+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0016p-1 started at 16:32:12 on 07-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0016p-1 in P-1 CELL 0.71073 6.1332 10.2547 13.7444 98.274 93.850 94.425 ZERR 2.00 0.0004 0.0007 0.0006 0.003 0.004 0.003 LATT 1 SFAC C H N S O UNIT 30 54 2 2 6 V = 850.21 F(000) = 328.0 Mu = 0.20 mm-1 Cell Wt = 602.87 Rho = 1.177 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 EQIV_$1 -x, -y, -z+1 HTAB N25 O1A_$1 EQIV_$2 x-1, y-1, z HTAB N25 O1B_$2 HTAB N25 O1A_$2 HTAB N25 S1_$2 EQIV_$3 x, y-1, z HTAB N25 O1C_$3 FMAP 2 PLAN 10 SIZE 0.01 0.05 0.14 ACTA BOND $H WGHT 0.03390 0.60820 L.S. 4 TEMP -153.00 FVAR 0.92436 MOLE 1 C4 1 0.458390 0.308665 0.959039 11.00000 0.04024 0.02269 = 0.02202 0.00353 -0.00502 -0.00633 C3 1 0.599318 0.314042 0.885200 11.00000 0.03148 0.02732 = 0.03138 0.00635 -0.00428 0.00387 AFIX 43 H3 2 0.736281 0.277382 0.891371 11.00000 -1.20000 AFIX 0 C2 1 0.546410 0.371585 0.802105 11.00000 0.02622 0.02749 = 0.02867 0.00421 0.00274 0.00218 AFIX 43 H2 2 0.645478 0.374066 0.752022 11.00000 -1.20000 AFIX 0 C1 1 0.345892 0.425502 0.793497 11.00000 0.02296 0.01880 = 0.02323 0.00262 0.00040 -0.00166 C6 1 0.203678 0.422957 0.866882 11.00000 0.02669 0.02584 = 0.02729 0.00053 0.00249 0.00059 AFIX 43 H6 2 0.067753 0.460885 0.861150 11.00000 -1.20000 AFIX 0 C5 1 0.259703 0.364865 0.949060 11.00000 0.03605 0.02987 = 0.02418 0.00262 0.00702 -0.00588 AFIX 43 H5 2 0.161119 0.363318 0.999405 11.00000 -1.20000 AFIX 0 C7 1 0.516173 0.240869 1.046540 11.00000 0.06231 0.03392 = 0.03124 0.01188 -0.00685 -0.00419 AFIX 137 H7A 2 0.476948 0.145478 1.029218 11.00000 -1.50000 H7B 2 0.435031 0.275889 1.102146 11.00000 -1.50000 H7C 2 0.674071 0.257207 1.065087 11.00000 -1.50000 AFIX 0 S1 4 0.277702 0.500127 0.688326 11.00000 0.02039 0.02382 = 0.02387 0.00584 -0.00196 0.00047 O1A 5 0.378184 0.426132 0.606943 11.00000 0.03813 0.03138 = 0.01968 0.00047 -0.00128 0.00524 O1B 5 0.373476 0.636856 0.709396 11.00000 0.02674 0.02142 = 0.02714 0.00447 0.00137 -0.00056 O1C 5 0.039619 0.489134 0.675870 11.00000 0.01976 0.03720 = 0.04879 0.01859 -0.00410 -0.00195 MOLE 2 C24 1 -0.159003 -0.206407 0.602009 11.00000 0.01922 0.01906 = 0.02388 0.00397 -0.00001 -0.00183 C23 1 -0.122260 -0.156840 0.713852 11.00000 0.02161 0.02451 = 0.02348 0.00376 0.00228 0.00017 AFIX 23 H23A 2 -0.045379 -0.225025 0.743173 11.00000 -1.20000 H23B 2 -0.269304 -0.157395 0.739499 11.00000 -1.20000 AFIX 0 C22 1 0.001672 -0.021823 0.757711 11.00000 0.02687 0.02251 = 0.02524 -0.00042 0.00196 -0.00116 C21 1 -0.039011 -0.001621 0.867306 11.00000 0.04114 0.03117 = 0.02689 -0.00104 0.00130 -0.00225 AFIX 137 H21A 2 0.044130 0.079976 0.900384 11.00000 -1.50000 H21B 2 0.008647 -0.076873 