+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005slh0403 started at 23:09:21 on 27-Apr-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005slh0403 in P2(1)/n CELL 0.71073 11.9856 17.7146 15.2383 90.000 101.808 90.000 ZERR 4.00 0.0009 0.0011 0.0005 0.000 0.004 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O P S CD UNIT 112 120 8 16 8 16 4 V = 3166.93 F(000) = 1544.0 Mu = 1.09 mm-1 Cell Wt = 3044.48 Rho = 1.596 MERG 2 OMIT -3.00 55.00 OMIT 0 1 2 OMIT 2 0 0 OMIT -1 1 2 OMIT -2 1 1 OMIT -1 2 2 EXTI 0.00057 FMAP 2 PLAN 5 SIZE 0.10 0.36 0.38 ACTA BOND $H WGHT 0.02690 2.29820 L.S. 6 TEMP -153.00 FVAR 0.25654 C1 1 0.235177 0.855518 0.755336 11.00000 0.01269 0.04026 = 0.03752 0.01782 0.00291 0.00485 AFIX 137 H1A 2 0.249681 0.907291 0.777392 11.00000 -1.50000 H1B 2 0.156486 0.841497 0.756809 11.00000 -1.50000 H1C 2 0.246765 0.852311 0.693621 11.00000 -1.50000 AFIX 0 C2 1 0.502046 0.738893 0.889762 11.00000 0.01664 0.01401 = 0.01582 -0.00007 0.00353 0.00001 C3 1 0.443544 0.708129 0.951978 11.00000 0.02041 0.02409 = 0.02439 0.00539 0.00950 0.00577 AFIX 43 H3 2 0.372194 0.728775 0.957614 11.00000 -1.20000 AFIX 0 C4 1 0.489006 0.647686 1.005496 11.00000 0.02455 0.02731 = 0.02527 0.00982 0.01181 0.00429 AFIX 43 H4 2 0.448201 0.626457 1.046789 11.00000 -1.20000 AFIX 0 C5 1 0.594365 0.618289 0.998538 11.00000 0.02274 0.01537 = 0.01692 0.00376 0.00141 0.00249 C6 1 0.654191 0.648792 0.937986 11.00000 0.01675 0.02119 = 0.02209 0.00262 0.00547 0.00380 AFIX 43 H6 2 0.726543 0.629049 0.933601 11.00000 -1.20000 AFIX 0 C7 1 0.606880 0.708556 0.883895 11.00000 0.01704 0.01895 = 0.02042 0.00281 0.00631 -0.00017 AFIX 43 H7 2 0.647293 0.729094 0.841938 11.00000 -1.20000 AFIX 0 C8 1 0.742966 0.530541 1.056179 11.00000 0.03094 0.02508 = 0.02296 0.00560 0.00492 0.01271 AFIX 137 H8A 2 0.746375 0.510395 0.996889 11.00000 -1.50000 H8B 2 0.760204 0.490209 1.100925 11.00000 -1.50000 H8C 2 0.798906 0.571254 1.071587 11.00000 -1.50000 AFIX 0 C9 1 0.901885 0.757949 0.692597 11.00000 0.02668 0.01680 = 0.03916 -0.00554 -0.00195 -0.00046 AFIX 137 H9A 2 0.876325 0.729802 0.740233 11.00000 -1.50000 H9B 2 0.954962 0.726807 0.667147 11.00000 -1.50000 H9C 2 0.835904 0.770847 0.645500 11.00000 -1.50000 AFIX 0 C10 1 0.989909 0.965043 0.788692 11.00000 0.01354 0.01568 = 0.01919 0.00009 0.00461 0.00147 C11 1 1.023075 1.004483 0.718273 11.00000 0.01980 0.01887 = 0.01559 -0.00095 0.00538 0.00067 AFIX 43 H11 2 0.991009 0.991245 0.657973 11.00000 -1.20000 AFIX 0 C12 1 1.101574 1.062139 0.735670 11.00000 0.02206 0.02090 = 0.01615 0.00225 0.00790 -0.00080 AFIX 43 H12 2 1.123956 1.088074 0.687497 11.00000 -1.20000 AFIX 0 C13 1 1.148336 1.082521 0.824172 11.00000 0.01661 0.01706 = 0.02246 -0.00017 0.00538 -0.00237 C14 1 1.115872 1.044434 0.894775 11.00000 0.02151 0.02549 = 0.01432 0.00016 0.00085 -0.00452 AFIX 43 H14 2 1.147151 1.058249 0.955025 11.00000 -1.20000 AFIX 0 C15 1 1.037018 0.985819 0.876241 11.00000 0.01845 0.02327 = 0.01709 0.00556 0.00404 -0.00127 AFIX 43 H15 2 1.015111 0.959603 0.924420 11.00000 -1.20000 AFIX 0 C16 1 1.264328 1.170767 0.921383 11.00000 0.04317 0.03959 = 0.02476 -0.00478 0.00233 -0.02331 AFIX 137 H16A 2 1.198993 1.187474 0.945919 11.00000 -1.50000 H16B 2 1.314738 1.213786 0.918151 11.00000 -1.50000 H16C 2 1.306303 1.131757 0.960311 11.00000 -1.50000 AFIX 0 C17 1 0.441674 1.074391 0.722114 11.00000 0.01747 0.01757 = 0.01578 0.00200 0.00526 -0.00112 AFIX 43 H17 2 0.423033 1.058651 0.776957 11.00000 -1.20000 AFIX 0 C18 1 0.393734 1.140409 0.682696 11.00000 0.01670 0.01530 = 0.01893 -0.00126 0.00426 0.00108 AFIX 43 H18 2 0.343157 1.168769 0.710381 11.00000 -1.20000 AFIX 0 C19 1 0.419604 1.165214 0.602583 11.00000 0.01436 0.01473 = 0.01691 0.00081 0.00120 0.00191 C20 1 0.491119 1.119264 0.563971 11.00000 0.02785 0.02779 = 0.01759 0.00770 0.01093 0.01214 AFIX 43 H20 2 0.509104 1.132614 0.508095 11.00000 -1.20000 AFIX 0 C21 1 0.535433 1.054346 0.607600 11.00000 0.02503 0.02289 = 0.02021 0.00128 0.00910 