+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0061p21c started at 16:23:24 on 07-Sep-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0061p21c in P2(1)/c CELL 0.71073 10.7285 7.7897 8.8064 90.000 106.793 90.000 ZERR 4.00 0.0004 0.0003 0.0003 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 24 44 4 12 V = 704.58 F(000) = 312.0 Mu = 0.11 mm-1 Cell Wt = 580.63 Rho = 1.368 MERG 2 OMIT -3.00 55.00 OMIT 1 0 0 OMIT -2 1 1 OMIT 0 2 0 OMIT -3 1 7 OMIT -4 1 5 OMIT -6 0 6 EXTI 0.04021 SHEL 7 0.77 HTAB N21 O1A HTAB N21 O1B EQIV_$1 x, -y+3/2, z+1/2 HTAB N21 O1B_$1 FMAP 2 PLAN 5 SIZE 0.21 0.28 0.39 ACTA BOND $H EQIV_$2 -x+1, -y+2, -z+1 MPLA C1 O1A O1B MPLA C1_$2 O1A_$2 O1B_$2 WGHT 0.05560 0.10350 L.S. 8 TEMP -153.00 FVAR 1.52169 MOLE 1 C1 1 0.628259 0.940090 0.699031 11.00000 0.01704 0.01896 = 0.01660 0.00084 0.00359 -0.00199 C2 1 0.547182 0.943770 0.528346 11.00000 0.02055 0.02207 = 0.01462 -0.00112 0.00405 -0.00049 AFIX 43 H2 2 0.564604 0.861215 0.457719 11.00000 0.03545 AFIX 0 O1A 4 0.597059 1.037000 0.796240 11.00000 0.02251 0.02721 = 0.01517 -0.00212 0.00237 0.00370 O1B 4 0.724638 0.839486 0.735335 11.00000 0.02209 0.02644 = 0.02205 -0.00286 -0.00066 0.00658 MOLE 2 C22 1 0.699443 1.086600 1.190576 11.00000 0.02172 0.02523 = 0.02236 -0.00139 0.00836 0.00162 AFIX 23 H22A 2 0.611163 1.054712 1.194734 11.00000 -1.20000 H22B 2 0.694701 1.202117 1.142363 11.00000 -1.20000 AFIX 0 C23 1 0.792234 1.089640 1.356468 11.00000 0.02752 0.02906 = 0.02179 -0.00569 0.00979 -0.00502 AFIX 23 H23A 2 0.762379 1.175772 1.420931 11.00000 -1.20000 H23B 2 0.792370 0.975883 1.406642 11.00000 -1.20000 AFIX 0 C25 1 0.968090 0.998623 1.271352 11.00000 0.01930 0.03050 = 0.02264 0.00052 0.00339 -0.00080 AFIX 23 H25A 2 0.967019 0.887299 1.325193 11.00000 -1.20000 H25B 2 1.059159 1.023835 1.274099 11.00000 -1.20000 AFIX 0 C26 1 0.884660 0.986070 1.100738 11.00000 0.01993 0.02515 = 0.01935 0.00127 0.00790 0.00040 AFIX 23 H26A 2 0.893607 1.092737 1.043666 11.00000 -1.20000 H26B 2 0.915081 0.889010 1.048136 11.00000 -1.20000 AFIX 0 N21 3 0.745716 0.959823 1.092360 11.00000 0.01877 0.02254 = 0.01559 0.00063 0.00417 -0.00067 AFIX 23 H21A 2 0.735129 0.850720 1.126682 11.00000 0.03625 H21B 2 0.695623 0.969094 0.988512 11.00000 0.03933 AFIX 0 O24 4 0.921180 1.130928 1.353671 11.00000 0.02624 0.03092 = 0.02356 -0.00706 0.00443 -0.00833 HKLF 4 Covalent radii and connectivity table for 06skc0061p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C2_$2 C1 O1A - C1 O1B - C1 C22 - N21 C23 C23 - O24 C22 C25 - O24 C26 C26 - N21 C25 N21 - C26 C22 O24 - C23 C25 Operators for generating equivalent atoms: $1 x, -y+3/2, z+1/2 $2 -x+1, -y+2, -z+1 8668 Reflections read, of which 649 rejected -13 =< h =< 13, -10 =< k =< 10, -11 =< l =< 11, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 1184 Unique reflections, of which 0 suppressed R(int) = 0.0455 R(sigma) = 0.0457 Friedel opposites merged Maximum memory for data reduction = 1446 / 12805 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 = 1709 / 124835 wR2 = 0.1106 before cycle 1 for 1184 data and 95 / 95 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.52173 