+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0028pccn started at 16:54:33 on 06-May-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0028pccn in Pccn CELL 0.71073 20.5769 7.3521 14.0383 90.000 90.000 90.000 ZERR 8.00 0.0012 0.0004 0.0008 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, 1/2 - Y, Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, - Y, 1/2 - Z SFAC C H N O UNIT 72 112 16 32 V = 2123.76 F(000) = 912.0 Mu = 0.11 mm-1 Cell Wt = 1713.78 Rho = 1.340 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 EQIV_$1 x, -y+1/2, z-1/2 HTAB O1B O4A_$1 EQIV_$2 -x+3/2, -y+1/2, z HTAB N23 O4A_$2 FMAP 2 PLAN 10 SIZE 0.03 0.07 0.08 ACTA CONF BOND $H WGHT 0.04890 1.78330 L.S. 4 TEMP -153.00 FVAR 0.34767 MOLE 1 C1 1 0.562114 0.271068 0.666069 11.00000 0.02574 0.03174 = 0.02897 0.00089 -0.00284 0.00498 C2 1 0.518837 0.171202 0.734567 11.00000 0.02883 0.03278 = 0.03169 0.00130 -0.00149 -0.00243 AFIX 23 H2A 2 0.518692 0.040664 0.717262 11.00000 -1.20000 H2B 2 0.473902 0.217122 0.727026 11.00000 -1.20000 AFIX 0 C3 1 0.538136 0.188615 0.838460 11.00000 0.03014 0.03257 = 0.02721 -0.00078 -0.00045 0.00102 AFIX 23 H3A 2 0.542703 0.319397 0.853859 11.00000 -1.20000 H3B 2 0.502443 0.139647 0.878190 11.00000 -1.20000 AFIX 0 C4 1 0.600580 0.092559 0.865810 11.00000 0.02918 0.03052 = 0.02772 0.00448 0.00356 0.00140 O1A 4 0.604427 0.377249 0.689317 11.00000 0.03833 0.04075 = 0.03428 -0.00384 -0.00240 -0.01019 O1B 4 0.547955 0.231302 0.576684 11.00000 0.03699 0.04238 = 0.02542 -0.00077 -0.00147 -0.01045 AFIX 147 H1 2 0.575705 0.278629 0.540468 11.00000 0.06848 AFIX 0 O4A 4 0.623446 0.134825 0.947969 11.00000 0.03502 0.04714 = 0.02613 -0.00245 -0.00451 0.00740 O4B 4 0.625040 -0.021921 0.812408 11.00000 0.04016 0.03861 = 0.03038 -0.00352 0.00262 0.01155 MOLE 2 C22 1 0.710672 0.540154 0.955901 11.00000 0.03335 0.02957 = 0.03869 0.00096 -0.00083 -0.00773 C24 1 0.748851 0.488652 1.100514 11.00000 0.04106 0.03572 = 0.03252 0.00194 -0.00631 -0.00222 AFIX 43 H24 2 0.777386 0.454621 1.150639 11.00000 -1.20000 AFIX 0 C25 1 0.688219 0.551452 1.109940 11.00000 0.04289 0.03890 = 0.03315 -0.00033 0.00717 -0.00051 AFIX 43 H25 2 0.665455 0.570086 1.168000 11.00000 -1.20000 AFIX 0 C26 1 0.601153 0.661037 0.997707 11.00000 0.03362 0.04746 = 0.06334 0.01265 0.00673 0.00963 AFIX 137 H26A 2 0.596367 0.676237 0.928709 11.00000 -1.50000 H26B 2 0.596971 0.779579 1.029036 11.00000 -1.50000 H26C 2 0.567271 0.578942 1.021338 11.00000 -1.50000 AFIX 0 C27 1 0.704864 0.547739 0.851742 11.00000 0.04268 0.05115 = 0.03506 -0.00140 0.00013 -0.00519 AFIX 137 H27A 2 0.674852 0.452864 0.830079 11.00000 -1.50000 H27B 2 0.747656 0.528176 0.822861 11.00000 -1.50000 H27C 2 0.688206 0.667240 0.832761 11.00000 -1.50000 AFIX 0 N21 3 0.664773 0.584353 1.018549 11.00000 0.02844 0.03024 = 0.03905 0.00114 0.00615 -0.00176 N23 3 0.762254 