0.00990 AFIX 43 H21 2 0.584340 1.023984 0.580499 11.00000 -1.20000 AFIX 0 C22 1 0.370375 1.236196 0.562081 11.00000 0.01480 0.01709 = 0.01759 -0.00169 0.00365 0.00400 C23 1 0.698920 1.063105 0.931936 11.00000 0.02084 0.01902 = 0.01756 0.00043 0.00683 -0.00485 AFIX 43 H23 2 0.648714 1.033619 0.958749 11.00000 -1.20000 AFIX 0 C24 1 0.753700 1.123489 0.979506 11.00000 0.02119 0.01941 = 0.01478 -0.00114 0.00563 -0.00340 AFIX 43 H24 2 0.741088 1.134770 1.037646 11.00000 -1.20000 AFIX 0 C25 1 0.827633 1.167790 0.941665 11.00000 0.01562 0.01433 = 0.01867 -0.00053 0.00309 -0.00110 C26 1 0.843223 1.147110 0.856544 11.00000 0.01951 0.01541 = 0.02073 0.00020 0.00911 -0.00238 AFIX 43 H26 2 0.893903 1.175009 0.828475 11.00000 -1.20000 AFIX 0 C27 1 0.784851 1.086060 0.813296 11.00000 0.02237 0.01648 = 0.01586 -0.00241 0.00708 -0.00005 AFIX 43 H27 2 0.796030 1.073284 0.755162 11.00000 -1.20000 AFIX 0 C28 1 0.884112 1.235553 0.984750 11.00000 0.02164 0.01751 = 0.02059 -0.00149 0.00804 -0.00536 N1 3 0.513111 1.031790 0.686342 11.00000 0.01484 0.01533 = 0.01703 0.00181 0.00160 0.00052 N2 3 0.713090 1.043982 0.849629 11.00000 0.01542 0.01496 = 0.01936 -0.00137 0.00305 -0.00205 O1 4 0.312811 0.804532 0.811697 11.00000 0.01125 0.02027 = 0.02036 0.00561 0.00341 -0.00078 O2 4 0.631252 0.559369 1.054917 11.00000 0.02669 0.02535 = 0.02333 0.01008 0.00647 0.00930 O3 4 0.958733 0.826511 0.729415 11.00000 0.01327 0.01616 = 0.02653 -0.00331 0.00290 0.00100 O4 4 1.224821 1.140516 0.833422 11.00000 0.02846 0.02648 = 0.02063 -0.00256 0.00534 -0.01347 P1 5 0.446863 0.819251 0.822793 11.00000 0.01165 0.01327 = 0.01593 0.00192 0.00478 -0.00002 P2 5 0.883825 0.891948 0.762233 11.00000 0.01161 0.01635 = 0.01600 0.00063 0.00309 0.00064 S1 6 0.489037 0.916053 0.890301 11.00000 0.01931 0.01552 = 0.01836 -0.00214 0.00805 -0.00200 S2 6 0.494574 0.818855 0.704931 11.00000 0.01820 0.01606 = 0.01569 0.00003 0.00672 -0.00108 S3 6 0.762467 0.923964 0.656960 11.00000 0.01247 0.02287 = 0.01468 0.00177 0.00267 0.00273 S4 6 0.820449 0.859339 0.866504 11.00000 0.01654 0.02406 = 0.01757 0.00509 0.00461 -0.00159 CD1 7 0.626504 0.935844 0.773911 11.00000 0.01250 0.01242 = 0.01562 0.00042 0.00451 -0.00080 H22 2 0.322872 1.261486 0.594625 11.00000 0.01933 H28 2 0.927055 1.262786 0.950630 11.00000 0.03271 HKLF 4 Covalent radii and connectivity table for 2005slh0403 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 S 1.030 CD 1.490 C1 - O1 C2 - C7 C3 P1 C3 - C4 C2 C4 - C3 C5 C5 - O2 C6 C4 C6 - C5 C7 C7 - C2 C6 C8 - O2 C9 - O3 C10 - C15 C11 P2 C11 - C12 C10 C12 - C11 C13 C13 - O4 C14 C12 C14 - C13 C15 C15 - C10 C14 C16 - O4 C17 - N1 C18 C18 - C17 C19 C19 - C18 C20 C22 C20 - C21 C19 C21 - N1 C20 C22 - C28_$2 C19 C23 - N2 C24 C24 - C23 C25 C25 - C24 C26 C28 C26 - C27 C25 C27 - N2 C26 C28 - C22_$1 C25 N1 - C17 C21 Cd1 N2 - C27 C23 Cd1 O1 - C1 P1 O2 - C5 C8 O3 - C9 P2 O4 - C13 C16 P1 - O1 C2 S2 S1 P2 - O3 C10 S4 S3 S1 - P1 Cd1 S2 - P1 Cd1 S3 - P2 Cd1 S4 - P2 Cd1 Cd1 - N2 N1 S3 S1 S2 S4 Operators for generating equivalent atoms: $1 x+1/2, -y+5/2, z+1/2 $2 x-1/2, -y+5/2, z-1/2 44788 Reflections read, of which 889 rejected -15 =< h =< 15, -22 =< k =< 22, -19 =< l =< 19, Max. 2-theta = 54.95 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -3 9 10 52.57 1.34 3 9.82 1 Inconsistent equivalents 7249 Unique reflections, of which 0 suppressed R(int) = 0.0397 R(sigma) = 0.0311 Friedel opposites merged Maximum memory for data reduction = 3587 / 71739 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 = 4627 / 491789 wR2 = 0.0638 before cycle 1 for 7249 data and 383 / 383 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 2.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25653 0.00024 -0.038 OSF 2 0.00058 0.00011 0.073 EXTI Mean shift/esd = 0.020 Maximum = -0.154 for U22 Cd1 Max. shift = 0.001 A for H28 Max. dU = 0.000 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4627 / 491789 wR2 = 0.0637 before cycle 2 for 7249 data and 383 / 383 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 2.