+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0011 started at 18:04:04 on 30-Jan-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0011 in P4(1) CELL 0.71073 11.4912 11.4912 16.7890 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0001 0.0002 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM - Y, X, 1/4 + Z SYMM Y, - X, 3/4 + Z SFAC C H N O P S UNIT 72 96 20 8 12 8 V = 2216.95 F(000) = 1040.0 Mu = 0.48 mm-1 Cell Wt = 1997.81 Rho = 1.496 MERG 2 OMIT -3.00 55.00 OMIT 0 0 -4 OMIT -1 2 2 OMIT 0 1 2 OMIT 0 1 -2 FMAP 2 TEMP -153 ACTA SIZE 0.45 0.45 0.4 PLAN 20 BOND WGHT 0.02830 0.48190 L.S. 4 FVAR 0.79377 C1 1 0.829660 0.709213 -0.037300 11.00000 0.01473 0.01192 = 0.01630 0.00275 0.00084 0.00261 C2 1 0.849035 0.708152 -0.119064 11.00000 0.02457 0.02114 = 0.01906 0.00258 0.00342 0.00126 AFIX 43 H2 2 0.791623 0.680730 -0.153300 11.00000 -1.20000 AFIX 0 C3 1 0.953781 0.747904 -0.149575 11.00000 0.03317 0.02667 = 0.02484 0.00599 0.01413 0.00666 AFIX 43 H3 2 0.967266 0.746494 -0.204186 11.00000 -1.20000 AFIX 0 C4 1 1.038455 0.789850 -0.098062 11.00000 0.01839 0.02392 = 0.05498 0.01606 0.01096 0.00464 AFIX 43 H4 2 1.108449 0.817530 -0.118420 11.00000 -1.20000 AFIX 0 C5 1 1.019521 0.790812 -0.016536 11.00000 0.01998 0.02193 = 0.04740 0.00938 -0.01068 -0.00470 AFIX 43 H5 2 1.077262 0.818005 0.017524 11.00000 -1.20000 AFIX 0 C6 1 0.914702 0.751342 0.014499 11.00000 0.02403 0.01664 = 0.02126 0.00168 -0.00483 0.00050 AFIX 43 H6 2 0.901367 0.752975 0.069124 11.00000 -1.20000 AFIX 0 C7 1 0.837099 0.291172 -0.055017 11.00000 0.02148 0.01677 = 0.01234 -0.00422 0.00060 -0.00032 C8 1 0.956552 0.292076 -0.068616 11.00000 0.02307 0.02015 = 0.02273 -0.00715 0.00518 -0.00424 AFIX 43 H8 2 0.991720 0.357446 -0.090687 11.00000 -1.20000 AFIX 0 C9 1 1.022962 0.195761 -0.049310 11.00000 0.02291 0.02848 = 0.03045 -0.00948 0.00219 0.00345 AFIX 43 H9 2 1.102850 0.196482 -0.058160 11.00000 -1.20000 AFIX 0 C10 1 0.970481 0.098254 -0.016799 11.00000 0.03890 0.01884 = 0.02856 -0.00596 -0.00533 0.00784 AFIX 43 H10 2 1.015222 0.033531 -0.003829 11.00000 -1.20000 AFIX 0 C11 1 0.851318 0.096852 -0.003522 11.00000 0.03899 0.01767 = 0.02585 0.00061 0.00134 -0.00669 AFIX 43 H11 2 0.816543 0.031118 0.018334 11.00000 -1.20000 AFIX 0 C12 1 0.783446 0.193292 -0.022725 11.00000 0.02415 0.02287 = 0.02152 -0.00367 0.00400 -0.00539 AFIX 43 H12 2 0.703505 0.192324 -0.014109 11.00000 -1.20000 AFIX 0 C13 1 1.060310 0.553684 0.194831 11.00000 0.01516 0.02087 = 0.02394 -0.00264 -0.00474 -0.00540 AFIX 23 H13A 2 1.089336 0.603448 0.237060 11.00000 -1.20000 H13B 2 1.046524 0.601674 0.148246 11.00000 -1.20000 AFIX 0 C14 1 1.150431 0.461703 0.175340 11.00000 0.01069 0.02334 = 0.02487 0.00449 -0.00498 -0.00192 AFIX 23 H14A 2 1.169693 0.419197 0.223484 11.00000 -1.20000 H14B 2 1.220743 0.499492 0.156549 11.00000 -1.20000 AFIX 0 C15 1 1.108385 0.376386 0.112371 11.00000 0.01025 0.02010 = 0.02395 0.00217 0.00157 0.00263 AFIX 23 H15A 2 1.093473 0.417184 0.062832 11.00000 -1.20000 H15B 2 1.167599 0.317930 0.102645 11.00000 -1.20000 AFIX 0 C16 1 0.483660 0.216288 0.143884 11.00000 0.01527 0.01485 = 0.01940 -0.00052 -0.00471 -0.00395 AFIX 23 H16A 2 0.467645 0.133582 