+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0042p21 started at 17:39:55 on 31-Jul-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0042p21 in P2(1) CELL 0.71069 7.5360 14.2180 9.7160 90.000 96.571 90.000 ZERR 4.00 0.0004 0.0008 0.0006 0.000 0.003 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O UNIT 36 56 8 16 V = 1034.20 F(000) = 456.0 Mu = 0.11 mm-1 Cell Wt = 856.89 Rho = 1.376 MERG 4 OMIT -3.00 55.00 SHEL 7 0.77 HTAB N23 O35A EQIV_$1 -x, y+1/2, -z HTAB O5A O1B_$1 EQIV_$2 x, y, z+1 HTAB N21 O1A_$2 EQIV_$3 -x+1, y+1/2, -z HTAB O35B O31A_$3 HTAB N43 O1B_$3 EQIV_$4 -x+1, y+1/2, -z+1 HTAB N41 O31A_$4 FMAP 2 PLAN 20 SIZE 0.03 0.07 0.13 ACTA BOND $H WGHT 0.01500 0.37270 L.S. 4 TEMP -153.00 FVAR 0.32998 MOLE 1 C1 1 0.107088 0.085837 -0.281208 11.00000 0.02264 0.01879 = 0.02796 0.00217 0.00331 -0.00119 C2 1 0.046612 0.107548 -0.142464 11.00000 0.02658 0.02282 = 0.02899 -0.00352 0.00738 0.00189 AFIX 23 H2A 2 0.133635 0.079943 -0.069516 11.00000 -1.20000 H2B 2 -0.069631 0.076158 -0.136981 11.00000 -1.20000 AFIX 0 C3 1 0.026042 0.211666 -0.111136 11.00000 0.02869 0.02079 = 0.02342 -0.00010 0.00585 0.00039 AFIX 23 H3A 2 -0.064666 0.239671 -0.180974 11.00000 -1.20000 H3B 2 0.140941 0.244215 -0.117540 11.00000 -1.20000 AFIX 0 C4 1 -0.030337 0.226244 0.033037 11.00000 0.03146 0.01925 = 0.02528 -0.00023 0.00963 -0.00038 AFIX 23 H4A 2 -0.149875 0.197990 0.036175 11.00000 -1.20000 H4B 2 0.054567 0.192671 0.101308 11.00000 -1.20000 AFIX 0 C5 1 -0.037053 0.328141 0.074494 11.00000 0.02545 0.02674 = 0.02263 0.00103 0.00360 -0.00054 O1A 4 0.133504 0.148872 -0.365085 11.00000 0.04071 0.01942 = 0.02593 0.00208 0.01261 -0.00273 O1B 4 0.130987 -0.001140 -0.306369 11.00000 0.04478 0.01811 = 0.02436 0.00116 0.01491 0.00289 O5A 4 -0.084704 0.337648 0.199819 11.00000 0.05347 0.02281 = 0.02741 -0.00568 0.01896 -0.00164 AFIX 147 H5 2 -0.093258 0.395073 0.218281 11.00000 0.06826 AFIX 0 O5B 4 -0.002081 0.393523 0.002989 11.00000 0.05651 0.02610 = 0.03058 -0.00171 0.01752 -0.00140 MOLE 2 C22 1 0.251611 0.363861 0.502066 11.00000 0.03202 0.02035 = 0.02486 -0.00189 0.00894 -0.00423 AFIX 43 H22 2 0.285902 0.324068 0.431141 11.00000 -1.20000 AFIX 0 C24 1 0.197682 0.490161 0.622169 11.00000 0.02438 0.01865 = 0.02158 -0.00357 0.00672 -0.00230 C25 1 0.155075 0.414164 0.693489 11.00000 0.03055 0.01874 = 0.02794 -0.00065 0.00945 -0.00049 AFIX 43 H25 2 0.110047 0.414247 0.780906 11.00000 -1.20000 AFIX 0 C26 1 0.186438 0.592884 0.652249 11.00000 0.03718 0.01479 = 0.02932 -0.00435 0.00649 0.00196 AFIX 137 H26A 2 0.144615 0.601734 0.743233 11.00000 -1.50000 H26B 2 0.102541 0.622851 0.580994 11.00000 -1.50000 H26C 2 0.304781 0.621457 0.652254 11.00000 -1.50000 AFIX 0 N21 3 0.188546 0.336159 0.616836 11.00000 0.03630 0.01962 = 0.02227 -0.00222 0.01002 -0.00322 AFIX 43 H21 2 0.170859 0.277424 0.640369 11.00000 0.02525 AFIX 0 N23 3 0.258579 0.457390 0.503436 11.00000 0.03192 0.01913 = 0.02124 0.00060 0.00545 -0.00017 AFIX 43 H23 2 0.296365 0.492681 0.438317 11.00000 0.04797 AFIX 0 MOLE 3 C31 1 0.422635 0.236516 0.157984 11.00000 0.02431 0.02277 = 0.02267 -0.00333 0.00483 -0.00286 C32 1 0.453982 0.329518 0.090657 11.00000 0.02526 0.01699 = 0.01990 -0.00049 0.00531 -0.00128 AFIX 23 H32A 2 0.372180 0.334770 0.003707 11.00000 -1.20000 H32B 2 0.577844 0.331065 0.066034 11.00000 -1.20000 AFIX 0 C33 1 0.425629 0.413425 0.181799 11.00000 0.02955 0.01502 = 0.02602 -0.00422 0.00753 -0.00098 AFIX 23 H33A 2 0.302228 0.411479 0.207359 11.00000 -1.20000 H33B 2 0.508479 0.408602 0.268255 11.00000 -1.20000 AFIX 0 C34 1 0.455038 0.506812 0.113361 11.00000 0.02828 0.01919 = 0.01914 -0.00090 0.00503 -0.00318 AFIX 23 H34A 2 0.576987 0.507668 0.084800 11.00000 -1.20000 H34B 2 0.369419 0.512345 0.028532 11.00000 -1.20000 AFIX 0 C35 1 0.433477 0.590289 0.203756 11.00000 0.02965 0.01592 = 0.02535 0.00248 0.00585 -0.00070 O31A 4 0.443671 0.161078 0.087303 11.00000 0.04337 0.01390 = 0.02384 -0.00136 0.01350 0.00256 O31B 4 0.375512 0.234088 0.275304 11.00000 0.05104 0.01786 = 0.02433 0.00038 0.01706 -0.00060 O35A 4 0.386863 0.583966 0.319424 11.00000 0.04737 0.02146 = 0.02540 0.00351 0.01505 -0.00088 O35B 4 0.465374 0.674074 0.152663 11.00000 0.05016 0.01492 = 0.02598 0.00240 0.01560 -0.00309 AFIX 147 H35 2 0.490751 0.668095 0.071156 11.00000 0.04112 AFIX 0 MOLE 4 C42 1 0.701775 0.548322 0.617831 11.00000 0.02955 0.01853 = 0.02822 -0.00287 0.00990 -0.00108 AFIX 43 H42 2 0.718338 0.612038 0.592770 11.00000 -1.20000 AFIX 0 C44 1 0.692305 0.393417 0.611398 11.00000 0.02422 0.01757 = 0.02433 0.00372 0.00217 -0.00010 C45 1 0.636719 0.420429 0.732204 11.00000 0.02904 0.02394 = 0.02483 0.00763 0.00547 0.00028 AFIX 43 H45 2 0.599729 0.380422 0.801863 11.00000 -1.20000 AFIX 0 C46 1 0.708951 0.298570 0.551185 11.00000 0.03874 0.01610 = 0.03379 -0.00115 0.00716 0.00226 AFIX 137 H46A 2 0.669438 0.251182 0.614295 11.00000 -1.50000 H46B 2 0.833934 0.286909 0.537621 11.00000 -1.50000 H46C 2 0.634494 0.294858 0.461795 11.00000 -1.50000 AFIX 0 N41 3 0.643923 0.518863 0.735415 11.00000 0.03331 0.02294 = 0.02156 -0.00190 0.00819 0.00123 AFIX 43 H41 2 0.615339 0.554979 0.803057 11.00000 0.04647 AFIX 0 N43 3 0.731954 0.474428 0.542602 11.00000 0.03007 0.01517 = 0.02094 -0.00051 0.00711 -0.00171 AFIX 43 H43 2 0.771420 0.476281 0.460833 11.00000 0.07398 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0042p21 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C1 C3 C3 - C2 C4 C4 - C5 C3 C5 - O5B O5A C4 O1A - C1 O1B - C1 O5A - C5 O5B - C5 C22 - N21 N23 C24 - C25 N23 C26 C25 - C24 N21 C26 - C24 N21 - C22 C25 N23 - C22 C24 C31 - O31B O31A C32 C32 - C31 C33 C33 - C34 C32 C34 - C35 C33 C35 - O35A O35B C34 O31A - C31 O31B - C31 O35A - C35 O35B - C35 C42 - N43 N41 C44 - C45 N43 C46 C45 - C44 N41 C46 - C44 N41 - C42 C45 N43 - C42 C44 Operators for generating equivalent atoms: $1 -x, y+1/2, -z $2 x, y, z+1 $3 -x+1, y+1/2, -z $4 -x+1, y+1/2, -z+1 Floating origin restraints generated 12072 Reflections read, of which 46 rejected -9 =< h =< 9, -18 =< k =< 17, -12 =< l =< 11, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -2 9 1 3.77 0.39 7 2.26 7 0 4 -0.25 0.41 3 2.55 4 8 4 -0.04 0.19 7 1.04 7 2 5 0.08 0.42 5 2.33 3 8 6 1.62 0.30 5 1.61 5 Inconsistent equivalents 2460 Unique reflections, of which 0 suppressed R(int) = 0.1295 R(sigma) = 0.1106 Friedel opposites merged Maximum memory for data reduction = 3031 / 24117 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 = 3840 / 350360 wR2 = 0.1108 before cycle 1 for 2460 data and 281 / 281 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0150 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.32984 0.00079 -0.172 OSF Mean shift/esd = 0.015 Maximum = -0.172 for OSF Max. shift = 0.001 A for H35 Max. dU = 0.001 for H35 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3840 / 350360 wR2 = 0.1108 before cycle 2 for 2460 data and 281 / 281 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0150 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.32981 0.00079 -0.041 OSF Mean shift/esd = 0.005 Maximum = -0.041 for OSF Max. shift = 0.001 A for H35 Max. dU = 0.000 for H35 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3840 / 350360 wR2 = 0.1108 before cycle 3 for 2460 data and 281 / 281 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0150 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.32981 0.00079 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.011 for U11 H35 Max. shift = 0.000 A for H35 Max. dU = 0.000 for H35 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3840 / 350360 wR2 = 0.1108 before cycle 4 for 2460 data and 281 / 281 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0150 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.32981 0.00079 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.004 for U11 H35 Max. shift = 0.000 A for H35 Max. dU = 0.000 for H35 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 0.1336 0.0799 -0.0695 23 0.990 0.000 C2 C1 C3 H2B -0.0696 0.0762 -0.1370 23 0.990 0.000 C2 C1 C3 H3A -0.0646 0.2397 -0.1810 23 0.990 0.000 C3 C2 C4 H3B 0.1410 0.2442 -0.1175 23 0.990 0.000 C3 C2 C4 H4A -0.1498 0.1980 0.0362 23 0.990 0.000 C4 C5 C3 H4B 0.0546 0.1927 0.1013 23 0.990 0.000 C4 C5 C3 H5 -0.0933 0.3951 0.2183 147 0.840 0.000 O5A C5 H5 H22 0.2859 0.3241 0.4311 43 0.950 0.000 C22 N21 N23 H25 0.1101 0.4142 0.7809 43 0.950 0.000 C25 C24 N21 H26A 0.1445 0.6017 0.7432 137 0.980 0.000 C26 C24 H26A H26B 0.1026 0.6228 0.5810 137 0.980 0.000 C26 C24 H26A H26C 0.3048 0.6214 0.6523 137 0.980 0.000 C26 C24 H26A H21 0.1708 0.2774 0.6404 43 0.880 0.000 N21 C22 C25 H23 0.2963 0.4927 0.4383 43 0.880 0.000 N23 C22 C24 H32A 0.3722 0.3348 0.0037 23 0.990 0.000 C32 C31 C33 H32B 0.5779 0.3311 0.0660 23 0.990 0.000 C32 C31 C33 H33A 0.3022 0.4115 0.2074 23 0.990 0.000 C33 C34 C32 H33B 0.5085 0.4086 0.2683 23 0.990 0.000 C33 C34 C32 H34A 0.5770 0.5077 0.0848 23 0.990 0.000 C34 C35 C33 H34B 0.3694 0.5123 0.0285 23 0.990 0.000 C34 C35 C33 H35 0.4911 0.6681 0.0712 147 0.840 0.000 O35B C35 H35 H42 0.7184 0.6120 0.5928 43 0.950 0.000 C42 N43 N41 H45 0.5998 0.3804 0.8019 43 0.950 0.000 C45 C44 N41 H46A 0.6694 0.2512 0.6142 137 0.980 0.000 C46 C44 H46A H46B 0.8340 0.2869 0.5377 137 0.980 0.000 C46 C44 H46A H46C 0.6346 0.2949 0.4617 137 0.980 0.000 C46 C44 H46A H41 0.6153 0.5550 0.8031 43 0.880 0.000 N41 C42 C45 H43 0.7714 0.4763 0.4608 43 0.880 0.000 N43 C42 C44 06skc0042p21 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.10708 0.08585 -0.28119 1.00000 0.02258 0.01882 0.02798 0.00209 0.00330 -0.00112 0.02310 0.00793 0.00048 0.00031 0.00047 0.00000 0.00189 0.00224 0.00246 0.00210 0.00169 0.00178 0.00092 C2 0.04662 0.10755 -0.14248 1.00000 0.02656 0.02273 0.02894 -0.00353 0.00742 0.00189 0.02575 0.00827 0.00053 0.00031 0.00047 0.00000 0.00201 0.00253 0.00263 0.00205 0.00178 0.00172 0.00103 H2A 0.13363 0.07993 -0.06954 1.00000 0.03089 0.00000 0.00000 H2B -0.06963 0.07616 -0.13701 1.00000 0.03089 0.00000 0.00000 C3 0.02606 0.21166 -0.11113 1.00000 0.02862 0.02079 0.02339 -0.00008 0.00584 0.00038 0.02404 0.00778 0.00053 0.00031 0.00044 0.00000 0.00213 0.00212 0.00235 0.00196 0.00175 0.00176 0.00093 H3A -0.06464 0.23968 -0.18096 1.00000 0.02885 0.00000 0.00000 H3B 