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25652 0.00024 -0.057 OSF 2 0.00058 0.00011 0.024 EXTI Mean shift/esd = 0.006 Maximum = -0.057 for OSF Max. shift = 0.000 A for H28 Max. dU = 0.000 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4627 / 491789 wR2 = 0.0637 before cycle 3 for 7249 data and 383 / 383 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 2.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25652 0.00024 -0.004 OSF 2 0.00058 0.00011 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.004 for OSF Max. shift = 0.000 A for H1C Max. dU = 0.000 for H28 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4627 / 491789 wR2 = 0.0637 before cycle 4 for 7249 data and 383 / 383 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 2.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25652 0.00024 -0.002 OSF 2 0.00058 0.00011 -0.003 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for EXTI Max. shift = 0.000 A for H1B Max. dU = 0.000 for C3 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4627 / 491789 wR2 = 0.0637 before cycle 5 for 7249 data and 383 / 383 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 2.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25652 0.00024 -0.001 OSF 2 0.00058 0.00011 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.003 for z Cd1 Max. shift = 0.000 A for H1C Max. dU = 0.000 for H22 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4627 / 491789 wR2 = 0.0637 before cycle 6 for 7249 data and 383 / 383 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 2.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25652 0.00024 0.002 OSF 2 0.00058 0.00011 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.003 for z Cd1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for C16 Largest correlation matrix elements 0.561 U22 Cd1 / OSF 0.550 U11 Cd1 / OSF 0.552 U33 Cd1 / OSF 0.537 EXTI / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.2497 0.9073 0.7774 137 0.980 0.000 C1 O1 H1A H1B 0.1565 0.8415 0.7569 137 0.980 0.000 C1 O1 H1A H1C 0.2467 0.8523 0.6936 137 0.980 0.000 C1 O1 H1A H3 0.3722 0.7288 0.9576 43 0.950 0.000 C3 C4 C2 H4 0.4482 0.6265 1.0468 43 0.950 0.000 C4 C3 C5 H6 0.7265 0.6291 0.9336 43 0.950 0.000 C6 C5 C7 H7 0.6473 0.7291 0.8419 43 0.950 0.000 C7 C2 C6 H8A 0.7464 0.5104 0.9969 137 0.980 0.000 C8 O2 H8A H8B 0.7602 0.4902 1.1009 137 0.980 0.000 C8 O2 H8A H8C 0.7989 0.5712 1.0716 137 0.980 0.000 C8 O2 H8A H9A 0.8763 0.7298 0.7402 137 0.980 0.000 C9 O3 H9A H9B 0.9550 0.7268 0.6671 137 0.980 0.000 C9 O3 H9A H9C 0.8359 0.7709 0.6455 137 0.980 0.000 C9 O3 H9A H11 0.9910 0.9912 0.6580 43 0.950 0.000 C11 C12 C10 H12 1.1240 1.0881 0.6875 43 0.950 0.000 C12 C11 C13 H14 1.1471 1.0583 0.9550 43 0.950 0.000 C14 C13 C15 H15 1.0151 0.9596 0.9244 43 0.950 0.000 C15 C10 C14 H16A 1.1990 1.1875 0.9459 137 0.980 0.000 C16 O4 H16A H16B 1.3148 1.2138 0.9181 137 0.980 0.000 C16 O4 H16A H16C 1.3063 1.1318 0.9603 137 0.980 0.000 C16 O4 H16A H17 0.4230 1.0586 0.7770 43 0.950 0.000 C17 N1 C18 H18 0.3432 1.1688 0.7104 43 0.950 0.000 C18 C17 C19 H20 0.5091 1.1326 0.5081 43 0.950 0.000 C20 C21 C19 H21 0.5844 1.0240 0.5805 43 0.950 0.000 C21 N1 C20 H23 0.6487 1.0336 0.9587 43 0.950 0.000 C23 N2 C24 H24 0.7411 1.1348 1.0377 43 0.950 0.000 C24 C23 C25 H26 0.8939 1.1750 0.8285 43 0.950 0.000 C26 C27 C25 H27 0.7960 1.0733 0.7552 43 0.950 0.000 C27 N2 C26 2005slh0403 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.23518 0.85551 0.75534 1.00000 0.01269 0.04021 0.03745 0.01777 0.00289 0.00481 0.03043 0.00501 0.00020 0.00015 0.00017 0.00000 0.00117 0.00147 0.00142 0.00118 0.00101 0.00104 0.00058 H1A 0.24973 0.90729 0.77736 1.00000 0.04565 0.00000 0.00000 H1B 0.15649 0.84152 0.75686 1.00000 0.04565 0.00000 0.00000 H1C 0.24671 0.85227 0.69361 1.00000 0.04565 0.00000 0.00000 C2 0.50204 0.73889 0.88976 1.00000 0.01660 0.01401 0.01582 -0.00007 0.00354 0.00004 0.01544 