0.140221 11.00000 -1.20000 H16B 2 0.458363 0.252589 0.094681 11.00000 -1.20000 AFIX 0 C17 1 0.416469 0.267863 0.213440 11.00000 0.01107 0.01664 = 0.02217 0.00177 -0.00119 -0.00178 AFIX 23 H17A 2 0.435989 0.225753 0.261698 11.00000 -1.20000 H17B 2 0.333709 0.258542 0.204021 11.00000 -1.20000 AFIX 0 C18 1 0.443777 0.396642 0.225049 11.00000 0.00991 0.01722 = 0.02266 -0.00136 0.00080 0.00099 AFIX 23 H18A 2 0.419690 0.440216 0.178394 11.00000 -1.20000 H18B 2 0.401404 0.426331 0.270700 11.00000 -1.20000 AFIX 0 N1 3 0.867908 0.489207 0.077704 11.00000 0.00975 0.01504 = 0.01488 0.00229 -0.00181 -0.00052 N2 3 0.785822 0.353146 0.198234 11.00000 0.01069 0.01814 = 0.01291 0.00296 -0.00169 0.00074 N3 3 0.638166 0.433749 0.083957 11.00000 0.01052 0.01796 = 0.01600 0.00454 -0.00344 -0.00167 N4 3 0.999341 0.319613 0.141176 11.00000 0.01193 0.01293 = 0.01872 0.00068 -0.00032 0.00080 N5 3 0.570069 0.411229 0.237798 11.00000 0.01056 0.01317 = 0.01640 -0.00395 -0.00037 -0.00088 O1 4 0.951733 0.500007 0.219852 11.00000 0.01252 0.01924 = 0.01525 -0.00410 -0.00359 -0.00168 O2 4 0.608883 0.234545 0.154279 11.00000 0.01382 0.01057 = 0.01745 -0.00245 0.00025 -0.00075 P1 5 0.744419 0.489165 0.035996 11.00000 0.01075 0.01226 = 0.01051 0.00083 -0.00222 0.00030 P2 5 0.892570 0.415079 0.156755 11.00000 0.00873 0.01186 = 0.01100 -0.00045 -0.00201 0.00056 P3 5 0.655907 0.363349 0.166291 11.00000 0.00954 0.01073 = 0.01119 -0.00002 -0.00140 -0.00027 S1 6 0.694770 0.658490 0.002276 11.00000 0.01355 0.01574 = 0.01628 0.00461 0.00198 0.00369 S2 6 0.753917 0.417876 -0.078753 11.00000 0.02579 0.02100 = 0.01187 -0.00314 -0.00364 0.00207 H4N 2 0.979647 0.260997 0.108701 11.00000 0.01140 H5N 2 0.587988 0.472498 0.257603 11.00000 0.02062 HKLF 4 Covalent radii and connectivity table for 2007src0011 in P4(1) C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 S 1.030 C1 - C2 C6 S1 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - C8 C12 S2 C8 - C9 C7 C9 - C8 C10 C10 - C9 C11 C11 - C10 C12 C12 - C7 C11 C13 - O1 C14 C14 - C13 C15 C15 - N4 C14 C16 - O2 C17 C17 - C16 C18 C18 - N5 C17 N1 - P1 P2 N2 - P2 P3 N3 - P1 P3 N4 - C15 P2 N5 - C18 P3 O1 - C13 P2 O2 - C16 P3 P1 - N1 N3 S2 S1 P2 - N2 O1 N1 N4 P3 - O2 N2 N3 N5 S1 - C1 P1 S2 - C7 P1 Floating origin restraints generated 41685 Reflections read, of which 66 rejected -14 =< h =< 14, -14 =< k =< 14, -21 =< l =< 21, Max. 2-theta = 54.99 0 Systematic absence violations 0 Inconsistent equivalents 5057 Unique reflections, of which 0 suppressed R(int) = 0.0308 R(sigma) = 0.0181 Friedel opposites not merged Maximum memory for data reduction = 2595 / 53781 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 = 3366 / 349795 wR2 = 0.0498 before cycle 1 for 5057 data and 279 / 279 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.79215 0.00062 -2.601 OSF Mean shift/esd = 0.356 Maximum = -2.601 for OSF Max. shift = 0.026 A for H5N Max. dU = 0.003 for H5N Least-squares cycle 2 Maximum vector length = 511 Memory required = 3366 / 349795 wR2 = 0.0494 before cycle 2 for 5057 data and 279 / 279 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.79152 0.00062 -1.025 OSF Mean shift/esd = 0.120 Maximum = -1.025 