+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0011p21c started at 15:25:33 on 21-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0011p21c in P2(1)/c CELL 0.71073 7.7814 22.3584 9.1957 90.000 103.329 90.000 ZERR 4.00 0.0003 0.0011 0.0005 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 48 88 16 24 V = 1556.77 F(000) = 680.0 Mu = 0.11 mm-1 Cell Wt = 1273.34 Rho = 1.358 MERG 2 OMIT -3.00 55.00 OMIT -1 2 1 SHEL 7 0.77 HTAB O6B O22 HTAB N23 O6A EQIV_$1 x+1, -y+1/2, z+1/2 HTAB O1A O32_$1 EQIV_$2 -x+1, y+1/2, -z+3/2 HTAB N21 O1B_$2 EQIV_$3 x-1, -y+1/2, z-1/2 HTAB N31 O1B_$3 EQIV_$4 -x+1, -y+1, -z+2 HTAB N33 O6A_$4 FMAP 2 MPLA C1 O1A O1B MPLA C6 O6A O6B PLAN 10 SIZE 0.04 0.06 0.13 ACTA BOND $H WGHT 0.01270 4.57130 L.S. 4 TEMP -153.00 FVAR 0.29161 MOLE 1 C1 1 0.903581 -0.028917 1.202119 11.00000 0.02372 0.02122 = 0.02284 0.00135 0.00096 0.00035 C2 1 0.893023 0.037360 1.166723 11.00000 0.02826 0.01439 = 0.02233 0.00263 0.00059 0.00220 AFIX 23 H2A 2 1.012091 0.051997 1.163271 11.00000 -1.20000 H2B 2 0.855365 0.058953 1.248104 11.00000 -1.20000 AFIX 0 C3 1 0.765178 0.051758 1.018942 11.00000 0.02364 0.01737 = 0.02320 0.00202 0.00198 -0.00055 AFIX 23 H3A 2 0.645216 0.038508 1.023747 11.00000 -1.20000 H3B 2 0.800206 0.029006 0.938035 11.00000 -1.20000 AFIX 0 C4 1 0.759842 0.118292 0.980831 11.00000 0.01803 0.01548 = 0.02191 -0.00044 0.00102 0.00139 AFIX 23 H4A 2 0.729753 0.141356 1.063460 11.00000 -1.20000 H4B 2 0.878237 0.131267 0.970888 11.00000 -1.20000 AFIX 0 C5 1 0.625164 0.131748 0.836399 11.00000 0.02683 0.01445 = 0.02703 -0.00006 -0.00138 -0.00037 AFIX 23 H5A 2 0.660344 0.110649 0.753154 11.00000 -1.20000 H5B 2 0.508895 0.115819 0.844127 11.00000 -1.20000 AFIX 0 C6 1 0.606514 0.197149 0.800287 11.00000 0.01978 0.02496 = 0.02010 0.00204 0.00209 0.00307 O1A 4 1.031473 -0.043090 1.315978 11.00000 0.03857 0.01787 = 0.03141 0.00305 -0.01527 -0.00010 AFIX 147 H1 2 1.032024 -0.080273 1.329159 11.00000 -1.5000 AFIX 0 O1B 4 0.802826 -0.065410 1.129882 11.00000 0.03731 0.01709 = 0.03293 0.00481 -0.01116 -0.00583 O6A 4 0.675108 0.236706 0.883720 11.00000 0.03046 0.01629 = 0.02708 -0.00086 -0.00401 0.00089 O6B 4 0.503452 0.207453 0.666205 11.00000 0.03741 0.01766 = 0.02665 0.00043 -0.00413 0.00291 AFIX 147 H6 2 0.492027 0.244509 0.652238 11.00000 -1.5000 AFIX 0 MOLE 2 C22 1 0.453894 0.362859 0.702913 11.00000 0.02300 0.01801 = 0.02464 0.00020 0.00185 0.00030 C24 1 0.546137 0.415660 0.922403 11.00000 0.04673 0.02116 = 0.02653 0.00179 -0.00249 0.00940 AFIX 23 H24A 2 0.660628 0.432579 0.976536 11.00000 -1.20000 H24B 2 0.473377 0.406252 0.994683 11.00000 -1.20000 AFIX 0 C25 1 0.449110 0.458131 0.799075 11.00000 0.03542 0.02169 = 0.02930 -0.00459 -0.00025 0.00350 AFIX 23 H25A 2 0.359709 0.482442 0.833378 11.00000 -1.20000 