0.00692 0.006 OSF 2 0.04031 0.01355 0.008 EXTI Mean shift/esd = 0.004 Maximum = 0.012 for z O1B Max. shift = 0.000 A for C23 Max. dU = 0.000 for H2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1709 / 124835 wR2 = 0.1106 before cycle 2 for 1184 data and 95 / 95 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.52172 0.00692 -0.002 OSF 2 0.04035 0.01357 0.002 EXTI Mean shift/esd = 0.001 Maximum = 0.005 for z O1B Max. shift = 0.000 A for O1A Max. dU = 0.000 for H2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1709 / 124835 wR2 = 0.1106 before cycle 3 for 1184 data and 95 / 95 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.52171 0.00692 -0.001 OSF 2 0.04034 0.01357 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H25B Max. dU = 0.000 for H2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1709 / 124835 wR2 = 0.1106 before cycle 4 for 1184 data and 95 / 95 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.52172 0.00692 0.000 OSF 2 0.04034 0.01357 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for z N21 Max. shift = 0.000 A for N21 Max. dU = 0.000 for H21B Least-squares cycle 5 Maximum vector length = 511 Memory required = 1709 / 124835 wR2 = 0.1106 before cycle 5 for 1184 data and 95 / 95 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.52172 0.00692 0.000 OSF 2 0.04034 0.01357 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O24 Max. shift = 0.000 A for C1 Max. dU = 0.000 for H21B Least-squares cycle 6 Maximum vector length = 511 Memory required = 1709 / 124835 wR2 = 0.1106 before cycle 6 for 1184 data and 95 / 95 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.52172 0.00692 0.000 OSF 2 0.04034 0.01357 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O24 Max. shift = 0.000 A for C1 Max. dU = 0.000 for H21A Least-squares cycle 7 Maximum vector length = 511 Memory required = 1709 / 124835 wR2 = 0.1106 before cycle 7 for 1184 data and 95 / 95 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.52172 0.00692 0.000 OSF 2 0.04034 0.01357 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O24 Max. shift = 0.000 A for C1 Max. dU = 0.000 for H21A Least-squares cycle 8 Maximum vector length = 511 Memory required = 1709 / 124835 wR2 = 0.1106 before cycle 8 for 1184 data and 95 / 95 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.52172 0.00692 0.000 OSF 2 0.04035 0.01357 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O24 Max. shift = 0.000 A for C1 Max. dU = 0.000 for H21A Largest correlation matrix elements 0.595 U13 C26 / U11 C26 0.551 U13 C23 / U33 C23 0.526 U13 C2 / U33 C2 0.581 U13 C25 / U11 C25 0.547 U13 C1 / U11 C1 0.515 U13 N21 / U33 N21 0.576 U13 C22 / U33 C22 0.546 U13 O1A / U11 O1A 0.514 z C23 / x C23 0.565 U13 N21 / U11 N21 0.543 U13 C23 / U11 C23 0.514 EXTI / OSF 0.562 U13 C2 / U11 C2 0.538 U13 C26 / U33 C26 0.511 z C26 / x C26 0.560 U13 C22 / U11 C22 0.527 U13 O24 / U11 O24 0.507 U13 O24 / U33 O24 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.5646 0.8612 0.4577 43 0.950 0.000 C2 C2_$2 C1 H22A 0.6112 1.0547 1.1947 23 0.990 0.000 C22 N21 C23 H22B 0.6947 1.2021 1.1424 23 0.990 0.000 C22 N21 C23 