+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0005cc started at 15:18:01 on 21-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0005cc in Cc CELL 0.71073 5.3007 19.3739 10.0780 90.000 94.012 90.000 ZERR 4.00 0.0004 0.0020 0.0009 0.000 0.006 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC C H N O UNIT 32 56 8 20 V = 1032.43 F(000) = 464.0 Mu = 0.12 mm-1 Cell Wt = 872.85 Rho = 1.404 MERG 4 OMIT -3.00 55.00 OMIT 1 3 1 OMIT 0 2 -1 EXTI 0.00675 SHEL 7 0.77 EQIV_$1 x, y, z+1 HTAB O1B O22_$1 EQIV_$2 x+1, y, z HTAB O5B O22_$2 EQIV_$3 x-1, y, z HTAB N21 O5A_$3 EQIV_$4 x, y, z-1 HTAB N23 O1A_$4 FMAP 2 PLAN 10 SIZE 0.09 0.20 0.25 ACTA BOND $H WGHT 0.06510 0.32370 L.S. 4 TEMP -153.00 FVAR 0.74580 MOLE 1 C1 1 -0.405949 0.408225 1.000098 11.00000 0.02439 0.02811 = 0.02412 -0.00294 0.00096 -0.00246 C2 1 -0.391053 0.442259 0.867020 11.00000 0.02705 0.02615 = 0.01960 -0.00004 0.00189 -0.00030 AFIX 23 H2A 2 -0.366273 0.492532 0.879794 11.00000 -1.20000 H2B 2 -0.552579 0.435225 0.813279 11.00000 -1.20000 AFIX 0 C3 1 -0.173891 0.413056 0.791995 11.00000 0.02706 0.02892 = 0.02469 0.00180 0.00335 0.00345 AFIX 23 H3A 2 -0.013377 0.419135 0.847101 11.00000 -1.20000 H3B 2 -0.200909 0.362929 0.778224 11.00000 -1.20000 AFIX 0 C4 1 -0.150332 0.447453 0.657952 11.00000 0.02654 0.02796 = 0.02342 0.00070 0.00375 0.00248 AFIX 23 H4A 2 -0.316029 0.445852 0.606222 11.00000 -1.20000 H4B 2 -0.103947 0.496543 0.671986 11.00000 -1.20000 AFIX 0 C5 1 0.045814 0.412794 0.579610 11.00000 0.02327 0.02472 = 0.02066 0.00125 0.00083 -0.00004 O1A 4 -0.262265 0.362682 1.040161 11.00000 0.04194 0.04281 = 0.02740 0.00831 0.00993 0.01522 O1B 4 -0.593111 0.431539 1.069102 11.00000 0.02935 0.03391 = 0.02554 0.00586 0.00724 0.00378 AFIX 147 H1 2 -0.590865 0.410887 1.142462 11.00000 -1.500 AFIX 0 O5A 4 0.194324 0.370007 0.627444 11.00000 0.03315 0.04586 = 0.02300 0.00500 0.00439 0.01308 O5B 4 0.041150 0.432960 0.453546 11.00000 0.03025 0.03646 = 0.02174 0.00461 0.00496 0.00599 AFIX 147 H5 2 0.167860 0.416996 0.418391 11.00000 -1.5000 AFIX 0 MOLE 2 C22 1 -0.448994 0.330059 0.359047 11.00000 0.02594 0.02587 = 0.02351 -0.00082 0.00118 -0.00091 C24 1 -0.128033 0.248813 0.368619 11.00000 0.02670 0.03017 = 0.02690 0.00245 0.00145 0.00462 AFIX 23 H24A 2 0.044571 0.268098 0.383580 11.00000 -1.20000 H24B 2 -0.117767 0.202374 0.328366 11.00000 -1.20000 AFIX 0 C25 1 -0.263546 0.246344 0.498805 11.00000 0.02828 0.02877 = 0.02929 0.00322 0.00004 0.00480 AFIX 23 H25A 2 -0.364007 0.203532 0.505018 11.00000 -1.20000 H25B 2 -0.141852 0.249849 0.577631 11.00000 -1.20000 AFIX 0 N21 3 -0.426843 0.307406 0.485574 11.00000 0.03569 0.03170 = 0.02467 0.00195 0.00335 0.00717 AFIX 43 H21 2 -0.500717 0.326719 0.551731 11.00000 -1.2000 AFIX 0 N23 3 -0.291757 0.294599 0.285338 11.00000 0.03423 0.03191 = 0.02489 -0.00001 0.00393 0.00876 AFIX 43 H23 2 -0.287733 0.298395 0.198498 