++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker Analytical X-ray Solutions All Rights Reserved + + 2007src1051 started at 11:28:49 on 14-Aug-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007SRC1051 in Pna2(1) CELL 0.71073 14.7643 13.3490 10.3953 90.000 90.000 90.000 ZERR 4.00 0.0007 0.0006 0.0003 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H N O S Cl UNIT 88 112 4 8 4 4 V = 2048.80 F(000) = 864.0 Mu = 0.31 mm-1 Cell Wt = 1623.86 Rho = 1.316 TEMP -153 SIZE 0.2x0.2x.01 BOND $H OMIT -3 55 SHEL 7 0.77 L.S. 6 FMAP 2 PLAN 20 ACTA WGHT 0.0390 0.3846 FVAR 0.15047 S1 5 0.80508 0.23438 0.86861 11.00000 0.01727 0.02452 = 0.02773 -0.00017 -0.00099 0.00232 CL1 6 1.00462 -0.03823 0.99379 11.00000 0.04820 0.02516 = 0.04656 0.00535 0.01634 -0.00008 O1 4 0.78189 0.27728 0.99095 11.00000 0.02341 0.02965 = 0.03359 -0.00529 0.00467 0.00267 O2 4 0.77149 0.27896 0.75209 11.00000 0.02479 0.03056 = 0.03431 0.00789 -0.00569 0.00428 C16 1 0.76825 0.10842 0.87318 11.00000 0.01422 0.02565 = 0.02813 0.00093 -0.00291 0.00130 N1 3 0.91445 0.23578 0.85701 11.00000 0.01473 0.02511 = 0.02302 0.00076 0.00128 0.00142 C18 1 0.73362 -0.04546 0.76428 11.00000 0.02932 0.03140 = 0.03906 -0.01087 -0.00824 -0.00085 AFIX 43 H18 2 0.73009 -0.08334 0.68707 11.00000 -1.20000 AFIX 0 C7 1 1.19832 -0.02463 0.86003 11.00000 0.02846 0.02978 = 0.04162 -0.00255 0.00047 0.00442 AFIX 137 H7A 2 1.18634 -0.05605 0.94351 11.00000 -1.50000 H7B 2 1.22188 0.04320 0.87346 11.00000 -1.50000 H7C 2 1.24307 -0.06445 0.81278 11.00000 -1.50000 AFIX 0 C20 1 0.71519 -0.03320 0.99201 11.00000 0.03014 0.03806 = 0.03476 0.00877 0.00053 -0.00519 AFIX 43 H20 2 0.69905 -0.06269 1.07196 11.00000 -1.20000 AFIX 0 C2 1 1.05072 0.14281 0.88756 11.00000 0.01740 0.02593 = 0.02136 0.00112 0.00109 0.00039 AFIX 13 H2 2 1.10812 0.14823 0.93815 11.00000 -1.20000 AFIX 0 C21 1 0.74411 0.06448 0.98931 11.00000 0.02543 0.03778 = 0.02488 0.00265 -0.00013 -0.00164 AFIX 43 H21 2 0.74763 0.10200 1.06681 11.00000 -1.20000 AFIX 0 C9 1 1.06172 0.24309 1.16295 11.00000 0.02614 0.02583 = 0.02774 0.00225 -0.00530 0.00151 AFIX 23 H9A 2 1.03540 0.18097 1.19911 11.00000 -1.20000 H9B 2 1.12284 0.22661 1.12999 11.00000 -1.20000 AFIX 0 C17 1 0.76318 0.05281 0.75903 11.00000 0.02408 0.03293 = 0.02907 -0.00256 0.00030 -0.00307 AFIX 43 H17 2 0.77980 0.08217 0.67920 11.00000 -1.20000 AFIX 0 C10 1 1.07101 0.31971 1.27009 11.00000 0.01745 0.02911 = 0.02560 -0.00360 0.00035 -0.00181 C19 1 0.70899 -0.08999 0.87990 11.00000 0.02025 0.02960 = 0.04798 0.00563 -0.00166 -0.00110 C5 1 1.03274 0.03311 0.85118 11.00000 0.02271 0.02588 = 0.02668 0.00006 -0.00231 0.00258 AFIX 13 H5 2 0.97912 0.03152 0.79244 11.00000 -1.20000 AFIX 0 C22 1 0.67324 -0.19579 0.88347 11.00000 0.03431 0.03082 = 0.07812 0.00430 -0.01037 -0.00569 AFIX 137 H22A 2 0.69339 -0.23183 0.80648 11.00000 -1.50000 H22B 2 0.60690 -0.19445 0.88589 11.00000 -1.50000 H22C 2 0.69620 -0.22985 0.96036 11.00000 -1.50000 AFIX 0 C11 1 1.09976 0.28823 1.39176 11.00000 0.02797 0.03122 = 0.03385 0.00619 0.00205 -0.00732 AFIX 43 H11 2 1.11276 0.21941 1.40593 11.00000 -1.20000 AFIX 0 C14 1 1.06200 0.48813 1.35355 11.00000 0.03273 0.02873 = 0.04670 -0.00693 -0.00550 0.00445 AFIX 43 H14 2 1.04773 0.55678 1.34055 11.00000 -1.20000 AFIX 0 C12 1 1.10954 0.35552 