0.482553 1.003536 11.00000 0.02977 0.03190 = 0.03915 -0.00120 0.00196 0.00091 AFIX 43 H23 2 0.799074 0.446272 0.977928 11.00000 0.07096 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0028pccn in Pccn C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C1 C3 C3 - C4 C2 C4 - O4B O4A C3 O1A - C1 O1B - C1 O4A - C4 O4B - C4 C22 - N23 N21 C27 C24 - C25 N23 C25 - C24 N21 C26 - N21 C27 - C22 N21 - C22 C25 C26 N23 - C22 C24 Operators for generating equivalent atoms: $1 x, -y+1/2, z-1/2 $2 -x+3/2, -y+1/2, z 47818 Reflections read, of which 3887 rejected -26 =< h =< 26, -9 =< k =< 9, -18 =< l =< 18, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2444 Unique reflections, of which 0 suppressed R(int) = 0.1637 R(sigma) = 0.0612 Friedel opposites merged Maximum memory for data reduction = 1771 / 24443 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 = 2176 / 177390 wR2 = 0.1560 before cycle 1 for 2444 data and 141 / 141 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0489 * P )^2 + 1.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34767 0.00109 -0.004 OSF Mean shift/esd = 0.002 Maximum = 0.004 for U12 C3 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H23 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2176 / 177390 wR2 = 0.1560 before cycle 2 for 2444 data and 141 / 141 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0489 * P )^2 + 1.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34766 0.00109 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.002 for U12 C3 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H23 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2176 / 177390 wR2 = 0.1560 before cycle 3 for 2444 data and 141 / 141 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0489 * P )^2 + 1.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34766 0.00109 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H26B Max. dU = 0.000 for H23 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2176 / 177390 wR2 = 0.1560 before cycle 4 for 2444 data and 141 / 141 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0489 * P )^2 + 1.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34766 0.00109 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z N21 Max. shift = 0.000 A for H26A Max. dU = 0.000 for H23 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 0.5187 0.0407 0.7173 23 0.990 0.000 C2 C1 C3 H2B 0.4739 0.2171 0.7270 23 0.990 0.000 C2 C1 C3 H3A 0.5427 0.3194 0.8539 23 0.990 0.000 C3 C4 C2 H3B 0.5024 0.1396 0.8782 23 0.990 0.000 C3 C4 C2 H1 0.5757 0.2786 0.5405 147 0.840 0.000 O1B C1 H1 H24 0.7774 0.4546 1.1506 43 0.950 0.000 C24 C25 N23 H25 0.6655 0.5701 1.1680 43 0.950 0.000 C25 C24 N21 H26A 0.5964 0.6762 0.9287 137 0.980 0.000 C26 N21 H26A H26B 0.5970 0.7796 1.0290 137 0.980 0.000 C26 N21 H26A H26C 0.5673 0.5789 1.0213 137 0.980 