.62 0 2 2 588.02 457.53 5.25 0.182 3.36 10 0 0 109.09 64.42 4.97 0.068 1.13 3 3 4 251.22 188.43 4.82 0.117 1.64 3 2 3 154.68 209.19 4.54 0.123 2.08 3 0 3 2442.77 2014.10 4.50 0.382 2.24 4 3 1 197.66 256.74 4.28 0.136 2.19 8 1 9 37.43 68.37 4.11 0.070 0.77 0 6 2 171.49 218.56 3.67 0.126 1.73 5 2 2 45.70 67.39 3.61 0.070 1.88 6 2 6 30.34 17.53 3.43 0.036 1.10 2 2 4 494.23 419.99 3.37 0.174 1.85 2 4 0 55.34 37.35 3.33 0.052 2.54 2 6 4 708.26 611.25 3.31 0.210 1.36 6 1 0 1109.01 1285.58 3.30 0.305 1.86 5 0 7 321.22 385.94 3.21 0.167 1.05 6 2 1 1390.77 1226.45 3.12 0.298 1.75 10 2 0 332.19 277.65 3.03 0.142 1.11 1 5 1 242.35 203.17 2.99 0.121 2.15 8 8 0 41.72 27.61 2.93 0.045 1.00 10 4 0 40.35 27.43 2.70 0.045 1.05 2 3 1 253.59 216.99 2.67 0.125 2.95 2 5 4 4.58 1.14 2.67 0.009 1.48 2 4 1 -0.73 1.65 2.61 0.011 2.43 13 3 2 21.28 32.90 2.57 0.049 0.83 0 9 1 175.23 148.22 2.42 0.104 1.25 1 2 5 1156.93 1276.29 2.39 0.304 1.58 1 13 1 140.84 169.63 2.36 0.111 0.87 5 2 7 1292.37 1426.47 2.36 0.321 1.04 2 3 5 489.51 547.46 2.33 0.199 1.47 2 6 5 161.21 137.24 2.33 0.100 1.22 1 3 6 365.63 324.62 2.27 0.153 1.30 3 4 5 353.86 398.11 2.27 0.170 1.34 3 9 6 331.06 288.15 2.27 0.144 0.91 1 5 6 401.98 450.25 2.25 0.180 1.18 1 7 3 9.03 4.53 2.23 0.018 1.39 3 5 4 75.91 92.70 2.23 0.082 1.42 10 1 2 6.22 2.81 2.22 0.014 1.09 14 0 0 33.87 20.67 2.21 0.039 0.81 1 5 2 11.01 6.25 2.21 0.021 1.97 5 1 8 204.41 235.90 2.16 0.131 0.94 7 11 3 31.00 42.61 2.16 0.056 0.83 1 2 4 -0.79 0.87 2.14 0.008 1.93 6 0 8 61.66 79.27 2.13 0.076 0.91 5 2 9 77.18 94.64 2.13 0.083 0.85 5 5 8 28.27 38.50 2.10 0.053 0.87 5 3 0 413.53 371.62 2.07 0.164 1.95 1 7 0 1633.53 1773.25 2.07 0.358 1.61 0 7 5 2982.37 2753.06 2.06 0.446 1.16 Bond lengths and angles C1 - Distance Angles O1 1.4435 (0.0023) H1A 0.9741 (0.0088) 110.59 (1.08) H1B 0.9712 (0.0096) 108.37 (1.49) 107.27 (1.27) C1 - O1 H1A C2 - Distance Angles O2 1.4462 (0.0024) H2A 0.9746 (0.0088) 110.60 (1.07) H2B 0.9773 (0.0096) 107.49 (1.52) 109.63 (1.29) C2 - O2 H2A C3 - Distance Angles N1 1.3403 (0.0014) C4 1.3841 (0.0018) 123.28 (0.12) H3 0.9500 118.36 118.36 C3 - N1 C4 C4 - Distance Angles C3 1.3841 (0.0018) C5 1.3970 (0.0015) 119.54 (0.12) H4 0.9500 120.23 120.23 C4 - C3 C5 C5 - Distance Angles C4 1.3970 (0.0015) C4_$1 1.3970 (0.0015) 116.99 (0.16) C5_$2 1.4803 (0.0034) 121.50 (0.08) 121.50 (0.08) C5 - C4 C4_$1 N1 - Distance Angles C3 1.3403 (0.0014) C3_$1 1.3403 (0.0014) 117.24 (0.15) Co1 2.1370 (0.0014) 121.13 (0.07) 121.13 (0.07) N1 - C3 C3_$1 O1 - Distance Angles C1 1.4435 (0.0023) P1 1.5977 (0.0013) 118.28 (0.11) O1 - C1 O2 - Distance Angles C2 1.4462 (0.0024) P1 1.5899 (0.0013) 118.52 (0.11) O2 - C2 P1 - Distance Angles O2 1.5899 (0.0013) O1 1.5977 (0.0013) 94.99 (0.07) S1 1.9841 (0.0004) 112.10 (0.03) 112.18 (0.03) S1_$1 1.9841 (0.0004) 112.10 (0.03) 112.18 (0.03) 112.19 (0.03) P1 - O2 O1 S1 S1 - Distance Angles P1 1.9841 (0.0004) Co1 2.5321 (0.0003) 83.34 (0.01) S1 - P1 Co1 - Distance Angles N1_$3 2.1370 (0.0014) N1 2.1370 (0.0014) 180.00 (0.01) S1_$1 2.5321 (0.0003) 89.60 (0.03) 90.40 (0.03) S1 2.5321 (0.0003) 89.60 (0.03) 90.40 (0.03) 81.14 (0.01) S1_$4 2.5321 (0.0003) 90.40 (0.03) 89.60 (0.03) 180.00 (0.02) 98.86 (0.01) S1_$3 2.5321 (0.0003) 90.40 (0.03) 89.60 (0.03) 98.86 (0.01) 180.00 81.14 (0.01) Co1 - N1_$3 N1 S1_$1 S1 S1_$4 FMAP and GRID set by program FMAP 2 3 12 GRID -2.778 -2 -1 2.778 2 1 R1 = 0.0203 for 1309 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.40 at 0.3666 0.4927 0.0000 [ 0.63 A from N1 ] Deepest hole -0.36 at 0.5057 0.2856 0.0000 [ 0.64 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 1794 / 16614 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3666 0.4927 0.0000 0.50000 0.05 0.40 0.63 N1 1.51 CO1 1.75 C3 2.14 H3 Q2 1 0.0988 0.4825 0.0700 1.00000 0.05 0.33 0.70 C4 0.71 C5 1.45 H4 1.81 C4 Q3 1 0.2803 0.4679 0.0620 1.00000 0.05 0.28 0.65 N1 0.73 C3 1.46 H3 1.70 C3 Q4 1 0.5205 0.2831 0.0943 1.00000 0.05 0.27 0.96 P1 1.02 S1 2.13 O2 2.19 O1 Q5 1 0.1865 0.4951 0.1311 1.00000 0.05 0.27 0.66 C4 0.75 C3 1.45 H4 1.50 H3 Shortest distances between peaks (including symmetry equivalents) 3 3 1.03 2 5 1.13 1 3 1.14 2 2 1.17 3 5 1.25 4 4 1.57 2 5 1.95 3 5 1.95 2 3 2.06 5 5 2.19 2 2 2.28 1 5 2.32 2 3 2.34 2 2 2.56 1 4 2.96 Time profile in seconds ----------------------- 0.05: 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. 0.64: 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 0.46: Structure factors and derivatives 0.13: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.05: Solve l.s. equations 0.00: Generate HTAB table 0.01: 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 +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005slh1124 finished at 16:42:38 Total CPU time: 1.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++