0.00379 0.00018 0.00011 0.00014 0.00000 0.00110 0.00099 0.00103 0.00079 0.00083 0.00081 0.00043 C3 0.44354 0.70813 0.95198 1.00000 0.02039 0.02410 0.02439 0.00543 0.00951 0.00577 0.02226 0.00436 0.00019 0.00013 0.00015 0.00000 0.00120 0.00119 0.00117 0.00094 0.00094 0.00093 0.00049 H3 0.37219 0.72877 0.95762 1.00000 0.02671 0.00000 0.00000 C4 0.48899 0.64769 1.00550 1.00000 0.02456 0.02726 0.02524 0.00979 0.01183 0.00430 0.02473 0.00463 0.00020 0.00013 0.00016 0.00000 0.00128 0.00124 0.00121 0.00098 0.00098 0.00099 0.00051 H4 0.44818 0.62645 1.04678 1.00000 0.02967 0.00000 0.00000 C5 0.59437 0.61829 0.99854 1.00000 0.02269 0.01537 0.01692 0.00376 0.00141 0.00252 0.01870 0.00403 0.00019 0.00012 0.00014 0.00000 0.00119 0.00102 0.00106 0.00082 0.00087 0.00087 0.00045 C6 0.65419 0.64879 0.93799 1.00000 0.01672 0.02115 0.02208 0.00262 0.00544 0.00379 0.01978 0.00412 0.00019 0.00012 0.00014 0.00000 0.00113 0.00111 0.00113 0.00088 0.00088 0.00088 0.00046 H6 0.72654 0.62905 0.93360 1.00000 0.02373 0.00000 0.00000 C7 0.60688 0.70855 0.88389 1.00000 0.01704 0.01891 0.02042 0.00279 0.00632 -0.00014 0.01844 0.00397 0.00018 0.00012 0.00014 0.00000 0.00112 0.00108 0.00109 0.00087 0.00087 0.00086 0.00045 H7 0.64729 0.72909 0.84193 1.00000 0.02212 0.00000 0.00000 C8 0.74295 0.53053 1.05618 1.00000 0.03095 0.02507 0.02296 0.00561 0.00492 0.01273 0.02641 0.00472 0.00021 0.00013 0.00016 0.00000 0.00137 0.00123 0.00120 0.00096 0.00100 0.00104 0.00053 H8A 0.74637 0.51041 0.99688 1.00000 0.03962 0.00000 0.00000 H8B 0.76017 0.49018 1.10090 1.00000 0.03962 0.00000 0.00000 H8C 0.79891 0.57124 1.07162 1.00000 0.03962 0.00000 0.00000 C9 0.90189 0.75796 0.69259 1.00000 0.02663 0.01676 0.03916 -0.00552 -0.00192 -0.00051 0.02875 0.00423 0.00021 0.00013 0.00017 0.00000 0.00134 0.00114 0.00144 0.00102 0.00109 0.00097 0.00056 H9A 0.87633 0.72981 0.74023 1.00000 0.04312 0.00000 0.00000 H9B 0.95496 0.72682 0.66714 1.00000 0.04312 0.00000 0.00000 H9C 0.83590 0.77086 0.64550 1.00000 0.04312 0.00000 0.00000 C10 0.98991 0.96504 0.78870 1.00000 0.01347 0.01570 0.01918 0.00010 0.00459 0.00149 0.01594 0.00389 0.00018 0.00012 0.00014 0.00000 0.00104 0.00100 0.00106 0.00082 0.00083 0.00082 0.00042 C11 1.02307 1.00448 0.71827 1.00000 0.01981 0.01887 0.01554 -0.00096 0.00540 0.00066 0.01782 0.00402 0.00018 0.00012 0.00014 0.00000 0.00113 0.00107 0.00104 0.00082 0.00085 0.00086 0.00044 H11 0.99100 0.99125 0.65797 1.00000 0.02139 0.00000 0.00000 C12 1.10158 1.06214 0.73567 1.00000 0.02203 0.02085 0.01615 0.00225 0.00789 -0.00082 0.01911 0.00409 0.00019 0.00012 0.00014 0.00000 0.00117 0.00111 0.00105 0.00086 0.00087 0.00090 0.00045 H12 1.12396 1.08808 0.68750 1.00000 0.02293 0.00000 0.00000 C13 1.14834 1.08252 0.82418 1.00000 0.01658 0.01705 0.02239 -0.00014 0.00534 -0.00236 0.01848 0.00400 0.00019 0.00012 0.00015 0.00000 0.00112 0.00105 0.00114 0.00086 0.00088 0.00084 0.00045 C14 1.11587 1.04443 0.89477 1.00000 0.02148 0.02548 0.01433 0.00017 0.00085 -0.00453 0.02083 0.00407 0.00019 0.00013 0.00014 0.00000 0.00119 0.00116 0.00105 0.00087 0.00087 0.00093 0.00047 H14 1.14714 1.05825 0.95502 1.00000 0.02500 0.00000 0.00000 C15 1.03702 0.98581 0.87624 1.00000 0.01846 0.02327 0.01707 0.00554 0.00402 -0.00130 0.01955 0.00406 0.00018 0.00012 0.00014 0.00000 0.00114 0.00113 0.00106 0.00087 0.00086 0.00090 0.00046 H15 1.01512 0.95960 0.92442 1.00000 0.02346 0.00000 0.00000 C16 1.26433 1.17077 0.92138 1.00000 0.04317 0.03959 0.02471 -0.00477 0.00232 -0.02332 0.03648 0.00437 0.00024 0.00015 0.00016 0.00000 0.00166 0.00153 0.00131 0.00113 0.00115 0.00128 0.00066 H16A 1.19899 1.18751 0.94590 1.00000 0.05472 0.00000 0.00000 H16B 1.31477 1.21377 0.91815 1.00000 0.05472 0.00000 0.00000 H16C 1.30626 1.13176 0.96033 1.00000 0.05472 0.00000 0.00000 C17 0.44168 1.07439 0.72212 1.00000 0.01747 0.01754 0.01576 0.00200 0.00524 -0.00114 0.01666 0.00388 0.00018 0.00011 0.00014 0.00000 0.00111 0.00105 0.00102 0.00081 0.00084 0.00084 0.00044 H17 0.42304 1.05864 