0.897252 11.00000 -1.50000 H21C 2 -0.195857 0.004968 0.874452 11.00000 -1.50000 AFIX 0 C28 1 0.049281 -0.210321 0.547483 11.00000 0.02140 0.02764 = 0.02576 0.00544 0.00204 -0.00211 AFIX 137 H28A 2 0.159137 -0.253387 0.583663 11.00000 -1.50000 H28B 2 0.106970 -0.119873 0.542606 11.00000 -1.50000 H28C 2 0.015661 -0.260218 0.481122 11.00000 -1.50000 AFIX 0 C29 1 -0.333356 -0.137947 0.548651 11.00000 0.02504 0.02547 = 0.02879 0.00431 -0.00226 0.00373 AFIX 137 H29A 2 -0.363543 -0.183118 0.480688 11.00000 -1.50000 H29B 2 -0.280120 -0.045479 0.548107 11.00000 -1.50000 H29C 2 -0.468274 -0.141319 0.582921 11.00000 -1.50000 AFIX 0 C27 1 -0.080687 0.094512 0.712510 11.00000 0.04289 0.02480 = 0.03396 0.00245 0.00077 -0.00173 AFIX 137 H27A 2 -0.240183 0.093039 0.714898 11.00000 -1.50000 H27B 2 -0.043875 0.087633 0.643773 11.00000 -1.50000 H27C 2 -0.010895 0.177578 0.749828 11.00000 -1.50000 AFIX 0 C26 1 0.250110 -0.021274 0.750230 11.00000 0.02848 0.03552 = 0.04130 -0.00707 -0.00167 -0.00579 AFIX 137 H26A 2 0.283182 -0.018154 0.681786 11.00000 -1.50000 H26B 2 0.301303 -0.101773 0.771294 11.00000 -1.50000 H26C 2 0.324593 0.056454 0.792828 11.00000 -1.50000 AFIX 0 N25 3 -0.253174 -0.348371 0.595123 11.00000 0.02007 0.02203 = 0.02167 0.00326 -0.00058 -0.00086 AFIX 137 H25A 2 -0.292750 -0.382057 0.530893 11.00000 -1.5 H25B 2 -0.373061 -0.351600 0.630569 11.00000 -1.5 H25C 2 -0.150400 -0.396918 0.619761 11.00000 -1.5 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0016p-1 in P-1 C 0.770 H 0.320 N 0.700 S 1.030 O 0.660 C4 - C3 C5 C7 C3 - C4 C2 C2 - C3 C1 C1 - C6 C2 S1 C6 - C1 C5 C5 - C6 C4 C7 - C4 S1 - O1C O1A O1B C1 O1A - S1 O1B - S1 O1C - S1 C24 - N25 C28 C29 C23 C23 - C24 C22 C22 - C27 C21 C26 C23 C21 - C22 C28 - C24 C29 - C24 C27 - C22 C26 - C22 N25 - C24 Operators for generating equivalent atoms: $1 -x, -y, -z+1 $2 x-1, y-1, z $3 x, y-1, z 15078 Reflections read, of which 53 rejected -7 =< h =< 7, -13 =< k =< 13, -17 =< l =< 17, 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) 5 0 6 85.95 3.81 3 21.51 -6 -1 7 -2.68 3.29 2 25.27 -7 0 7 0.41 4.97 2 28.23 -7 3 8 0.32 7.33 2 44.07 4 Inconsistent equivalents 3857 Unique reflections, of which 0 suppressed R(int) = 0.0775 R(sigma) = 0.0790 Friedel opposites merged Maximum memory for data reduction = 2540 / 37973 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 = 3130 / 234295 wR2 = 0.1242 before cycle 1 for 3857 data and 188 / 188 parameters GooF = S = 1.028; Restrained GooF = 1.028 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0339 * P )^2 + 0.61 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92429 0.00181 -0.037 OSF Mean shift/esd = 0.015 Maximum = -0.227 for U11 N25 Max. shift = 0.001 A for H25B Max. dU = 0.000 