0.14096 0.24421 -0.11753 1.00000 0.02885 0.00000 0.00000 C4 -0.03032 0.22624 0.03305 1.00000 0.03143 0.01912 0.02530 -0.00021 0.00964 -0.00033 0.02479 0.00788 0.00054 0.00029 0.00045 0.00000 0.00228 0.00250 0.00246 0.00193 0.00178 0.00177 0.00101 H4A -0.14985 0.19798 0.03619 1.00000 0.02975 0.00000 0.00000 H4B 0.05460 0.19268 0.10132 1.00000 0.02975 0.00000 0.00000 C5 -0.03707 0.32813 0.07449 1.00000 0.02541 0.02677 0.02266 0.00094 0.00356 -0.00054 0.02488 0.00786 0.00053 0.00032 0.00045 0.00000 0.00209 0.00254 0.00245 0.00228 0.00171 0.00191 0.00098 O1A 0.13351 0.14887 -0.36508 1.00000 0.04071 0.01937 0.02586 0.00211 0.01261 -0.00273 0.02797 0.00554 0.00037 0.00020 0.00032 0.00000 0.00162 0.00159 0.00181 0.00139 0.00136 0.00128 0.00073 O1B 0.13096 -0.00114 -0.30637 1.00000 0.04475 0.01810 0.02436 0.00116 0.01496 0.00288 0.02822 0.00604 0.00040 0.00020 0.00033 0.00000 0.00174 0.00173 0.00180 0.00137 0.00141 0.00125 0.00076 O5A -0.08471 0.33766 0.19981 1.00000 0.05348 0.02274 0.02732 -0.00563 0.01896 -0.00164 0.03341 0.00610 0.00044 0.00023 0.00033 0.00000 0.00193 0.00181 0.00185 0.00152 0.00147 0.00155 0.00080 H5 -0.09325 0.39509 0.21826 1.00000 0.06768 0.00000 0.01993 O5B -0.00208 0.39351 0.00299 1.00000 0.05652 0.02596 0.03055 -0.00161 0.01750 -0.00135 0.03671 0.00633 0.00046 0.00020 0.00035 0.00000 0.00193 0.00200 0.00187 0.00167 0.00150 0.00153 0.00085 C22 0.25162 0.36387 0.50207 1.00000 0.03201 0.02040 0.02485 -0.00189 0.00894 -0.00419 0.02531 0.00824 0.00057 0.00032 0.00046 0.00000 0.00234 0.00227 0.00247 0.00191 0.00189 0.00183 0.00102 H22 0.28594 0.32408 0.43115 1.00000 0.03038 0.00000 0.00000 C24 0.19767 0.49016 0.62216 1.00000 0.02438 0.01861 0.02155 -0.00356 0.00674 -0.00229 0.02120 0.00777 0.00053 0.00028 0.00046 0.00000 0.00196 0.00264 0.00247 0.00190 0.00173 0.00162 0.00101 C25 0.15507 0.41416 0.69349 1.00000 0.03048 0.01867 0.02785 -0.00073 0.00944 -0.00054 0.02520 0.00840 0.00051 0.00034 0.00048 0.00000 0.00211 0.00217 0.00272 0.00216 0.00180 0.00213 0.00100 H25 0.11005 0.41425 0.78091 1.00000 0.03023 0.00000 0.00000 C26 0.18642 0.59287 0.65225 1.00000 0.03712 0.01475 0.02922 -0.00435 0.00644 0.00193 0.02683 0.00818 0.00055 0.00031 0.00050 0.00000 0.00224 0.00224 0.00252 0.00215 0.00185 0.00189 0.00100 H26A 0.14455 0.60172 0.74322 1.00000 0.04024 0.00000 0.00000 H26B 0.10256 0.62285 0.58098 1.00000 0.04024 0.00000 0.00000 H26C 0.30477 0.62145 0.65230 1.00000 0.04024 0.00000 0.00000 N21 0.18853 0.33616 0.61684 1.00000 0.03629 0.01957 0.02230 -0.00221 0.01001 -0.00319 0.02554 0.00646 0.00044 0.00026 0.00036 0.00000 0.00201 0.00221 0.00206 0.00177 0.00157 0.00160 0.00087 H21 0.17083 0.27742 0.64036 1.00000 0.02540 0.00000 0.01258 N23 0.25856 0.45740 0.50344 1.00000 0.03186 0.01902 0.02121 0.00063 0.00541 -0.00020 0.02385 0.00655 0.00044 0.00026 0.00037 0.00000 0.00191 0.00181 0.00221 0.00171 0.00158 0.00153 0.00084 H23 0.29634 0.49270 0.43832 1.00000 0.04802 0.00000 0.01635 C31 0.42262 0.23650 0.15799 1.00000 0.02427 0.02275 0.02270 -0.00331 0.00484 -0.00288 0.02307 0.00774 0.00052 0.00032 0.00046 0.00000 0.00206 0.00220 0.00235 0.00212 0.00165 0.00183 0.00094 C32 0.45399 0.32952 0.09066 1.00000 0.02521 0.01698 0.01982 -0.00047 0.00530 -0.00129 0.02046 0.00756 0.00051 0.00028 0.00043 0.00000 0.00201 0.00227 0.00211 0.00199 0.00158 0.00177 0.00090 H32A 0.37219 0.33477 0.00370 1.00000 0.02455 0.00000 0.00000 H32B 0.57785 