11.00000 -1.2000 AFIX 0 O22 4 -0.597300 0.377269 0.315042 11.00000 0.02985 0.03321 = 0.02432 0.00363 0.00439 0.00694 HKLF 4 Covalent radii and connectivity table for 07skc0005cc in Cc C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C1 C3 C3 - C4 C2 C4 - C5 C3 C5 - O5A O5B C4 O1A - C1 O1B - C1 O5A - C5 O5B - C5 C22 - O22 N23 N21 C24 - N23 C25 C25 - N21 C24 N21 - C22 C25 N23 - C22 C24 O22 - C22 Operators for generating equivalent atoms: $1 x, y, z+1 $2 x+1, y, z $3 x-1, y, z $4 x, y, z-1 Floating origin restraints generated 8927 Reflections read, of which 148 rejected -6 =< h =< 6, -24 =< k =< 24, -13 =< l =< 13, Max. 2-theta = 54.90 0 Systematic absence violations 0 Inconsistent equivalents 1186 Unique reflections, of which 0 suppressed R(int) = 0.0563 R(sigma) = 0.0387 Friedel opposites merged Maximum memory for data reduction = 1740 / 13746 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 = 2137 / 175061 wR2 = 0.1115 before cycle 1 for 1186 data and 139 / 139 parameters GooF = S = 1.076; Restrained GooF = 1.075 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0651 * P )^2 + 0.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74475 0.00326 -0.323 OSF 2 0.00626 0.00425 -0.116 EXTI Mean shift/esd = 0.143 Maximum = -1.083 for U33 N23 Max. shift = 0.014 A for H1 Max. dU = 0.000 for C24 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2137 / 175061 wR2 = 0.1111 before cycle 2 for 1186 data and 139 / 139 parameters GooF = S = 1.073; Restrained GooF = 1.072 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0651 * P )^2 + 0.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74434 0.00324 -0.125 OSF 2 0.00605 0.00420 -0.050 EXTI Mean shift/esd = 0.044 Maximum = -0.250 for U33 N23 Max. shift = 0.006 A for H1 Max. dU = 0.000 for C24 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2137 / 175061 wR2 = 0.1110 before cycle 3 for 1186 data and 139 / 139 parameters GooF = S = 1.072; Restrained GooF = 1.071 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0651 * P )^2 + 0.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74432 0.00324 -0.006 OSF 2 0.00603 0.00419 -0.004 EXTI Mean shift/esd = 0.003 Maximum = 0.015 for U23 C2 Max. shift = 0.001 A for H1 Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2137 / 175061 wR2 = 0.1110 before cycle 4 for 1186 data and 139 / 139 parameters GooF = S = 1.072; Restrained GooF = 1.071 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0651 * P )^2 + 0.