+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009skc0160p21c started at 12:40:51 on 17-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009skc0160p21c in P2(1)/c CELL 0.71073 12.1273 11.4724 11.5592 90.000 90.735 90.000 ZERR 8.00 0.0003 0.0004 0.0004 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O UNIT 56 128 16 V = 1608.09 F(000) = 592.0 Mu = 0.08 mm-1 Cell Wt = 1057.58 Rho = 1.092 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB O2 O22 EQIV_$1 x+1, y, z HTAB O21 O1_$1 EQIV_$2 -x+1, -y, -z+2 HTAB O22 O21_$2 EQIV_$3 -x, -y, -z+2 HTAB O1 O2_$3 FMAP 2 PLAN 10 ACTA SIZE 0.18 0.09 0.05 BOND $H WGHT 0.00000 3.53550 L.S. 8 TEMP -153.00 FVAR 0.79066 MOLE 1 C1 1 -0.000953 0.106433 0.764323 11.00000 0.02037 0.02284 = 0.02765 0.00198 0.00358 -0.00198 C2 1 -0.076652 0.171790 0.846466 11.00000 0.03044 0.04891 = 0.05329 -0.00306 0.01477 0.00146 AFIX 23 H2A 2 -0.031912 0.203334 0.911506 11.00000 -1.20000 H2B 2 -0.110178 0.238593 0.804755 11.00000 -1.20000 AFIX 0 C3 1 0.058566 0.009684 0.830835 11.00000 0.02343 0.04048 = 0.05006 0.01080 -0.00072 -0.00257 AFIX 23 H3A 2 0.004149 -0.050520 0.852599 11.00000 -1.20000 H3B 2 0.112854 -0.027393 0.779244 11.00000 -1.20000 AFIX 0 C4 1 0.082561 0.196414 0.719967 11.00000 0.02870 0.03481 = 0.05584 0.01124 0.00441 -0.00174 AFIX 23 H4A 2 0.041178 0.264819 0.690404 11.00000 -1.20000 H4B 2 0.128315 0.223108 0.786381 11.00000 -1.20000 AFIX 0 C5 1 0.159475 0.154293 0.624946 11.00000 0.02991 0.08557 = 0.04204 0.01805 0.01049 -0.00293 AFIX 137 H5A 2 0.201540 0.086755 0.652850 11.00000 -1.50000 H5B 2 0.210433 0.217086 0.604510 11.00000 -1.50000 H5C 2 0.115768 0.132032 0.556554 11.00000 -1.50000 AFIX 0 C6 1 -0.066682 0.048809 0.666804 11.00000 0.03102 0.05663 = 0.03891 -0.00407 -0.00025 -0.00538 AFIX 23 H6A 2 -0.115341 -0.011330 0.700309 11.00000 -1.20000 H6B 2 -0.014814 0.008930 0.614511 11.00000 -1.20000 AFIX 0 C7 1 -0.137864 0.134454 0.595096 11.00000 0.04539 0.13272 = 0.05480 0.04759 -0.02102 -0.02127 AFIX 137 H7A 2 -0.199414 0.161978 0.641937 11.00000 -1.50000 H7B 2 -0.166725 0.094751 0.526017 11.00000 -1.50000 H7C 2 -0.092678 0.201047 0.571776 11.00000 -1.50000 AFIX 0 O1 3 -0.162852 0.100569 0.892148 11.00000 0.02296 0.07924 = 0.04755 0.02235 0.01135 0.00260 AFIX 147 H1 2 -0.136695 0.056585 0.943707 11.00000 -1.50000 AFIX 0 O2 3 0.114216 0.049199 0.932600 11.00000 0.02761 0.09744 = 0.04325 0.02619 -0.00875 -0.01913 AFIX 147 H2 2 0.175850 0.076917 0.914897 11.00000 -1.50000 AFIX 0 MOLE 2 C21 1 0.495540 0.228305 0.887726 11.00000 0.01794 0.02705 = 0.02534 0.00238 0.00071 -0.00215 C22 1 0.568157 0.158896 0.972015 11.00000 0.02370 0.04167 = 0.02512 0.00240 0.00194 -0.00307 AFIX 23 H22A 2 0.626464 0.210791 1.003474 11.00000 -1.20000 H22B 2 0.522633 0.132658 1.037556 11.00000 -1.20000 AFIX 0 C23 1 0.404726 0.147806 0.839535 11.00000 0.02400 0.03728 = 0.03380 