0.33106 0.06604 1.00000 0.02455 0.00000 0.00000 C33 0.42563 0.41341 0.18181 1.00000 0.02949 0.01496 0.02600 -0.00416 0.00756 -0.00097 0.02314 0.00787 0.00051 0.00031 0.00047 0.00000 0.00201 0.00198 0.00256 0.00200 0.00174 0.00193 0.00093 H33A 0.30223 0.41146 0.20736 1.00000 0.02777 0.00000 0.00000 H33B 0.50847 0.40858 0.26827 1.00000 0.02777 0.00000 0.00000 C34 0.45505 0.50681 0.11338 1.00000 0.02816 0.01912 0.01920 -0.00086 0.00503 -0.00313 0.02198 0.00810 0.00055 0.00029 0.00046 0.00000 0.00209 0.00206 0.00236 0.00200 0.00175 0.00172 0.00093 H34A 0.57700 0.50767 0.08483 1.00000 0.02638 0.00000 0.00000 H34B 0.36944 0.51235 0.02854 1.00000 0.02638 0.00000 0.00000 C35 0.43347 0.59027 0.20377 1.00000 0.02960 0.01589 0.02537 0.00242 0.00584 -0.00074 0.02342 0.00778 0.00051 0.00030 0.00045 0.00000 0.00208 0.00214 0.00246 0.00210 0.00176 0.00188 0.00094 O31A 0.44368 0.16108 0.08730 1.00000 0.04335 0.01383 0.02378 -0.00141 0.01349 0.00252 0.02624 0.00565 0.00037 0.00021 0.00031 0.00000 0.00170 0.00145 0.00183 0.00140 0.00138 0.00129 0.00073 O31B 0.37552 0.23410 0.27531 1.00000 0.05098 0.01782 0.02429 0.00040 0.01707 -0.00061 0.03005 0.00588 0.00042 0.00021 0.00030 0.00000 0.00186 0.00172 0.00178 0.00135 0.00143 0.00137 0.00078 O35A 0.38685 0.58397 0.31943 1.00000 0.04736 0.02139 0.02538 0.00347 0.01509 -0.00089 0.03053 0.00579 0.00039 0.00022 0.00031 0.00000 0.00162 0.00158 0.00181 0.00154 0.00136 0.00144 0.00073 O35B 0.46538 0.67408 0.15266 1.00000 0.05010 0.01482 0.02601 0.00242 0.01564 -0.00310 0.02944 0.00611 0.00042 0.00019 0.00035 0.00000 0.00188 0.00153 0.00192 0.00133 0.00152 0.00133 0.00077 H35 0.49107 0.66808 0.07125 1.00000 0.04243 0.00000 0.01525 C42 0.70178 0.54832 0.61783 1.00000 0.02956 0.01851 0.02815 -0.00288 0.00993 -0.00107 0.02489 0.00778 0.00050 0.00032 0.00045 0.00000 0.00215 0.00226 0.00261 0.00195 0.00193 0.00173 0.00103 H42 0.71836 0.61204 0.59277 1.00000 0.02987 0.00000 0.00000 C44 0.69228 0.39341 0.61139 1.00000 0.02421 0.01758 0.02423 0.00376 0.00219 -0.00007 0.02205 0.00799 0.00052 0.00028 0.00045 0.00000 0.00203 0.00261 0.00230 0.00201 0.00161 0.00167 0.00097 C45 0.63672 0.42044 0.73222 1.00000 0.02896 0.02383 0.02487 0.00769 0.00543 0.00028 0.02570 0.00890 0.00054 0.00036 0.00048 0.00000 0.00214 0.00232 0.00253 0.00207 0.00176 0.00194 0.00100 H45 0.59976 0.38043 0.80189 1.00000 0.03084 0.00000 0.00000 C46 0.70897 0.29858 0.55117 1.00000 0.03875 0.01604 0.03377 -0.00117 0.00720 0.00228 0.02928 0.00903 0.00062 0.00030 0.00053 0.00000 0.00251 0.00239 0.00303 0.00209 0.00207 0.00182 0.00111 H46A 0.66942 0.25118 0.61424 1.00000 0.04393 0.00000 0.00000 H46B 0.83398 0.28693 0.53765 1.00000 0.04393 0.00000 0.00000 H46C 0.63458 0.29488 0.46175 1.00000 0.04393 0.00000 0.00000 N41 0.64390 0.51887 0.73542 1.00000 0.03331 0.02289 0.02153 -0.00184 0.00823 0.00124 0.02552 0.00642 0.00043 0.00026 0.00036 0.00000 0.00190 0.00209 0.00205 0.00171 0.00160 0.00158 0.00085 H41 0.61530 0.55498 0.80305 1.00000 0.04607 0.00000 0.01516 N43 0.73195 0.47443 0.54260 1.00000 0.03007 0.01511 0.02091 -0.00049 0.00711 -0.00170 0.02171 0.00629 0.00041 0.00024 0.00038 0.00000 0.00180 0.00182 0.00210 0.00158 0.00154 0.00149 0.00080 H43 0.77142 0.47628 0.46083 1.00000 0.07429 0.00000 0.02076 Final Structure Factor Calculation for 06skc0042p21 in P2(1) Total number of l.s. parameters = 281 Maximum vector length = 511 Memory required = 3561 / 25046 wR2 = 0.1108 before cycle 5 for 2460 data and 2 / 281 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0150 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0559 for 1739 Fo > 4sig(Fo) and 0.0980 for all 2460 data wR2 = 0.1108, GooF = S = 1.038, Restrained GooF = 1.038 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 30.