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74432 0.00324 0.000 OSF 2 0.00603 0.00419 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.009 for U33 N23 Max. shift = 0.000 A for H1 Max. dU = 0.000 for N23 Largest correlation matrix elements 0.544 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A -0.3662 0.4925 0.8798 23 0.990 0.000 C2 C1 C3 H2B -0.5526 0.4352 0.8133 23 0.990 0.000 C2 C1 C3 H3A -0.0135 0.4190 0.8470 23 0.990 0.000 C3 C4 C2 H3B -0.2013 0.3629 0.7780 23 0.990 0.000 C3 C4 C2 H4A -0.3158 0.4459 0.6061 23 0.990 0.000 C4 C5 C3 H4B -0.1036 0.4965 0.6719 23 0.990 0.000 C4 C5 C3 H1 -0.5933 0.4102 1.1416 147 0.840 0.000 O1B C1 H1 H5 0.1670 0.4167 0.4182 147 0.840 0.000 O5B C5 H5 H24A 0.0448 0.2680 0.3835 23 0.990 0.000 C24 N23 C25 H24B -0.1177 0.2023 0.3282 23 0.990 0.000 C24 N23 C25 H25A -0.3640 0.2035 0.5049 23 0.990 0.000 C25 N21 C24 H25B -0.1418 0.2498 0.5776 23 0.990 0.000 C25 N21 C24 H21 -0.5007 0.3267 0.5518 43 0.880 0.000 N21 C22 C25 H23 -0.2877 0.2985 0.1986 43 0.880 0.000 N23 C22 C24 07skc0005cc in Cc ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.40586 0.40824 1.00016 1.00000 0.02416 0.02806 0.02375 -0.00272 0.00105 -0.00240 0.02535 0.00528 0.00058 0.00015 0.00029 0.00000 0.00152 0.00161 0.00150 0.00126 0.00118 0.00131 0.00067 C2 -0.39103 0.44225 0.86701 1.00000 0.02687 0.02632 0.01923 -0.00008 0.00165 -0.00025 0.02414 0.00521 0.00057 0.00016 0.00030 0.00000 0.00161 0.00154 0.00144 0.00113 0.00117 0.00118 0.00065 H2A -0.36619 0.49252 0.87976 1.00000 0.02896 0.00000 0.00000 H2B -0.55263 0.43523 0.81333 1.00000 0.02896 0.00000 0.00000 C3 -0.17402 0.41304 0.79183 1.00000 0.02664 0.02874 0.02469 0.00226 0.00355 0.00355 0.02661 0.00605 0.00062 0.00017 0.00032 0.00000 0.00147 0.00149 0.00147 0.00120 0.00112 0.00127 0.00064 H3A -0.01348 0.41904 0.84695 1.00000 0.03193 0.00000 0.00000 H3B -0.20126 0.36293 0.77797 1.00000 0.03193 0.00000 0.00000 C4 -0.15015 0.44746 0.65785 1.00000 0.02642 0.02785 0.02345 0.00052 0.00399 0.00270 0.02580 0.00560 0.00058 0.00016 0.00032 0.00000 0.00156 0.00155 0.00145 0.00123 0.00117 0.00128 0.00065 H4A -0.31578 0.44592 0.60605 1.00000 0.03096 0.00000 0.00000 H4B -0.10356 0.49653 0.67194 1.00000 0.03096 0.00000 0.00000 C5 0.04573 0.41278 0.57970 1.00000 0.02308 0.02487 0.02031 0.00118 0.00096 0.00011 0.02278 0.00500 0.00053 0.00015 0.00029 0.00000 0.00151 0.00150 0.00139 0.00113 0.00110 0.00119 0.00063 O1A -0.26227 0.36267 1.04004 1.00000 0.04158 0.04279 0.02749 0.00836 0.00993 0.01499 0.03694 0.00467 0.00044 0.00013 0.00023 0.00000 0.00141 0.00138 0.00118 0.00098 0.00100 0.00110 0.00061 O1B -0.59305 0.43159 1.06914 1.00000 0.02938 0.03330 0.02582 0.00581 0.00739 0.00408 0.02925 0.00419 0.00041 0.00012 0.00022 0.00000 0.00120 0.00121 0.00114 0.00092 0.00087 0.00094 0.00053 H1 -0.59330 0.41020 1.14163 1.00000 0.04387 0.00000 0.00000 O5A 0.19422 0.36998 0.62748 1.00000 0.03315 0.04598 0.02293 0.00506 0.00432 0.01299 0.03391 0.00431 0.00041 0.00013 0.00023 0.00000 0.00127 0.00140 0.00105 0.00095 0.00090 0.00103 0.00058 O5B 0.04100 0.43294 0.45357 1.00000 0.02990 0.03617 0.02196 0.00433 0.00516 0.00606 0.02918 0.00402 0.00040 0.00012 0.00021 0.00000 0.00127 0.00122 0.00112 0.00092 0.00084 0.00096 0.00052 H5 0.16696 0.41666 0.41820 1.00000 0.04378 0.00000 0.00000 