+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0027pna21 started at 16:26:49 on 21-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0027pna21 in Pna2(1) CELL 0.71073 11.4966 18.7024 3.9535 90.000 90.000 90.000 ZERR 4.00 0.0019 0.0027 0.0005 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H N O UNIT 28 40 8 16 V = 850.06 F(000) = 392.0 Mu = 0.12 mm-1 Cell Wt = 744.68 Rho = 1.455 MERG 4 OMIT -3.00 55.00 SHEL 7 0.77 HTAB O1B O3A HTAB N21 O1A EQIV_$1 -x+3/2, y-1/2, z-3/2 HTAB N23 O3B_$1 FMAP 2 PLAN 10 SIZE 0.01 0.04 0.19 ACTA BOND $H WGHT 0.00000 1.86310 L.S. 4 TEMP -153.00 FVAR 0.89722 MOLE 1 C1 1 0.867197 0.349992 0.278666 11.00000 0.03192 0.02467 = 0.02787 -0.00514 0.00344 -0.00719 C2 1 0.905004 0.416272 0.473076 11.00000 0.02652 0.02222 = 0.02573 0.00062 0.00501 -0.00003 AFIX 23 H2A 2 0.947602 0.400251 0.677080 11.00000 -1.20000 H2B 2 0.960996 0.442829 0.330206 11.00000 -1.20000 AFIX 0 C3 1 0.811795 0.468131 0.585092 11.00000 0.03174 0.02130 = 0.03028 0.00532 0.00624 0.00332 O1A 4 0.940022 0.304328 0.207138 11.00000 0.03366 0.02370 = 0.04508 -0.00739 0.00254 0.00253 O1B 4 0.759406 0.345661 0.196276 11.00000 0.02950 0.02584 = 0.05659 -0.01275 -0.00551 0.00081 AFIX 147 H1 2 0.724436 0.382690 0.260445 11.00000 -1.50000 AFIX 0 O3A 4 0.706812 0.455129 0.482954 11.00000 0.02048 0.03179 = 0.04497 -0.00645 0.00011 -0.00018 O3B 4 0.838263 0.520020 0.759958 11.00000 0.03490 0.02859 = 0.05033 -0.01782 -0.00122 0.00202 MOLE 2 C22 1 0.805973 0.160180 -0.285970 11.00000 0.02922 0.02249 = 0.02880 0.00226 -0.00062 -0.00516 C24 1 0.947761 0.086919 -0.433687 11.00000 0.03558 0.02134 = 0.03426 -0.00107 0.00372 -0.00001 AFIX 43 H24 2 0.988369 0.047616 -0.529751 11.00000 -1.20000 AFIX 0 C25 1 0.994209 0.140557 -0.255921 11.00000 0.02347 0.02711 = 0.02879 0.00180 -0.00159 0.00168 AFIX 43 H25 2 1.074090 0.146430 -0.201060 11.00000 -1.20000 AFIX 0 C26 1 0.690030 0.191628 -0.238826 11.00000 0.03370 0.02823 = 0.04465 0.00017 -0.00411 0.00470 AFIX 137 H26A 2 0.697762 0.239279 -0.138193 11.00000 -1.50000 H26B 2 0.644003 0.161052 -0.088457 11.00000 -1.50000 H26C 2 0.650966 0.195534 -0.458371 11.00000 -1.50000 AFIX 0 N21 3 0.904842 0.185665 -0.167207 11.00000 0.02487 0.02224 = 0.02761 -0.00684 -0.00012 -0.00180 AFIX 43 H21 2 0.912423 0.225338 -0.049577 11.00000 -1.20000 AFIX 0 N23 3 0.829942 0.099404 -0.451232 11.00000 0.02806 0.01864 = 0.03329 -0.00330 -0.00400 -0.00482 AFIX 43 H23 2 0.778775 0.071981 -0.554074 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 07skc0027pna21 in Pna2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C3 C1 C3 - O3B O3A C2 O1A - C1 O1B - C1 O3A - C3 O3B - C3 C22 - N21 N23 C26 C24 - C25 N23 C25 - C24 N21 C26 - C22 N21 - C22 C25 N23 - C22 C24 Operators for generating equivalent atoms: $1 -x+3/2, y-1/2, z-3/2 Floating origin restraints generated h k l Fo^2 Sigma Why rejected 11 0 3 83.66 20.21 observed but should be systematically absent 5732 Reflections read, of which 291 rejected -14 =< h =< 14, -24 =< k =< 23, -4 =< l =< 5, Max. 