for OSF Max. shift = 0.008 A for H5N Max. dU = 0.001 for H5N Least-squares cycle 3 Maximum vector length = 511 Memory required = 3366 / 349795 wR2 = 0.0493 before cycle 3 for 5057 data and 279 / 279 parameters GooF = S = 1.039; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.79151 0.00062 -0.024 OSF Mean shift/esd = 0.005 Maximum = 0.079 for z H4N Max. shift = 0.002 A for H4N Max. dU = 0.000 for H4N Least-squares cycle 4 Maximum vector length = 511 Memory required = 3366 / 349795 wR2 = 0.0493 before cycle 4 for 5057 data and 279 / 279 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.79151 0.00062 -0.002 OSF Mean shift/esd = 0.002 Maximum = -0.028 for x H5N Max. shift = 0.001 A for H5N Max. dU = 0.000 for H5N 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 H2 0.7905 0.6799 -0.1540 43 0.950 0.000 C2 C3 C1 H3 0.9674 0.7470 -0.2053 43 0.950 0.000 C3 C2 C4 H4 1.1100 0.8180 -0.1189 43 0.950 0.000 C4 C5 C3 H5 1.0786 0.8186 0.0182 43 0.950 0.000 C5 C4 C6 H6 0.9011 0.7530 0.0703 43 0.950 0.000 C6 C5 C1 H8 0.9925 0.3590 -0.0910 43 0.950 0.000 C8 C9 C7 H9 1.1047 0.1963 -0.0584 43 0.950 0.000 C9 C8 C10 H10 1.0161 0.0321 -0.0034 43 0.950 0.000 C10 C9 C11 H11 0.8157 0.0295 0.0186 43 0.950 0.000 C11 C10 C12 H12 0.7018 0.1924 -0.0137 43 0.950 0.000 C12 C7 C11 H13A 1.0897 0.6045 0.2379 23 0.990 0.000 C13 O1 C14 H13B 1.0461 0.6026 0.1473 23 0.990 0.000 C13 O1 C14 H14A 1.1703 0.4185 0.2245 23 0.990 0.000 C14 C13 C15 H14B 1.2222 0.5005 0.1561 23 0.990 0.000 C14 C13 C15 H15A 1.0932 0.4178 0.0617 23 0.990 0.000 C15 N4 C14 H15B 1.1688 0.3165 0.1025 23 0.990 0.000 C15 N4 C14 H16A 0.4673 0.1319 0.1401 23 0.990 0.000 C16 O2 C17 H16B 0.4578 0.2534 0.0937 23 0.990 0.000 C16 O2 C17 H17A 0.4364 0.2249 0.2627 23 0.990 0.000 C17 C16 C18 H17B 0.3320 0.2584 0.2039 23 0.990 0.000 C17 C16 C18 H18A 0.4193 0.4411 0.1774 23 0.990 0.000 C18 N5 C17 H18B 0.4006 0.4270 0.2716 23 0.990 0.000 C18 N5 C17 2007src0011 in P4(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.82967 0.70920 -0.03729 1.00000 0.01462 0.01140 0.01599 0.00253 0.00099 0.00262 0.01400 0.00246 0.00012 0.00012 0.00009 0.00000 0.00062 0.00061 0.00065 0.00049 0.00051 0.00048 0.00026 C2 0.84908 0.70813 -0.11901 1.00000 0.02467 0.02062 0.01874 0.00221 0.00344 0.00145 0.02134 0.00282 0.00014 0.00013 0.00009 0.00000 0.00075 0.00072 0.00073 0.00056 0.00059 0.00059 0.00031 H2 0.79054 0.67995 -0.15399 1.00000 0.02561 0.00000 0.00000 C3 0.95378 0.74816 -0.14948 1.00000 0.03255 0.02628 0.02476 0.00635 0.01365 0.00647 0.02786 0.00331 0.00015 0.00014 0.00011 0.00000 0.00089 0.00083 0.00083 0.00066 0.00069 0.00067 0.00035 H3 0.96742 0.74702 -0.20528 1.00000 0.03344 0.00000 0.00000 C4 1.03847 0.78984 -0.09812 1.00000 0.01841 0.02339 0.05500 0.01628 0.01102 0.00430 0.03227 0.00354 0.00014 0.00015 0.00013 0.00000 0.00072 0.00079 0.00119 0.00079 0.00076 0.00059 0.00041 H4 1.11001 0.81796 -0.11895 1.00000 0.03872 0.00000 0.00000 C5 1.01960 0.79083 -0.01660 1.00000 0.02012 0.02181 0.04750 0.00887 -0.01042 -0.00463 0.02981 0.00301 0.00014 0.00014 0.00012 0.00000 0.00076 0.00077 0.00110 0.00074 0.00071 0.00060 0.00038 H5 1.07859 0.81862 0.01818 1.00000 0.03577 0.00000 0.00000 C6 0.91471 0.75134 