1.49151 11.00000 0.03247 0.04428 = 0.02436 0.00247 0.00231 -0.01109 AFIX 43 H12 2 1.12937 0.33260 1.57332 11.00000 -1.20000 AFIX 0 C6 1 1.11111 -0.01935 0.78314 11.00000 0.02859 0.03419 = 0.02906 -0.00451 -0.00171 0.00574 AFIX 23 H6A 2 1.09208 -0.08841 0.76134 11.00000 -1.20000 H6B 2 1.12347 0.01613 0.70137 11.00000 -1.20000 AFIX 0 C8 1 1.00272 0.27789 1.05030 11.00000 0.02904 0.02256 = 0.02623 -0.00020 -0.00467 0.00157 AFIX 23 H8A 2 0.94836 0.31185 1.08504 11.00000 -1.20000 H8B 2 1.03709 0.32772 0.99938 11.00000 -1.20000 AFIX 0 C4 1 0.95819 0.22830 0.72945 11.00000 0.01965 0.03755 = 0.02494 0.00224 0.00182 -0.00148 AFIX 23 H4A 2 0.95181 0.29144 0.68032 11.00000 -1.20000 H4B 2 0.93256 0.17243 0.67850 11.00000 -1.20000 AFIX 0 C13 1 1.09076 0.45591 1.47354 11.00000 0.03562 0.04810 = 0.02504 -0.01400 0.00348 -0.00309 AFIX 43 H13 2 1.09745 0.50216 1.54235 11.00000 -1.20000 AFIX 0 C1 1 0.97225 0.19340 0.96085 11.00000 0.01918 0.02504 = 0.02469 0.00241 -0.00206 -0.00061 AFIX 13 H1 2 0.93749 0.14210 1.01062 11.00000 -1.20000 AFIX 0 C15 1 1.05390 0.42142 1.25273 11.00000 0.02918 0.02909 = 0.03253 -0.00240 -0.00723 0.00036 AFIX 43 H15 2 1.03639 0.44523 1.17028 11.00000 -1.20000 AFIX 0 C3 1 1.05651 0.20852 0.76488 11.00000 0.02103 0.03227 = 0.02985 0.00386 0.00331 0.00017 AFIX 23 H3A 2 1.08885 0.27198 0.78268 11.00000 -1.20000 H3B 2 1.08819 0.17255 0.69480 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2007SRC1051 in Pna2(1) C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 CL 0.990 S1 - O1 O2 N1 C16 Cl1 - C5 O1 - S1 O2 - S1 C16 - C21 C17 S1 N1 - C4 C1 S1 C18 - C17 C19 C7 - C6 C20 - C21 C19 C2 - C5 C1 C3 C21 - C20 C16 C9 - C10 C8 C17 - C18 C16 C10 - C15 C11 C9 C19 - C18 C20 C22 C5 - C6 C2 Cl1 C22 - C19 C11 - C12 C10 C14 - C15 C13 C12 - C11 C13 C6 - C7 C5 C8 - C1 C9 C4 - N1 C3 C13 - C12 C14 C1 - N1 C8 C2 C15 - C14 C10 C3 - C4 C2 Floating origin restraints generated 17636 Reflections read, of which 836 rejected -17 =< h =< 19, -17 =< k =< 17, -13 =< l =< 13, 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 2 -12 -0.05 0.03 2 0.75 13 3 -6 2.32 1.13 2 14.38 2 Inconsistent equivalents 4515 Unique reflections, of which 0 suppressed R(int) = 0.0836 R(sigma) = 0.0874 Friedel opposites not merged Maximum memory for data reduction = 2766 / 45563 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 = 3504 / 307324 wR2 = 0.1143 before cycle 1 for 4515 data and 246 / 246 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0390 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15043 0.00026 -0.171 OSF Mean shift/esd = 0.018 Maximum = -0.171 for OSF Max. shift = 0.001 A for H22A Max. dU = 0.000 for C11 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3504 / 307324 wR2 = 0.1143 before cycle 2 for 4515 data and 246 / 246 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0390 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15041 0.00026 -0.056 OSF Mean shift/esd = 0.006 Maximum = -0.056 for OSF Max. shift = 0.001 A for H22A Max. dU = 0.000 for C11 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3504 / 307324 wR2 = 0.1143 before cycle 3 for 4515 data and 246 / 246 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0390 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15041 0.00026 