0.00449 -0.00226 -0.00494 AFIX 23 H23A 2 0.365372 0.188508 0.775769 11.00000 -1.20000 H23B 2 0.439518 0.077303 0.806734 11.00000 -1.20000 AFIX 0 C24 1 0.445849 0.330045 0.955597 11.00000 0.02820 0.03891 = 0.03821 -0.00263 0.00307 -0.00231 AFIX 23 H24A 2 0.405791 0.297778 1.022465 11.00000 -1.20000 H24B 2 0.506999 0.378437 0.986640 11.00000 -1.20000 AFIX 0 C25 1 0.367435 0.408689 0.887708 11.00000 0.03451 0.04189 = 0.07295 0.00801 0.00169 0.00802 AFIX 137 H25A 2 0.405544 0.440823 0.820602 11.00000 -1.50000 H25B 2 0.342860 0.472535 0.937456 11.00000 -1.50000 H25C 2 0.303394 0.363363 0.861340 11.00000 -1.50000 AFIX 0 C26 1 0.561994 0.268868 0.782508 11.00000 0.02693 0.03955 = 0.02535 0.00669 0.00165 -0.00238 AFIX 23 H26A 2 0.593316 0.199271 0.744403 11.00000 -1.20000 H26B 2 0.510592 0.306175 0.726530 11.00000 -1.20000 AFIX 0 C27 1 0.655498 0.353693 0.808809 11.00000 0.02480 0.03883 = 0.04655 0.01243 0.00359 -0.00323 AFIX 137 H27A 2 0.625938 0.423095 0.846902 11.00000 -1.50000 H27B 2 0.690880 0.376469 0.736490 11.00000 -1.50000 H27C 2 0.709883 0.316132 0.859970 11.00000 -1.50000 AFIX 0 O21 3 0.619050 0.059162 0.920265 11.00000 0.02341 0.03635 = 0.04658 0.00768 0.00585 0.00506 AFIX 147 H21 2 0.680864 0.078139 0.894245 11.00000 -1.50000 AFIX 0 O22 3 0.326374 0.112848 0.924045 11.00000 0.02092 0.04221 = 0.05352 0.01679 0.00072 -0.00580 AFIX 147 H22 2 0.355667 0.064439 0.969474 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2009skc0160p21c in P2(1)/c C 0.770 H 0.320 O 0.660 C1 - C6 C2 C3 C4 C2 - O1 C1 C3 - O2 C1 C4 - C5 C1 C5 - C4 C6 - C1 C7 C7 - C6 O1 - C2 O2 - C3 C21 - C22 C24 C23 C26 C22 - O21 C21 C23 - O22 C21 C24 - C25 C21 C25 - C24 C26 - C27 C21 C27 - C26 O21 - C22 O22 - C23 Operators for generating equivalent atoms: $1 x+1, y, z $2 -x+1, -y, -z+2 $3 -x, -y, -z+2 h k l Fo^2 Sigma Why rejected -2 0 5 29.16 7.03 observed but should be systematically absent -2 0 3 36.34 7.96 observed but should be systematically absent -2 0 3 30.01 6.39 observed but should be systematically absent 2 0 3 36.68 6.62 observed but should be systematically absent 2 0 3 33.95 5.77 observed but should be systematically absent 2 0 3 46.02 6.20 observed but should be systematically absent 2 0 5 15.24 3.71 observed but should be systematically absent 10 0 3 17.89 3.95 observed but should be systematically absent 18069 Reflections read, of which 648 rejected -15 =< h =< 15, -14 =< k =< 14, -15 =< l =< 14, Max. 2-theta = 54.96 8 Systematic absence violations 0 Inconsistent equivalents 3671 Unique reflections, of which 0 suppressed R(int) = 0.0690 R(sigma) = 0.0644 Friedel opposites merged Maximum memory for data reduction = 2549 / 36050 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 = 3128 / 211783 wR2 = 0.1888 before cycle 1 for 3671 data and 171 / 171 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.79066 