for N25 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3130 / 234295 wR2 = 0.1242 before cycle 2 for 3857 data and 188 / 188 parameters GooF = S = 1.028; Restrained GooF = 1.028 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0339 * P )^2 + 0.61 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92427 0.00181 -0.013 OSF Mean shift/esd = 0.006 Maximum = -0.084 for U11 N25 Max. shift = 0.000 A for H25B Max. dU = 0.000 for N25 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3130 / 234295 wR2 = 0.1242 before cycle 3 for 3857 data and 188 / 188 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0339 * P )^2 + 0.61 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92427 0.00181 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.004 for U23 N25 Max. shift = 0.000 A for H7C Max. dU = 0.000 for C29 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3130 / 234295 wR2 = 0.1242 before cycle 4 for 3857 data and 188 / 188 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0339 * P )^2 + 0.61 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92427 0.00181 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H7A Max. shift = 0.000 A for H7C Max. dU = 0.000 for C29 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 H3 0.7363 0.2774 0.8914 43 0.950 0.000 C3 C4 C2 H2 0.6455 0.3741 0.7520 43 0.950 0.000 C2 C3 C1 H6 0.0677 0.4609 0.8611 43 0.950 0.000 C6 C1 C5 H5 0.1611 0.3633 0.9994 43 0.950 0.000 C5 C6 C4 H7A 0.4769 0.1455 1.0292 137 0.980 0.000 C7 C4 H7A H7B 0.4351 0.2759 1.1021 137 0.980 0.000 C7 C4 H7A H7C 0.6741 0.2572 1.0651 137 0.980 0.000 C7 C4 H7A H23A -0.0454 -0.2250 0.7432 23 0.990 0.000 C23 C24 C22 H23B -0.2693 -0.1574 0.7395 23 0.990 0.000 C23 C24 C22 H21A 0.0442 0.0800 0.9004 137 0.980 0.000 C21 C22 H21A H21B 0.0086 -0.0769 0.8972 137 0.980 0.000 C21 C22 H21A H21C -0.1958 0.0050 0.8745 137 0.980 0.000 C21 C22 H21A H28A 0.1591 -0.2534 0.5837 137 0.980 0.000 C28 C24 H28A H28B 0.1070 -0.1199 0.5426 137 0.980 0.000 C28 C24 H28A H28C 0.0157 -0.2602 0.4811 137 0.980 0.000 C28 C24 H28A H29A -0.3636 -0.1831 0.4807 137 0.980 0.000 C29 C24 H29A H29B -0.2801 -0.0455 0.5481 137 0.980 0.000 C29 C24 H29A H29C -0.4683 -0.1413 0.5829 137 0.980 0.000 C29 C24 H29A H27A -0.2402 0.0930 0.7149 137 0.980 0.000 C27 C22 H27A H27B -0.0439 0.0876 0.6438 137 0.980 0.000 C27 C22 H27A H27C -0.0109 0.1776 0.7498 137 0.980 0.000 C27 C22 H27A H26A 0.2832 -0.0182 0.6818 137 0.980 0.000 C26 C22 H26A H26B 0.3013 -0.1017 0.7713 137 0.980 0.000 C26 C22 H26A H26C 0.3246 0.0565 0.7928 137 0.980 0.000 C26 C22 H26A H25A -0.2927 -0.3820 0.5309 137 0.910 0.000 N25 C24 H25A H25B -0.3731 -0.3516 0.6305 137 0.910 0.000 N25 C24 H25A H25C -0.1504 -0.3969 0.6197 137 0.910 0.000 N25 C24 