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.008 for tors H22A Max. shift = 0.000 A for H22A Max. dU = 0.000 for C17 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3504 / 307324 wR2 = 0.1143 before cycle 4 for 4515 data and 246 / 246 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0390 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15041 0.00026 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.003 for tors H22A Max. shift = 0.000 A for H22A Max. dU = 0.000 for C13 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3504 / 307324 wR2 = 0.1143 before cycle 5 for 4515 data and 246 / 246 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0390 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15041 0.00026 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H22A Max. shift = 0.000 A for H22A Max. dU = 0.000 for C12 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3504 / 307324 wR2 = 0.1143 before cycle 6 for 4515 data and 246 / 246 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0390 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15041 0.00026 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for x Cl1 Max. shift = 0.000 A for H22C Max. dU = 0.000 for C15 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H18 0.7301 -0.0834 0.6871 43 0.950 0.000 C18 C17 C19 H7A 1.1863 -0.0561 0.9435 137 0.980 0.000 C7 C6 H7A H7B 1.2219 0.0432 0.8735 137 0.980 0.000 C7 C6 H7A H7C 1.2431 -0.0644 0.8128 137 0.980 0.000 C7 C6 H7A H20 0.6991 -0.0627 1.0720 43 0.950 0.000 C20 C21 C19 H2 1.1081 0.1482 0.9381 13 1.000 0.000 C2 C5 C1 C3 H21 0.7476 0.1020 1.0668 43 0.950 0.000 C21 C20 C16 H9A 1.0354 0.1810 1.1991 23 0.990 0.000 C9 C10 C8 H9B 1.1228 0.2266 1.1300 23 0.990 0.000 C9 C10 C8 H17 0.7798 0.0822 0.6792 43 0.950 0.000 C17 C18 C16 H5 0.9791 0.0315 0.7924 13 1.000 0.000 C5 C6 C2 Cl1 H22A 0.6935 -0.2319 0.8066 137 0.980 0.000 C22 C19 H22A H22B 0.6069 -0.1945 0.8857 137 0.980 0.000 C22 C19 H22A H22C 0.6961 -0.2298 0.9604 137 0.980 0.000 C22 C19 H22A H11 1.1128 0.2194 1.4059 43 0.950 0.000 C11 C12 C10 H14 1.0477 0.5568 1.3406 43 0.950 0.000 C14 C15 C13 H12 1.1294 0.3326 1.5733 43 0.950 0.000 C12 C11 C13 H6A 1.0921 -0.0884 0.7613 23 0.990 0.000 C6 C7 C5 H6B 1.1235 0.0161 0.7014 23 0.990 0.000 C6 C7 C5 H8A 0.9484 0.3118 1.0851 23 0.990 0.000 C8 C1 C9 H8B 1.0371 0.3277 0.9994 23 0.990 0.000 C8 C1 C9 H4A 0.9518 0.2914 0.6803 23 0.990 0.000 C4 N1 C3 H4B 0.9326 0.1724 0.6785 23 0.990 0.000 C4 N1 C3 H13 1.0975 0.5022 1.5423 43 0.950 0.000 C13 C12 C14 H1 0.9375 0.1421 1.0106 13 1.000 0.000 C1 N1 C8 C2 H15 1.0364 0.4452 1.1703 43 0.950 0.000 C15 C14 C10 H3A 1.0888 0.2720 0.7827 23 0.990 0.000 C3 C4 C2 H3B 1.0882 0.1726 0.6948 23 0.990 0.000 C3 C4 C2 2007SRC1051 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.80508 0.23438 0.86861 1.00000 0.01724 0.02449 0.02771 -0.00015 -0.00100 0.00232 0.02314 0.00126 0.00005 0.00005 0.00008 0.00000 0.00035 0.00038 0.00037 0.00038 0.00037 0.00030 0.00017 Cl1 1.00463 -0.03822 0.99380 1.00000 0.04816 0.02516 0.04652 0.00535 0.01634 -0.00009 0.03995 0.00178 0.00007 0.00006 0.00010 0.00000 0.00054 0.00040 0.00044 0.00044 0.00042 0.00039 0.00022 O1 0.78188 0.27728 0.99095 1.00000 0.02337 0.02961 0.03354 -0.00533 0.00468 0.00268 0.02884 0.00390 0.00016 0.00016 