0.77696 1.00000 0.01999 0.00000 0.00000 C18 0.39373 1.14041 0.68270 1.00000 0.01668 0.01527 0.01889 -0.00122 0.00425 0.00109 0.01686 0.00384 0.00018 0.00012 0.00014 0.00000 0.00111 0.00101 0.00107 0.00083 0.00085 0.00083 0.00044 H18 0.34315 1.16877 0.71039 1.00000 0.02023 0.00000 0.00000 C19 0.41961 1.16522 0.60258 1.00000 0.01434 0.01470 0.01688 0.00080 0.00120 0.00191 0.01559 0.00380 0.00018 0.00011 0.00014 0.00000 0.00105 0.00099 0.00104 0.00080 0.00081 0.00081 0.00042 C20 0.49112 1.11927 0.56397 1.00000 0.02781 0.02775 0.01755 0.00768 0.01091 0.01211 0.02348 0.00459 0.00020 0.00013 0.00015 0.00000 0.00130 0.00122 0.00111 0.00092 0.00095 0.00100 0.00051 H20 0.50910 1.13261 0.50809 1.00000 0.02818 0.00000 0.00000 C21 0.53544 1.05435 0.60760 1.00000 0.02501 0.02286 0.02016 0.00128 0.00908 0.00988 0.02204 0.00437 0.00020 0.00013 0.00015 0.00000 0.00125 0.00117 0.00112 0.00091 0.00093 0.00094 0.00049 H21 0.58436 1.02400 0.58051 1.00000 0.02645 0.00000 0.00000 C22 0.37037 1.23620 0.56208 1.00000 0.01477 0.01704 0.01758 -0.00167 0.00364 0.00399 0.01641 0.00393 0.00018 0.00012 0.00014 0.00000 0.00109 0.00105 0.00107 0.00083 0.00085 0.00084 0.00044 C23 0.69892 1.06311 0.93194 1.00000 0.02083 0.01899 0.01752 0.00044 0.00681 -0.00484 0.01870 0.00398 0.00019 0.00012 0.00014 0.00000 0.00116 0.00108 0.00106 0.00084 0.00087 0.00088 0.00045 H23 0.64871 1.03362 0.95875 1.00000 0.02244 0.00000 0.00000 C24 0.75370 1.12349 0.97951 1.00000 0.02123 0.01936 0.01475 -0.00116 0.00564 -0.00342 0.01817 0.00391 0.00018 0.00012 0.00014 0.00000 0.00118 0.00107 0.00103 0.00083 0.00086 0.00088 0.00045 H24 0.74109 1.13477 1.03765 1.00000 0.02180 0.00000 0.00000 C25 0.82763 1.16779 0.94166 1.00000 0.01558 0.01429 0.01866 -0.00056 0.00309 -0.00111 0.01623 0.00381 0.00018 0.00011 0.00014 0.00000 0.00108 0.00100 0.00106 0.00082 0.00083 0.00081 0.00043 C26 0.84323 1.14711 0.85655 1.00000 0.01947 0.01539 0.02070 0.00021 0.00909 -0.00238 0.01781 0.00396 0.00019 0.00012 0.00014 0.00000 0.00115 0.00102 0.00110 0.00084 0.00088 0.00085 0.00044 H26 0.89391 1.17501 0.82848 1.00000 0.02137 0.00000 0.00000 C27 0.78485 1.08606 0.81330 1.00000 0.02233 0.01647 0.01584 -0.00237 0.00706 -0.00007 0.01776 0.00396 0.00019 0.00012 0.00014 0.00000 0.00118 0.00102 0.00104 0.00081 0.00088 0.00087 0.00045 H27 0.79604 1.07329 0.75517 1.00000 0.02132 0.00000 0.00000 C28 0.88411 1.23555 0.98475 1.00000 0.02162 0.01750 0.02055 -0.00151 0.00801 -0.00537 0.01936 0.00404 0.00019 0.00012 0.00015 0.00000 0.00120 0.00108 0.00113 0.00087 0.00092 0.00090 0.00046 N1 0.51311 1.03179 0.68635 1.00000 0.01482 0.01530 0.01698 0.00182 0.00156 0.00051 0.01594 0.00320 0.00015 0.00010 0.00011 0.00000 0.00091 0.00086 0.00089 0.00069 0.00070 0.00070 0.00037 N2 0.71309 1.04398 0.84963 1.00000 0.01542 0.01494 0.01932 -0.00136 0.00306 -0.00203 0.01663 0.00318 0.00015 0.00010 0.00012 0.00000 0.00092 0.00085 0.00092 0.00070 0.00072 0.00070 0.00037 O1 0.31281 0.80453 0.81170 1.00000 0.01119 0.02025 0.02039 0.00558 0.00341 -0.00079 0.01725 0.00270 0.00012 0.00008 0.00010 0.00000 0.00073 0.00075 0.00076 0.00061 0.00058 0.00059 0.00031 O2 0.63126 0.55937 1.05492 1.00000 0.02668 0.02531 0.02329 0.01008 0.00648 0.00930 0.02490 0.00313 0.00014 0.00009 0.00010 0.00000 0.00090 0.00086 0.00083 0.00067 0.00068 0.00069 0.00036 O3 0.95874 0.82651 0.72941 1.00000 0.01326 0.01611 0.02650 -0.00331 0.00290 0.00102 0.01879 0.00265 0.00012 0.00008 0.00010 0.00000 0.00076 0.00074 0.00083 0.00062 0.00062 0.00059 0.00032 O4 1.22482 1.14051 0.83342 1.00000 0.02843 0.02647 0.02060 -0.00257 0.00534 -0.01348 0.02512 0.00278 0.00014 0.00009 0.00010 0.00000 0.00092 0.00086 0.00081 0.00066 0.00068 0.00071 0.00036 P1 0.44686 0.81925 0.82279 1.00000 0.01163 0.01325 0.01592 0.00193 0.00478 -0.00003 0.01332 0.00098 0.00004 0.00003 0.00003 0.00000 0.00027 0.00025 0.00026 0.00020 0.00020 0.00020 0.00011 P2 0.88382 0.89195 0.76223 1.00000 0.01158 0.01633 0.01598 0.00062 0.00309 0.00065 0.01459 0.00100 