H25B 2 0.532541 0.485017 0.764383 11.00000 -1.20000 AFIX 0 N21 3 0.366883 0.416124 0.683001 11.00000 0.03158 0.02264 = 0.02013 0.00246 -0.00723 0.00360 AFIX 43 H21 2 0.322902 0.425845 0.593048 11.00000 -1.2000 AFIX 0 N23 3 0.570659 0.363381 0.835318 11.00000 0.03285 0.01766 = 0.02493 -0.00050 -0.00584 0.00923 AFIX 43 H23 2 0.618312 0.332855 0.876123 11.00000 -1.20000 AFIX 0 O22 4 0.425640 0.320805 0.611140 11.00000 0.02718 0.01761 = 0.02452 0.00040 0.00129 0.00107 MOLE 3 C32 1 0.006388 0.696526 0.806394 11.00000 0.02261 0.02000 = 0.02559 -0.00480 0.00334 -0.00045 C34 1 -0.036115 0.795239 0.732728 11.00000 0.02834 0.01788 = 0.02958 -0.00208 -0.00258 -0.00053 AFIX 23 H34A 2 0.050671 0.811016 0.678860 11.00000 -1.20000 H34B 2 -0.091281 0.829026 0.774679 11.00000 -1.20000 AFIX 0 C35 1 -0.175686 0.755950 0.630612 11.00000 0.02377 0.01983 = 0.02835 -0.00195 0.00256 0.00048 AFIX 23 H35A 2 -0.294410 0.762485 0.649657 11.00000 -1.20000 H35B 2 -0.180090 0.763677 0.523808 11.00000 -1.20000 AFIX 0 N31 3 -0.111276 0.696084 0.674027 11.00000 0.02913 0.01828 = 0.03047 -0.00575 -0.00547 -0.00217 AFIX 43 H31 2 -0.167590 0.662956 0.646351 11.00000 -1.2000 AFIX 0 N33 3 0.045196 0.753022 0.848343 11.00000 0.03310 0.01682 = 0.02220 -0.00451 -0.00400 -0.00390 AFIX 43 H33 2 0.122682 0.762488 0.919060 11.00000 -1.2000 AFIX 0 O32 4 0.072950 0.651694 0.881639 11.00000 0.03617 0.01706 = 0.03206 -0.00517 -0.00530 0.00218 HKLF 4 Covalent radii and connectivity table for 07skc0011p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C1 C3 C3 - C2 C4 C4 - C5 C3 C5 - C6 C4 C6 - O6A O6B C5 O1A - C1 O1B - C1 O6A - C6 O6B - C6 C22 - O22 N23 N21 C24 - N23 C25 C25 - N21 C24 N21 - C22 C25 N23 - C22 C24 O22 - C22 C32 - O32 N33 N31 C34 - N33 C35 C35 - N31 C34 N31 - C32 C35 N33 - C32 C34 O32 - C32 Operators for generating equivalent atoms: $1 x+1, -y+1/2, z+1/2 $2 -x+1, y+1/2, -z+3/2 $3 x-1, -y+1/2, z-1/2 $4 -x+1, -y+1, -z+2 14939 Reflections read, of which 265 rejected -10 =< h =< 9, -27 =< k =< 29, -11 =< l =< 11, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 7 9 0 2.50 0.33 4 1.70 -6 2 1 0.98 0.44 2 2.50 2 Inconsistent equivalents 3521 Unique reflections, of which 0 suppressed R(int) = 0.0880 R(sigma) = 0.0856 Friedel opposites merged Maximum memory for data reduction = 2468 / 34777 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 = 3062 / 249120 wR2 = 0.1897 before cycle 1 for 3521 data and 201 / 201 parameters GooF = S = 1.144; Restrained GooF = 1.144 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0127 * P )^2 + 4.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29161 0.00085 -0.004 OSF Mean shift/esd = 0.207 Maximum = 2.151 for U33 N21 Max. shift = 0.008 A for N21 Max. dU = 0.000 for N21 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3062 / 249120 wR2 = 0.1881 before cycle 2 for 3521 data and 201 / 201 parameters GooF = S = 1.134; Restrained GooF = 1.134 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0127 * P )^2 + 4.