0.00022 0.00000 0.00126 0.00130 0.00120 0.00112 0.00109 0.00095 0.00052 O2 0.77149 0.27897 0.75209 1.00000 0.02477 0.03057 0.03421 0.00791 -0.00570 0.00428 0.02985 0.00395 0.00016 0.00016 0.00021 0.00000 0.00136 0.00131 0.00129 0.00103 0.00107 0.00105 0.00055 C16 0.76825 0.10842 0.87319 1.00000 0.01422 0.02556 0.02812 0.00094 -0.00294 0.00131 0.02263 0.00519 0.00019 0.00021 0.00034 0.00000 0.00137 0.00151 0.00138 0.00147 0.00150 0.00118 0.00059 N1 0.91445 0.23578 0.85700 1.00000 0.01463 0.02507 0.02296 0.00077 0.00129 0.00141 0.02089 0.00426 0.00015 0.00017 0.00026 0.00000 0.00114 0.00130 0.00123 0.00116 0.00125 0.00100 0.00052 C18 0.73363 -0.04547 0.76428 1.00000 0.02928 0.03137 0.03900 -0.01090 -0.00823 -0.00084 0.03322 0.00579 0.00024 0.00026 0.00035 0.00000 0.00198 0.00186 0.00197 0.00163 0.00153 0.00162 0.00082 H18 0.73012 -0.08336 0.68709 1.00000 0.03986 0.00000 0.00000 C7 1.19832 -0.02463 0.86004 1.00000 0.02846 0.02977 0.04158 -0.00250 0.00044 0.00447 0.03327 0.00584 0.00021 0.00024 0.00038 0.00000 0.00177 0.00172 0.00188 0.00185 0.00169 0.00143 0.00073 H7A 1.18634 -0.05607 0.94351 1.00000 0.04990 0.00000 0.00000 H7B 1.22186 0.04321 0.87350 1.00000 0.04990 0.00000 0.00000 H7C 1.24308 -0.06443 0.81278 1.00000 0.04990 0.00000 0.00000 C20 0.71519 -0.03321 0.99201 1.00000 0.03003 0.03802 0.03476 0.00881 0.00050 -0.00519 0.03427 0.00631 0.00023 0.00026 0.00038 0.00000 0.00188 0.00202 0.00176 0.00177 0.00168 0.00160 0.00078 H20 0.69905 -0.06270 1.07196 1.00000 0.04113 0.00000 0.00000 C2 1.05072 0.14282 0.88756 1.00000 0.01733 0.02588 0.02133 0.00115 0.00111 0.00039 0.02151 0.00528 0.00021 0.00022 0.00028 0.00000 0.00152 0.00160 0.00150 0.00126 0.00123 0.00122 0.00064 H2 1.10812 0.14824 0.93815 1.00000 0.02581 0.00000 0.00000 C21 0.74412 0.06448 0.98929 1.00000 0.02539 0.03770 0.02485 0.00260 -0.00009 -0.00162 0.02931 0.00601 0.00022 0.00025 0.00034 0.00000 0.00179 0.00193 0.00157 0.00156 0.00156 0.00148 0.00073 H21 0.74763 0.10200 1.06679 1.00000 0.03518 0.00000 0.00000 C9 1.06172 0.24309 1.16295 1.00000 0.02612 0.02575 0.02775 0.00221 -0.00530 0.00149 0.02654 0.00548 0.00023 0.00024 0.00030 0.00000 0.00189 0.00174 0.00167 0.00133 0.00136 0.00149 0.00073 H9A 1.03540 0.18097 1.19911 1.00000 0.03185 0.00000 0.00000 H9B 1.12284 0.22661 1.12998 1.00000 0.03185 0.00000 0.00000 C17 0.76318 0.05282 0.75904 1.00000 0.02402 0.03293 0.02897 -0.00256 0.00029 -0.00307 0.02864 0.00561 0.00023 0.00025 0.00033 0.00000 0.00180 0.00185 0.00173 0.00144 0.00142 0.00151 0.00075 H17 0.77979 0.08220 0.67921 1.00000 0.03437 0.00000 0.00000 C10 1.07102 0.31972 1.27009 1.00000 0.01741 0.02907 0.02558 -0.00360 0.00034 -0.00186 0.02402 0.00522 0.00021 0.00024 0.00029 0.00000 0.00162 0.00174 0.00161 0.00136 0.00128 0.00139 0.00067 C19 0.70899 -0.09000 0.87990 1.00000 0.02022 0.02948 0.04800 0.00560 -0.00170 -0.00109 0.03256 0.00598 0.00021 0.00024 0.00039 0.00000 0.00175 0.00175 0.00201 0.00181 0.00171 0.00132 0.00076 C5 1.03273 0.03311 0.85118 1.00000 0.02263 0.02586 0.02666 0.00012 -0.00228 0.00255 0.02505 0.00530 0.00021 0.00022 0.00030 0.00000 0.00159 0.00169 0.00163 0.00139 0.00135 0.00129 0.00067 H5 0.97911 0.03153 0.79244 1.00000 0.03006 0.00000 0.00000 C22 0.67325 -0.19580 0.88347 1.00000 0.03423 0.03086 0.07802 0.00435 -0.01033 -0.00574 0.04770 0.00676 0.00026 0.00026 0.00046 0.00000 0.00206 0.00192 0.00286 0.00219 0.00222 0.00163 0.00099 H22A 0.69351 -0.23187 0.80657 1.00000 0.07155 0.00000 0.00000 H22B 0.60691 -0.19447 0.88570 1.00000 0.07155 0.00000 0.00000 H22C 0.69612 -0.22981 0.96045 1.00000 0.07155 0.00000 0.00000 C11 1.09976 0.28824 1.39175 1.00000 0.02794 0.03113 0.03374 0.00622 0.00202 -0.00732 0.03094 0.00548 0.00023 0.00026 0.00029 0.00000 0.00185 0.00184 0.00205 0.00145 0.00145 0.00141 0.00079 H11 1.11275 0.21942 1.40591 1.00000 0.03713 0.00000 0.00000 C14 1.06200 0.48812 1.35354 1.00000 0.03269 0.02866 0.04671 -0.00693 -0.00547 0.00442 0.03602 0.00576 0.00022 0.00026 0.00036 0.00000 0.00191 0.00179 0.00220 0.00170 0.00186 0.00152 0.00081 H14 1.04773 0.55677 1.34055 1.00000 0.04323 0.00000 0.00000 C12 1.10953 0.35552 1.49150 1.00000 0.03243 0.04427 0.02432 0.00247 0.00235 -0.01114 0.03367 0.00587 0.00023 0.00026 0.00033 0.00000 0.00192 0.00215 0.00154 0.00163 0.00160 0.00162 0.00077 H12 1.12936 0.33259 1.57330 1.00000 0.04041 0.00000 0.00000 C6 1.11110 -0.01935 0.78313 1.00000 0.02854 0.03415 0.02900 -0.00455 -0.00172 0.00574 0.03056 0.00573 0.00023 0.00026 0.00030 0.00000 0.00192 0.00193 0.00174 0.00145 0.00135 0.00157 0.00077 H6A 1.09207 -0.08841 0.76134 1.00000 0.03668 0.00000 0.00000 H6B 1.12346 0.01613 0.70136 1.00000 0.03668 0.00000 0.00000 C8 1.00272 0.27789 1.05031 1.00000 0.02900 0.02256 0.02616 -0.00019 -0.00467 0.00156 0.02591 0.00533 0.00023 0.00023 0.00029 0.00000 0.00193 0.00167 0.00156 0.00126 0.00137 0.00142 0.00072 H8A 0.94836 0.31184 1.08505 1.00000 0.03109 0.00000 0.00000 H8B 1.03709 0.32772 0.99939 1.00000 0.03109 0.00000 0.00000 C4 0.95820 0.22831 0.72944 1.00000 0.01963 0.03756 0.02491 0.00225 0.00182 -0.00147 0.02737 0.00575 0.00023 0.00025 0.00029 0.00000 0.00168 0.00198 0.00163 0.00140 0.00127 0.00150 0.00073 H4A 0.95182 0.29145 0.68031 1.00000 0.03284 0.00000 0.00000 H4B 0.93256 0.17243 0.67848 1.00000 0.03284 0.00000 0.00000 C13 1.09076 0.45591 1.47353 1.00000 0.03558 0.04809 0.02495 -0.01400 0.00348 -0.00307 0.03620 0.00600 0.00025 0.00029 0.00030 0.00000 0.00209 0.00235 0.00183 0.00161 0.00153 0.00174 0.00088 H13 1.09746 0.50216 1.54233 1.00000 0.04345 0.00000 0.00000 C1 0.97226 0.19341 0.96085 1.00000 0.01917 0.02497 0.02467 0.00241 -0.00209 -0.00058 0.02294 0.00532 0.00021 0.00025 0.00027 0.00000 0.00167 0.00171 0.00162 0.00123 0.00118 0.00140 0.00069 H1 0.93750 0.14211 1.01062 1.00000 0.02753 0.00000 0.00000 C15 1.05390 0.42142 1.25274 1.00000 0.02915 0.02906 0.03245 -0.00243 -0.00721 0.00037 0.03022 0.00560 0.00023 0.00024 0.00032 0.00000 0.00191 0.00180 0.00172 0.00148 0.00151 0.00154 0.00076 H15 1.03639 0.44524 1.17029 1.00000 0.03627 0.00000 0.00000 C3 1.05651 0.20852 0.76489 1.00000 0.02098 0.03224 0.02973 0.00385 0.00327 0.00019 0.02765 0.00582 0.00022 0.00025 0.00031 0.00000 0.00176 0.00181 0.00169 0.00145 0.00135 0.00144 0.00073 H3A 1.08885 0.27199 0.78269 1.00000 0.03318 0.00000 0.00000 H3B 1.08820 0.17255 0.69481 1.00000 0.03318 0.00000 0.00000 Final Structure Factor Calculation for 2007SRC1051 in Pna2(1) Total number of l.s. parameters = 246 Maximum vector length = 511 Memory required = 3260 / 27090 wR2 = 0.1143 before cycle 7 for 4515 data and 2 / 246 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0390 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0504 for 3393 Fo > 4sig(Fo) and 0.0832 for all 4515 data wR2 = 0.1143, GooF = S = 1.052, Restrained GooF = 1.052 for all data Flack x parameter = 0.0971 with esd 0.0776 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 27.