0.000 C26 N21 H26A H27A 0.6749 0.4529 0.8301 137 0.980 0.000 C27 C22 H27A H27B 0.7477 0.5282 0.8229 137 0.980 0.000 C27 C22 H27A H27C 0.6882 0.6672 0.8328 137 0.980 0.000 C27 C22 H27A H23 0.7991 0.4463 0.9779 43 0.880 0.000 N23 C22 C24 06skc0028pccn in Pccn ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.56211 0.27107 0.66607 1.00000 0.02574 0.03174 0.02897 0.00089 -0.00284 0.00498 0.02882 0.00453 0.00012 0.00036 0.00018 0.00000 0.00131 0.00142 0.00141 0.00112 0.00111 0.00116 0.00059 C2 0.51884 0.17120 0.73457 1.00000 0.02883 0.03278 0.03169 0.00129 -0.00149 -0.00243 0.03110 0.00445 0.00012 0.00036 0.00018 0.00000 0.00141 0.00143 0.00145 0.00116 0.00112 0.00112 0.00062 H2A 0.51869 0.04066 0.71726 1.00000 0.03732 0.00000 0.00000 H2B 0.47390 0.21712 0.72703 1.00000 0.03732 0.00000 0.00000 C3 0.53814 0.18862 0.83846 1.00000 0.03013 0.03257 0.02721 -0.00078 -0.00045 0.00103 0.02997 0.00448 0.00013 0.00036 0.00018 0.00000 0.00139 0.00144 0.00134 0.00109 0.00108 0.00113 0.00060 H3A 0.54270 0.31940 0.85386 1.00000 0.03596 0.00000 0.00000 H3B 0.50244 0.13965 0.87819 1.00000 0.03596 0.00000 0.00000 C4 0.60058 0.09256 0.86581 1.00000 0.02918 0.03052 0.02772 0.00448 0.00356 0.00140 0.02914 0.00459 0.00012 0.00035 0.00019 0.00000 0.00136 0.00136 0.00136 0.00114 0.00111 0.00113 0.00059 O1A 0.60443 0.37725 0.68932 1.00000 0.03833 0.04075 0.03428 -0.00384 -0.00240 -0.01019 0.03779 0.00310 0.00009 0.00026 0.00013 0.00000 0.00111 0.00111 0.00105 0.00088 0.00084 0.00093 0.00049 O1B 0.54796 0.23130 0.57668 1.00000 0.03699 0.04238 0.02542 -0.00077 -0.00147 -0.01045 0.03493 0.00300 0.00009 0.00027 0.00013 0.00000 0.00111 0.00113 0.00101 0.00083 0.00084 0.00090 0.00048 H1 0.57571 0.27862 0.54047 1.00000 0.06849 0.00000 0.01194 O4A 0.62345 0.13483 0.94797 1.00000 0.03502 0.04714 0.02613 -0.00245 -0.00451 0.00740 0.03610 0.00318 0.00009 0.00026 0.00012 0.00000 0.00104 0.00116 0.00099 0.00085 0.00080 0.00093 0.00048 O4B 0.62504 -0.02192 0.81241 1.00000 0.04015 0.03861 0.03038 -0.00352 0.00262 0.01155 0.03638 0.00330 0.00009 0.00025 0.00013 0.00000 0.00107 0.00109 0.00097 0.00084 0.00087 0.00090 0.00048 C22 0.71067 0.54015 0.95590 1.00000 0.03335 0.02956 0.03869 0.00096 -0.00083 -0.00773 0.03387 0.00453 0.00013 0.00036 0.00019 0.00000 0.00151 0.00138 0.00156 0.00118 0.00124 0.00120 0.00064 C24 0.74885 0.48865 1.10051 1.00000 0.04106 0.03571 0.03252 0.00194 -0.00631 -0.00222 0.03643 0.00473 0.00015 0.00037 0.00019 0.00000 0.00157 0.00153 0.00147 0.00120 0.00131 0.00131 0.00065 H24 0.77739 0.45462 1.15064 1.00000 0.04371 0.00000 0.00000 C25 0.68822 0.55145 1.10994 1.00000 0.04289 0.03890 0.03315 -0.00033 0.00717 -0.00051 0.03831 0.00490 0.00014 0.00037 0.00020 0.00000 0.00164 0.00159 0.00155 0.00124 0.00130 0.00136 0.00068 H25 0.66545 0.57009 1.16800 1.00000 0.04597 0.00000 0.00000 C26 0.60115 0.66104 0.99771 