2-theta = 54.90 1 Systematic absence violations 0 Inconsistent equivalents 1107 Unique reflections, of which 0 suppressed R(int) = 0.0767 R(sigma) = 0.0764 Friedel opposites merged Maximum memory for data reduction = 1413 / 10808 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 = 1749 / 153135 wR2 = 0.1429 before cycle 1 for 1107 data and 120 / 120 parameters GooF = S = 1.163; Restrained GooF = 1.162 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.89722 0.00329 0.000 OSF Mean shift/esd = 0.003 Maximum = -0.010 for U12 C24 Max. shift = 0.000 A for H26A Max. dU = 0.000 for O3A Least-squares cycle 2 Maximum vector length = 511 Memory required = 1749 / 153135 wR2 = 0.1429 before cycle 2 for 1107 data and 120 / 120 parameters GooF = S = 1.163; Restrained GooF = 1.162 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.89722 0.00329 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.003 for U13 C1 Max. shift = 0.000 A for H26B Max. dU = 0.000 for O3A Least-squares cycle 3 Maximum vector length = 511 Memory required = 1749 / 153135 wR2 = 0.1429 before cycle 3 for 1107 data and 120 / 120 parameters GooF = S = 1.163; Restrained GooF = 1.162 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.89721 0.00329 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H26A Max. shift = 0.000 A for H26B Max. dU = 0.000 for O3A Least-squares cycle 4 Maximum vector length = 511 Memory required = 1749 / 153135 wR2 = 0.1429 before cycle 4 for 1107 data and 120 / 120 parameters GooF = S = 1.163; Restrained GooF = 1.162 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.89721 0.00329 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H26A Max. shift = 0.000 A for H26B Max. dU = 0.000 for N21 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 H2A 0.9476 0.4003 0.6771 23 0.990 0.000 C2 C3 C1 H2B 0.9610 0.4428 0.3302 23 0.990 0.000 C2 C3 C1 H1 0.7244 0.3827 0.2605 147 0.840 0.000 O1B C1 H1 H24 0.9884 0.0476 -0.5297 43 0.950 0.000 C24 C25 N23 H25 1.0741 0.1464 -0.2011 43 0.950 0.000 C25 C24 N21 H26A 0.6978 0.2393 -0.1381 137 0.980 0.000 C26 C22 H26A H26B 0.6440 0.1610 -0.0885 137 0.980 0.000 C26 C22 H26A H26C 0.6510 0.1955 -0.4584 137 0.980 0.000 C26 C22 H26A H21 0.9124 0.2253 -0.0496 43 0.880 0.000 N21 C22 C25 H23 0.7788 0.0720 -0.5541 43 0.880 0.000 N23 C22 C24 07skc0027pna21 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.86720 0.34999 0.27866 1.00000 0.03193 0.02466 0.02787 -0.00517 0.00348 -0.00719 0.02815 0.01044 0.00055 0.00029 0.00167 0.00000 0.00328 0.00279 0.00411 0.00300 0.00316 0.00243 0.00147 C2 0.90500 0.41627 0.47308 1.00000 0.02655 0.02223 0.02572 0.00062 0.00502 -0.00003 0.02483 0.01022 0.00051 0.00028 0.00165 0.00000 0.00310 0.00271 0.00365 0.00257 0.00297 0.00239 0.00138 H2A 0.94760 0.40025 0.67708 1.00000 0.02980 0.00000 0.00000 H2B 0.96099 0.44283 0.33021 1.00000 0.02980 0.00000 0.00000 C3 0.81179 0.46813 0.58510 1.00000 0.03176 0.02129 0.03028 0.00529 0.00624 0.00332 0.02778 0.01124 0.00053 0.00028 0.00167 0.00000 0.00355 0.00267 