0.00005 0.00003 0.00004 0.00000 0.00027 0.00026 0.00026 0.00020 0.00020 0.00020 0.00012 S1 0.48904 0.91605 0.89030 1.00000 0.01930 0.01551 0.01833 -0.00214 0.00805 -0.00200 0.01711 0.00098 0.00005 0.00003 0.00004 0.00000 0.00028 0.00025 0.00026 0.00020 0.00021 0.00020 0.00011 S2 0.49457 0.81886 0.70493 1.00000 0.01817 0.01605 0.01568 0.00003 0.00672 -0.00107 0.01617 0.00097 0.00005 0.00003 0.00003 0.00000 0.00028 0.00025 0.00025 0.00019 0.00020 0.00020 0.00011 S3 0.76247 0.92396 0.65696 1.00000 0.01245 0.02285 0.01465 0.00178 0.00267 0.00273 0.01666 0.00098 0.00004 0.00003 0.00003 0.00000 0.00026 0.00027 0.00025 0.00020 0.00020 0.00020 0.00011 S4 0.82045 0.85934 0.86650 1.00000 0.01651 0.02404 0.01755 0.00509 0.00460 -0.00158 0.01921 0.00102 0.00005 0.00003 0.00004 0.00000 0.00028 0.00028 0.00026 0.00021 0.00021 0.00022 0.00012 Cd1 0.62650 0.93584 0.77391 1.00000 0.01249 0.01240 0.01560 0.00042 0.00451 -0.00079 0.01327 0.00027 0.00001 0.00001 0.00001 0.00000 0.00009 0.00008 0.00009 0.00006 0.00006 0.00006 0.00006 H22 0.32285 1.26151 0.59469 1.00000 0.01935 0.04287 0.00200 0.00133 0.00153 0.00000 0.00609 H28 0.92712 1.26283 0.95061 1.00000 0.03273 0.04796 0.00224 0.00149 0.00173 0.00000 0.00726 Final Structure Factor Calculation for 2005slh0403 in P2(1)/n Total number of l.s. parameters = 383 Maximum vector length = 511 Memory required = 4244 / 26061 wR2 = 0.0637 before cycle 7 for 7249 data and 0 / 383 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 2.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0273 for 5988 Fo > 4sig(Fo) and 0.0399 for all 7249 data wR2 = 0.0637, GooF = S = 1.064, Restrained GooF = 1.064 for all data Occupancy sum of asymmetric unit = 41.00 for non-hydrogen and 30.00 for hydrogen atoms Principal mean square atomic displacements U 0.0568 0.0230 0.0115 C1 0.0166 0.0157 0.0140 C2 0.0327 0.0188 0.0152 C3 0.0385 0.0214 0.0142 C4 0.0245 0.0199 0.0117 C5 0.0252 0.0197 0.0144 C6 0.0228 0.0182 0.0143 C7 0.0411 0.0243 0.0138 C8 0.0466 0.0244 0.0152 C9 0.0193 0.0163 0.0122 C10 0.0203 0.0191 0.0141 C11 0.0234 0.0216 0.0123 C12 0.0225 0.0189 0.0141 C13 0.0291 0.0197 0.0137 C14 0.0269 0.0185 0.0132 C15 0.0654 0.0281 0.0160 C16 0.0189 0.0183 0.0127 C17 0.0193 0.0173 0.0140 C18 0.0185 0.0161 0.0121 C19 0.0420 0.0157 0.0128 C20 0.0343 0.0197 0.0122 C21 0.0209 0.0172 0.0111 C22 0.0250 0.0184 0.0127 C23 0.0240 0.0168 0.0137 C24 0.0189 0.0162 0.0136 C25 0.0244 0.0167 0.0123 C26 0.0232 0.0177 0.0124 C27 0.0267 0.0182 0.0132 C28 0.0189 0.0156 0.0133 N1 0.0198 0.0171 0.0130 N2 0.0262 0.0149 0.0107 O1 0.0383 0.0235 0.0130 O2 0.0281 0.0155 0.0128 O3 0.0410 0.0205 0.0139 O4 0.0172 0.0128 0.0100 P1 0.0168 0.0156 0.0114 P2 0.0232 0.0146 0.0134 S1 0.0200 0.0160 0.0124 S2 0.0237 0.0145 0.0118 S3 0.0272 0.0175 0.0130 S4 0.0160 0.0130 0.0108 Cd1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.031 0.047 0.063 0.082 0.104 0.129 0.162 0.220 1.000 Number in group 773. 719. 714. 720. 706. 744. 705. 719. 725. 724. GooF 0.945 1.085 1.134 1.142 1.060 1.043 1.054 0.933 1.077 1.158 K 0.768 0.884 0.897 0.944 0.964 0.976 0.986 1.002 1.012 1.012 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 733. 742. 728. 727. 713. 711. 724. 727. 723. 721. GooF 1.015 1.042 1.036 1.032 0.955 0.966 0.982 0.923 1.085 1.498 K 0.967 1.000 0.990 0.993 1.011 1.017 1.025 1.022 1.015 0.988 R1 0.096 0.077 0.065 0.052 0.039 0.032 0.028 0.022 0.020 0.022 Recommended weighting scheme: WGHT 0.0265 2.3235 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 0 17 4903.90 6526.07 5.69 0.205 0.89 -4 0 2 6692.16 8033.02 4.83 0.227 2.94 4 0 0 2.02 125.46 4.77 0.028 2.93 -2 3 3 530.98 356.72 4.70 0.048 3.45 -4 7 4 250.59 123.25 4.53 0.028 1.81 -4 3 7 861.03 632.61 4.41 0.064 1.83 -1 6 8 45.58 181.84 4.18 0.034 1.60 1 6 5 187.24 96.94 4.14 0.025 2.02 -2 2 8 4068.51 4806.00 4.10 0.176 1.85 2 9 0 130.01 271.54 4.09 0.042 1.87 -8 0 2 970.29 1282.27 4.07 0.091 1.50 0 1 7 1887.94 2297.32 4.05 0.121 2.12 -1 1 9 886.89 679.85 