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0284 0.0229 0.0180 C1 0.0321 0.0264 0.0188 C2 0.0296 0.0218 0.0207 C3 0.0348 0.0204 0.0191 C4 0.0271 0.0255 0.0221 C5 0.0440 0.0233 0.0166 O1A 0.0487 0.0182 0.0177 O1B 0.0587 0.0256 0.0160 O5A 0.0604 0.0263 0.0235 O5B 0.0358 0.0211 0.0190 C22 0.0283 0.0192 0.0161 C24 0.0348 0.0222 0.0186 C25 0.0377 0.0297 0.0131 C26 0.0390 0.0196 0.0181 N21 0.0321 0.0207 0.0187 N23 0.0285 0.0213 0.0194 C31 0.0263 0.0183 0.0168 C32 0.0325 0.0234 0.0135 C33 0.0295 0.0184 0.0181 C34 0.0306 0.0245 0.0151 C35 0.0464 0.0196 0.0127 O31A 0.0548 0.0183 0.0170 O31B 0.0508 0.0242 0.0166 O35A 0.0535 0.0219 0.0129 O35B 0.0352 0.0219 0.0175 C42 0.0262 0.0241 0.0159 C44 0.0326 0.0283 0.0162 C45 0.0400 0.0322 0.0156 C46 0.0347 0.0239 0.0179 N41 0.0315 0.0188 0.0149 N43 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.012 0.016 0.020 0.024 0.030 0.037 0.047 0.065 1.000 Number in group 260. 235. 279. 245. 216. 271. 246. 228. 236. 244. GooF 0.984 0.968 1.051 1.096 1.008 1.072 1.140 0.999 0.976 1.060 K 2.689 1.779 1.175 1.026 1.039 1.056 1.012 1.005 1.008 1.020 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.33 1.68 inf Number in group 250. 252. 236. 252. 240. 250. 241. 246. 247. 246. GooF 1.052 1.006 1.006 1.152 1.050 1.078 0.954 0.974 0.989 1.098 K 1.066 1.193 1.059 1.179 0.989 1.018 1.015 0.995 1.014 1.023 R1 0.310 0.261 0.212 0.186 0.111 0.081 0.047 0.039 0.039 0.027 Recommended weighting scheme: WGHT 0.0127 0.3825 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) -6 3 3 134.98 80.73 5.66 0.031 1.17 -2 0 2 50.97 19.27 5.04 0.015 3.14 3 7 7 55.65 114.06 3.64 0.037 1.00 -8 4 1 97.28 52.44 3.38 0.025 0.91 -2 12 4 86.08 122.07 3.37 0.038 1.04 -2 10 7 10.92 31.52 3.36 0.019 0.98 -8 7 6 31.59 62.51 3.31 0.027 0.79 -2 9 10 150.44 69.04 3.22 0.029 0.82 3 6 8 97.21 171.24 3.21 0.045 0.95 2 6 7 146.89 223.98 3.20 0.051 1.10 -5 2 11 238.38 141.77 3.20 0.041 0.79 -2 3 1 385.50 445.53 3.19 0.073 2.88 0 5 1 39.68 59.66 3.18 0.027 2.73 1 6 10 230.82 111.38 3.18 0.036 0.88 0 9 3 493.30 407.75 3.17 0.069 1.42 -1 0 11 233.87 94.02 3.17 0.033 0.88 0 3 6 398.12 286.03 3.10 0.058 1.52 3 13 3 0.88 24.16 3.08 0.017 0.94 -6 9 4 41.19 95.18 3.02 0.034 0.94 1 1 10 43.14 122.63 3.01 0.038 0.94 -2 14 5 16.64 2.92 2.89 0.006 0.88 6 14 0 43.07 14.81 2.86 0.013 0.79 0 0 8 37.65 95.38 2.85 0.034 1.21 0 6 3 572.67 466.41 2.83 0.074 1.91 -8 1 5 2.46 19.55 2.81 0.015 0.88 -3 0 10 92.77 57.39 2.71 0.026 0.94 4 15 2 -5.79 38.99 2.64 0.021 0.83 7 5 3 20.91 0.31 2.63 0.002 0.93 0 6 9 65.14 41.43 2.63 0.022 0.98 -5 1 11 -1.63 22.10 2.59 0.016 0.80 4 14 3 78.16 15.02 2.58 0.013 0.85 -1 7 7 543.98 643.88 2.58 0.087 1.14 -4 12 5 15.05 32.54 2.58 0.020 0.91 6 0 3 3367.77 2752.38 2.56 0.180 1.12 -7 6 5 437.61 363.76 2.55 0.066 0.91 -4 0 2 46.70 33.16 2.54 0.020 1.82 -1 10 4 169.11 140.46 2.54 0.041 1.22 2 12 6 71.66 31.99 2.52 0.019 0.91 5 4 6 60.97 9.40 2.52 0.011 1.00 6 5 7 71.35 46.28 2.50 0.023 0.84 -2 13 6 28.63 47.18 2.50 0.024 0.89 2 0 3 217.66 262.81 2.49 0.056 2.31 8 1 2 292.66 366.65 