1.00000 0.03362 0.04746 0.06334 0.01265 0.00673 0.00964 0.04814 0.00587 0.00013 0.00043 0.00024 0.00000 0.00162 0.00180 0.00211 0.00158 0.00148 0.00137 0.00081 H26A 0.59637 0.67623 0.92871 1.00000 0.07221 0.00000 0.00000 H26B 0.59697 0.77958 1.02903 1.00000 0.07221 0.00000 0.00000 H26C 0.56727 0.57894 1.02134 1.00000 0.07221 0.00000 0.00000 C27 0.70486 0.54774 0.85174 1.00000 0.04268 0.05114 0.03506 -0.00140 0.00013 -0.00519 0.04296 0.00504 0.00015 0.00044 0.00019 0.00000 0.00172 0.00183 0.00162 0.00138 0.00130 0.00144 0.00074 H27A 0.67485 0.45287 0.83008 1.00000 0.06444 0.00000 0.00000 H27B 0.74766 0.52817 0.82286 1.00000 0.06444 0.00000 0.00000 H27C 0.68821 0.66724 0.83276 1.00000 0.06444 0.00000 0.00000 N21 0.66477 0.58435 1.01855 1.00000 0.02844 0.03024 0.03905 0.00114 0.00615 -0.00176 0.03258 0.00379 0.00010 0.00029 0.00016 0.00000 0.00116 0.00116 0.00130 0.00101 0.00100 0.00095 0.00053 N23 0.76225 0.48255 1.00354 1.00000 0.02977 0.03190 0.03914 -0.00120 0.00196 0.00091 0.03360 0.00374 0.00011 0.00029 0.00016 0.00000 0.00125 0.00122 0.00133 0.00100 0.00105 0.00099 0.00055 H23 0.79907 0.44627 0.97793 1.00000 0.07097 0.00000 0.01176 Final Structure Factor Calculation for 06skc0028pccn in Pccn Total number of l.s. parameters = 141 Maximum vector length = 511 Memory required = 2035 / 22995 wR2 = 0.1560 before cycle 5 for 2444 data and 0 / 141 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0489 * P )^2 + 1.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0685 for 1643 Fo > 4sig(Fo) and 0.1161 for all 2444 data wR2 = 0.1560, GooF = S = 1.107, Restrained GooF = 1.107 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0346 0.0301 0.0218 C1 0.0350 0.0308 0.0275 C2 0.0331 0.0298 0.0271 C3 0.0356 0.0283 0.0235 C4 0.0499 0.0367 0.0268 O1A 0.0505 0.0295 0.0248 O1B 0.0513 0.0327 0.0242 O4A 0.0510 0.0336 0.0245 O4B 0.0403 0.0378 0.0235 C22 0.0453 0.0349 0.0291 C24 0.0467 0.0388 0.0294 C25 0.0732 0.0425 0.0287 C26 0.0537 0.0403 0.0349 C27 0.0419 0.0310 0.0248 N21 0.0397 0.0322 0.0289 N23 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.005 0.011 0.015 0.021 0.027 0.036 0.046 0.062 0.096 1.000 Number in group 265. 279. 192. 271. 233. 240. 250. 229. 240. 245. GooF 1.224 1.255 1.181 1.016 1.045 1.011 1.169 0.961 0.973 1.163 K 16.721 2.838 1.533 1.214 1.117 0.974 1.024 0.983 1.012 0.992 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.66 inf Number in group 247. 244. 248. 242. 246. 246. 240. 244. 243. 