0.01447 1.00000 0.02356 0.01630 0.02134 0.00227 -0.00459 0.00039 0.02040 0.00257 0.00013 0.00012 0.00010 0.00000 0.00074 0.00067 0.00077 0.00056 0.00058 0.00055 0.00031 H6 0.90111 0.75302 0.07027 1.00000 0.02448 0.00000 0.00000 C7 0.83700 0.29120 -0.05501 1.00000 0.02133 0.01654 0.01232 -0.00434 0.00039 -0.00057 0.01673 0.00243 0.00013 0.00012 0.00008 0.00000 0.00068 0.00067 0.00063 0.00051 0.00054 0.00053 0.00027 C8 0.95654 0.29215 -0.06858 1.00000 0.02292 0.02019 0.02225 -0.00686 0.00493 -0.00417 0.02179 0.00255 0.00013 0.00013 0.00009 0.00000 0.00075 0.00071 0.00074 0.00059 0.00060 0.00057 0.00031 H8 0.99247 0.35898 -0.09104 1.00000 0.02615 0.00000 0.00000 C9 1.02310 0.19563 -0.04932 1.00000 0.02303 0.02781 0.03007 -0.00951 0.00241 0.00329 0.02697 0.00289 0.00014 0.00015 0.00011 0.00000 0.00077 0.00085 0.00087 0.00068 0.00066 0.00065 0.00034 H9 1.10469 0.19628 -0.05843 1.00000 0.03236 0.00000 0.00000 C10 0.97046 0.09820 -0.01675 1.00000 0.03876 0.01901 0.02810 -0.00623 -0.00475 0.00771 0.02863 0.00291 0.00016 0.00014 0.00010 0.00000 0.00093 0.00075 0.00087 0.00064 0.00073 0.00068 0.00035 H10 1.01614 0.03211 -0.00339 1.00000 0.03435 0.00000 0.00000 C11 0.85124 0.09675 -0.00354 1.00000 0.03872 0.01802 0.02565 0.00087 0.00115 -0.00626 0.02746 0.00287 0.00015 0.00014 0.00010 0.00000 0.00091 0.00072 0.00082 0.00063 0.00072 0.00065 0.00034 H11 0.81566 0.02953 0.01865 1.00000 0.03295 0.00000 0.00000 C12 0.78346 0.19330 -0.02265 1.00000 0.02383 0.02273 0.02124 -0.00366 0.00388 -0.00473 0.02260 0.00265 0.00014 0.00013 0.00009 0.00000 0.00075 0.00076 0.00076 0.00060 0.00060 0.00060 0.00031 H12 0.70183 0.19237 -0.01373 1.00000 0.02712 0.00000 0.00000 C13 1.06017 0.55367 0.19483 1.00000 0.01424 0.02073 0.02433 -0.00303 -0.00451 -0.00514 0.01977 0.00249 0.00012 0.00013 0.00010 0.00000 0.00066 0.00069 0.00076 0.00059 0.00057 0.00054 0.00030 H13A 1.08968 0.60454 0.23791 1.00000 0.02372 0.00000 0.00000 H13B 1.04605 0.60259 0.14726 1.00000 0.02372 0.00000 0.00000 C14 1.15053 0.46183 0.17538 1.00000 0.01071 0.02365 0.02403 0.00330 -0.00467 -0.00202 0.01947 0.00251 0.00012 0.00013 0.00009 0.00000 0.00059 0.00072 0.00075 0.00060 0.00056 0.00052 0.00029 H14A 1.17032 0.41855 0.22453 1.00000 0.02336 0.00000 0.00000 H14B 1.22219 0.50051 0.15613 1.00000 0.02336 0.00000 0.00000 C15 1.10837 0.37624 0.11235 1.00000 0.01018 0.01993 0.02347 0.00201 0.00172 0.00226 0.01786 0.00254 0.00012 0.00013 0.00009 0.00000 0.00062 0.00069 0.00075 0.00059 0.00054 0.00052 0.00028 H15A 1.09324 0.41777 0.06174 1.00000 0.02143 0.00000 0.00000 H15B 1.16875 0.31649 0.10252 1.00000 0.02143 0.00000 0.00000 C16 0.48367 0.21634 0.14388 1.00000 0.01447 0.01471 0.01936 -0.00062 -0.00454 -0.00386 0.01618 0.00231 0.00012 0.00012 0.00009 0.00000 0.00063 0.00062 0.00070 0.00054 0.00052 0.00050 0.00027 H16A 0.46732 0.13193 0.14013 1.00000 0.01941 0.00000 0.00000 H16B 0.45783 0.25341 0.09368 1.00000 0.01941 0.00000 0.00000 C17 0.41646 0.26790 0.21349 1.00000 0.01098 0.01654 0.02178 0.00163 -0.00089 -0.00228 0.01643 0.00242 0.00012 0.00012 0.00009 0.00000 0.00062 0.00064 0.00074 0.00054 0.00052 0.00052 0.00028 H17A 0.43642 0.22494 0.26274 1.00000 0.01972 0.00000 0.00000 