2.48 0.066 0.90 -6 0 10 44.77 4.47 2.46 0.007 0.81 -1 13 3 57.39 75.95 2.43 0.030 1.03 -6 1 7 92.74 112.99 2.43 0.037 0.98 0 6 11 93.83 20.68 2.42 0.016 0.82 3 8 8 86.46 17.06 2.40 0.014 0.90 -7 8 7 1.75 18.94 2.40 0.015 0.80 -2 15 2 31.54 0.17 2.39 0.001 0.91 Bond lengths and angles C1 - Distance Angles O1A 1.2426 (0.0050) O1B 1.2776 (0.0054) 122.40 (0.40) C2 1.5032 (0.0055) 121.86 (0.39) 115.73 (0.38) C1 - O1A O1B C2 - Distance Angles C1 1.5032 (0.0055) C3 1.5228 (0.0058) 115.28 (0.37) H2A 0.9900 108.45 108.45 H2B 0.9900 108.45 108.45 107.49 C2 - C1 C3 H2A C3 - Distance Angles C2 1.5228 (0.0058) C4 1.5238 (0.0054) 111.20 (0.35) H3A 0.9900 109.39 109.39 H3B 0.9900 109.39 109.39 108.01 C3 - C2 C4 H3A C4 - Distance Angles C5 1.5060 (0.0060) C3 1.5238 (0.0054) 113.46 (0.35) H4A 0.9900 108.88 108.88 H4B 0.9900 108.88 108.88 107.72 C4 - C5 C3 H4A C5 - Distance Angles O5B 1.2076 (0.0050) O5A 1.3153 (0.0050) 123.64 (0.42) C4 1.5060 (0.0060) 124.78 (0.38) 111.57 (0.39) C5 - O5B O5A O1A - Distance Angles C1 1.2426 (0.0051) O1A - O1B - Distance Angles C1 1.2776 (0.0054) O1B - O5A - Distance Angles C5 1.3153 (0.0050) H5 0.8400 109.47 O5A - C5 O5B - Distance Angles C5 1.2076 (0.0050) O5B - C22 - Distance Angles N21 1.3214 (0.0054) N23 1.3309 (0.0054) 107.88 (0.40) H22 0.9500 126.06 126.06 C22 - N21 N23 C24 - Distance Angles C25 1.3424 (0.0061) N23 1.3708 (0.0054) 106.49 (0.37) C26 1.4937 (0.0058) 131.58 (0.39) 121.93 (0.37) C24 - C25 N23 C25 - Distance Angles C24 1.3424 (0.0061) N21 1.3753 (0.0058) 107.46 (0.35) H25 0.9500 126.27 126.27 C25 - C24 N21 C26 - Distance Angles C24 1.4937 (0.0058) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C24 H26A H26B N21 - Distance Angles C22 1.3214 (0.0054) C25 1.3753 (0.0058) 108.82 (0.38) H21 0.8800 125.59 125.59 N21 - C22 C25 N23 - Distance Angles C22 1.3309 (0.0054) C24 1.3708 (0.0054) 109.35 (0.37) H23 0.8800 125.32 125.32 N23 - C22 C24 C31 - Distance Angles O31B 1.2325 (0.0049) O31A 1.2931 (0.0053) 122.28 (0.44) C32 1.5060 (0.0063) 120.15 (0.40) 117.56 (0.35) C31 - O31B O31A C32 - Distance Angles C31 1.5060 (0.0063) C33 1.5153 (0.0057) 113.44 (0.33) H32A 0.9900 108.88 108.88 H32B 0.9900 108.88 108.88 107.72 C32 - C31 C33 H32A C33 - Distance Angles C34 1.5128 (0.0057) C32 1.5153 (0.0057) 113.37 (0.34) H33A 0.9900 108.90 108.90 H33B 0.9900 108.90 108.90 107.73 C33 - C34 C32 H33A C34 - Distance Angles C35 1.4962 (0.0059) C33 1.5128 (0.0057) 114.02 (0.33) H34A 0.9900 108.75 108.75 H34B 0.9900 108.75 108.75 107.65 C34 - C35 C33 H34A C35 - Distance Angles O35A 1.2184 (0.0049) O35B 1.3234 (0.0049) 119.75 (0.39) C34 1.4962 (0.0059) 123.04 (0.39) 117.21 (0.33) C35 - O35A O35B O31A - Distance Angles C31 1.2931 (0.0053) O31A - O31B - Distance Angles C31 1.2325 (0.0049) O31B - O35A - Distance Angles C35 1.2184 (0.0049) O35A - O35B - Distance Angles C35 1.3234 (0.0049) H35 0.8400 109.47 O35B - C35 C42 - Distance Angles N43 1.3145 (0.0053) N41 1.3360 (0.0052) 108.61 (0.40) H42 0.9500 125.69 125.69 C42 - N43 N41 C44 - Distance Angles C45 1.3467 (0.0060) N43 1.3815 (0.0051) 106.85 (0.39) C46 1.4809 (0.0059) 130.78 (0.40) 122.35 (0.36) C44 - C45 N43 C45 - Distance Angles C44 1.3467 (0.0060) N41 1.4007 (0.0061) 106.82 (0.38) H45 0.9500 126.59 126.59 C45 - C44 N41 C46 - Distance Angles C44 1.4809 (0.0059) H46A 0.9800 109.47 H46B 0.9800 109.47 109.47 H46C 0.9800 109.47 109.47 109.47 C46 - C44 H46A H46B N41 - Distance