244. GooF 1.083 0.987 1.051 1.106 0.995 1.033 0.938 1.108 1.208 1.469 K 0.972 1.209 1.153 1.090 1.039 1.031 1.002 0.996 1.018 0.991 R1 0.396 0.290 0.281 0.212 0.133 0.098 0.063 0.065 0.055 0.040 Recommended weighting scheme: WGHT 0.0488 1.7819 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 6 0 342.14 154.51 5.63 0.045 1.15 1 1 0 589.14 1144.99 5.47 0.124 6.92 9 3 0 236.83 127.14 4.25 0.041 1.67 4 0 0 1426.04 1060.47 3.79 0.119 5.14 1 0 2 237.07 146.87 3.66 0.044 6.64 4 3 3 42.66 13.50 3.42 0.013 2.00 12 1 6 31.56 3.14 3.35 0.006 1.36 9 3 3 25.07 0.26 3.32 0.002 1.57 1 4 3 27.52 3.35 3.31 0.007 1.70 3 3 9 35.88 6.39 3.30 0.009 1.29 4 5 4 24.06 1.65 3.22 0.005 1.31 4 1 8 39.33 10.34 3.16 0.012 1.62 5 7 4 32.74 1.23 2.99 0.004 0.98 9 0 8 178.46 267.02 2.99 0.060 1.39 3 3 6 29.86 5.85 2.98 0.009 1.64 14 1 13 58.15 0.11 2.94 0.001 0.86 2 1 7 93.42 53.07 2.93 0.027 1.90 3 4 5 29.55 6.16 2.90 0.009 1.50 14 2 2 28.46 4.08 2.88 0.007 1.34 5 6 2 21.16 0.57 2.87 0.003 1.16 4 3 1 38.21 14.01 2.85 0.014 2.19 5 5 0 3122.99 2580.46 2.78 0.186 1.38 2 5 2 126.93 78.43 2.77 0.032 1.43 8 3 14 58.25 123.88 2.76 0.041 0.87 16 7 1 55.22 136.63 2.69 0.043 0.81 1 2 2 603.36 483.08 2.69 0.080 3.22 11 4 14 125.23 33.14 2.64 0.021 0.80 6 4 16 -24.98 58.63 2.63 0.028 0.77 9 1 15 272.51 178.94 2.58 0.049 0.86 20 2 2 60.16 10.37 2.57 0.012 0.98 3 1 17 136.18 63.88 2.57 0.029 0.81 3 7 12 -26.95 30.73 2.57 0.020 0.78 2 7 10 46.64 125.77 2.56 0.041 0.84 20 6 3 94.68 7.62 2.56 0.010 0.78 3 4 6 26.58 6.29 2.55 0.009 1.41 24 2 6 151.08 60.40 2.53 0.028 0.79 7 1 2 23.82 6.16 2.53 0.009 2.54 2 3 3 2527.73 2157.49 2.52 0.170 2.12 6 3 3 952.38 791.79 2.49 0.103 1.83 7 3 15 193.47 109.38 2.46 0.038 0.84 6 1 2 1805.80 2124.36 2.46 0.169 2.84 3 3 0 74.97 42.61 2.45 0.024 2.31 10 3 4 18.46 0.00 2.43 0.000 1.44 10 3 7 23.41 3.40 2.42 0.007 1.24 1 0 4 651.68 793.23 2.41 0.103 3.46 4 1 3 39.15 18.13 2.41 0.016 3.13 9 1 4 100.72 65.14 2.40 0.030 1.85 2 0 2 19315.48 22363.52 2.40 0.547 5.80 3 3 3 263.67 201.77 2.40 0.052 2.07 0 3 16 107.30 15.73 2.39 0.015 0.83 Bond lengths and angles C1 - Distance Angles O1A 1.2141 (0.0030) O1B 1.3210 (0.0030) 123.77 (0.24) C2 1.5023 (0.0036) 124.56 (0.24) 111.66 (0.22) C1 - O1A O1B C2 - Distance Angles C1 1.5023 (0.0036) C3 1.5170 (0.0035) 114.77 (0.22) H2A 0.9900 108.57 108.57 H2B 0.9900 108.57 108.57 107.55 C2 - C1 C3 H2A C3 - Distance Angles C4 1.5156 (0.0036) C2 1.5170 (0.0035) 115.22 (0.22) H3A 0.9900 108.47 108.47 H3B 0.9900 108.47 108.47 107.49 C3 - C4 C2 H3A C4 - Distance Angles O4B 1.2344 (0.0031) O4A 1.2838 (0.0031) 124.14 (0.24) C3 1.5156 (0.0036) 120.63 (0.23) 115.18 (0.22) C4 - O4B O4A O1A - Distance Angles C1 1.2141 (0.0031) O1A - O1B - Distance Angles C1 1.3210 (0.0030) H1 0.8400 109.47 O1B - C1 O4A - Distance Angles C4 1.2838 (0.0031) O4A - O4B - Distance Angles C4 1.2344 (0.0031) O4B - C22 - Distance Angles N23 1.3240 (0.0035) N21 1.3308 (0.0034) 108.25 (0.24) C27 1.4682 (0.0038) 125.48 (0.26) 126.24 (0.26) C22 - N23 N21 C24 - Distance Angles C25 1.3369 (0.0042) N23 1.3898 (0.0035) 107.06 (0.24) H24 0.9500 126.47 126.47 C24 - C25 N23 C25 - Distance Angles C24 1.3369 (0.0042) N21 1.3919 (0.0036) 106.99 (0.23) H25 0.9500 126.50 126.50 C25 - C24 N21 C26 - Distance