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29169 0.00084 0.098 OSF Mean shift/esd = 0.079 Maximum = 0.924 for U33 N21 Max. shift = 0.003 A for N21 Max. dU = 0.000 for N21 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3062 / 249120 wR2 = 0.1879 before cycle 3 for 3521 data and 201 / 201 parameters GooF = S = 1.133; Restrained GooF = 1.133 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0127 * P )^2 + 4.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29173 0.00084 0.042 OSF Mean shift/esd = 0.011 Maximum = -0.097 for z N21 Max. shift = 0.001 A for H1 Max. dU = 0.000 for N21 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3062 / 249120 wR2 = 0.1880 before cycle 4 for 3521 data and 201 / 201 parameters GooF = S = 1.133; Restrained GooF = 1.133 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0127 * P )^2 + 4.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29173 0.00084 0.002 OSF Mean shift/esd = 0.003 Maximum = 0.024 for U13 N21 Max. shift = 0.000 A for H1 Max. dU = 0.000 for N31 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 1.0122 0.0520 1.1633 23 0.990 0.000 C2 C1 C3 H2B 0.8556 0.0590 1.2482 23 0.990 0.000 C2 C1 C3 H3A 0.6452 0.0385 1.0238 23 0.990 0.000 C3 C2 C4 H3B 0.8001 0.0290 0.9380 23 0.990 0.000 C3 C2 C4 H4A 0.7294 0.1413 1.0636 23 0.990 0.000 C4 C5 C3 H4B 0.8782 0.1313 0.9713 23 0.990 0.000 C4 C5 C3 H5A 0.6606 0.1107 0.7533 23 0.990 0.000 C5 C6 C4 H5B 0.5089 0.1158 0.8440 23 0.990 0.000 C5 C6 C4 H1 1.0327 -0.0802 1.3288 147 0.840 0.000 O1A C1 H1 H6 0.4930 0.2445 0.6517 147 0.840 0.000 O6B C6 H6 H24A 0.6609 0.4325 0.9762 23 0.990 0.000 C24 N23 C25 H24B 0.4736 0.4065 0.9949 23 0.990 0.000 C24 N23 C25 H25A 0.3595 0.4823 0.8333 23 0.990 0.000 C25 N21 C24 H25B 0.5328 0.4852 0.7650 23 0.990 0.000 C25 N21 C24 H21 0.2760 0.4242 0.6088 43 0.880 0.000 N21 C22 C25 H23 0.6503 0.3353 0.8664 43 0.880 0.000 N23 C22 C24 H34A 0.0504 0.8112 0.6788 23 0.990 0.000 C34 N33 C35 H34B -0.0913 0.8290 0.7750 23 0.990 0.000 C34 N33 C35 H35A -0.2945 0.7626 0.6494 23 0.990 0.000 C35 N31 C34 H35B -0.1797 0.7635 0.5239 23 0.990 0.000 C35 N31 C34 H31 -0.1461 0.6637 0.6215 43 0.880 0.000 N31 C32 C35 H33 0.1132 0.7634 0.9352 43 0.880 0.000 N33 C32 C34 07skc0011p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.90362 -0.02891 1.20221 1.00000 0.02445 0.02098 0.02236 0.00109 0.00079 0.00011 0.02334 0.00713 0.00049 0.00017 0.00044 0.00000 0.00198 0.00200 0.00215 0.00157 0.00159 0.00156 0.00085 C2 0.89313 0.03736 1.16682 1.00000 0.02864 0.01444 0.02186 0.00290 0.00025 0.00240 0.02255 0.00704 0.00050 0.00016 