H23A 0.7624 1.1758 1.4209 23 0.990 0.000 C23 O24 C22 H23B 0.7924 0.9759 1.4066 23 0.990 0.000 C23 O24 C22 H25A 0.9670 0.8873 1.3252 23 0.990 0.000 C25 O24 C26 H25B 1.0592 1.0238 1.2741 23 0.990 0.000 C25 O24 C26 H26A 0.8936 1.0927 1.0437 23 0.990 0.000 C26 N21 C25 H26B 0.9151 0.8890 1.0481 23 0.990 0.000 C26 N21 C25 H21A 0.7351 0.8507 1.1267 23 0.920 0.000 N21 C26 C22 H21B 0.6956 0.9691 0.9885 23 0.920 0.000 N21 C26 C22 06skc0061p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.62826 0.94009 0.69903 1.00000 0.01704 0.01895 0.01660 0.00084 0.00359 -0.00199 0.01780 0.00299 0.00015 0.00018 0.00017 0.00000 0.00069 0.00073 0.00070 0.00055 0.00058 0.00054 0.00035 C2 0.54718 0.94377 0.52835 1.00000 0.02054 0.02206 0.01462 -0.00112 0.00405 -0.00049 0.01929 0.00294 0.00015 0.00019 0.00017 0.00000 0.00076 0.00075 0.00073 0.00055 0.00064 0.00054 0.00036 H2 0.56461 0.86121 0.45772 1.00000 0.03541 0.00000 0.00512 O1A 0.59706 1.03700 0.79624 1.00000 0.02251 0.02721 0.01516 -0.00212 0.00237 0.00370 0.02227 0.00217 0.00011 0.00014 0.00012 0.00000 0.00060 0.00061 0.00053 0.00043 0.00047 0.00045 0.00031 O1B 0.72464 0.83949 0.73534 1.00000 0.02209 0.02644 0.02205 -0.00286 -0.00066 0.00658 0.02500 0.00222 0.00011 0.00014 0.00013 0.00000 0.00062 0.00061 0.00056 0.00046 0.00047 0.00045 0.00032 C22 0.69944 1.08660 1.19058 1.00000 0.02172 0.02522 0.02236 -0.00139 0.00836 0.00162 0.02268 0.00317 0.00015 0.00021 0.00018 0.00000 0.00076 0.00077 0.00077 0.00063 0.00067 0.00063 0.00037 H22A 0.61116 1.05471 1.19473 1.00000 0.02722 0.00000 0.00000 H22B 0.69470 1.20212 1.14236 1.00000 0.02722 0.00000 0.00000 C23 0.79223 1.08964 1.35647 1.00000 0.02752 0.02905 0.02179 -0.00569 0.00979 -0.00503 0.02556 0.00335 0.00016 0.00022 0.00019 0.00000 0.00087 0.00081 0.00076 0.00067 0.00067 0.00069 0.00038 H23A 0.76238 1.17577 1.42093 1.00000 0.03067 0.00000 0.00000 H23B 0.79237 0.97588 1.40664 1.00000 0.03067 0.00000 0.00000 C25 0.96809 0.99862 1.27135 1.00000 0.01929 0.03050 0.02264 0.00052 0.00338 -0.00080 0.02471 0.00320 0.00015 0.00021 0.00019 0.00000 0.00083 0.00087 0.00078 0.00068 0.00069 0.00064 0.00039 H25A 0.96702 0.88730 1.32519 1.00000 0.02965 0.00000 0.00000 H25B 1.05916 1.02383 1.27410 1.00000 0.02965 0.00000 0.00000 C26 0.88466 0.98607 1.10074 1.00000 0.01992 0.02515 0.01935 0.00127 0.00790 0.00040 0.02101 0.00314 0.00015 0.00020 0.00017 0.00000 0.00081 0.00078 0.00075 0.00059 0.00067 0.00059 0.00038 H26A 0.89361 1.09274 1.04367 1.00000 0.02521 0.00000 0.00000 H26B 0.91508 0.88901 1.04814 1.00000 0.02521 0.00000 0.00000 N21 0.74572 0.95982 1.09236 1.00000 0.01877 0.02254 0.01558 0.00063 0.00417 -0.00067 0.01913 0.00256 0.00012 0.00016 0.00015 0.00000 0.00069 0.00064 0.00064 0.00049 0.00055 0.00049 0.00034 H21A 0.73513 0.85072 1.12668 1.00000 0.03624 0.00000 0.00550 H21B 0.69562 0.96909 0.98851 1.00000 0.03932 0.00000 0.00569 O24 0.92118 1.13093 1.35367 1.00000 0.02623 0.03092 0.02357 -0.00706 0.00443 -0.00833 0.02749 0.00219 0.00011 0.00015 0.00013 0.00000 0.00068 0.00067 0.00058 0.00049 0.00053 0.00048 0.00034 Final Structure Factor Calculation for 06skc0061p21c in P2(1)/c Total number of l.s. parameters = 95 Maximum vector length = 511 Memory required = 1614 / 22995 wR2 = 0.1106 before cycle 9 for 1184 data and 0 / 95 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0407 for 915 Fo > 4sig(Fo) and 0.0606 for all 1184 data wR2 = 0.1106, GooF = S = 1.091, Restrained GooF = 1.091 for all data Occupancy sum of asymmetric unit = 10.00 for non-hydrogen and 11.00 for hydrogen atoms Principal mean square atomic displacements U 0.0212 0.0165 0.0156 C1 0.0222 0.0212 0.0144 C2 0.0311 0.0211 0.0146 O1A 0.0377 0.0215 0.0158 O1B 0.0261 0.0236 0.0183 C22 0.0348 0.0236 0.0183 C23 0.0307 0.0250 0.0184 C25 0.0255 0.0211 0.0164 C26 0.0228 0.0191 0.0155 N21 0.0376 0.0285 0.0164 O24 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.025 0.041 0.056 0.070 0.090 0.111 0.138 0.206 1.000 Number in group 131. 107. 120. 118. 116. 127. 113. 116. 119. 117. GooF 0.873 0.751 1.164 1.136 1.243 1.106 1.360 0.894 1.150 1.093 K 0.337 0.933 0.877 0.914 0.961 0.967 0.982 1.004 1.044 1.017 Resolution(A) 0.77 0.79 0.82 0.85 0.88 0.93 0.99 1.07 1.21 1.47 inf Number in group 121. 119. 115. 123. 116. 117. 117. 119. 118. 119. GooF 0.926 0.915 1.056 0.961 1.181 1.081 1.147 1.016 1.016 1.496 K 1.001 1.028 1.046 0.994 0.995 1.035 1.041 1.017 1.007 1.003 R1 0.135 0.110 0.095 0.087 0.071 0.060 0.050 0.031 0.045 0.033 Recommended weighting scheme: WGHT 0.0553 0.1047 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) 2 1 7 9.29 17.35 4.53 0.060 1.09 0 1 1 3.96 8.15 4.25 0.041 5.72 -1 0 2 480.40 635.86 4.25 0.361 4.37 -4 2 4 61.55 45.08 4.19 0.096 1.73 5 0 6 31.06 48.20 4.00 0.099 1.03 -11 1 3 34.04 48.30 3.88 0.100 0.97 1 2 0 78.45 59.80 3.75 0.111 3.64 0 4 0 1.56 4.90 3.53 0.032 1.95 1 3 10 77.43 54.56 3.50 0.106 0.78 -1 2 9 35.70 56.96 3.43 0.108 0.93 -1 3 4 35.90 48.02 3.35 0.099 1.68 0 1 9 6.52 11.85 3.31 0.049 0.93 1 6 7 -3.66 20.00 3.31 0.064 0.86 -11 3 1 13.56 22.82 3.19 0.068 0.90 9 1 2 37.63 19.18 2.98 0.063 1.02 1 2 3 47.47 60.45 2.96 0.111 2.12 -7 4 8 5.15 10.13 2.95 0.046 0.89 -11 1 8 -0.34 4.91 2.91 0.032 0.82 7 1 5 0.89 5.98 2.90 0.035 0.97 4 3 0 44.62 35.39 2.82 0.085 1.83 4 5 0 6.35 10.21 2.61 0.046 1.33 -5 6 6 6.17 11.27 2.60 0.048 0.94 3 3 0 14.43 19.38 2.59 0.063 2.07 2 2 6 18.28 24.48 2.58 0.071 1.20 2 3 0 103.31 123.84 2.57 0.159 2.32 1 0 2 345.98 410.27 2.51 0.290 3.56 -4 7 6 16.67 24.81 2.45 0.071 0.88 5 4 7 176.07 141.37 2.42 0.170 0.84 0 5 2 143.36 122.07 2.37 0.158 1.46 -11 1 5 147.99 125.66 2.35 0.161 0.93 -1 2 3 13.37 17.55 2.35 0.060 2.34 7 4 6 34.50 49.99 2.34 0.101 0.81 -10 3 6 38.80 47.92 2.29 0.099 0.91 9 5 1 360.01 298.85 2.29 0.248 0.89 6 1 8 49.32 37.42 2.28 0.088 0.80 0 2 10 241.53 202.51 2.28 0.204 0.82 4 3 7 17.92 23.77 2.25 0.070 0.92 -7 5 7 22.07 27.95 2.23 0.076 0.90 -8 7 3 20.18 26.54 2.22 0.074 0.85 -3 8 5 4.09 9.28 2.21 0.044 0.85 -12 3 2 4.55 9.45 2.21 0.044 0.84 -6 4 6 18.56 23.25 2.19 0.069 1.07 2 0 0 616.14 709.87 2.16 0.382 5.14 3 9 0 184.26 155.76 2.15 0.179 0.84 6 2 0 242.43 211.22 2.15 0.208 1.57 3 2 6 10.83 14.85 2.14 0.055 1.13 -1 2 2 350.79 402.18 2.12 0.287 2.91 -4 4 5 109.57 127.73 2.11 0.162 1.26 -3 6 5 19.36 24.20 2.07 0.070 1.04 -10 0 4 237.15 206.39 