0.00393 0.00289 0.00301 0.00260 0.00150 O1A 0.94002 0.30433 0.20714 1.00000 0.03366 0.02372 0.04508 -0.00739 0.00255 0.00253 0.03416 0.00759 0.00035 0.00020 0.00132 0.00000 0.00225 0.00191 0.00300 0.00223 0.00250 0.00181 0.00109 O1B 0.75941 0.34566 0.19628 1.00000 0.02949 0.02584 0.05661 -0.01277 -0.00550 0.00079 0.03731 0.00730 0.00035 0.00020 0.00142 0.00000 0.00238 0.00208 0.00332 0.00251 0.00255 0.00174 0.00120 H1 0.72443 0.38269 0.26051 1.00000 0.05597 0.00000 0.00000 O3A 0.70681 0.45513 0.48295 1.00000 0.02047 0.03179 0.04494 -0.00646 0.00013 -0.00017 0.03240 0.00727 0.00033 0.00020 0.00123 0.00000 0.00214 0.00216 0.00293 0.00222 0.00230 0.00179 0.00109 O3B 0.83826 0.52002 0.75995 1.00000 0.03488 0.02860 0.05033 -0.01783 -0.00122 0.00203 0.03793 0.00763 0.00036 0.00021 0.00139 0.00000 0.00247 0.00209 0.00320 0.00244 0.00273 0.00177 0.00120 C22 0.80597 0.16018 -0.28596 1.00000 0.02921 0.02250 0.02881 0.00226 -0.00058 -0.00516 0.02684 0.01080 0.00050 0.00028 0.00190 0.00000 0.00318 0.00249 0.00355 0.00287 0.00333 0.00246 0.00136 C24 0.94776 0.08692 -0.43368 1.00000 0.03558 0.02134 0.03424 -0.00107 0.00370 -0.00004 0.03039 0.01059 0.00054 0.00029 0.00175 0.00000 0.00360 0.00282 0.00390 0.00298 0.00330 0.00259 0.00153 H24 0.98837 0.04762 -0.52974 1.00000 0.03646 0.00000 0.00000 C25 0.99421 0.14056 -0.25593 1.00000 0.02348 0.02711 0.02876 0.00180 -0.00160 0.00168 0.02645 0.01036 0.00050 0.00027 0.00172 0.00000 0.00294 0.00267 0.00364 0.00303 0.00313 0.00231 0.00132 H25 1.07409 0.14643 -0.20107 1.00000 0.03174 0.00000 0.00000 C26 0.69003 0.19162 -0.23883 1.00000 0.03372 0.02822 0.04464 0.00016 -0.00413 0.00471 0.03553 0.01118 0.00052 0.00030 0.00189 0.00000 0.00351 0.00292 0.00475 0.00375 0.00359 0.00267 0.00167 H26A 0.69776 0.23927 -0.13811 1.00000 0.05329 0.00000 0.00000 H26B 0.64399 0.16104 -0.08853 1.00000 0.05329 0.00000 0.00000 H26C 0.65098 0.19555 -0.45839 1.00000 0.05329 0.00000 0.00000 N21 0.90484 0.18567 -0.16721 1.00000 0.02487 0.02224 0.02759 -0.00681 -0.00012 -0.00180 0.02490 0.00791 0.00040 0.00023 0.00123 0.00000 0.00270 0.00232 0.00325 0.00225 0.00235 0.00211 0.00122 H21 0.91243 0.22534 -0.04959 1.00000 0.02988 0.00000 0.00000 N23 0.82994 0.09940 -0.45123 1.00000 0.02805 0.01863 0.03328 -0.00330 -0.00400 -0.00482 0.02666 0.00861 0.00042 0.00022 0.00144 0.00000 0.00266 0.00207 0.00311 0.00241 0.00247 0.00208 0.00117 H23 0.77877 0.07198 -0.55408 1.00000 0.03199 0.00000 0.00000 Final Structure Factor Calculation for 07skc0027pna21 in Pna2(1) Total number of l.s. parameters = 120 Maximum vector length = 511 Memory required = 1631 / 25046 wR2 = 0.1429 before cycle 5 for 1107 data and 2 / 120 parameters GooF = S = 1.163; Restrained GooF = 1.162 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0802 for 779 Fo > 4sig(Fo) and 0.1277 for all 1107 data wR2 = 0.1429, GooF = S = 1.163, Restrained GooF = 1.162 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0393 0.0259 0.0193 C1 0.0312 0.0224 0.0209 C2 0.0393 0.0252 0.0188 C3 0.0476 0.0342 0.0206 O1A 0.0621 0.0287 0.0211 O1B 0.0476 0.0292 0.0205 O3A 0.0605 0.0348 0.0185 O3B 0.0327 0.0284 0.0194 C22 0.0387 0.0312 0.0212 C24 0.0299 0.0273 0.0221 C25 0.0461 0.0352 0.0253 C26 0.0323 0.0251 0.0173 N21 0.0355 0.0291 0.0154 N23 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.028 0.038 0.047 0.057 0.068 0.087 0.115 0.166 1.000 Number in group 113. 