0.00043 0.00000 0.00204 0.00175 0.00214 0.00153 0.00158 0.00151 0.00083 H2A 1.01219 0.05198 1.16329 1.00000 0.02706 0.00000 0.00000 H2B 0.85556 0.05897 1.24822 1.00000 0.02706 0.00000 0.00000 C3 0.76511 0.05173 1.01899 1.00000 0.02389 0.01726 0.02292 0.00205 0.00186 -0.00035 0.02193 0.00692 0.00049 0.00016 0.00043 0.00000 0.00196 0.00188 0.00214 0.00151 0.00155 0.00146 0.00083 H3A 0.64518 0.03846 1.02382 1.00000 0.02632 0.00000 0.00000 H3B 0.80014 0.02901 0.93804 1.00000 0.02632 0.00000 0.00000 C4 0.75975 0.11830 0.98105 1.00000 0.01829 0.01528 0.02206 -0.00033 0.00107 0.00074 0.01912 0.00659 0.00046 0.00015 0.00041 0.00000 0.00181 0.00177 0.00209 0.00144 0.00146 0.00139 0.00079 H4A 0.72941 0.14132 1.06364 1.00000 0.02295 0.00000 0.00000 H4B 0.87819 0.13131 0.97133 1.00000 0.02295 0.00000 0.00000 C5 0.62524 0.13175 0.83642 1.00000 0.02640 0.01472 0.02670 -0.00028 -0.00148 -0.00039 0.02384 0.00696 0.00051 0.00016 0.00044 0.00000 0.00203 0.00182 0.00228 0.00158 0.00162 0.00150 0.00086 H5A 0.66061 0.11066 0.75325 1.00000 0.02861 0.00000 0.00000 H5B 0.50892 0.11581 0.84398 1.00000 0.02861 0.00000 0.00000 C6 0.60663 0.19715 0.80032 1.00000 0.01986 0.02515 0.01972 0.00209 0.00207 0.00318 0.02198 0.00707 0.00047 0.00017 0.00042 0.00000 0.00186 0.00203 0.00206 0.00161 0.00150 0.00155 0.00082 O1A 1.03148 -0.04297 1.31595 1.00000 0.03940 0.01650 0.03228 0.00320 -0.01565 -0.00020 0.03327 0.00492 0.00038 0.00012 0.00033 0.00000 0.00168 0.00137 0.00176 0.00123 0.00130 0.00122 0.00074 H1 1.03271 -0.08018 1.32884 1.00000 0.04991 0.00000 0.00000 O1B 0.80271 -0.06541 1.12994 1.00000 0.03719 0.01683 0.03295 0.00467 -0.01083 -0.00583 0.03206 0.00493 0.00037 0.00011 0.00033 0.00000 0.00163 0.00140 0.00174 0.00119 0.00129 0.00120 0.00072 O6A 0.67510 0.23670 0.88381 1.00000 0.02961 0.01664 0.02763 -0.00083 -0.00445 0.00086 0.02642 0.00482 0.00035 0.00011 0.00030 0.00000 0.00148 0.00135 0.00164 0.00112 0.00118 0.00109 0.00065 O6B 0.50350 0.20743 0.66616 1.00000 0.03788 0.01760 0.02672 0.00049 -0.00416 0.00300 0.02928 0.00492 0.00037 0.00012 0.00031 0.00000 0.00166 0.00137 0.00164 0.00117 0.00124 0.00121 0.00068 H6 0.49299 0.24448 0.65175 1.00000 0.04393 0.00000 0.00000 C22 0.45391 0.36287 0.70292 1.00000 0.02284 0.01788 0.02571 0.00028 0.00195 0.00014 0.02274 0.00713 0.00049 0.00016 0.00045 0.00000 0.00195 0.00190 0.00220 0.00157 0.00156 0.00150 0.00084 C24 0.54622 0.41567 0.92237 1.00000 0.04690 0.02173 0.02589 0.00158 -0.00271 0.00924 0.03331 0.00808 0.00060 0.00017 0.00048 0.00000 0.00257 0.00207 0.00240 0.00175 0.00189 0.00187 0.00102 H24A 0.66093 0.43252 0.97622 1.00000 0.03997 0.00000 0.00000 H24B 0.47364 0.40646 0.99492 1.00000 0.03997 0.00000 0.00000 C25 0.44933 0.45812 0.79916 1.00000 0.03621 0.02176 0.02953 -0.00456 0.00000 0.00332 