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0279 0.0251 0.0165 S1 0.0640 0.0329 0.0229 Cl1 0.0377 0.0294 0.0194 O1 0.0407 0.0312 0.0176 O2 0.0289 0.0256 0.0134 C16 0.0256 0.0228 0.0143 N1 0.0488 0.0309 0.0199 C18 0.0421 0.0333 0.0244 C7 0.0462 0.0320 0.0246 C20 0.0262 0.0213 0.0170 C2 0.0384 0.0252 0.0243 C21 0.0324 0.0269 0.0203 C9 0.0350 0.0279 0.0230 C17 0.0315 0.0234 0.0171 C10 0.0497 0.0280 0.0201 C19 0.0283 0.0264 0.0205 C5 0.0809 0.0358 0.0264 C22 0.0399 0.0332 0.0198 C11 0.0514 0.0314 0.0253 C14 0.0510 0.0284 0.0217 C12 0.0398 0.0272 0.0246 C6 0.0326 0.0233 0.0217 C8 0.0380 0.0252 0.0188 C4 0.0556 0.0349 0.0182 C13 0.0277 0.0227 0.0185 C1 0.0387 0.0289 0.0231 C15 0.0354 0.0278 0.0198 C3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.020 0.029 0.037 0.046 0.055 0.066 0.082 0.103 0.144 1.000 Number in group 470. 459. 450. 449. 433. 464. 458. 436. 441. 455. GooF 0.874 1.077 1.044 1.103 1.151 1.159 1.037 0.950 1.050 1.053 K 1.522 0.956 0.895 0.946 0.970 0.984 1.003 1.017 1.019 0.992 Resolution(A) 0.77 0.80 0.84 0.88 0.92 0.98 1.05 1.17 1.33 1.67 inf Number in group 459. 454. 445. 455. 451. 443. 452. 452. 455. 449. GooF 0.955 0.984 0.996 1.017 0.975 1.125 1.075 0.982 1.028 1.337 K 0.954 1.006 0.980 1.007 1.012 1.017 1.013 1.022 1.018 0.978 R1 0.237 0.194 0.162 0.125 0.089 0.073 0.048 0.037 0.034 0.030 Recommended weighting scheme: WGHT 0.0381 0.3925 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 6 0 126.16 59.63 4.55 0.035 2.20 2 4 -4 59.26 22.21 4.51 0.021 1.98 6 1 -3 66.64 32.67 3.82 0.026 1.98 6 1 1 220.11 147.48 3.69 0.055 2.36 3 7 7 84.46 135.76 3.59 0.052 1.14 10 10 6 71.61 168.05 3.58 0.058 0.86 14 3 0 402.64 266.25 3.49 0.073 1.03 3 5 0 1208.65 992.57 3.46 0.142 2.35 2 4 0 255.93 166.70 3.42 0.058 3.04 3 2 -2 75.67 45.44 3.42 0.030 3.15 7 10 0 32.39 101.96 3.42 0.045 1.13 2 4 4 61.18 27.91 3.20 0.024 1.98 11 7 -7 119.63 23.36 3.20 0.022 0.88 18 0 1 -21.66 99.30 3.18 0.045 0.82 1 1 4 174.48 227.25 3.15 0.068 2.51 1 3 -1 215.74 276.54 3.15 0.075 3.94 6 2 12 93.27 214.78 3.14 0.066 0.81 0 8 0 81.93 32.29 3.11 0.026 1.67 18 2 1 -58.13 64.67 3.08 0.036 0.81 4 1 5 202.71 158.53 3.06 0.057 1.80 5 7 7 48.03 93.07 3.06 0.043 1.09 4 5 -7 494.76 392.79 3.05 0.089 1.22 3 6 4 445.75 546.33 3.04 0.105 1.60 6 4 -8 180.59 119.37 3.01 0.049 1.09 3 3 0 197.79 141.59 2.99 0.053 3.30 9 12 6 337.70 160.96 2.96 0.057 0.81 0 4 -2 3830.88 4495.26 2.93 0.301 2.81 6 11 -4 85.96 158.50 2.93 0.057 1.00 12 6 -4 71.25 31.36 2.91 0.025 0.99 0 4 0 42886.13 49568.49 2.89 1.000 3.34 1 1 -4 180.33 227.96 2.88 0.068 2.51 4 10 8 48.15 167.68 2.84 0.058 0.90 12 7 -5 127.11 65.12 2.83 0.036 0.93 10 2 7 169.23 113.89 2.81 0.048 1.03 4 6 10 2.92 80.03 2.81 0.040 0.91 14 0 -7 -150.51 138.10 2.80 0.053 0.86 12 5 -4 347.18 439.76 2.79 0.094 1.03 5 7 -7 48.34 91.75 2.78 0.043 1.09 5 5 -5 182.19 131.30 2.78 0.051 1.43 6 7 9 76.61 121.20 2.77 0.049 0.92 2 7 2 1057.03 893.09 2.77 0.134 1.74 2 8 6 56.33 21.48 