0.00206 0.002 OSF Mean shift/su = 0.001 Maximum = -0.003 for U13 C21 Max. shift = 0.000 A for H5B Max. dU = 0.000 for C23 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3128 / 211783 wR2 = 0.1888 before cycle 2 for 3671 data and 171 / 171 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.79066 0.00206 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for U13 O22 Max. shift = 0.000 A for H25C Max. dU = 0.000 for C23 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3128 / 211783 wR2 = 0.1888 before cycle 3 for 3671 data and 171 / 171 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.79066 0.00206 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C22 Max. shift = 0.000 A for H2 Max. dU = 0.000 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3128 / 211783 wR2 = 0.1888 before cycle 4 for 3671 data and 171 / 171 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.79066 0.00206 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for H2 Max. dU = 0.000 for C7 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3128 / 211783 wR2 = 0.1888 before cycle 5 for 3671 data and 171 / 171 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.79066 0.00206 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C25 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3128 / 211783 wR2 = 0.1888 before cycle 6 for 3671 data and 171 / 171 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.79066 0.00206 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for H27A Max. dU = 0.000 for C7 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3128 / 211783 wR2 = 0.1888 before cycle 7 for 3671 data and 171 / 171 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.79066 0.00206 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for H22 Max. dU = 0.000 for C7 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3128 / 211783 wR2 = 0.1888 before cycle 8 for 3671 data and 171 / 171 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.79066 0.00206 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z O21 Max. shift = 0.000 A for C26 Max. dU = 0.000 for C7 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A -0.0319 0.2033 0.9115 23 0.990 0.000 C2 O1 C1 H2B -0.1102 0.2386 0.8048 23 0.990 0.000 C2 O1 C1 H3A 0.0041 -0.0505 0.8526 23 0.990 0.000 C3 O2 C1 H3B 0.1129 -0.0274 0.7792 23 0.990 0.000 C3 O2 C1 H4A 0.0412 0.2648 0.6904 23 0.990 0.000 C4 C5 C1 H4B 0.1283 0.2231 0.7864 23 0.990 0.000 C4 C5 C1 H5A 0.2015 0.0868 0.6528 137 0.980 0.000 C5 C4 H5A H5B 0.2104 0.2171 0.6045 137 0.980 0.000 C5 C4 H5A H5C 0.1158 0.1320 0.5566 137 0.980 0.000 C5 C4 H5A H6A -0.1153 -0.0113 0.7003 23 0.990 0.000 C6 C1 C7 H6B -0.0148 0.0089 0.6145 23 0.990 0.000 C6 C1 C7 H7A -0.1994 0.1620 0.6419 137 0.980 0.000 C7 C6 H7A H7B -0.1667 0.0948 0.5260 137 0.980 0.000 C7 C6 H7A H7C -0.0927 0.2010 0.5718 137 0.980 0.000 