0.03040 0.00754 0.00057 0.00017 0.00047 0.00000 0.00232 0.00201 0.00241 0.00174 0.00181 0.00171 0.00095 H25A 0.35947 0.48226 0.83332 1.00000 0.03648 0.00000 0.00000 H25B 0.53277 0.48519 0.76504 1.00000 0.03648 0.00000 0.00000 N21 0.36767 0.41618 0.68213 1.00000 0.02798 0.02168 0.02617 0.00074 -0.00819 0.00359 0.02762 0.00596 0.00043 0.00014 0.00038 0.00000 0.00176 0.00172 0.00198 0.00142 0.00138 0.00138 0.00079 H21 0.27598 0.42420 0.60877 1.00000 0.03314 0.00000 0.00000 N23 0.57018 0.36318 0.83575 1.00000 0.03026 0.02008 0.02482 -0.00241 -0.00531 0.00936 0.02695 0.00591 0.00043 0.00014 0.00037 0.00000 0.00185 0.00166 0.00194 0.00138 0.00143 0.00136 0.00079 H23 0.65026 0.33533 0.86636 1.00000 0.03234 0.00000 0.00000 O22 0.42553 0.32078 0.61117 1.00000 0.02697 0.01768 0.02433 0.00050 0.00161 0.00102 0.02369 0.00479 0.00034 0.00011 0.00030 0.00000 0.00140 0.00132 0.00157 0.00112 0.00110 0.00109 0.00061 C32 0.00633 0.69651 0.80639 1.00000 0.02317 0.02022 0.02500 -0.00473 0.00375 -0.00070 0.02309 0.00695 0.00049 0.00017 0.00044 0.00000 0.00192 0.00191 0.00215 0.00161 0.00157 0.00152 0.00083 C34 -0.03607 0.79529 0.73280 1.00000 0.02869 0.01796 0.02933 -0.00217 -0.00268 -0.00083 0.02685 0.00700 0.00052 0.00017 0.00046 0.00000 0.00215 0.00189 0.00234 0.00166 0.00168 0.00158 0.00090 H34A 0.05044 0.81119 0.67881 1.00000 0.03222 0.00000 0.00000 H34B -0.09132 0.82900 0.77498 1.00000 0.03222 0.00000 0.00000 C35 -0.17569 0.75594 0.63066 1.00000 0.02356 0.01967 0.02843 -0.00236 0.00293 0.00081 0.02438 0.00707 0.00050 0.00016 0.00046 0.00000 0.00196 0.00193 0.00226 0.00163 0.00160 0.00152 0.00085 H35A -0.29451 0.76262 0.64936 1.00000 0.02926 0.00000 0.00000 H35B -0.17971 0.76353 0.52386 1.00000 0.02926 0.00000 0.00000 N31 -0.11178 0.69607 0.67458 1.00000 0.03063 0.01835 0.02906 -0.00795 -0.00562 -0.00067 0.02804 0.00583 0.00042 0.00014 0.00038 0.00000 0.00183 0.00165 0.00200 0.00142 0.00145 0.00138 0.00080 H31 -0.14612 0.66366 0.62153 1.00000 0.03365 0.00000 0.00000 N33 0.04579 0.75303 0.84825 1.00000 0.03496 0.01673 0.02054 -0.00452 -0.00271 -0.00317 0.02556 0.00577 0.00043 0.00013 0.00036 0.00000 0.00187 0.00159 0.00179 0.00133 0.00140 0.00137 0.00076 H33 0.11317 0.76343 0.93516 1.00000 0.03067 0.00000 0.00000 O32 0.07281 0.65166 0.88163 1.00000 0.03666 0.01667 0.03217 -0.00517 -0.00571 0.00228 0.03071 0.00491 0.00037 0.00011 0.00032 0.00000 0.00161 0.00138 0.00175 0.00119 0.00126 0.00119 0.00070 Final Structure Factor Calculation for 07skc0011p21c in P2(1)/c Total number of l.s. parameters = 201 Maximum vector length = 511 Memory required = 2861 / 22995 wR2 = 0.1880 before cycle 5 for 3521 data and 0 / 201 parameters GooF = S = 1.133; Restrained GooF = 1.133 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0127 * P )^2 + 4.