C22 -0.44884 0.33005 0.35903 1.00000 0.02552 0.02551 0.02378 -0.00073 0.00119 -0.00058 0.02496 0.00505 0.00054 0.00015 0.00029 0.00000 0.00152 0.00151 0.00149 0.00124 0.00111 0.00122 0.00064 C24 -0.12782 0.24876 0.36857 1.00000 0.02644 0.03001 0.02642 0.00209 0.00134 0.00442 0.02765 0.00601 0.00061 0.00017 0.00033 0.00000 0.00149 0.00164 0.00145 0.00127 0.00119 0.00129 0.00068 H24A 0.04482 0.26803 0.38353 1.00000 0.03318 0.00000 0.00000 H24B -0.11769 0.20234 0.32824 1.00000 0.03318 0.00000 0.00000 C25 -0.26346 0.24630 0.49877 1.00000 0.02835 0.02859 0.02887 0.00319 0.00040 0.00475 0.02868 0.00575 0.00060 0.00016 0.00033 0.00000 0.00159 0.00164 0.00153 0.00130 0.00121 0.00135 0.00069 H25A -0.36397 0.20349 0.50495 1.00000 0.03442 0.00000 0.00000 H25B -0.14179 0.24978 0.57761 1.00000 0.03442 0.00000 0.00000 N21 -0.42678 0.30739 0.48561 1.00000 0.03570 0.03135 0.02467 0.00170 0.00361 0.00774 0.03050 0.00495 0.00053 0.00014 0.00026 0.00000 0.00147 0.00137 0.00143 0.00110 0.00112 0.00121 0.00063 H21 -0.50065 0.32669 0.55177 1.00000 0.03660 0.00000 0.00000 N23 -0.29172 0.29463 0.28546 1.00000 0.03490 0.03235 0.02307 0.00018 0.00349 0.00867 0.03004 0.00502 0.00052 0.00014 0.00026 0.00000 0.00147 0.00140 0.00136 0.00104 0.00110 0.00118 0.00062 H23 -0.28772 0.29846 0.19863 1.00000 0.03604 0.00000 0.00000 O22 -0.59743 0.37720 0.31504 1.00000 0.02962 0.03332 0.02404 0.00378 0.00418 0.00694 0.02888 0.00399 0.00041 0.00011 0.00022 0.00000 0.00115 0.00120 0.00107 0.00091 0.00083 0.00096 0.00052 Final Structure Factor Calculation for 07skc0005cc in Cc Total number of l.s. parameters = 139 Maximum vector length = 511 Memory required = 2000 / 25046 wR2 = 0.1110 before cycle 5 for 1186 data and 2 / 139 parameters GooF = S = 1.072; Restrained GooF = 1.071 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0651 * P )^2 + 0.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0418 for 1005 Fo > 4sig(Fo) and 0.0556 for all 1186 data wR2 = 0.1110, GooF = S = 1.072, Restrained GooF = 1.071 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0299 0.0247 0.0215 C1 0.0270 0.0262 0.0192 C2 0.0323 0.0240 0.0235 C3 0.0303 0.0252 0.0219 C4 0.0252 0.0232 0.0200 C5 0.0602 0.0272 0.0234 O1A 0.0398 0.0271 0.0209 O1B 0.0547 0.0251 0.0219 O5A 0.0411 0.0263 0.0202 O5B 0.0261 0.0254 0.0233 C22 0.0332 0.0269 0.0229 C24 0.0335 0.0303 0.0223 C25 0.0417 0.0255 0.0243 N21 0.0424 0.0253 0.0224 N23 0.0396 0.0244 0.0227 O22 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.023 0.035 0.046 0.058 0.072 0.090 0.113 0.141 0.201 1.000 Number in group 122. 119. 122. 112. 121. 118. 119. 116. 118. 119. GooF 1.044 1.035 1.041 1.128 1.117 0.958 1.191 0.969 1.156 1.061 K 1.077 0.936 0.929 0.969 0.952 1.000 1.002 1.019 1.022 1.024 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.98 1.05 1.15 1.31 1.66 inf Number in group 120. 118. 123. 116. 119. 118. 116. 118. 