C7 C6 H7A H1 -0.1367 0.0566 0.9437 147 0.840 0.000 O1 C2 H1 H2 0.1759 0.0769 0.9149 147 0.840 0.000 O2 C3 H2 H22A 0.6265 0.2108 1.0035 23 0.990 0.000 C22 O21 C21 H22B 0.5226 0.1327 1.0376 23 0.990 0.000 C22 O21 C21 H23A 0.3654 0.1885 0.7758 23 0.990 0.000 C23 O22 C21 H23B 0.4395 0.0773 0.8067 23 0.990 0.000 C23 O22 C21 H24A 0.4058 0.2978 1.0225 23 0.990 0.000 C24 C25 C21 H24B 0.5070 0.3784 0.9866 23 0.990 0.000 C24 C25 C21 H25A 0.4055 0.4408 0.8206 137 0.980 0.000 C25 C24 H25A H25B 0.3429 0.4725 0.9375 137 0.980 0.000 C25 C24 H25A H25C 0.3034 0.3634 0.8613 137 0.980 0.000 C25 C24 H25A H26A 0.5933 0.1993 0.7444 23 0.990 0.000 C26 C27 C21 H26B 0.5106 0.3062 0.7265 23 0.990 0.000 C26 C27 C21 H27A 0.6259 0.4231 0.8469 137 0.980 0.000 C27 C26 H27A H27B 0.6909 0.3765 0.7365 137 0.980 0.000 C27 C26 H27A H27C 0.7099 0.3161 0.8600 137 0.980 0.000 C27 C26 H27A H21 0.6809 0.0781 0.8942 147 0.840 0.000 O21 C22 H21 H22 0.3557 0.0644 0.9695 147 0.840 0.000 O22 C23 H22 2009skc0160p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.00095 0.10643 0.76432 1.00000 0.02037 0.02284 0.02765 0.00198 0.00358 -0.00198 0.02359 0.00506 0.00023 0.00025 0.00025 0.00000 0.00128 0.00145 0.00152 0.00121 0.00114 0.00115 0.00061 C2 -0.07665 0.17179 0.84647 1.00000 0.03044 0.04891 0.05329 -0.00306 0.01477 0.00146 0.04409 0.00680 0.00028 0.00034 0.00033 0.00000 0.00171 0.00223 0.00227 0.00181 0.00163 0.00161 0.00090 H2A -0.03191 0.20333 0.91151 1.00000 0.05291 0.00000 0.00000 H2B -0.11018 0.23859 0.80475 1.00000 0.05291 0.00000 0.00000 C3 0.05857 0.00968 0.83083 1.00000 0.02343 0.04048 0.05006 0.01080 -0.00072 -0.00257 0.03800 0.00608 0.00026 0.00031 0.00031 0.00000 0.00152 0.00196 0.00214 0.00165 0.00145 0.00142 0.00081 H3A 0.00415 -0.05052 0.85260 1.00000 0.04560 0.00000 0.00000 H3B 0.11285 -0.02739 0.77924 1.00000 0.04560 0.00000 0.00000 C4 0.08256 0.19641 0.71997 1.00000 0.02870 0.03481 0.05584 0.01124 0.00441 -0.00174 0.03975 0.00650 0.00027 0.00031 0.00033 0.00000 0.00163 0.00190 0.00224 0.00166 0.00155 0.00144 0.00084 H4A 0.04118 0.26482 0.69040 1.00000 0.04770 0.00000 0.00000 H4B 0.12831 0.22311 0.78638 1.00000 0.04770 0.00000 0.00000 C5 0.15948 0.15429 0.62495 1.00000 0.02991 0.08557 0.04204 0.01805 0.01049 -0.00293 0.05242 0.00750 0.00029 0.00041 0.00033 0.00000 0.00178 0.00316 0.00208 0.00211 0.00158 0.00192 0.00109 H5A 0.20154 0.08675 0.65285 1.00000 0.07863 0.00000 0.00000 H5B 0.21043 0.21709 0.60451 1.00000 0.07863 0.00000 0.00000 H5C 0.11577 0.13203 0.55655 1.00000 0.07863 0.00000 0.00000 C6 -0.06668 0.04881 0.66680 1.00000 0.03102 0.05663 0.03891 -0.00407 -0.00025 -0.00538 0.04219 0.00606 0.00028 0.00035 0.00030 0.00000 0.00170 0.00237 0.00197 0.00175 0.00148 0.00165 0.00087 H6A -0.11534 -0.01133 0.70031 1.00000 0.05063 0.00000 0.00000 H6B -0.01481 0.00893 0.61451 1.00000 0.05063 0.00000 0.00000 C7 -0.13786 