H25A 06skc0016p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C4 0.45838 0.30866 0.95904 1.00000 0.04026 0.02268 0.02199 0.00353 -0.00501 -0.00633 0.02911 0.00443 0.00043 0.00023 0.00016 0.00000 0.00154 0.00129 0.00115 0.00097 0.00106 0.00111 0.00057 C3 0.59932 0.31404 0.88520 1.00000 0.03145 0.02734 0.03136 0.00636 -0.00428 0.00387 0.03010 0.00462 0.00042 0.00024 0.00017 0.00000 0.00141 0.00136 0.00129 0.00105 0.00108 0.00110 0.00056 H3 0.73628 0.27737 0.89137 1.00000 0.03612 0.00000 0.00000 C2 0.54642 0.37159 0.80210 1.00000 0.02622 0.02751 0.02866 0.00420 0.00275 0.00220 0.02745 0.00455 0.00039 0.00023 0.00017 0.00000 0.00135 0.00134 0.00122 0.00102 0.00101 0.00105 0.00054 H2 0.64549 0.37407 0.75202 1.00000 0.03294 0.00000 0.00000 C1 0.34589 0.42550 0.79350 1.00000 0.02297 0.01880 0.02322 0.00263 0.00040 -0.00168 0.02197 0.00417 0.00037 0.00022 0.00016 0.00000 0.00123 0.00118 0.00110 0.00091 0.00092 0.00095 0.00049 C6 0.20367 0.42296 0.86688 1.00000 0.02666 0.02585 0.02726 0.00053 0.00248 0.00059 0.02700 0.00442 0.00040 0.00023 0.00016 0.00000 0.00132 0.00131 0.00120 0.00100 0.00100 0.00104 0.00053 H6 0.06774 0.46088 0.86114 1.00000 0.03240 0.00000 0.00000 C5 0.25970 0.36487 0.94906 1.00000 0.03605 0.02988 0.02417 0.00261 0.00702 -0.00587 0.03042 0.00458 0.00042 0.00024 0.00017 0.00000 0.00151 0.00139 0.00120 0.00103 0.00106 0.00114 0.00058 H5 0.16112 0.36332 0.99941 1.00000 0.03651 0.00000 0.00000 C7 0.51618 0.24086 1.04653 1.00000 0.06230 0.03393 0.03125 0.01190 -0.00685 -0.00421 0.04273 0.00535 0.00052 0.00027 0.00019 0.00000 0.00198 0.00155 0.00138 0.00118 0.00132 0.00139 0.00071 H7A 0.47692 0.14548 1.02922 1.00000 0.06409 0.00000 0.00000 H7B 0.43507 0.27590 1.10215 1.00000 0.06409 0.00000 0.00000 H7C 0.67409 0.25718 1.06507 1.00000 0.06409 0.00000 0.00000 S1 0.27770 0.50013 0.68833 1.00000 0.02039 0.02380 0.02386 0.00583 -0.00197 0.00047 0.02271 0.00109 0.00009 0.00006 0.00004 0.00000 0.00031 0.00032 0.00029 0.00023 0.00022 0.00023 0.00016 O1A 0.37819 0.42614 0.60694 1.00000 0.03810 0.03138 0.01967 0.00047 -0.00129 0.00526 0.03010 0.00307 0.00028 0.00016 0.00011 0.00000 0.00103 0.00098 0.00079 0.00069 0.00071 0.00079 0.00041 O1B 0.37347 0.63686 0.70940 1.00000 0.02675 0.02142 0.02713 0.00444 0.00135 -0.00057 0.02520 0.00294 0.00025 0.00015 0.00011 0.00000 0.00091 0.00087 0.00082 0.00067 0.00068 0.00070 0.00037 O1C 0.03962 0.48913 0.67587 1.00000 0.01977 0.03721 0.04881 0.01861 -0.00410 -0.00198 0.03461 0.00332 0.00026 0.00017 0.00013 0.00000 0.00091 0.00106 0.00106 0.00084 0.00077 0.00076 0.00044 C24 -0.15901 -0.20641 0.60201 1.00000 0.01923 0.01907 0.02385 0.00396 0.00000 -0.00183 0.02090 0.00413 0.00036 0.00022 0.00016 0.00000 0.00116 0.00115 0.00111 