H17B 0.33199 0.25839 0.20390 1.00000 0.01972 0.00000 0.00000 C18 0.44382 0.39663 0.22502 1.00000 0.00942 0.01679 0.02263 -0.00171 0.00041 0.00089 0.01628 0.00243 0.00012 0.00012 0.00009 0.00000 0.00060 0.00066 0.00072 0.00054 0.00052 0.00050 0.00028 H18A 0.41926 0.44107 0.17738 1.00000 0.01954 0.00000 0.00000 H18B 0.40059 0.42701 0.27160 1.00000 0.01954 0.00000 0.00000 N1 0.86790 0.48911 0.07770 1.00000 0.00962 0.01463 0.01462 0.00251 -0.00190 -0.00036 0.01296 0.00194 0.00009 0.00010 0.00007 0.00000 0.00049 0.00053 0.00056 0.00043 0.00043 0.00041 0.00022 N2 0.78575 0.35315 0.19822 1.00000 0.01027 0.01746 0.01279 0.00295 -0.00163 0.00069 0.01350 0.00201 0.00010 0.00010 0.00007 0.00000 0.00052 0.00055 0.00054 0.00044 0.00042 0.00042 0.00023 N3 0.63816 0.43377 0.08397 1.00000 0.01033 0.01732 0.01546 0.00432 -0.00368 -0.00179 0.01437 0.00198 0.00010 0.00010 0.00007 0.00000 0.00051 0.00055 0.00057 0.00044 0.00044 0.00041 0.00023 N4 0.99932 0.31969 0.14117 1.00000 0.01126 0.01271 0.01890 0.00049 -0.00021 0.00085 0.01429 0.00213 0.00010 0.00010 0.00007 0.00000 0.00054 0.00053 0.00059 0.00047 0.00045 0.00041 0.00023 N5 0.57017 0.41113 0.23776 1.00000 0.01021 0.01313 0.01649 -0.00419 -0.00047 -0.00109 0.01328 0.00207 0.00010 0.00010 0.00007 0.00000 0.00052 0.00055 0.00058 0.00046 0.00044 0.00042 0.00023 O1 0.95169 0.49993 0.21983 1.00000 0.01267 0.01894 0.01500 -0.00431 -0.00342 -0.00198 0.01554 0.00164 0.00008 0.00009 0.00006 0.00000 0.00045 0.00048 0.00047 0.00038 0.00038 0.00037 0.00020 O2 0.60887 0.23459 0.15424 1.00000 0.01325 0.01062 0.01737 -0.00241 -0.00003 -0.00094 0.01375 0.00158 0.00008 0.00008 0.00006 0.00000 0.00044 0.00043 0.00049 0.00037 0.00037 0.00034 0.00019 P1 0.74443 0.48918 0.03601 1.00000 0.01067 0.01207 0.01028 0.00081 -0.00227 0.00030 0.01101 0.00058 0.00003 0.00003 0.00002 0.00000 0.00015 0.00015 0.00015 0.00012 0.00012 0.00012 0.00007 P2 0.89259 0.41507 0.15676 1.00000 0.00859 0.01160 0.01079 -0.00041 -0.00206 0.00057 0.01033 0.00055 0.00003 0.00003 0.00002 0.00000 0.00014 0.00015 0.00015 0.00012 0.00012 0.00011 0.00007 P3 0.65592 0.36334 0.16628 1.00000 0.00928 0.01050 0.01102 -0.00001 -0.00139 -0.00029 0.01027 0.00056 0.00003 0.00003 0.00002 0.00000 0.00015 0.00015 0.00015 0.00012 0.00012 0.00011 0.00007 S1 0.69478 0.65851 0.00226 1.00000 0.01338 0.01559 0.01614 0.00466 0.00195 0.00377 0.01504 0.00061 0.00003 0.00003 0.00002 0.00000 0.00015 0.00016 0.00016 0.00012 0.00013 0.00012 0.00007 S2 0.75390 0.41788 -0.07875 1.00000 0.02552 0.02079 0.01173 -0.00313 -0.00372 0.00216 0.01935 0.00061 0.00003 0.00003 0.00002 0.00000 0.00018 0.00017 0.00015 0.00013 0.00013 0.00014 0.00008 H4N 0.97924 0.26237 0.10956 1.00000 0.01541 0.03246 0.00151 0.00154 0.00110 0.00000 0.00417 H5N 0.58959 0.47174 0.25596 1.00000 0.02510 0.03635 0.00168 0.00174 0.00121 0.00000 0.00495 Final Structure Factor Calculation for 2007src0011 in P4(1) Total number of l.s. parameters = 279 Maximum vector length = 511 Memory required = 3089 / 27090 wR2 = 0.0494 before cycle 5 for 5057 data and 2 / 279 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0188 for 4976 Fo > 4sig(Fo) and 0.0193 for all 5057 data wR2 = 0.0494, GooF = S = 1.039, Restrained GooF = 1.039 for all data Flack x parameter = 0.0128 with esd 0.0357 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 = 30.