112. 109. 112. 115. 107. 107. 110. 113. 109. GooF 1.206 1.409 1.276 1.257 1.159 1.173 1.083 1.008 0.922 1.051 K 2.918 1.819 1.230 1.089 1.008 0.988 1.044 1.006 0.992 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.06 1.18 1.35 1.73 inf Number in group 113. 112. 109. 113. 106. 112. 111. 110. 110. 111. GooF 1.284 1.255 1.396 1.222 1.185 1.174 1.038 1.002 0.981 1.012 K 1.201 1.261 1.148 1.063 0.987 1.007 1.006 0.972 1.025 1.000 R1 0.359 0.359 0.274 0.181 0.161 0.111 0.082 0.074 0.047 0.027 Recommended weighting scheme: WGHT 0.0000 1.8664 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) 12 8 1 44.08 1.90 3.35 0.013 0.87 0 4 0 2605.05 2925.87 3.24 0.497 4.68 13 6 1 41.71 7.73 3.14 0.026 0.83 7 13 3 0.17 40.36 3.01 0.058 0.84 2 1 5 67.31 3.62 2.95 0.018 0.78 11 5 1 -7.28 14.51 2.78 0.035 0.98 3 1 5 109.83 16.08 2.76 0.037 0.77 0 22 0 70.04 7.94 2.71 0.026 0.85 6 4 4 70.71 7.67 2.61 0.025 0.86 8 11 1 115.00 164.59 2.55 0.118 1.06 10 12 1 2.71 36.38 2.54 0.055 0.90 9 3 1 12.47 38.46 2.54 0.057 1.19 7 20 1 39.25 5.28 2.53 0.021 0.80 4 5 0 1370.55 1161.07 2.52 0.313 2.28 11 11 0 -17.45 19.22 2.47 0.040 0.89 0 6 2 5101.05 4732.91 2.47 0.633 1.67 8 20 0 34.29 0.00 2.47 0.000 0.78 0 23 1 54.86 17.71 2.47 0.039 0.80 14 4 1 43.25 7.16 2.45 0.025 0.79 6 17 2 50.07 18.03 2.43 0.039 0.86 10 1 3 216.05 146.87 2.42 0.111 0.87 3 1 4 -26.74 22.73 2.42 0.044 0.96 5 10 0 -5.49 14.08 2.40 0.035 1.45 5 1 4 224.41 145.03 2.37 0.111 0.91 2 18 2 -10.05 9.53 2.37 0.028 0.91 13 8 0 100.30 23.63 2.35 0.045 0.83 3 13 3 6.22 34.63 2.35 0.054 0.94 2 19 2 40.31 14.92 2.35 0.036 0.87 12 4 1 73.48 33.31 2.34 0.053 0.91 7 16 1 68.41 34.37 2.32 0.054 0.93 7 8 3 30.19 5.44 2.30 0.021 0.94 8 1 1 112.98 159.17 2.28 0.116 1.35 5 19 2 38.24 13.18 2.27 0.033 0.82 3 20 0 50.58 12.61 2.27 0.033 0.91 2 4 4 49.64 21.67 2.22 0.043 0.95 9 4 3 -12.39 36.30 2.21 0.055 0.90 1 18 1 73.94 42.80 2.14 0.060 1.00 9 7 2 33.53 9.96 2.13 0.029 1.00 4 18 0 -3.77 26.73 2.12 0.048 0.98 12 11 1 30.60 5.00 2.12 0.021 0.82 3 2 5 49.88 2.03 2.11 0.013 0.77 12 10 2 16.87 50.33 2.11 0.065 0.78 4 4 3 19.31 2.88 2.11 0.016 1.16 2 23 1 -0.64 22.01 2.10 0.043 0.79 4 9 0 1260.57 1128.47 2.10 0.309 1.68 12 11 0 35.02 0.21 2.10 0.004 0.83 3 16 3 23.16 0.95 2.08 0.009 0.85 4 11 4 30.94 77.37 2.07 0.081 0.82 3 10 4 26.82 54.06 2.06 0.068 0.85 8 16 1 20.37 50.32 2.06 0.065 0.88 Bond lengths and angles C1 - Distance Angles O1A 1.2289 (0.0067) O1B 1.2839 (0.0070) 123.74 (0.55) C2 1.5220 (0.0077) 119.19 (0.55) 117.07 (0.51) C1 - O1A O1B C2 - Distance Angles C3 1.5116 (0.0076) C1 1.5220 (0.0077) 117.91 (0.52) H2A 0.9900 107.83 107.83 H2B 0.9900 107.83 107.83 107.16 C2 - C3 C1 H2A C3 - Distance Angles O3B 1.2298 (0.0069) O3A 1.2957 (0.0073) 123.63 (0.54) C2 1.5116 (0.0076) 119.71 (0.56) 116.65 (0.52) C3 - O3B O3A O1A - Distance Angles C1 1.2289 (0.0067) O1A - O1B - Distance Angles C1 1.2839 (0.0070) H1 0.8400 109.47 O1B - C1 O3A - Distance Angles C3 1.2957 (0.0073) O3A - O3B - Distance Angles C3 1.2298 (0.0069) O3B - C22 - Distance Angles N21 1.3189 (0.0072) N23 1.3397 (0.0072) 107.64 (0.50) C26 1.4688 (0.0079) 126.32 (0.54) 126.03 (0.55) C22 - N21 N23 C24 - Distance Angles C25 1.3361 (0.0078) N23 1.3763 (0.0076) 107.00 (0.53) H24 0.9500 126.50 126.50 C24 - C25 N23 C25 - Distance Angles C24 1.3361 (0.0078) N21 1.3748 (0.0069) 107.23 (0.52) H25 0.9500 126.38 126.38 C25 - C24 N21 C26 - Distance Angles C22 1.4688 (0.0079) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C22 H26A H26B N21 - Distance Angles C22 1.3189 (0.0072) C25 1.3748 (0.0069) 109.35 (0.47) H21 0.8800 125.32 125.32 N21 - C22 C25 N23 - Distance Angles C22 1.3397 (0.0072) C24 1.3763 (0.0076) 108.77 (0.51) H23 0.8800 125.62 125.62 N23 - C22 C24 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.63 2.417(6) 155.4 O1B-H1...O3A 0.88 1.82 2.698(6) 175.0 N21-H21...O1A 0.88 1.82 2.692(6) 174.0 N23-H23...O3B_$1 FMAP and GRID set by program FMAP 2 3 12 GRID -5.556 -2 24 5.556 2 1 R1 = 0.1277 for 1107 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.33 at 0.7589 0.2939 0.2656 [ 1.01 A from O1B ] Deepest hole -0.34 at 0.1798 0.5719 0.2253 [ 0.94 A from C3 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 2158 / 21984 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7589 0.2939 0.2656 1.00000 0.05 0.33 1.01 O1B 1.63 C1 1.71 H1 2.02 H26A Q2 1 0.7765 0.5282 0.6007 1.00000 0.05 0.29 0.96 O3B 1.20 C3 1.65 O3A 1.71 H23 Q3 1 0.7025 0.4267 0.2139 1.00000 0.05 0.29 0.88 H1 1.19 O3A 1.65 O1B 2.08 C3 Q4 1 0.8256 0.2033 -0.2641 1.00000 0.05 0.26 0.84 C22 1.04 N21 1.37 H21 1.58 C26 Q5 1 0.8767 0.2738 -0.0840 1.00000 0.05 0.25 1.00 H21 1.48 O1A 1.71 N21 2.02 C1 Q6 1 1.0300 0.0310 -0.2872 1.00000 0.05 0.25 1.12 H24 1.52 C24 1.80 H24 2.09 C25 Q7 1 0.8545 0.5688 0.7431 1.00000 0.05 0.24 0.93 O3B 1.73 H23 2.04 C3 2.16 H2B Q8 1 0.6672 0.0747 -0.2789 1.00000 0.05 0.24 1.68 H23 1.80 H26B 2.04 N23 2.09 O3B Q9 1 1.0508 0.0183 -0.3078 1.00000 0.05 0.24 1.26 H24 1.71 H24 1.82 C24 2.04 O3A Q10 1 1.0421 0.1179 -0.0382 1.00000 0.05 0.24 0.91 H25 1.11 C25 1.99 C24 2.09 N21 Shortest distances between peaks (including symmetry equivalents) 6 9 0.35 2 7 1.30 4 5 1.61 2 8 1.85 6 10 1.91 7 8 1.91 1 5 1.97 9 10 2.15 3 10 2.26 6 9 2.30 6 6 2.39 9 9 2.40 1 3 2.58 2 3 2.58 1 4 2.63 2 9 2.76 3 9 2.77 3 6 2.91 9 10 2.91 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. 0.27: 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 0.20: Structure factors and derivatives 0.14: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.05: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0027pna21 finished at 16:26:49 Total CPU time: 0.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++