0.00091 0.00091 0.00092 0.00048 C23 -0.12226 -0.15684 0.71385 1.00000 0.02160 0.02452 0.02346 0.00376 0.00229 0.00017 0.02325 0.00421 0.00037 0.00022 0.00016 0.00000 0.00122 0.00125 0.00111 0.00094 0.00092 0.00097 0.00050 H23A -0.04538 -0.22503 0.74317 1.00000 0.02791 0.00000 0.00000 H23B -0.26931 -0.15740 0.73950 1.00000 0.02791 0.00000 0.00000 C22 0.00167 -0.02182 0.75771 1.00000 0.02684 0.02250 0.02524 -0.00043 0.00195 -0.00116 0.02544 0.00434 0.00038 0.00023 0.00016 0.00000 0.00131 0.00126 0.00116 0.00096 0.00098 0.00101 0.00052 C21 -0.03900 -0.00162 0.86731 1.00000 0.04112 0.03115 0.02689 -0.00105 0.00131 -0.00223 0.03393 0.00476 0.00044 0.00026 0.00017 0.00000 0.00158 0.00147 0.00126 0.00108 0.00112 0.00120 0.00061 H21A 0.04419 0.07995 0.90039 1.00000 0.05090 0.00000 0.00000 H21B 0.00859 -0.07690 0.89724 1.00000 0.05090 0.00000 0.00000 H21C -0.19584 0.00501 0.87446 1.00000 0.05090 0.00000 0.00000 C28 0.04928 -0.21032 0.54749 1.00000 0.02136 0.02764 0.02576 0.00545 0.00202 -0.00215 0.02500 0.00443 0.00036 0.00023 0.00016 0.00000 0.00126 0.00132 0.00117 0.00099 0.00096 0.00101 0.00052 H28A 0.15912 -0.25341 0.58365 1.00000 0.03749 0.00000 0.00000 H28B 0.10699 -0.11987 0.54263 1.00000 0.03749 0.00000 0.00000 H28C 0.01565 -0.26019 0.48112 1.00000 0.03749 0.00000 0.00000 C29 -0.33336 -0.13795 0.54864 1.00000 0.02504 0.02546 0.02877 0.00433 -0.00227 0.00374 0.02652 0.00448 0.00038 0.00023 0.00017 0.00000 0.00130 0.00131 0.00122 0.00101 0.00100 0.00102 0.00053 H29A -0.36356 -0.18314 0.48069 1.00000 0.03978 0.00000 0.00000 H29B -0.28011 -0.04549 0.54809 1.00000 0.03978 0.00000 0.00000 H29C -0.46827 -0.14131 0.58292 1.00000 0.03978 0.00000 0.00000 C27 -0.08069 0.09451 0.71251 1.00000 0.04288 0.02482 0.03392 0.00243 0.00078 -0.00176 0.03442 0.00499 0.00045 0.00024 0.00018 0.00000 0.00161 0.00136 0.00135 0.00108 0.00117 0.00117 0.00061 H27A -0.24019 0.09304 0.71490 1.00000 0.05163 0.00000 0.00000 H27B -0.04387 0.08765 0.64378 1.00000 0.05163 0.00000 0.00000 H27C -0.01091 0.17758 0.74984 1.00000 0.05163 0.00000 0.00000 C26 0.25011 -0.02127 0.75023 1.00000 0.02845 0.03554 0.04128 -0.00707 -0.00167 -0.00575 0.03701 0.00481 0.00041 0.00027 0.00020 0.00000 0.00144 0.00155 0.00147 0.00119 0.00116 0.00118 0.00064 H26A 0.28318 -0.01820 0.68178 1.00000 0.05551 0.00000 0.00000 H26B 0.30131 -0.10175 0.77133 1.00000 0.05551 0.00000 0.00000 H26C 0.32458 0.05648 0.79280 1.00000 0.05551 0.00000 0.00000 N25 -0.25319 -0.34836 0.59509 1.00000 0.01975 0.02212 0.02184 0.00349 -0.00046 -0.00068 0.02145 0.00337 0.00030 0.00017 0.00013 0.00000 0.00100 0.00103 0.00092 0.00078 0.00076 0.00080 0.00042 H25A -0.29270 -0.38203 0.53085 1.00000 0.03217 0.00000 0.00000 H25B -0.37311 -0.35160 0.63051 1.00000 