0.13445 0.59510 1.00000 0.04539 0.13272 0.05480 0.04759 -0.02102 -0.02127 0.07782 0.00873 0.00035 0.00051 0.00039 0.00000 0.00237 0.00485 0.00267 0.00298 0.00204 0.00276 0.00173 H7A -0.19941 0.16198 0.64194 1.00000 0.11674 0.00000 0.00000 H7B -0.16672 0.09475 0.52602 1.00000 0.11674 0.00000 0.00000 H7C -0.09268 0.20105 0.57178 1.00000 0.11674 0.00000 0.00000 O1 -0.16285 0.10057 0.89215 1.00000 0.02296 0.07924 0.04755 0.02235 0.01135 0.00260 0.04983 0.00502 0.00018 0.00027 0.00022 0.00000 0.00114 0.00204 0.00158 0.00141 0.00107 0.00123 0.00073 H1 -0.13669 0.05659 0.94371 1.00000 0.07474 0.00000 0.00000 O2 0.11422 0.04920 0.93260 1.00000 0.02761 0.09744 0.04325 0.02619 -0.00875 -0.01913 0.05618 0.00477 0.00020 0.00029 0.00022 0.00000 0.00124 0.00237 0.00150 0.00152 0.00108 0.00140 0.00083 H2 0.17585 0.07692 0.91490 1.00000 0.08427 0.00000 0.00000 C21 0.49554 0.22830 0.88773 1.00000 0.01794 0.02705 0.02534 0.00238 0.00071 -0.00215 0.02344 0.00493 0.00022 0.00026 0.00024 0.00000 0.00133 0.00154 0.00148 0.00121 0.00112 0.00113 0.00062 C22 0.56816 0.15890 0.97201 1.00000 0.02370 0.04167 0.02512 0.00240 0.00194 -0.00307 0.03015 0.00547 0.00024 0.00029 0.00026 0.00000 0.00144 0.00188 0.00154 0.00136 0.00121 0.00134 0.00070 H22A 0.62646 0.21079 1.00347 1.00000 0.03618 0.00000 0.00000 H22B 0.52263 0.13266 1.03756 1.00000 0.03618 0.00000 0.00000 C23 0.40473 0.14781 0.83953 1.00000 0.02400 0.03728 0.03380 0.00449 -0.00226 -0.00494 0.03171 0.00542 0.00024 0.00030 0.00027 0.00000 0.00147 0.00184 0.00170 0.00142 0.00129 0.00133 0.00072 H23A 0.36537 0.18851 0.77577 1.00000 0.03805 0.00000 0.00000 H23B 0.43952 0.07730 0.80673 1.00000 0.03805 0.00000 0.00000 C24 0.44585 0.33004 0.95560 1.00000 0.02820 0.03891 0.03821 -0.00263 0.00307 -0.00231 0.03508 0.00577 0.00026 0.00030 0.00029 0.00000 0.00158 0.00191 0.00184 0.00150 0.00138 0.00141 0.00076 H24A 0.40579 0.29778 1.02247 1.00000 0.04210 0.00000 0.00000 H24B 0.50700 0.37844 0.98664 1.00000 0.04210 0.00000 0.00000 C25 0.36743 0.40869 0.88771 1.00000 0.03451 0.04189 0.07295 0.00801 0.00169 0.00802 0.04977 0.00727 0.00030 0.00034 0.00037 0.00000 0.00187 0.00219 0.00277 0.00195 0.00184 0.00164 0.00100 H25A 0.40554 0.44082 0.82060 1.00000 0.07466 0.00000 0.00000 H25B 0.34286 0.47254 0.93746 1.00000 0.07466 0.00000 0.00000 H25C 0.30339 0.36336 0.86134 1.00000 0.07466 0.00000 0.00000 C26 0.56199 0.26887 0.78251 1.00000 0.02693 0.03955 0.02535 0.00669 0.00165 -0.00238 0.03060 0.00552 0.00025 0.00030 0.00026 0.00000 0.00154 0.00185 0.00155 0.00137 0.00123 0.00136 0.00071 H26A 0.59332 0.19927 0.74440 1.00000 0.03672 0.00000 0.00000 H26B 0.51059 0.30618 0.72653 1.00000 0.03672 0.00000 0.00000 C27 0.65550 0.35369 0.80881 1.00000 0.02480 0.03883 0.04655 0.01243 0.00359 -0.00323 0.03670 0.00600 0.00025 0.00030 0.00031 0.00000 0.00152 0.00190 0.00201 0.00159 0.00142 0.00140 0.00079 