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0934 for 2194 Fo > 4sig(Fo) and 0.1552 for all 3521 data wR2 = 0.1880, GooF = S = 1.133, Restrained GooF = 1.133 for all data Occupancy sum of asymmetric unit = 22.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0296 0.0213 0.0191 C1 0.0335 0.0214 0.0128 C2 0.0284 0.0209 0.0166 C3 0.0254 0.0169 0.0151 C4 0.0364 0.0204 0.0147 C5 0.0266 0.0228 0.0165 C6 0.0673 0.0184 0.0141 O1A 0.0614 0.0196 0.0152 O1B 0.0431 0.0196 0.0166 O6A 0.0489 0.0222 0.0168 O6B 0.0293 0.0211 0.0179 C22 0.0570 0.0259 0.0171 C24 0.0450 0.0266 0.0196 C25 0.0461 0.0225 0.0143 N21 0.0468 0.0202 0.0138 N23 0.0315 0.0221 0.0175 O22 0.0287 0.0233 0.0172 C32 0.0413 0.0222 0.0171 C34 0.0315 0.0227 0.0190 C35 0.0473 0.0241 0.0127 N31 0.0421 0.0223 0.0123 N33 0.0533 0.0238 0.0151 O32 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.004 0.008 0.012 0.016 0.021 0.027 0.035 0.048 0.069 1.000 Number in group 414. 348. 357. 323. 361. 347. 324. 361. 334. 352. GooF 1.127 1.210 1.134 1.149 1.142 1.281 1.050 1.064 1.009 1.131 K 11.957 2.814 1.537 1.279 1.100 1.097 1.018 1.001 1.007 1.016 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.65 inf Number in group 359. 352. 346. 354. 355. 351. 353. 346. 350. 355. GooF 1.257 1.282 1.115 1.116 1.092 1.088 1.004 1.063 1.016 1.249 K 1.173 1.234 1.117 1.063 1.048 1.029 0.991 0.989 1.019 1.021 R1 0.393 0.324 0.300 0.223 0.196 0.136 0.109 0.099 0.073 0.052 Recommended weighting scheme: WGHT 0.0107 5.4310 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) 1 3 0 208.21 352.06 3.42 0.057 5.31 -8 5 8 94.94 0.42 3.20 0.002 0.81 -6 3 3 46.52 5.22 3.15 0.007 1.25 -7 13 7 207.99 76.74 3.14 0.027 0.82 -2 12 6 171.48 61.50 3.12 0.024 1.17 -3 0 2 340.98 508.60 3.05 0.069 2.45 -3 5 11 118.19 1.99 2.99 0.004 0.82 -3 3 6 89.28 184.89 2.97 0.042 1.41 -4 3 1 3.79 54.05 2.95 0.022 1.88 -2 1 9 228.54 46.97 2.90 0.021 1.02 -2 15 7 82.71 196.81 2.85 0.043 0.98 -2 6 11 -16.88 61.36 2.84 0.024 0.82 2 0 4 7088.38 6199.51 2.83 0.241 1.76 -5 17 8 165.56 4.10 2.82 0.006 0.81 1 9 2 5901.29 5219.31 2.82 0.221 2.03 2 0 0 14262.85 15980.98 2.81 0.387 3.79 -5 7 11 -42.54 70.30 2.78 0.026 0.77 7 11 3 60.93 8.13 2.75 0.009 0.86 1 13 7 164.76 75.06 2.74 0.026 0.99 -5 10 8 78.28 4.03 2.73 0.006 0.93 4 23 4 94.00 3.05 2.73 0.005 0.78 1 18 1 45.61 4.22 2.72 0.006 1.21 -6 17 4 -18.52 59.65 2.70 0.024 0.90 -2 1 10 172.24 60.05 2.70 0.024 0.92 4 25 2 254.28 115.99 2.69 0.033 0.78 -1 15 5 71.03 149.61 2.67 0.037 1.16 -1 22 7 157.40 42.99 2.67 0.020 0.80 -9 11 2 122.56 24.66 2.67 0.015 0.79 -1 5 4 14.71 67.27 2.67 0.025 2.04 -2 28 1 193.64 33.86 2.64 0.018 0.78 -6 5 9 84.01 2.34 2.64 0.005 0.87 -1 3 2 5700.36 6438.17 2.64 0.245 3.73 -9 4 2 164.45 38.60 2.62 0.019 0.85 -2 8 3 45.65 108.70 2.61 0.032 1.93 -8 