119. 119. GooF 1.054 0.951 1.065 1.175 1.003 1.071 0.978 0.977 0.978 1.396 K 1.030 1.049 1.018 1.029 0.995 1.014 1.021 1.044 1.041 1.004 R1 0.166 0.111 0.125 0.095 0.063 0.045 0.034 0.033 0.030 0.028 Recommended weighting scheme: WGHT 0.0651 0.3364 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) 0 2 1 263.73 570.40 7.51 0.180 6.98 1 9 0 250.57 187.01 3.73 0.103 1.99 2 0 0 160.84 217.25 3.58 0.111 2.64 -5 7 6 106.25 159.68 3.15 0.095 0.88 -2 12 7 171.04 226.58 3.04 0.113 1.01 1 17 4 2.05 15.59 3.01 0.030 1.01 -2 8 3 268.63 212.75 2.97 0.110 1.61 5 15 2 22.31 43.70 2.90 0.050 0.80 -3 21 4 46.99 84.75 2.87 0.069 0.78 -3 3 5 -0.83 5.21 2.86 0.017 1.34 1 9 2 26.10 15.79 2.79 0.030 1.84 5 11 4 23.75 4.39 2.78 0.016 0.84 0 8 1 32.81 46.99 2.72 0.052 2.35 6 0 0 982.85 749.53 2.70 0.206 0.88 2 8 9 9.55 45.69 2.67 0.051 0.93 0 18 3 64.52 89.96 2.54 0.071 1.02 -1 15 9 3.35 28.75 2.53 0.040 0.84 -2 8 8 214.09 269.72 2.49 0.124 1.05 2 20 2 47.70 75.12 2.44 0.065 0.89 -3 7 9 26.73 41.99 2.43 0.049 0.92 3 15 8 38.46 76.34 2.38 0.066 0.79 1 1 0 1245.65 1484.26 2.34 0.290 5.10 -3 19 2 -7.84 12.56 2.33 0.027 0.87 3 13 6 4.56 21.56 2.27 0.035 0.92 -2 10 7 55.21 72.57 2.27 0.064 1.08 2 4 3 1192.64 1023.50 2.24 0.241 1.86 1 21 4 147.88 113.88 2.24 0.080 0.85 2 8 2 10424.77 8977.37 2.22 0.713 1.66 -1 17 2 37.76 53.77 2.21 0.055 1.09 -2 12 5 29.79 41.33 2.19 0.048 1.16 2 16 6 29.92 47.47 2.18 0.052 0.91 6 0 4 309.89 233.27 2.17 0.115 0.81 4 8 2 126.50 156.34 2.15 0.094 1.12 -5 1 6 20.34 29.67 2.13 0.041 0.92 4 2 2 90.47 111.07 2.12 0.079 1.25 -2 4 5 144.95 119.70 2.12 0.082 1.57 2 14 1 179.98 216.77 2.12 0.111 1.21 4 12 4 150.09 181.82 2.09 0.101 0.93 -2 10 10 11.23 31.22 2.08 0.042 0.86 0 6 4 208.14 175.59 2.08 0.100 1.98 -1 1 11 13.49 23.57 2.08 0.037 0.91 -4 12 6 15.94 27.48 2.06 0.039 0.89 -3 3 7 1290.92 1117.02 2.05 0.251 1.14 3 1 1 556.47 645.01 2.04 0.191 1.71 1 7 4 16.16 23.85 2.04 0.037 1.73 6 2 1 726.82 570.92 2.03 0.180 0.87 2 8 11 229.98 188.62 2.01 0.103 0.80 1 3 8 135.17 162.62 2.00 0.096 1.18 6 6 0 9.59 23.48 1.99 0.036 0.85 3 11 2 113.94 90.13 1.98 0.071 1.20 Bond lengths and angles C1 - Distance Angles O1A 1.2154 (0.0037) O1B 1.3301 (0.0039) 123.16 (0.28) C2 1.5020 (0.0041) 122.91 (0.27) 113.91 (0.26) C1 - O1A O1B C2 - Distance Angles C1 1.5020 (0.0041) C3 1.5295 (0.0043) 111.62 (0.25) H2A 0.9900 109.30 109.30 H2B 0.9900 109.30 109.30 107.95 C2 - C1 C3 H2A C3 - Distance Angles C4 1.5191 (0.0044) C2 1.5295 (0.0043) 112.96 (0.25) H3A 0.9900 108.99 108.99 H3B 0.9900 108.99 108.99 107.78 C3 - C4 C2 H3A C4 - Distance Angles C5 1.5048 (0.0042) C3 1.5191 (0.0044) 111.88 (0.25) H4A 0.9900 109.24 109.24 H4B 0.9900 109.24 109.24 107.92 C4 - C5 C3 H4A C5 - Distance Angles O5A 1.2190 (0.0036) O5B 1.3284 (0.0036) 123.13 (0.27) C4 1.5048 (0.0042) 123.17 (0.26) 113.71 (0.24) C5 - O5A O5B O1A - Distance Angles C1 1.2154 (0.0037) O1A - O1B - Distance Angles C1 1.3301 (0.0039) H1 0.8400 109.47 O1B - C1 O5A - Distance Angles C5 1.2190 (0.0036) O5A - O5B - Distance Angles C5 1.3284 (0.0036) H5 0.8400 109.47 O5B - C5 C22 - Distance Angles O22 1.2660 (0.0036) N23 1.3419 (0.0039) 124.79 (0.27) N21 1.3465 (0.0039) 125.29 (0.27) 109.91 (0.26) C22 - O22 N23 C24 - Distance Angles N23 1.4643 (0.0042) C25 1.5405 (0.0043) 102.26 (0.24) H24A 0.9900 111.32 111.32 H24B 0.9900 111.32 111.32 109.20 C24 - N23 C25 H24A C25 - Distance Angles N21 1.4668 (0.0039) C24 1.5405 (0.0043) 101.87 (0.24) H25A 0.9900 111.40 111.40 H25B 0.9900 111.40 111.40 109.26 C25 - N21 C24 H25A N21 - Distance Angles C22 1.3465 (0.0039) C25 1.4668 (0.0039) 111.12 (0.25) H21 0.8800 124.44 124.44 N21 - C22 C25 N23 - Distance Angles C22 1.3419 (0.0039) C24 1.4643 (0.0042) 111.14 (0.25) H23 0.8800 124.43 124.43 N23 - C22 C24 O22 - Distance Angles C22 1.2660 (0.0036) O22 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.86 2.694(3) 170.5 O1B-H1...O22_$1 0.84 1.85 2.676(3) 169.7 O5B-H5...O22_$2 0.88 2.02 2.820(3) 150.9 N21-H21...O5A_$3 0.88 2.04 2.817(3) 147.1 N23-H23...O1A_$4 FMAP and GRID set by program FMAP 2 1 15 GRID -4.167 -1 -2 4.167 1 2 R1 = 0.0556 for 1186 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.21 at 0.4529 0.1409 0.3361 [ 0.97 A from H3B ] Deepest hole -0.25 at 0.2066 0.2139 0.6905 [ 0.25 A from H23 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2430 / 23724 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0471 0.3591 0.8361 1.00000 0.05 0.21 0.97 H3B 1.18 H3A 1.31 C3 2.25 H25A Q2 1 -0.4266 0.4258 0.9280 1.00000 0.05 0.20 0.73 C2 0.80 C1 1.31 H2B 1.43 H2A Q3 1 -0.3029 0.4301 0.8359 1.00000 0.05 0.20 0.63 C2 0.90 C3 1.33 H2B 1.34 H2A Q4 1 -0.0953 0.3086 1.0899 1.00000 0.05 0.18 1.44 O1A 1.56 H23 1.56 H25A 2.30 C25 Q5 1 -0.5818 0.3171 0.5372 1.00000 0.05 0.18 0.48 H21 1.02 N21 1.85 O5A 1.99 C22 Q6 1 -0.3896 0.2542 0.6419 1.00000 0.05 0.18 1.51 H25B 1.64 C25 1.71 H25A 1.75 H21 Q7 1 0.1555 0.4393 0.2749 1.00000 0.05 0.18 1.51 H5 1.80 O22 1.94 O5B 2.04 H1 Q8 1 -0.1783 0.4316 0.6996 1.00000 0.05 0.17 0.55 C4 1.00 C3 1.18 H4A 1.35 H4B Q9 1 -0.2479 0.3202 0.2151 1.00000 0.05 0.17 0.49 H23 0.91 N23 1.87 C22 1.94 O1A Q10 1 -0.4493 0.4988 0.7059 1.00000 0.05 0.16 1.63 H4A 1.75 H2B 1.78 H2A 1.89 H4B Shortest distances between peaks (including symmetry equivalents) 2 3 1.18 4 9 1.56 3 8 1.56 4 6 1.69 5 6 1.87 1 3 1.93 8 10 1.94 3 10 1.99 1 8 2.05 4 5 2.49 6 9 2.53 7 10 2.55 1 2 2.61 2 10 2.64 2 8 2.73 1 4 2.77 Time profile in seconds ----------------------- 0.06: 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. 0.50: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.22: Structure factors and derivatives 0.16: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0005cc finished at 15:18:02 Total CPU time: 1.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++