H27A 0.62594 0.42309 0.84690 1.00000 0.05505 0.00000 0.00000 H27B 0.69088 0.37647 0.73649 1.00000 0.05505 0.00000 0.00000 H27C 0.70988 0.31613 0.85997 1.00000 0.05505 0.00000 0.00000 O21 0.61905 0.05916 0.92026 1.00000 0.02341 0.03635 0.04658 0.00768 0.00585 0.00506 0.03540 0.00414 0.00017 0.00020 0.00021 0.00000 0.00106 0.00128 0.00139 0.00108 0.00098 0.00095 0.00055 H21 0.68086 0.07814 0.89425 1.00000 0.05310 0.00000 0.00000 O22 0.32637 0.11285 0.92404 1.00000 0.02092 0.04221 0.05352 0.01679 0.00072 -0.00580 0.03888 0.00428 0.00017 0.00021 0.00021 0.00000 0.00105 0.00143 0.00152 0.00118 0.00101 0.00099 0.00059 H22 0.35567 0.06444 0.96947 1.00000 0.05832 0.00000 0.00000 Final Structure Factor Calculation for 2009skc0160p21c in P2(1)/c Total number of l.s. parameters = 171 Maximum vector length = 511 Memory required = 2957 / 21973 wR2 = 0.1888 before cycle 9 for 3671 data and 0 / 171 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0964 for 2485 Fo > 4sig(Fo) and 0.1426 for all 3671 data wR2 = 0.1888, GooF = S = 1.105, Restrained GooF = 1.105 for all data Occupancy sum of asymmetric unit = 18.00 for non-hydrogen and 32.00 for hydrogen atoms Principal mean square atomic displacements U 0.0291 0.0239 0.0177 C1 0.0603 0.0488 0.0232 C2 0.0573 0.0337 0.0230 C3 0.0609 0.0324 0.0259 C4 0.0921 0.0434 0.0218 C5 0.0585 0.0384 0.0297 C6 0.1626 0.0459 0.0250 C7 0.0915 0.0399 0.0180 O1 0.1134 0.0328 0.0223 O2 0.0290 0.0240 0.0173 C21 0.0424 0.0262 0.0218 C22 0.0421 0.0308 0.0223 C23 0.0420 0.0359 0.0273 C24 0.0751 0.0451 0.0291 C25 0.0424 0.0276 0.0218 C26 0.0557 0.0323 0.0221 C27 0.0524 0.0325 0.0213 O21 0.0659 0.0322 0.0186 O22 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.015 0.022 0.030 0.040 0.052 0.067 0.089 0.140 1.000 Number in group 417. 361. 342. 364. 384. 363. 353. 353. 364. 370. GooF 1.271 1.228 1.122 1.207 1.069 0.997 1.048 1.055 0.929 1.048 K 15.373 3.327 1.754 1.384 1.145 1.090 1.035 1.040 1.002 0.998 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 367. 377. 362. 362. 377. 362. 366. 362. 368. 368. GooF 1.161 1.132 1.099 1.067 1.065 0.953 0.966 0.997 0.993 1.504 K 1.296 1.186 1.184 1.150 1.023 1.009 0.990 1.000 1.021 1.003 R1 0.363 0.329 0.282 0.253 0.202 0.143 0.106 0.077 0.069 0.053 Recommended weighting scheme: WGHT 0.0000 3.5354 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)/su Fc/Fc(max) Resolution(A) -2 1 2 46.77 0.03 5.30 0.001 3.95 -2 3 2 290.18 143.24 4.84 0.097 2.83 -2 1 6 58.60 2.68 4.70 0.013 1.82 -2 3 4 52.45 2.46 4.62 0.013 2.16 4 4 3 59.32 0.39 4.44 0.005 1.83 -4 3 2 216.56 113.07 3.86 0.086 2.21 -4 4 4 87.61 13.28 3.85 0.029 1.70 2 1 6 34.11 3.01 3.78 0.014 1.81 -2 2 4 179.86 91.97 3.58 0.078 2.38 4 1 3 49.69 11.30 3.44 0.027 2.32 0 6 0 36.10 4.36 3.34 0.017 1.91 2 1 3 130.78 65.76 3.29 0.066 3.11 3 0 2 261.24 153.36 3.27 0.100 3.29 4 4 1 21.48 0.18 