16 1 99.24 0.26 2.60 0.002 0.79 -3 11 7 268.43 166.39 2.59 0.039 1.07 -5 9 8 3.26 48.48 2.59 0.021 0.94 5 4 4 46.49 0.06 2.58 0.001 1.12 -3 1 1 258.51 165.27 2.57 0.039 2.57 -2 2 1 418.76 300.23 2.57 0.053 3.61 4 21 1 76.71 12.40 2.57 0.011 0.91 5 6 2 127.25 65.28 2.55 0.025 1.26 4 17 6 92.19 19.85 2.54 0.014 0.82 -6 12 8 60.76 5.50 2.54 0.007 0.85 -4 17 4 345.54 492.91 2.53 0.068 1.03 -6 16 1 163.22 66.26 2.53 0.025 0.95 -7 14 7 62.96 0.89 2.53 0.003 0.81 1 26 2 -13.43 32.05 2.52 0.017 0.84 2 11 6 579.80 771.37 2.52 0.085 1.09 2 4 8 5.52 62.26 2.52 0.024 1.00 Bond lengths and angles C1 - Distance Angles O1B 1.2179 (0.0044) O1A 1.3050 (0.0044) 123.54 (0.34) C2 1.5151 (0.0050) 122.82 (0.34) 113.64 (0.32) C1 - O1B O1A C2 - Distance Angles C1 1.5151 (0.0050) C3 1.5229 (0.0050) 112.94 (0.31) H2A 0.9900 109.00 109.00 H2B 0.9900 109.00 109.00 107.78 C2 - C1 C3 H2A C3 - Distance Angles C2 1.5229 (0.0050) C4 1.5270 (0.0047) 112.79 (0.30) H3A 0.9900 109.03 109.03 H3B 0.9900 109.03 109.03 107.80 C3 - C2 C4 H3A C4 - Distance Angles C5 1.5209 (0.0049) C3 1.5270 (0.0047) 111.69 (0.29) H4A 0.9900 109.28 109.28 H4B 0.9900 109.28 109.28 107.95 C4 - C5 C3 H4A C5 - Distance Angles C6 1.4991 (0.0051) C4 1.5209 (0.0049) 113.48 (0.31) H5A 0.9900 108.87 108.87 H5B 0.9900 108.87 108.87 107.71 C5 - C6 C4 H5A C6 - Distance Angles O6A 1.2110 (0.0044) O6B 1.3275 (0.0044) 123.10 (0.35) C5 1.4991 (0.0051) 124.47 (0.34) 112.42 (0.32) C6 - O6A O6B O1A - Distance Angles C1 1.3050 (0.0044) H1 0.8400 109.47 O1A - C1 O1B - Distance Angles C1 1.2179 (0.0044) O1B - O6A - Distance Angles C6 1.2110 (0.0044) O6A - O6B - Distance Angles C6 1.3275 (0.0044) H6 0.8400 109.47 O6B - C6 C22 - Distance Angles O22 1.2491 (0.0044) N23 1.3420 (0.0048) 126.57 (0.34) N21 1.3596 (0.0047) 124.12 (0.35) 109.32 (0.33) C22 - O22 N23 C24 - Distance Angles N23 1.4543 (0.0050) C25 1.5360 (0.0055) 101.40 (0.32) H24A 0.9900 111.49 111.49 H24B 0.9900 111.49 111.49 109.32 C24 - N23 C25 H24A C25 - Distance Angles N21 1.4580 (0.0049) C24 1.5360 (0.0055) 101.73 (0.30) H25A 0.9900 111.42 111.42 H25B 0.9900 111.43 111.42 109.28 C25 - N21 C24 H25A N21 - Distance Angles C22 1.3596 (0.0047) C25 1.4580 (0.0050) 110.06 (0.31) H21 0.8800 124.97 124.97 N21 - C22 C25 N23 - Distance Angles C22 1.3420 (0.0049) C24 1.4543 (0.0050) 110.98 (0.31) H23 0.8800 124.51 124.51 N23 - C22 C24 O22 - Distance Angles C22 1.2491 (0.0044) O22 - C32 - Distance Angles O32 1.2596 (0.0045) N33 1.3361 (0.0046) 123.83 (0.35) N31 1.3418 (0.0048) 126.83 (0.35) 109.34 (0.34) C32 - O32 N33 C34 - Distance Angles N33 1.4539 (0.0048) C35 1.5381 (0.0051) 101.72 (0.29) H34A 0.9900 111.43 111.43 H34B 0.9900 111.43 111.43 109.28 C34 - N33 C35 H34A C35 - Distance Angles N31 1.4525 (0.0048) C34 1.5381 (0.0052) 102.06 (0.30) H35A 