2.76 0.021 1.19 3 16 1 688.24 503.70 2.76 0.101 0.82 14 2 -1 85.92 38.10 2.76 0.028 1.04 4 0 10 171.40 270.54 2.75 0.074 1.00 13 2 3 166.08 236.52 2.75 0.069 1.07 7 16 1 -265.87 233.54 2.75 0.069 0.77 13 11 0 62.71 155.72 2.75 0.056 0.83 12 7 2 8.34 50.49 2.75 0.032 1.01 6 6 -9 277.43 368.96 2.74 0.086 0.95 Bond lengths and angles S1 - Distance Angles O1 1.4362 (0.0024) O2 1.4379 (0.0022) 119.91 (0.12) N1 1.6194 (0.0024) 107.41 (0.14) 106.04 (0.14) C16 1.7678 (0.0029) 106.38 (0.15) 108.08 (0.15) 108.65 (0.13) S1 - O1 O2 N1 Cl1 - Distance Angles C5 1.8102 (0.0032) Cl1 - O1 - Distance Angles S1 1.4362 (0.0024) O1 - O2 - Distance Angles S1 1.4379 (0.0022) O2 - C16 - Distance Angles C21 1.3884 (0.0047) C17 1.4016 (0.0045) 119.91 (0.28) S1 1.7678 (0.0029) 120.27 (0.26) 119.82 (0.25) C16 - C21 C17 N1 - Distance Angles C4 1.4784 (0.0040) C1 1.4879 (0.0038) 112.00 (0.23) S1 1.6194 (0.0024) 120.11 (0.21) 120.90 (0.21) N1 - C4 C1 C18 - Distance Angles C17 1.3838 (0.0046) C19 1.3893 (0.0051) 121.49 (0.32) H18 0.9500 119.26 119.26 C18 - C17 C19 C7 - Distance Angles C6 1.5174 (0.0046) 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 C20 - Distance Angles C21 1.3726 (0.0047) C19 1.3932 (0.0052) 121.34 (0.34) H20 0.9500 119.33 119.33 C20 - C21 C19 C2 - Distance Angles C5 1.5356 (0.0041) C1 1.5422 (0.0043) 114.17 (0.25) C3 1.5500 (0.0042) 110.28 (0.24) 101.54 (0.24) H2 1.0000 110.18 110.18 110.18 C2 - C5 C1 C3 C21 - Distance Angles C20 1.3726 (0.0047) C16 1.3884 (0.0047) 119.94 (0.33) H21 0.9500 120.03 120.03 C21 - C20 C16 C9 - Distance Angles C10 1.5184 (0.0043) C8 1.5315 (0.0042) 114.08 (0.26) H9A 0.9900 108.73 108.73 H9B 0.9900 108.73 108.73 107.64 C9 - C10 C8 H9A C17 - Distance Angles C18 1.3838 (0.0046) C16 1.4016 (0.0045) 119.05 (0.31) H17 0.9500 120.48 120.48 C17 - C18 C16 C10 - Distance Angles C15 1.3927 (0.0045) C11 1.3985 (0.0044) 117.72 (0.29) C9 1.5184 (0.0043) 123.04 (0.28) 119.23 (0.28) C10 - C15 C11 C19 - Distance Angles C18 1.3893 (0.0051) C20 1.3932 (0.0052) 118.27 (0.29) C22 1.5082 (0.0045) 120.90 (0.37) 120.80 (0.36) C19 - C18 C20 C5 - Distance Angles C6 1.5263 (0.0043) C2 1.5356 (0.0041) 114.87 (0.26) Cl1 1.8102 (0.0032) 108.18 (0.21) 109.85 (0.20) H5 1.0000 107.90 107.90 107.90 C5 - C6 C2 Cl1 C22 - Distance Angles C19 1.5082 (0.0045) H22A 0.9800 109.47 H22B 0.9800 109.47 109.47 H22C 0.9800 109.47 109.47 109.47 C22 - C19 H22A H22B C11 - Distance Angles C12 1.3794 (0.0045) C10 1.3985 (0.0044) 121.06 (0.32) H11 0.9500 119.47 119.47 C11 - C12 C10 C14 - Distance Angles C15 1.3803 (0.0047) C13 1.3860 (0.0050) 120.64 (0.32) H14 0.9500 119.68 119.68 C14 - C15 C13 C12 - Distance Angles C11 1.3794 (0.0045) C13 1.3813 (0.0049) 120.60 (0.33) H12 0.9500 119.70 119.70 C12 - C11 C13 C6 - Distance Angles C7 1.5174 (0.0046) C5 1.5263 (0.0043) 114.86 (0.27) H6A 0.9900 108.55 108.55 H6B 0.9900 108.55 108.55 107.54 C6 - C7 C5 H6A C8 - Distance Angles C1 1.5293 (0.0043) C9 1.5315 (0.0042) 114.11 (0.25) H8A 0.9900 108.73 108.73 H8B 0.9900 108.73 108.73 107.63 C8 - C1 C9 H8A C4 - Distance Angles N1 1.4784 (0.0039) C3 1.5206 (0.0045) 102.20 (0.24) H4A 0.9900 111.33 111.33 H4B 0.9900 111.33 111.33 109.21 C4 - N1 C3 H4A C13 - Distance Angles C12 1.3813 (0.0049) C14 1.3860 (0.0050) 118.96 (0.31) H13 0.9500 120.52 120.52 C13 - C12 C14 C1 - Distance Angles N1 1.4879 (0.0038) C8 1.5293 (0.0043) 109.24 (0.25) C2 1.5422 (0.0043) 103.82 (0.23) 113.73 (0.26) H1 1.0000 109.95 109.96 109.96 C1 - N1 C8 C2 C15 - Distance Angles C14 1.3803 (0.0047) C10 1.3927 (0.0045) 120.98 (0.31) H15 0.9500 119.51 119.51 C15 - C14 C10 C3 - Distance Angles C4 1.5206 (0.0045) C2 1.5500 (0.0042) 104.18 (0.25) H3A 0.9900 110.92 110.92 H3B 0.9900 110.92 110.92 108.94 C3 - C4 C2 H3A FMAP and GRID set by program FMAP 2 1 19 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.0705 for 2465 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.0154 0.1641 0.9217 [ 0.69 A from C2 ] Deepest hole -0.40 at 0.0137 0.0637 0.4416 [ 0.69 A from CL1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3273 / 22538 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.0154 0.1641 0.9217 1.00000 0.05 0.27 0.69 C2 0.85 C1 1.40 H2 1.50 H1 Q2 1 1.3108 0.0555 0.9139 1.00000 0.05 0.25 1.39 H7B 2.03 H13 2.05 C7 2.07 C13 Q3 1 1.1320 -0.1388 0.7779 1.00000 0.05 0.24 0.91 H6A 1.62 C6 1.95 H7C 1.97 H22A Q4 1 1.0816 0.1431 0.9101 1.00000 0.05 0.23 0.49 H2 0.51 C2 1.75 C5 1.78 C3 Q5 1 0.7649 0.2626 1.0042 1.00000 0.05 0.23 0.35 O1 1.57 S1 2.26 H21 2.47 C16 Q6 1 0.9982 -0.0371 0.7290 1.00000 0.05 0.22 1.16 H5 1.58 H6A 1.66 C5 1.78 C6 Q7 1 0.9503 -0.0804 0.7810 1.00000 0.05 0.22 1.56 H5 1.60 H9A 2.08 C5 2.11 H6A Q8 1 1.1711 -0.0906 0.7986 1.00000 0.05 0.22 1.13 H7C 1.16 C7 1.23 H6A 1.31 C6 Q9 1 1.1307 0.3955 0.8655 1.00000 0.05 0.22 1.96 H3A 2.03 C16 2.16 H8B 2.18 C21 Q10 1 0.7910 0.1567 0.8795 1.00000 0.05 0.21 0.73 C16 1.06 S1 1.82 C21 1.91 C17 Q11 1 1.1330 0.1643 0.8185 1.00000 0.05 0.21 1.31 H2 1.39 C3 1.44 C2 1.45 H3B Q12 1 0.7392 0.1078 0.8751 1.00000 0.05 0.21 0.43 C16 1.32 C21 1.46 C17 1.95 S1 Q13 1 1.0825 0.2596 0.8671 1.00000 0.05 0.21 0.90 H3A 1.32 C3 1.64 C2 1.70 H2 Q14 1 1.0178 0.2186 1.3767 1.00000 0.05 0.21 1.43 H11 1.53 C11 1.91 C10 1.93 H9A Q15 1 0.7293 0.3465 0.6419 1.00000 0.05 0.20 1.58 O2 1.77 H20 2.17 H3B 2.38 C20 Q16 1 0.7943 0.1022 0.8219 1.00000 0.05 0.20 0.66 C16 1.04 C17 1.52 H17 1.84 S1 Q17 1 1.2015 0.1740 1.1613 1.00000 0.05 0.20 1.40 H9B 1.60 H18 2.23 O1 2.24 C18 Q18 1 1.0944 0.4818 1.3687 1.00000 0.05 0.20 0.51 C14 1.14 C13 1.25 H14 1.57 C15 Q19 1 0.6095 -0.2876 0.9583 1.00000 0.05 0.20 1.45 H22B 1.49 H22C 1.73 C22 2.14 H22A Q20 1 0.9064 0.0628 0.7693 1.00000 0.05 0.20 1.18 H5 1.78 H4B 2.09 C5 2.11 H17 Shortest distances between peaks (including symmetry equivalents) 3 8 0.89 10 16 0.94 12 16 0.99 10 12 1.01 1 4 1.02 6 7 1.06 4 11 1.25 11 13 1.56 9 12 1.61 4 13 1.62 1 13 1.71 2 18 1.77 16 20 1.82 6 20 1.95 9 13 1.95 5 10 1.96 7 20 2.02 1 11 2.04 14 19 2.06 5 17 2.06 3 19 2.14 7 14 2.15 11 15 2.33 10 20 2.41 3 6 2.45 9 16 2.46 9 10 2.47 5 12 2.49 8 19 2.50 1 20 2.63 3 14 2.66 2 5 2.69 6 8 2.75 12 20 2.77 3 7 2.79 7 17 2.85 6 14 2.88 5 16 2.89 5 11 2.91 12 13 2.91 Time profile in seconds ----------------------- 0.02: 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. 0.14: 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 0.02: Generate idealized H-atoms 2.05: Structure factors and derivatives 1.66: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src1051 finished at 11:28:53 Total CPU time: 4.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++