3.20 0.003 2.05 3 2 3 81.97 33.20 3.13 0.047 2.50 6 1 4 43.67 11.43 3.08 0.027 1.63 -6 5 2 33.33 3.41 3.06 0.015 1.47 -3 4 2 479.30 346.32 3.06 0.150 2.17 -1 8 4 25.04 2.77 3.06 0.013 1.28 -3 0 4 568.71 413.07 2.88 0.164 2.37 5 4 13 143.87 6.42 2.87 0.020 0.80 2 2 1 302.49 207.51 2.86 0.116 3.91 6 1 7 22.76 0.00 2.85 0.000 1.26 4 6 2 20.55 0.97 2.84 0.008 1.55 -4 8 4 23.68 0.58 2.83 0.006 1.19 -3 2 2 1406.22 1653.36 2.81 0.329 2.88 -10 3 7 36.20 2.21 2.81 0.012 0.95 4 5 1 33.80 7.56 2.78 0.022 1.80 -1 11 6 22.15 0.59 2.74 0.006 0.91 8 9 6 98.60 41.83 2.74 0.052 0.87 -2 5 1 26.83 0.98 2.72 0.008 2.11 -4 7 12 55.61 10.17 2.72 0.026 0.80 -4 0 12 21.99 76.56 2.72 0.071 0.92 -3 14 3 197.06 85.94 2.67 0.075 0.79 1 5 2 12.85 0.07 2.66 0.002 2.10 -11 10 2 52.20 9.67 2.65 0.025 0.79 -1 1 13 66.35 14.55 2.64 0.031 0.88 9 10 1 46.84 7.00 2.63 0.021 0.87 1 6 5 18.84 1.74 2.62 0.011 1.46 -5 3 5 268.93 184.10 2.62 0.110 1.54 5 1 6 437.83 325.38 2.61 0.146 1.49 0 13 4 37.39 1.43 2.59 0.010 0.84 -2 11 7 7.01 51.63 2.59 0.058 0.87 -3 8 12 31.62 1.42 2.56 0.010 0.79 -11 3 10 -8.34 21.84 2.56 0.038 0.79 9 8 3 29.26 0.75 2.54 0.007 0.95 12 4 3 183.33 272.86 2.53 0.133 0.92 -2 0 10 -6.19 19.03 2.53 0.035 1.14 10 8 2 36.20 1.87 2.51 0.011 0.91 -1 2 2 962.60 1140.24 2.51 0.273 3.87 Bond lengths and angles C1 - Distance Angles C6 1.5232 (0.0044) C2 1.5261 (0.0043) 111.13 (0.27) C3 1.5264 (0.0043) 107.26 (0.27) 109.16 (0.27) C4 1.5387 (0.0041) 112.65 (0.27) 106.35 (0.26) 110.28 (0.25) C1 - C6 C2 C3 C2 - Distance Angles O1 1.4330 (0.0040) C1 1.5261 (0.0043) 113.37 (0.30) H2A 0.9900 108.90 108.90 H2B 0.9900 108.90 108.90 107.73 C2 - O1 C1 H2A C3 - Distance Angles O2 1.4228 (0.0042) C1 1.5264 (0.0043) 113.64 (0.30) H3A 0.9900 108.84 108.84 H3B 0.9900 108.84 108.84 107.69 C3 - O2 C1 H3A C4 - Distance Angles C5 1.5285 (0.0049) C1 1.5387 (0.0041) 115.96 (0.31) H4A 0.9900 108.29 108.29 H4B 0.9900 108.29 108.29 107.40 C4 - C5 C1 H4A C5 - Distance Angles C4 1.5285 (0.0049) H5A 0.9800 109.47 H5B 0.9800 109.47 109.47 H5C 0.9800 109.47 109.47 109.47 C5 - C4 H5A H5B C6 - Distance Angles C1 1.5232 (0.0044) C7 1.5425 (0.0056) 113.90 (0.35) H6A 0.9900 108.78 108.78 H6B 0.9900 108.78 108.78 107.66 C6 - C1 C7 H6A C7 - Distance Angles C6 1.5425 (0.0056) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C6 H7A H7B O1 - Distance Angles C2 1.4330 (0.0041) H1 0.8400 109.47 O1 - C2 O2 - Distance Angles C3 1.4228 (0.0042) H2 0.8400 109.47 O2 - C3 C21 - Distance Angles C22 1.5287 (0.0041) C24 1.5340 (0.0043) 107.29 (0.24) C23 1.5363 (0.0041) 108.81 (0.25) 111.00 (0.24) C26 1.5396 (0.0039) 110.97 (0.23) 112.77 (0.26) 105.98 (0.24) C21 - C22 C24 C23 C22 - Distance Angles O21 1.4344 (0.0038) C21 1.5287 (0.0041) 113.40 (0.24) H22A 0.9900 108.89 108.89 H22B 0.9900 108.89 108.89 107.73 C22 - O21 C21 H22A C23 - Distance Angles O22 1.4289 (0.0036) C21 