0.03217 0.00000 0.00000 H25C -0.15044 -0.39692 0.61974 1.00000 0.03217 0.00000 0.00000 Final Structure Factor Calculation for 06skc0016p-1 in P-1 Total number of l.s. parameters = 188 Maximum vector length = 511 Memory required = 2942 / 24017 wR2 = 0.1242 before cycle 5 for 3857 data and 0 / 188 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0339 * P )^2 + 0.61 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0568 for 2713 Fo > 4sig(Fo) and 0.0932 for all 3857 data wR2 = 0.1242, GooF = S = 1.027, Restrained GooF = 1.027 for all data Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 27.00 for hydrogen atoms Principal mean square atomic displacements U 0.0469 0.0221 0.0184 C4 0.0388 0.0288 0.0228 C3 0.0288 0.0275 0.0260 C2 0.0256 0.0232 0.0171 C1 0.0312 0.0265 0.0233 C6 0.0446 0.0255 0.0212 C5 0.0696 0.0346 0.0240 C7 0.0281 0.0218 0.0182 S1 0.0402 0.0311 0.0190 O1A 0.0287 0.0266 0.0203 O1B 0.0577 0.0274 0.0187 O1C 0.0252 0.0216 0.0159 C24 0.0256 0.0235 0.0206 C23 0.0305 0.0263 0.0196 C22 0.0441 0.0341 0.0235 C21 0.0305 0.0254 0.0191 C28 0.0322 0.0260 0.0214 C29 0.0447 0.0347 0.0239 C27 0.0541 0.0368 0.0201 C26 0.0247 0.0217 0.0180 N25 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.024 0.034 0.047 0.060 0.076 0.095 0.123 0.169 1.000 Number in group 422. 387. 363. 399. 370. 388. 375. 384. 385. 384. GooF 0.946 0.967 0.967 1.079 1.039 1.084 1.111 1.049 1.026 0.998 K 7.915 1.523 1.304 1.050 1.039 1.023 0.996 1.015 0.997 1.006 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.67 inf Number in group 394. 383. 389. 381. 380. 385. 388. 383. 390. 384. GooF 0.907 0.921 0.953 0.985 0.969 1.016 1.042 0.909 1.002 1.458 K 0.975 1.093 1.100 1.089 1.022 1.021 1.004 0.995 1.006 1.006 R1 0.238 0.209 0.180 0.168 0.112 0.088 0.058 0.044 0.042 0.039 Recommended weighting scheme: WGHT 0.0344 0.5988 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 9 1 22.56 78.68 6.14 0.084 1.11 -3 3 0 130.84 60.44 5.33 0.074 1.81 -3 -3 3 76.38 30.27 5.04 0.052 1.65 0 3 0 34.74 5.24 4.66 0.022 3.37 1 3 1 41.79 77.17 4.62 0.083 2.70 5 0 6 100.61 214.82 4.09 0.139 1.04 2 -3 1 554.95 429.46 4.05 0.197 2.35 0 0 6 340.30 270.14 3.78 0.156 2.26 2 -2 2 31.58 13.81 3.76 0.035 2.53 -3 2 0 2842.22 2432.37 3.62 0.469 1.95 -2 10 1 30.14 6.51 3.57 0.024 0.97 -1 -3 2 47.58 72.64 3.55 0.081 2.79 3 -2 2 333.82 265.40 3.52 0.155 1.86 0 2 3 151.15 110.73 3.35 0.100 3.14 -4 5 7 81.79 41.84 3.35 0.061 1.05 -2 -1 3 27.31 13.87 3.29 0.035 2.55 -7 -5 3 34.01 7.33 3.27 0.026 0.78 6 -1 1 41.26 0.03 3.20 0.002 1.01 0 -4 3 16.71 31.86 3.19 0.054 2.36 5 -1 7 100.91 150.71 3.18 0.117 1.01 -3 1 2 25.82 12.56 3.11 0.034 1.97 -2 2 3 10.63 22.42 3.08 0.045 2.32 6 -2 1 6.83 23.36 3.03 0.046 1.01 -5 -1 9 18.72 32.87 