Angles C42 1.3360 (0.0052) C45 1.4007 (0.0061) 108.04 (0.36) H41 0.8800 125.98 125.98 N41 - C42 C45 N43 - Distance Angles C42 1.3145 (0.0053) C44 1.3815 (0.0051) 109.67 (0.34) H43 0.8800 125.16 125.16 N43 - C42 C44 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.91 2.787(5) 170.9 N23-H23...O35A 0.84 1.75 2.555(4) 161.3 O5A-H5...O1B_$1 0.88 1.85 2.704(4) 163.3 N21-H21...O1A_$2 0.84 1.67 2.511(4) 175.6 O35B-H35...O31A_$3 0.88 1.77 2.646(4) 169.9 N43-H43...O1B_$3 0.88 1.93 2.784(4) 163.9 N41-H41...O31A_$4 FMAP and GRID set by program FMAP 2 1 19 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0980 for 2460 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.0578 0.4775 0.9416 [ 1.43 A from O5B ] Deepest hole -0.23 at 0.2157 0.8408 0.1292 [ 1.58 A from H45 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3528 / 22547 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0578 0.4775 -0.0584 1.00000 0.05 0.27 1.43 O5B 1.88 H25 2.35 H2B 2.45 H34B Q2 1 0.8807 0.3840 0.5859 1.00000 0.05 0.25 1.48 C44 1.49 H46B 1.73 N43 1.78 C46 Q3 1 0.4628 0.7498 0.0759 1.00000 0.05 0.24 1.18 H35 1.31 O35B 1.80 H32B 1.96 H32A Q4 1 0.8175 0.4016 0.3675 1.00000 0.05 0.23 1.46 H43 1.57 O1B 1.67 H5 2.07 O5A Q5 1 0.7746 0.1564 0.5777 1.00000 0.05 0.22 1.62 H46A 1.95 H26B 1.95 O35A 1.96 H46B Q6 1 0.6225 0.3001 0.7823 1.00000 0.05 0.22 1.17 H45 1.79 C45 1.85 H46A 2.04 O35B Q7 1 -0.1053 0.2243 0.2524 1.00000 0.05 0.21 1.70 O5A 1.77 H26A 2.05 H4B 2.12 H4A Q8 1 0.0534 0.0178 -0.4153 1.00000 0.05 0.21 1.18 O1B 1.56 H43 1.64 C1 2.00 O1A Q9 1 0.0620 0.3477 0.8711 1.00000 0.05 0.21 1.37 H25 1.56 O5B 1.59 H3B 1.85 H3A Q10 1 0.3118 0.4566 0.3165 1.00000 0.05 0.20 1.23 H33A 1.31 H23 1.74 H33B 1.76 C33 Q11 1 0.5307 0.4605 0.7982 1.00000 0.05 0.20 1.22 C45 1.25 H45 1.38 N41 1.49 H41 Q12 1 0.4460 0.4997 0.3055 1.00000 0.05 0.20 1.29 O35A 1.44 H33B 1.62 C35 1.71 C33 Q13 1 0.5623 0.3391 0.2116 1.00000 0.05 0.20 1.22 H33B 1.36 C32 1.44 H32B 1.48 C33 Q14 1 -0.1351 0.4194 0.2287 1.00000 0.05 0.20 0.49 H5 1.26 O5A 1.36 O1B 2.17 C5 Q15 1 0.4850 0.4613 -0.0182 1.00000 0.05 0.20 1.26 H34B 1.33 H34A 1.47 C34 2.01 H32A Q16 1 0.7909 0.2806 0.4720 1.00000 0.05 0.20 0.69 H46B 1.07 C46 1.19 H46C 1.79 H46A Q17 1 0.4619 0.5985 0.8061 1.00000 0.05 0.20 1.31 H41 1.48 O31A 1.83 H26C 1.96 N41 Q18 1 0.6586 0.5192 0.6543 1.00000 0.05 0.20 0.65 C42 0.81 N41 1.42 N43 1.54 H42 Q19 1 0.1009 0.6529 0.8227 1.00000 0.05 0.20 1.14 H26A 1.52 H4A 1.56 H4B 1.87 C4 Q20 1 0.3508 0.6633 0.2159 1.00000 0.05 0.19 1.13 O35B 1.22 C35 1.51 O35A 1.85 H35 Shortest distances between peaks (including symmetry equivalents) 10 12 1.20 7 19 1.25 4 14 1.46 3 6 1.74 11 15 1.85 2 16 1.92 4 8 1.95 6 20 1.96 1 9 1.97 11 18 1.97 4 16 2.02 11 17 2.03 5 16 2.05 3 20 2.08 2 4 2.14 5 20 2.31 8 14 2.32 6 11 2.39 4 13 2.47 17 18 2.48 7 16 2.49 13 14 2.54 12 20 2.56 15 17 2.58 2 8 2.61 12 13 2.64 2 18 2.68 1 19 2.78 7 14 2.79 10 13 2.80 13 15 2.84 4 7 2.85 17 19 2.85 5 8 2.88 7 13 2.98 2 9 2.99 Time profile in seconds ----------------------- 0.08: 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. 0.58: 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 0.72: Structure factors and derivatives 1.27: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.25: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0042p21 finished at 17:39:58 Total CPU time: 3.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++