1.5363 (0.0041) 113.62 (0.26) H23A 0.9900 108.84 108.84 H23B 0.9900 108.84 108.84 107.70 C23 - O22 C21 H23A C24 - Distance Angles C25 1.5215 (0.0047) C21 1.5340 (0.0043) 115.75 (0.29) H24A 0.9900 108.34 108.34 H24B 0.9900 108.34 108.34 107.43 C24 - C25 C21 H24A C25 - Distance Angles C24 1.5215 (0.0048) H25A 0.9800 109.47 H25B 0.9800 109.47 109.47 H25C 0.9800 109.47 109.47 109.47 C25 - C24 H25A H25B C26 - Distance Angles C27 1.5220 (0.0043) C21 1.5396 (0.0039) 115.57 (0.26) H26A 0.9900 108.39 108.39 H26B 0.9900 108.39 108.39 107.45 C26 - C27 C21 H26A C27 - Distance Angles C26 1.5220 (0.0043) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C26 H27A H27B O21 - Distance Angles C22 1.4344 (0.0038) H21 0.8400 109.47 O21 - C22 O22 - Distance Angles C23 1.4289 (0.0036) H22 0.8400 109.47 O22 - C23 Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.87 2.678(3) 159.9 O2-H2...O22 0.84 1.91 2.711(3) 158.2 O21-H21...O1_$1 0.84 1.93 2.746(3) 164.1 O22-H22...O21_$2 0.84 1.89 2.715(4) 166.1 O1-H1...O2_$3 FMAP and GRID set by program FMAP 2 2 16 GRID -1.923 -2 -2 1.923 2 2 R1 = 0.1426 for 3671 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.34 at 0.9005 0.0108 0.8158 [ 1.37 A from H6A ] Deepest hole -0.24 at 0.9469 0.2261 0.8157 [ 0.72 A from H2B ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3033 / 20289 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0995 0.0108 0.8158 1.00000 0.05 0.34 1.37 H6A 1.50 H3A 1.56 O1 1.64 H1 Q2 1 -0.0693 0.2266 0.7191 1.00000 0.05 0.33 1.12 H2B 1.45 H4A 1.60 C2 1.69 C1 Q3 1 0.3356 0.3742 0.8050 1.00000 0.05 0.26 0.77 H25C 1.10 C25 1.15 H25A 1.90 H25B Q4 1 0.0680 0.1687 0.8635 1.00000 0.05 0.25 1.32 H4B 1.40 H2A 1.58 C1 1.68 O2 Q5 1 0.0693 0.0381 0.6715 1.00000 0.05 0.23 1.25 H6B 1.54 H3B 1.59 C1 1.65 C6 Q6 1 -0.0985 0.0936 0.9723 1.00000 0.05 0.22 0.71 H1 1.21 O1 1.66 H2A 1.73 C2 Q7 1 0.6198 -0.0407 0.8452 1.00000 0.05 0.21 1.44 O21 1.65 H21 1.95 H25A 2.18 H22 Q8 1 0.6046 0.0985 0.9638 1.00000 0.05 0.21 0.70 O21 0.83 C22 1.25 H21 1.38 H22B Q9 1 0.3555 0.0625 0.7191 1.00000 0.05 0.20 1.44 H23B 1.59 H23A 1.79 H27A 1.80 C23 Q10 1 0.5423 0.1790 0.9046 1.00000 0.05 0.20 0.82 C21 0.87 C22 1.57 H22A 1.65 H22B Shortest distances between peaks (including symmetry equivalents) 8 10 1.37 1 6 2.04 3 7 2.07 7 8 2.11 2 4 2.43 4 6 2.54 1 5 2.68 4 5 2.68 1 2 2.74 1 4 2.77 7 10 2.78 2 5 2.80 Time profile in seconds ----------------------- 0.05: 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 0.02: 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. 0.84: 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 1.67: Structure factors and derivatives 1.50: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.19: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009skc0160p21c finished at 12:40:56 Total CPU time: 4.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++