4.02 0.066 1.68 2 0 6 81.78 177.81 3.96 0.034 2.14 -8 18 3 805.02 1255.01 3.93 0.090 0.82 -4 7 6 1172.57 1465.31 3.84 0.097 1.63 -1 1 8 4124.83 4797.33 3.83 0.175 1.89 -4 4 4 307.60 448.55 3.79 0.054 2.23 3 10 0 219.28 128.49 3.71 0.029 1.61 2 4 10 -26.62 47.61 3.64 0.017 1.32 -3 4 5 1744.80 2088.46 3.61 0.116 2.27 -14 8 1 -61.13 253.59 3.60 0.040 0.79 8 0 8 241.12 84.52 3.57 0.023 1.05 1 4 12 1655.05 2051.18 3.56 0.115 1.17 1 7 1 1961.28 2319.99 3.56 0.122 2.42 1 8 2 387.75 530.42 3.55 0.058 2.07 -10 9 10 83.69 370.73 3.53 0.049 0.91 -4 5 5 1903.31 1602.77 3.44 0.101 1.96 -8 11 11 140.21 293.40 3.38 0.043 0.92 4 2 1 1078.46 1302.61 3.33 0.091 2.65 5 19 6 259.71 514.16 3.26 0.057 0.80 -6 2 1 1807.68 1534.17 3.24 0.099 1.94 1 0 3 4925.85 5620.94 3.22 0.190 4.27 -6 3 3 178.44 284.35 3.20 0.043 1.86 -5 2 1 558.70 709.24 3.20 0.067 2.31 1 2 9 2680.96 3084.73 3.19 0.141 1.57 -3 2 8 5669.97 6382.03 3.16 0.202 1.80 4 2 2 3665.04 4146.20 3.12 0.163 2.46 -2 3 4 6222.59 6974.45 3.12 0.211 3.00 -12 14 5 1543.96 1987.91 3.11 0.113 0.78 -6 2 2 436.72 323.60 3.09 0.046 1.95 5 6 4 249.48 356.66 3.08 0.048 1.55 -7 1 19 553.10 31.28 3.06 0.014 0.77 2 6 6 307.52 415.72 3.05 0.052 1.73 2 5 0 11315.24 12517.67 3.01 0.283 3.03 -2 0 2 15647.66 17423.95 3.01 0.334 5.15 1 5 5 216.75 139.03 2.99 0.030 2.18 0 20 1 986.70 1252.06 2.98 0.090 0.88 1 3 6 2356.77 2057.27 2.98 0.115 2.17 -6 6 4 6995.46 6287.04 2.97 0.201 1.60 Bond lengths and angles C1 - Distance Angles O1 1.4463 (0.0026) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - O1 H1A H1B C2 - Distance Angles C7 1.3863 (0.0030) C3 1.3999 (0.0030) 118.62 (0.19) P1 1.7969 (0.0021) 120.24 (0.16) 121.06 (0.16) C2 - C7 C3 C3 - Distance Angles C4 1.3879 (0.0031) C2 1.3999 (0.0030) 120.50 (0.21) H3 0.9500 119.75 119.75 C3 - C4 C2 C4 - Distance Angles C3 1.3879 (0.0031) C5 1.3902 (0.0032) 119.85 (0.21) H4 0.9500 120.08 120.08 C4 - C3 C5 C5 - Distance Angles O2 1.3665 (0.0025) C6 1.3885 (0.0031) 124.78 (0.20) C4 1.3902 (0.0032) 114.85 (0.20) 120.37 (0.19) C5 - O2 C6 C6 - Distance Angles C5 1.3885 (0.0031) C7 1.3894 (0.0030) 119.16 (0.20) H6 0.9500 120.42 120.42 C6 - C5 C7 C7 - Distance Angles C2 1.3863 (0.0030) C6 1.3894 (0.0030) 121.50 (0.20) H7 0.9500 119.25 119.25 C7 - C2 C6 C8 - Distance Angles O2 1.4294 (0.0028) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - O2 H8A H8B C9 - Distance Angles O3 1.4482 (0.0026) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - O3 H9A H9B C10 - Distance Angles C15 1.3876 (0.0030) C11 1.4045 (0.0030) 118.66 (0.20) P2 1.8017 (0.0022) 122.37 (0.16) 118.92 (0.16) C10 - C15 C11 C11 - Distance Angles C12 1.3772 (0.0030) C10 1.4045 (0.0030) 120.72 (0.20) H11 0.9500 119.64 119.64 C11 - C12 C10 C12 - Distance Angles C11 1.3772 (0.0030) C13 1.3979 (0.0031) 120.04 (0.20) H12 0.9500 119.98 119.98 C12 - C11 C13 C13 - Distance Angles O4 1.3648 (0.0026) C14 1.3911 (0.0031) 125.00 (0.20) C12 1.3979 (0.0031) 114.97 (0.19) 120.03 (0.20) C13 - O4 C14 C14 - Distance Angles C13 1.3911 (0.0031) C15 1.3936 (0.0031) 119.35 (0.20) H14 0.9500 120.33 120.33 C14 - C13 C15 C15 - Distance Angles C10 1.3876 (0.0030) C14 1.3936 (0.0031) 121.20 (0.20) H15 0.9500 119.40 119.40 C15 - C10 C14 C16 - Distance Angles O4 1.4313 (0.0028) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - O4 H16A H16B C17 - Distance Angles N1 1.3381 (0.0028) C18 1.3848 (0.0029) 122.89 (0.20) H17 0.9500 118.56 118.56 C17 - N1 C18 C18 - Distance Angles C17 1.3848 (0.0029) C19 1.3910 (0.0029) 120.01 (0.20) H18 0.9500 119.99 119.99 C18 - C17 C19 C19 - Distance Angles C18 1.3910 (0.0029) C20 1.3964 (0.0030) 116.88 (0.19) C22 1.4701 (0.0028) 119.75 (0.19) 123.36 (0.19) C19 - C18 C20 C20 - Distance Angles C21 1.3792 (0.0030) C19 1.3964 (0.0030) 119.47 (0.20) H20 0.9500 120.27 120.27 C20 - C21 C19 C21 - Distance Angles N1 1.3426 (0.0028) C20 1.3792 (0.0030) 123.47 (0.20) H21 0.9500 118.26 118.26 C21 - N1 C20 C22 - Distance Angles C28_$2 1.3212 (0.0032) C19 1.4701 (0.0028) 125.86 (0.21) H22 0.9424 (0.0241) 119.29 (1.41) 114.81 (1.41) C22 - C28_$2 C19 C23 - Distance Angles N2 1.3431 (0.0028) C24 1.3805 (0.0029) 123.25 (0.20) H23 0.9500 118.37 118.37 C23 - N2 C24 C24 - Distance Angles C23 1.3805 (0.0029) C25 1.3940 (0.0029) 119.56 (0.20) H24 0.9500 120.22 120.22 C24 - C23 C25 C25 - Distance Angles C24 1.3940 (0.0029) C26 1.3966 (0.0029) 116.98 (0.19) C28 1.4657 (0.0029) 123.38 (0.19) 119.57 (0.19) C25 - C24 C26 C26 - Distance Angles C27 1.3801 (0.0029) C25 1.3966 (0.0029) 119.86 (0.20) H26 0.9500 120.07 120.07 C26 - C27 C25 C27 - Distance Angles N2 1.3405 (0.0028) C26 1.3801 (0.0029) 122.96 (0.20) H27 0.9500 118.52 118.52 C27 - N2 C26 C28 - Distance Angles C22_$1 1.3212 (0.0032) C25 1.4657 (0.0029) 125.40 (0.21) H28 0.9379 (0.0274) 118.85 (1.62) 115.43 (1.59) C28 - C22_$1 C25 N1 - Distance Angles C17 1.3381 (0.0028) C21 1.3426 (0.0028) 117.22 (0.18) Cd1 2.4030 (0.0017) 120.60 (0.14) 120.88 (0.14) N1 - C17 C21 N2 - Distance Angles C27 1.3405 (0.0028) C23 1.3431 (0.0028) 117.38 (0.18) Cd1 2.3638 (0.0017) 120.25 (0.14) 122.24 (0.14) N2 - C27 C23 O1 - Distance Angles C1 1.4463 (0.0026) P1 1.6022 (0.0015) 118.06 (0.13) O1 - C1 O2 - Distance Angles C5 1.3665 (0.0025) C8 1.4294 (0.0028) 117.58 (0.18) O2 - C5 O3 - Distance Angles C9 1.4482 (0.0026) P2 1.6075 (0.0015) 118.48 (0.14) O3 - C9 O4 - Distance Angles C13 1.3648 (0.0026) C16 1.4313 (0.0028) 117.72 (0.18) O4 - C13 P1 - Distance Angles O1 1.6022 (0.0015) C2 1.7969 (0.0021) 100.11 (0.09) S2 1.9933 (0.0007) 111.76 (0.06) 111.64 (0.07) S1 2.0103 (0.0007) 109.55 (0.06) 111.12 (0.07) 112.06 (0.03) P1 - O1 C2 S2 P2 - Distance Angles O3 1.6075 (0.0015) C10 1.8017 (0.0022) 100.04 (0.09) S4 1.9822 (0.0008) 111.67 (0.06) 113.50 (0.07) S3 2.0139 (0.0007) 108.28 (0.06) 109.72 (0.07) 112.82 (0.03) P2 - O3 C10 S4 S1 - Distance Angles P1 2.0103 (0.0007) Cd1 2.6794 (0.0006) 84.10 (0.02) S1 - P1 S2 - Distance Angles P1 1.9933 (0.0007) Cd1 2.6870 (0.0006) 84.21 (0.02) S2 - P1 S3 - Distance Angles P2 2.0139 (0.0007) Cd1 2.6579 (0.0006) 86.00 (0.02) S3 - P2 S4 - Distance Angles P2 1.9822 (0.0008) Cd1 2.8087 (0.0006) 82.54 (0.02) S4 - P2 Cd1 - Distance Angles N2 2.3638 (0.0017) N1 2.4030 (0.0017) 80.78 (0.06) S3 2.6579 (0.0006) 97.08 (0.05) 92.20 (0.04) S1 2.6794 (0.0006) 92.92 (0.05) 96.06 (0.04) 167.93 (0.02) S2 2.6870 (0.0006) 168.64 (0.05) 96.18 (0.04) 93.96 (0.02) 76.45 (0.02) S4 2.8087 (0.0006) 84.85 (0.04) 159.42 (0.04) 74.97 (0.02) 99.33 (0.02) 100.64 (0.02) Cd1 - N2 N1 S3 S1 S2 FMAP and GRID set by program FMAP 2 2 23 GRID -1.250 -2 -2 1.250 2 2 R1 = 0.0392 for 7249 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.74 at 0.8780 0.0638 0.3229 [ 1.82 A from H11 ] Deepest hole -0.63 at 0.3231 0.0883 0.2360 [ 0.78 A from CD1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4211 / 30536 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.1220 0.9362 0.6771 1.00000 0.05 0.74 1.82 H11 1.89 C11 1.89 O2 2.00 H1A Q2 1 0.4248 0.8644 0.6808 1.00000 0.05 0.56 1.17 S2 2.19 H1C 2.27 P1 2.31 H8C Q3 1 0.7982 0.8219 0.7235 1.00000 0.05 0.54 1.63 H9C 1.64 P2 1.81 C9 1.87 H9A Q4 1 0.8754 0.6958 0.7230 1.00000 0.05 0.49 0.66 H9A 1.26 C9 1.51 H9B 1.78 H9C Q5 1 1.0163 0.7105 0.6169 1.00000 0.05 0.45 1.20 H9B 2.14 C9 2.20 H16B 2.53 H9C Shortest distances between peaks (including symmetry equivalents) 3 4 2.42 4 5 2.58 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.01: 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. 2.21: 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 4.98: Structure factors and derivatives 11.92: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.74: Solve l.s. equations 0.00: Generate HTAB table 0.04: Other dependent quantities, CIF, tables 0.18: Analysis of variance 0.07: Merge reflections for Fourier and .fcf 0.07: Fourier summations 0.09: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005slh0403 finished at 23:09:42 Total CPU time: 20.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++