2.95 0.054 0.98 -5 10 2 68.80 134.61 2.95 0.110 0.80 4 7 7 45.01 13.54 2.94 0.035 0.84 3 1 0 43.67 26.70 2.93 0.049 1.96 2 -9 11 46.98 22.90 2.93 0.045 0.87 -1 0 14 10.23 2.13 2.93 0.014 0.97 -2 3 16 41.90 96.33 2.89 0.093 0.79 -4 -1 2 49.45 30.60 2.88 0.053 1.48 -6 2 1 86.28 58.46 2.87 0.073 1.01 0 3 2 93.92 124.53 2.83 0.106 2.85 -5 5 1 51.91 20.70 2.83 0.043 1.08 1 -3 1 27.67 42.92 2.81 0.062 3.05 0 -6 6 27.14 13.02 2.81 0.034 1.46 -1 -2 1 192.11 233.95 2.78 0.145 3.76 -2 8 4 92.66 134.01 2.77 0.110 1.10 -2 5 1 90.56 66.42 2.74 0.077 1.72 -3 -10 2 103.94 58.51 2.72 0.073 0.89 4 -7 12 142.89 95.32 2.72 0.093 0.81 3 3 0 6.17 0.20 2.72 0.004 1.68 -6 -5 3 21.75 0.02 2.69 0.001 0.88 2 8 4 155.21 215.25 2.67 0.139 1.02 3 7 2 3.06 19.01 2.67 0.041 1.09 -5 2 6 9.93 21.03 2.66 0.044 1.09 -3 0 9 73.25 101.53 2.63 0.096 1.26 -1 0 4 1563.30 1757.77 2.60 0.398 3.07 -2 -1 6 146.59 78.09 2.58 0.084 1.88 5 -3 12 74.94 43.37 2.58 0.063 0.81 Bond lengths and angles C4 - Distance Angles C3 1.3808 (0.0034) C5 1.3945 (0.0036) 118.05 (0.21) C7 1.5089 (0.0033) 120.72 (0.24) 121.22 (0.23) C4 - C3 C5 C3 - Distance Angles C4 1.3808 (0.0034) C2 1.3899 (0.0032) 121.85 (0.23) H3 0.9500 119.08 119.08 C3 - C4 C2 C2 - Distance Angles C3 1.3899 (0.0032) C1 1.3916 (0.0033) 118.89 (0.22) H2 0.9500 120.56 120.56 C2 - C3 C1 C1 - Distance Angles C6 1.3788 (0.0031) C2 1.3916 (0.0033) 120.35 (0.21) S1 1.7710 (0.0022) 120.39 (0.18) 119.25 (0.17) C1 - C6 C2 C6 - Distance Angles C1 1.3788 (0.0031) C5 1.3864 (0.0033) 119.77 (0.23) H6 0.9500 120.11 120.11 C6 - C1 C5 C5 - Distance Angles C6 1.3864 (0.0033) C4 1.3945 (0.0036) 121.09 (0.22) H5 0.9500 119.46 119.46 C5 - C6 C4 C7 - Distance Angles C4 1.5089 (0.0033) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C4 H7A H7B S1 - Distance Angles O1C 1.4525 (0.0017) O1A 1.4585 (0.0017) 113.44 (0.10) O1B 1.4588 (0.0016) 113.00 (0.10) 111.18 (0.10) C1 1.7710 (0.0022) 105.87 (0.10) 105.98 (0.10) 106.74 (0.10) S1 - O1C O1A O1B O1A - Distance Angles S1 1.4585 (0.0017) O1A - O1B - Distance Angles S1 1.4588 (0.0016) O1B - O1C - Distance Angles S1 1.4525 (0.0017) O1C - C24 - Distance Angles N25 1.5115 (0.0027) C28 1.5241 (0.0030) 106.26 (0.18) C29 1.5274 (0.0031) 105.13 (0.17) 111.05 (0.18) C23 1.5436 (0.0030) 104.35 (0.16) 114.90 (0.18) 114.08 (0.19) C24 - N25 C28 C29 C23 - Distance Angles C24 1.5436 (0.0030) C22 1.5473 (0.0031) 123.26 (0.18) H23A 0.9900 106.52 106.52 H23B 0.9900 106.52 106.52 106.52 C23 - C24 C22 H23A C22 - Distance Angles C27 1.5259 (0.0033) C21 1.5307 (0.0032) 108.24 (0.20) C26 1.5337 (0.0034) 108.97 (0.20) 107.65 (0.20) C23 1.5473 (0.0031) 113.72 (0.20) 105.55 (0.18) 112.41 (0.20) C22 - C27 C21 C26 C21 - Distance Angles C22 1.5307 (0.0032) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - C22 H21A H21B C28 - Distance Angles C24 1.5241 (0.0030) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C24 H28A H28B C29 - Distance Angles C24 1.5274 (0.0031) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - C24 H29A H29B C27 - Distance Angles C22 1.5259 (0.0033) 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 C26 - Distance Angles C22 1.5337 (0.0034) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C22 H26A H26B N25 - Distance Angles C24 1.5115 (0.0027) H25A 0.9100 109.47 H25B 0.9100 109.47 109.47 H25C 0.9100 109.47 109.47 109.47 N25 - C24 H25A H25B Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.91 2.814(2) 171.5 N25-H25A...O1A_$1 0.91 1.96 2.869(2) 177.9 N25-H25B...O1B_$2 0.91 2.61 3.136(2) 117.6 N25-H25B...O1A_$2 0.91 2.76 3.5655(18) 148.5 N25-H25B...S1_$2 0.91 1.92 2.822(2) 173.7 N25-H25C...O1C_$3 FMAP and GRID set by program FMAP 2 1 17 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0924 for 3857 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.3083 0.4615 0.7579 [ 0.69 A from C1 ] Deepest hole -0.42 at 0.2193 0.5283 0.7366 [ 0.80 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3047 / 21148 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3083 0.4615 0.7579 1.00000 0.05 0.29 0.69 C1 1.10 S1 1.75 C6 1.90 C2 Q2 1 -0.2520 -0.1723 0.5763 1.00000 0.05 0.24 0.75 C29 0.78 C24 1.39 H29C 1.43 H29A Q3 1 -0.0625 -0.0862 0.7461 1.00000 0.05 0.24 0.73 C22 0.84 C23 1.40 H23B 1.43 H23A Q4 1 0.3503 0.5784 0.6628 1.00000 0.05 0.23 0.81 O1B 1.01 S1 1.66 O1A 1.90 H25B Q5 1 0.1065 -0.0380 0.7635 1.00000 0.05 0.22 0.68 C22 0.92 C26 1.41 H26B 1.58 H26C Q6 1 0.4579 0.6522 0.7999 1.00000 0.05 0.22 1.30 O1B 1.52 H7B 2.19 H7C 2.20 S1 Q7 1 0.3204 0.3823 0.5540 1.00000 0.05 0.22 0.84 O1A 1.17 H25A 2.04 N25 2.07 H29A Q8 1 0.5416 0.3683 0.9550 1.00000 0.05 0.22 0.78 C4 1.13 C3 1.72 C5 1.77 H3 Q9 1 -0.1471 0.0645 0.9410 1.00000 0.05 0.22 1.04 H21C 1.34 H21A 1.37 C21 1.85 H21B Q10 1 0.4771 0.2878 0.9006 1.00000 0.05 0.22 0.82 C4 0.83 C3 1.61 H3 1.73 C5 Shortest distances between peaks (including symmetry equivalents) 8 10 1.06 3 5 1.11 1 4 1.91 4 6 1.98 1 6 2.08 4 7 2.31 2 3 2.54 2 7 2.58 1 7 2.81 9 9 2.87 8 8 2.90 3 9 2.99 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 0.02: 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. 0.69: 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 0.66: Structure factors and derivatives 0.92: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.11: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.00: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0016p-1 finished at 16:32:14 Total CPU time: 2.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++