Angles N21 1.4551 (0.0034) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - N21 H26A H26B C27 - Distance Angles C22 1.4682 (0.0038) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C22 H27A H27B N21 - Distance Angles C22 1.3308 (0.0035) C25 1.3919 (0.0036) 108.71 (0.23) C26 1.4551 (0.0034) 126.89 (0.24) 124.37 (0.23) N21 - C22 C25 N23 - Distance Angles C22 1.3240 (0.0035) C24 1.3898 (0.0035) 108.99 (0.23) H23 0.8800 125.51 125.51 N23 - C22 C24 Selected torsion angles -9.19 ( 0.38) O1A - C1 - C2 - C3 171.71 ( 0.22) O1B - C1 - C2 - C3 -69.24 ( 0.30) C1 - C2 - C3 - C4 -15.01 ( 0.36) C2 - C3 - C4 - O4B 167.34 ( 0.22) C2 - C3 - C4 - O4A -0.24 ( 0.30) N23 - C24 - C25 - N21 -0.61 ( 0.30) N23 - C22 - N21 - C25 177.55 ( 0.27) C27 - C22 - N21 - C25 177.23 ( 0.25) N23 - C22 - N21 - C26 -4.61 ( 0.46) C27 - C22 - N21 - C26 0.53 ( 0.31) C24 - C25 - N21 - C22 -177.37 ( 0.25) C24 - C25 - N21 - C26 0.46 ( 0.30) N21 - C22 - N23 - C24 -177.72 ( 0.27) C27 - C22 - N23 - C24 -0.12 ( 0.31) C25 - C24 - N23 - C22 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.75 2.578(3) 169.2 O1B-H1...O4A_$1 0.88 1.75 2.624(3) 169.7 N23-H23...O4A_$2 FMAP and GRID set by program FMAP 2 2 11 GRID -3.125 -2 24 3.125 2 1 R1 = 0.1160 for 2444 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.34 at 0.3373 0.0820 0.5967 [ 1.16 A from C27 ] Deepest hole -0.23 at 0.7346 0.1181 0.0379 [ 0.89 A from N23 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2786 / 25234 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6627 0.5820 0.9033 1.00000 0.05 0.34 1.16 C27 1.27 C22 1.28 H27C 1.42 H27A Q2 1 0.7515 0.4633 0.9395 1.00000 0.05 0.26 0.94 N23 1.04 C22 1.12 H23 1.68 C27 Q3 1 0.7174 0.5187 1.0365 1.00000 0.05 0.23 1.07 N23 1.13 C24 1.15 C22 1.21 N21 Q4 1 0.5938 0.6897 1.0662 1.00000 0.05 0.23 0.84 H26B 1.00 C26 1.17 H26C 1.78 N21 Q5 1 0.6017 -0.0060 0.7536 1.00000 0.05 0.22 0.96 O4B 1.73 C4 1.82 H2A 1.84 H25 Q6 1 0.7500 0.7500 1.0515 0.50000 0.05 0.20 2.04 C24 2.09 N23 2.10 C25 2.18 N21 Q7 1 0.5918 0.6857 1.1135 1.00000 0.05 0.20 1.38 H26B 1.59 H26C 1.65 C26 1.90 H25 Q8 1 0.6492 0.1277 0.9928 1.00000 0.05 0.19 0.82 O4A 1.21 H23 1.79 H1 2.00 N23 Q9 1 0.5654 0.5013 0.9404 1.00000 0.05 0.18 1.27 H26C 1.44 H26A 1.60 C26 1.87 H3A Q10 1 0.6062 0.1487 1.0085 1.00000 0.05 0.18 0.93 O4A 0.94 H1 1.77 O1B 2.05 C4 Shortest distances between peaks (including symmetry equivalents) 4 7 0.67 8 10 0.93 2 3 1.58 3 6 1.84 1 2 2.09 1 9 2.15 1 3 2.23 2 8 2.27 4 9 2.32 5 7 2.38 2 6 2.63 1 4 2.80 7 9 2.84 3 4 2.87 9 10 2.89 4 5 2.96 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. 2.16: 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 0.59: Structure factors and derivatives 0.39: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0028pccn finished at 16:54:36 Total CPU time: 3.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++