2.07 0.206 1.05 Bond lengths and angles C1 - Distance Angles O1A 1.2571 (0.0017) O1B 1.2627 (0.0019) 124.05 (0.15) C2 1.5037 (0.0020) 118.58 (0.13) 117.37 (0.12) C1 - O1A O1B C2 - Distance Angles C2_$2 1.3227 (0.0030) C1 1.5037 (0.0020) 123.27 (0.16) H2 0.9500 118.37 118.37 C2 - C2_$2 C1 O1A - Distance Angles C1 1.2571 (0.0017) O1A - O1B - Distance Angles C1 1.2627 (0.0019) O1B - C22 - Distance Angles N21 1.4893 (0.0017) C23 1.5118 (0.0023) 109.55 (0.13) H22A 0.9900 109.76 109.76 H22B 0.9900 109.76 109.76 108.22 C22 - N21 C23 H22A C23 - Distance Angles O24 1.4274 (0.0019) C22 1.5118 (0.0023) 110.96 (0.12) H23A 0.9900 109.45 109.45 H23B 0.9900 109.45 109.45 108.04 C23 - O24 C22 H23A C25 - Distance Angles O24 1.4324 (0.0018) C26 1.5136 (0.0022) 110.82 (0.13) H25A 0.9900 109.48 109.48 H25B 0.9900 109.48 109.48 108.06 C25 - O24 C26 H25A C26 - Distance Angles N21 1.4852 (0.0019) C25 1.5136 (0.0022) 110.82 (0.11) H26A 0.9900 109.48 109.48 H26B 0.9900 109.48 109.48 108.06 C26 - N21 C25 H26A N21 - Distance Angles C26 1.4852 (0.0019) C22 1.4893 (0.0017) 112.21 (0.12) H21A 0.9200 109.16 109.16 H21B 0.9200 109.16 109.16 107.88 N21 - C26 C22 H21A O24 - Distance Angles C23 1.4274 (0.0019) C25 1.4324 (0.0018) 109.30 (0.11) O24 - C23 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.92 1.80 2.7023(17) 167.2 N21-H21B...O1A 0.92 2.55 3.2256(16) 130.9 N21-H21B...O1B 0.92 1.78 2.6902(16) 167.4 N21-H21A...O1B_$1 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 7.1238 (0.0101) x + 5.6258 (0.0039) y - 3.3222 (0.0189) z = 7.4421 (0.0192) * 0.0000 (0.0000) C1 * 0.0000 (0.0000) O1A * 0.0000 (0.0000) O1B Rms deviation of fitted atoms = 0.0000 7.1238 (0.0101) x + 5.6258 (0.0039) y - 3.3222 (0.0188) z = 7.6112 (0.0076) Angle to previous plane (with approximate esd) = 0.00 ( 0.17 ) * 0.0000 (0.0000) C1_$2 * 0.0000 (0.0000) O1A_$2 * 0.0000 (0.0000) O1B_$2 Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 2 13 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.0606 for 1184 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.17 at 0.4217 0.0502 0.3962 [ 0.65 A from C2 ] Deepest hole -0.17 at 0.3318 0.0540 0.9407 [ 0.78 A from H21B ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 1773 / 14600 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5783 0.9498 0.6038 1.00000 0.05 0.17 0.65 C2 0.86 C1 1.43 H2 1.72 C2 Q2 1 0.4753 0.9566 0.5132 1.00000 0.05 0.17 0.75 C2 0.86 C2 1.41 H2 1.53 H2 Q3 1 0.5585 0.9216 0.3210 1.00000 0.05 0.15 1.28 H2 1.72 O1A 1.73 H22A 1.87 C2 Q4 1 0.7554 1.0808 1.2668 1.00000 0.05 0.13 0.76 C22 0.78 C23 1.44 H23B 1.45 H22B Q5 1 0.9055 1.1388 1.2570 1.00000 0.05 0.13 0.82 O24 1.27 C25 1.73 C23 1.78 C26 Shortest distances between peaks (including symmetry equivalents) 2 2 0.93 1 2 1.16 1 2 1.26 4 5 1.70 2 3 1.86 1 3 2.04 2 3 2.15 1 1 2.24 1 3 2.45 3 4 2.61 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. 0.39: 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 0.30: Structure factors and derivatives 0.19: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0061p21c finished at 16:23:25 Total CPU time: 1.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++