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0183 0.0143 0.0094 C1 0.0271 0.0204 0.0166 C2 0.0468 0.0225 0.0143 C3 0.0649 0.0166 0.0153 C4 0.0541 0.0195 0.0159 C5 0.0273 0.0191 0.0148 C6 0.0215 0.0190 0.0096 C7 0.0325 0.0186 0.0143 C8 0.0385 0.0256 0.0167 C9 0.0442 0.0270 0.0148 C10 0.0405 0.0257 0.0161 C11 0.0310 0.0186 0.0182 C12 0.0264 0.0235 0.0094 C13 0.0285 0.0208 0.0092 C14 0.0248 0.0192 0.0096 C15 0.0224 0.0169 0.0093 C16 0.0224 0.0167 0.0102 C17 0.0231 0.0165 0.0093 C18 0.0175 0.0125 0.0089 N1 0.0189 0.0127 0.0090 N2 0.0220 0.0127 0.0084 N3 0.0189 0.0131 0.0108 N4 0.0193 0.0114 0.0091 N5 0.0217 0.0164 0.0085 O1 0.0182 0.0135 0.0096 O2 0.0129 0.0121 0.0080 P1 0.0125 0.0111 0.0073 P2 0.0118 0.0105 0.0085 P3 0.0224 0.0127 0.0101 S1 0.0277 0.0202 0.0102 S2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.062 0.092 0.118 0.148 0.172 0.200 0.236 0.281 0.369 1.000 Number in group 516. 508. 496. 521. 494. 503. 507. 499. 507. 506. GooF 1.092 1.093 1.178 1.035 1.062 0.944 0.953 1.031 0.963 1.016 K 1.029 0.979 0.978 0.987 1.002 1.002 1.002 1.010 1.008 0.994 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.64 inf Number in group 507. 504. 508. 514. 503. 510. 498. 499. 510. 504. GooF 0.953 0.906 0.871 0.880 0.853 0.913 0.898 0.901 1.012 1.825 K 0.989 1.000 1.008 1.004 1.010 1.012 1.006 1.002 0.999 0.989 R1 0.034 0.027 0.023 0.021 0.018 0.018 0.015 0.013 0.013 0.022 Recommended weighting scheme: WGHT 0.0245 0.5587 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) -4 5 -3 138.03 89.94 5.78 0.073 1.71 -4 5 3 133.74 86.85 5.52 0.072 1.71 0 5 0 481.26 380.08 5.28 0.151 2.30 1 5 0 209.61 279.54 5.10 0.129 2.25 3 5 0 429.19 539.55 5.03 0.180 1.97 4 4 0 949.69 1138.86 4.82 0.261 2.03 1 5 -4 1284.34 1081.47 4.70 0.255 1.99 -3 5 0 564.19 462.49 4.66 0.166 1.97 -1 3 3 1769.33 2061.02 4.43 0.351 3.05 2 5 0 27.08 12.21 4.40 0.027 2.13 -1 3 -3 1732.10 2009.24 4.31 0.347 3.05 0 3 9 863.03 1018.00 4.26 0.247 1.68 -1 5 5 1671.42 1936.41 4.25 0.341 1.87 -1 2 6 250.46 197.76 4.22 0.109 2.46 1 4 0 360.56 440.06 4.17 0.162 2.79 0 2 -4 497.43 414.82 4.13 0.158 3.39 -2 7 0 787.85 926.20 4.12 0.236 1.58 0 3 -5 489.83 407.15 4.11 0.156 2.52 1 5 4 1265.14 1093.15 4.09 0.256 1.99 -1 2 -6 260.97 208.06 4.00 0.112 2.46 0 2 4 472.42 395.73 3.97 0.154 3.39 -2 5 0 277.02 224.29 3.94 0.116 2.13 0 3 5 443.55 370.04 3.92 0.149 2.52 -5 6 0 415.95 498.31 3.91 0.173 1.47 0 3 -9 920.14 1071.30 3.89 0.253 1.68 3 3 4 480.63 403.90 3.85 0.156 2.28 3 3 -4 498.21 421.02 3.82 0.159 2.28 -4 9 -2 26.96 46.74 3.74 0.053 1.16 -1 5 -5 1735.07 1972.37 3.72 0.344 1.87 3 3 -5 763.14 658.85 3.69 0.199 2.11 1 5 5 73.88 52.42 3.61 0.056 1.87 1 3 -7 260.65 315.89 3.59 0.138 2.00 3 3 5 777.46 675.47 3.56 0.201 2.11 1 5 -5 73.83 52.34 3.51 0.056 1.87 1 1 7 1317.50 1491.49 3.42 0.299 2.30 0 0 -8 2921.52 3333.24 3.39 0.447 2.10 -1 7 -18 159.27 216.80 3.38 0.114 0.81 2 6 -4 176.25 140.73 3.37 0.092 1.67 0 5 1 276.86 231.44 3.36 0.118 2.28 -2 6 3 208.42 169.92 3.35 0.101 1.73 -3 5 -6 591.01 679.57 3.32 0.202 1.61 -2 4 0 292.65 346.42 3.32 0.144 2.57 0 2 -1 11115.74 12353.01 3.32 0.860 5.44 -3 5 6 582.71 671.48 3.30 0.201 1.61 0 2 1 11135.10 12407.22 3.27 0.862 5.44 -3 5 2 7248.08 6565.34 3.26 0.627 1.92 0 0 8 2924.49 3286.78 3.26 0.444 2.10 -3 5 -2 7313.48 6633.57 3.25 0.631 1.92 2 6 4 167.40 135.00 3.23 0.090 1.67 1 3 7 278.80 329.26 3.18 0.140 2.00 Bond lengths and angles C1 - Distance Angles C2 1.3901 (0.0021) C6 1.3944 (0.0021) 120.37 (0.14) S1 1.7840 (0.0014) 120.26 (0.12) 119.36 (0.11) C1 - C2 C6 C2 - Distance Angles C3 1.3859 (0.0023) C1 1.3901 (0.0021) 120.05 (0.15) C2 - C3 C3 - Distance Angles C2 1.3859 (0.0023) C4 1.3857 (0.0028) 119.65 (0.16) C3 - C2 C4 - Distance Angles C5 1.3857 (0.0029) C3 1.3857 (0.0028) 120.50 (0.16) C4 - C5 C5 - Distance Angles C4 1.3857 (0.0029) C6 1.3895 (0.0023) 120.25 (0.16) C5 - C4 C6 - Distance Angles C5 1.3895 (0.0023) C1 1.3944 (0.0021) 119.17 (0.15) C6 - C5 C7 - Distance Angles C8 1.3924 (0.0021) C12 1.3926 (0.0021) 120.40 (0.14) S2 1.7861 (0.0015) 118.98 (0.11) 120.61 (0.12) C7 - C8 C12 C8 - Distance Angles C9 1.3855 (0.0023) C7 1.3924 (0.0021) 120.01 (0.14) C8 - C9 C9 - Distance Angles C8 1.3855 (0.0023) C10 1.3851 (0.0025) 119.88 (0.15) C9 - C8 C10 - Distance Angles C9 1.3851 (0.0025) C11 1.3879 (0.0025) 120.26 (0.16) C10 - C9 C11 - Distance Angles C10 1.3879 (0.0025) C12 1.3930 (0.0024) 120.37 (0.15) C11 - C10 C12 - Distance Angles C7 1.3926 (0.0021) C11 1.3930 (0.0024) 119.09 (0.15) C12 - C7 C13 - Distance Angles O1 1.4530 (0.0017) C14 1.5160 (0.0020) 110.73 (0.11) C13 - O1 C14 - Distance Angles C13 1.5160 (0.0020) C15 1.5238 (0.0021) 112.40 (0.11) C14 - C13 C15 - Distance Angles N4 1.4922 (0.0017) C14 1.5238 (0.0021) 108.84 (0.12) C15 - N4 C16 - Distance Angles O2 1.4643 (0.0016) C17 1.5209 (0.0021) 110.60 (0.11) C16 - O2 C17 - Distance Angles C16 1.5209 (0.0021) C18 1.5247 (0.0019) 111.77 (0.12) C17 - C16 C18 - Distance Angles N5 1.4770 (0.0017) C17 1.5247 (0.0019) 109.30 (0.11) C18 - N5 N1 - Distance Angles P1 1.5820 (0.0011) P2 1.6019 (0.0012) 121.71 (0.07) N1 - P1 N2 - Distance Angles P2 1.5806 (0.0012) P3 1.5896 (0.0011) 123.18 (0.07) N2 - P2 N3 - Distance Angles P1 1.5953 (0.0012) P3 1.6145 (0.0012) 122.37 (0.07) N3 - P1 N4 - Distance Angles C15 1.4922 (0.0017) P2 1.6656 (0.0012) 112.51 (0.09) N4 - C15 N5 - Distance Angles C18 1.4770 (0.0017) P3 1.6470 (0.0012) 116.42 (0.10) N5 - C18 O1 - Distance Angles C13 1.4530 (0.0017) P2 1.5916 (0.0010) 115.74 (0.09) O1 - C13 O2 - Distance Angles C16 1.4643 (0.0016) P3 1.5881 (0.0009) 118.88 (0.08) O2 - C16 P1 - Distance Angles N1 1.5820 (0.0011) N3 1.5953 (0.0012) 117.58 (0.06) S2 2.0965 (0.0005) 111.09 (0.05) 110.34 (0.05) S1 2.1054 (0.0005) 111.25 (0.05) 107.29 (0.05) 97.35 (0.02) P1 - N1 N3 S2 P2 - Distance Angles N2 1.5806 (0.0012) O1 1.5916 (0.0010) 108.32 (0.06) N1 1.6019 (0.0012) 117.81 (0.06) 107.54 (0.06) N4 1.6656 (0.0012) 110.18 (0.06) 101.15 (0.06) 110.47 (0.06) P2 - N2 O1 N1 P3 - Distance Angles O2 1.5881 (0.0009) N2 1.5896 (0.0011) 107.08 (0.06) N3 1.6145 (0.0012) 108.36 (0.06) 116.38 (0.06) N5 1.6470 (0.0012) 101.52 (0.06) 109.89 (0.06) 112.39 (0.06) P3 - O2 N2 N3 S1 - Distance Angles C1 1.7840 (0.0014) P1 2.1054 (0.0005) 99.58 (0.05) S1 - C1 S2 - Distance Angles C7 1.7861 (0.0015) P1 2.0965 (0.0005) 98.12 (0.05) S2 - C7 FMAP and GRID set by program FMAP 2 3 21 GRID -1.389 -2 -2 1.389 2 2 R1 = 0.0181 for 2615 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.16 at 0.7610 0.8123 0.1990 [ 0.67 A from C7 ] Deepest hole -0.27 at 0.9033 0.3744 0.1870 [ 0.70 A from P2 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 2922 / 20559 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8123 0.2390 -0.0510 1.00000 0.05 0.16 0.67 C7 0.78 C12 1.51 H12 1.79 C8 Q2 1 1.1027 0.5022 0.1786 1.00000 0.05 0.15 0.72 C14 0.81 C13 1.42 H14B 1.43 H13B Q3 1 0.8959 0.2957 -0.0639 1.00000 0.05 0.15 0.70 C7 0.70 C8 1.40 H8 1.88 C9 Q4 1 0.8341 0.7152 -0.0767 1.00000 0.05 0.15 0.67 C1 0.73 C2 1.45 H2 1.84 C6 Q5 1 0.8127 0.3348 -0.0643 1.00000 0.05 0.13 0.59 C7 1.19 S2 1.73 C8 1.80 C12 Q6 1 0.4524 0.2412 0.1772 1.00000 0.05 0.13 0.72 C16 0.80 C17 1.41 H16B 1.41 H16A Q7 1 0.6126 0.2002 0.2365 1.00000 0.05 0.13 1.44 O2 1.80 H15A 2.09 H17A 2.14 H15B Q8 1 1.0076 0.5225 0.2042 1.00000 0.05 0.12 0.72 C13 0.74 O1 1.40 H13B 1.45 H13A Q9 1 0.8159 0.3932 0.2006 1.00000 0.05 0.12 0.58 N2 1.18 P2 1.96 P3 2.01 O1 Q10 1 0.7342 0.5560 -0.1679 1.00000 0.05 0.12 1.58 H2 1.86 H18B 2.13 H14A 2.19 S2 Q11 1 0.8673 0.7271 -0.0160 1.00000 0.05 0.12 0.60 C1 0.80 C6 1.53 H6 1.76 C2 Q12 1 0.5994 0.5288 -0.0275 1.00000 0.05 0.12 1.92 S1 2.03 P1 2.06 H18A 2.08 H5N Q13 1 0.7961 0.6583 -0.0264 1.00000 0.05 0.12 0.72 C1 1.26 S1 1.76 C2 1.86 C6 Q14 1 0.5964 0.1395 -0.0535 1.00000 0.05 0.12 1.51 H12 1.57 O1 2.22 P2 2.29 H13B Q15 1 1.1716 0.2703 0.2082 1.00000 0.05 0.11 1.73 H14A 1.85 H17B 1.85 H15B 2.14 C15 Q16 1 1.1801 0.6438 0.1341 1.00000 0.05 0.11 1.63 H13B 1.76 H14B 2.00 C13 2.08 H13A Q17 1 0.6108 0.5944 -0.0842 1.00000 0.05 0.11 1.89 S1 1.97 H18A 2.44 H18B 2.46 H14B Q18 1 0.6739 0.4478 0.0557 1.00000 0.05 0.11 0.65 N3 1.00 P1 2.10 P3 2.31 N1 Q19 1 0.4205 0.3283 0.2147 1.00000 0.05 0.11 0.70 C17 0.85 C18 1.31 H17B 1.44 H18A Q20 1 0.6152 0.2902 0.1551 1.00000 0.05 0.11 0.64 O2 0.98 P3 1.74 C16 2.03 N5 Shortest distances between peaks (including symmetry equivalents) 3 5 1.06 4 11 1.10 1 5 1.12 11 13 1.15 4 13 1.15 1 3 1.18 2 8 1.20 12 17 1.22 6 19 1.24 7 20 1.71 12 18 1.88 8 14 1.90 6 20 1.99 2 16 2.00 10 17 2.04 6 7 2.15 9 14 2.39 13 17 2.45 19 20 2.49 18 20 2.55 4 16 2.58 4 10 2.65 8 9 2.66 16 17 2.67 7 19 2.68 8 16 2.69 9 20 2.70 12 13 2.71 1 14 2.73 10 13 2.74 2 15 2.82 10 12 2.84 5 18 2.88 4 17 2.92 15 19 2.94 13 16 2.96 10 19 2.97 17 18 2.98 9 18 2.99 Time profile in seconds ----------------------- 0.07: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.01: 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 0.01: Analyse other restraints etc. 6.14: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.80: Structure factors and derivatives 3.93: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.52: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.07: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.06: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0011 finished at 18:05:49 Total CPU time: 14.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++