0.9900 111.36 111.36 H35B 0.9900 111.36 111.36 109.23 C35 - N31 C34 H35A N31 - Distance Angles C32 1.3418 (0.0049) C35 1.4525 (0.0048) 111.33 (0.31) H31 0.8800 124.33 124.33 N31 - C32 C35 N33 - Distance Angles C32 1.3361 (0.0046) C34 1.4539 (0.0048) 111.80 (0.31) H33 0.8800 124.10 124.10 N33 - C32 C34 O32 - Distance Angles C32 1.2596 (0.0045) O32 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.80 2.628(4) 168.9 O6B-H6...O22 0.88 2.22 2.948(4) 140.4 N23-H23...O6A 0.84 1.68 2.507(4) 168.2 O1A-H1...O32_$1 0.88 2.15 2.900(4) 142.6 N21-H21...O1B_$2 0.88 2.24 3.003(4) 145.4 N31-H31...O1B_$3 0.88 2.05 2.894(4) 159.1 N33-H33...O6A_$4 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 6.0718 (0.0106) x + 2.6296 (0.1717) y + 7.1505 (0.0202) z = 3.0338 (0.0386) * 0.0000 (0.0000) C1 * 0.0000 (0.0000) O1A * 0.0000 (0.0000) O1B Rms deviation of fitted atoms = 0.0000 - 7.1250 (0.0078) x + 0.6642 (0.1546) y + 5.5284 (0.0213) z = 0.2332 (0.0236) Angle to previous plane (with approximate esd) = 15.37 ( 0.29 ) * 0.0000 (0.0000) C6 * 0.0000 (0.0000) O6A * 0.0000 (0.0000) O6B Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 1 21 GRID -2.778 24 -2 2.778 1 2 R1 = 0.1552 for 3521 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.55 at 0.3434 0.4281 0.5792 [ 0.65 A from H21 ] Deepest hole -0.37 at 0.2417 0.4294 0.6103 [ 0.29 A from H21 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 3155 / 31071 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3434 0.4281 0.5792 1.00000 0.05 0.55 0.65 H21 0.96 N21 1.93 C22 2.00 O1B Q2 1 0.2037 0.4284 0.9944 1.00000 0.05 0.47 2.16 H24B 2.44 H25A 2.73 H1 2.88 O1A Q3 1 0.5852 0.3250 0.8870 1.00000 0.05 0.42 0.62 H23 0.97 N23 1.96 C22 2.09 C24 Q4 1 0.6335 0.2880 0.8020 1.00000 0.05 0.32 1.20 H23 1.37 O6A 1.80 N23 1.83 H6 Q5 1 -0.2067 0.6663 0.6638 1.00000 0.05 0.32 0.68 H31 0.98 N31 1.98 C32 2.05 C35 Q6 1 0.8336 -0.0493 1.0309 1.00000 0.05 0.31 1.06 O1B 1.49 H21 1.61 C1 1.94 H3B Q7 1 0.5424 0.2994 0.6482 1.00000 0.05 0.31 1.01 O22 1.29 H6 1.70 C22 2.09 O6B Q8 1 0.7552 0.0823 0.9647 1.00000 0.05 0.31 0.82 C4 0.84 C3 1.28 H3B 1.45 H4B Q9 1 0.2661 0.3991 1.0260 1.00000 0.05 0.30 1.71 H24B 2.60 C24 2.78 H25A 2.97 H1 Q10 1 0.1954 0.7470 1.0371 1.00000 0.05 0.29 1.07 H33 1.16 O6A 1.86 N33 2.26 C6 Shortest distances between peaks (including symmetry equivalents) 2 9 0.83 3 4 1.25 4 7 1.45 1 6 1.59 4 10 1.91 3 7 2.22 3 10 2.33 5 6 2.93 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.70: 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 0.80: Structure factors and derivatives 0.97: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.11: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0011p21c finished at 15:25:36 Total CPU time: 2.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++