+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src1313 started at 15:31:11 on 11-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src1313 in P2(1)/c CELL 0.71073 20.7923 10.7114 8.4013 90.000 94.923 90.000 ZERR 4.00 0.0009 0.0005 0.0003 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N F P UNIT 64 80 8 36 4 V = 1864.19 F(000) = 904.0 Mu = 0.24 mm-1 Cell Wt = 1769.24 Rho = 1.576 MERG 2 OMIT -3.00 55.00 OMIT 3 1 1 OMIT 0 2 0 OMIT 3 0 0 OMIT 1 1 7 FMAP 2 PLAN 20 SIZE 0.04 0.20 0.40 WPDB ACTA BOND WGHT 0.06760 1.30830 L.S. 4 TEMP -153.00 FVAR 0.63910 MOLE 1 C1 1 -0.329894 0.604692 -0.105188 11.00000 0.03323 0.02846 = 0.04360 -0.00284 0.00493 0.00034 AFIX 23 H1A 2 -0.300904 0.652646 -0.170012 11.00000 -1.20000 H1B 2 -0.314279 0.612793 0.009020 11.00000 -1.20000 AFIX 0 C2 1 -0.398439 0.650397 -0.134113 11.00000 0.03705 0.03476 = 0.06474 -0.00348 0.00139 0.00340 AFIX 23 H2A 2 -0.399595 0.739380 -0.166090 11.00000 -1.20000 H2B 2 -0.421840 0.640458 -0.037121 11.00000 -1.20000 AFIX 0 C3 1 -0.427887 0.567617 -0.269724 11.00000 0.03171 0.03983 = 0.04783 0.00558 0.00061 0.00324 AFIX 23 H3A 2 -0.475243 0.561023 -0.266341 11.00000 -1.20000 H3B 2 -0.418545 0.601530 -0.374912 11.00000 -1.20000 AFIX 0 C4 1 -0.395585 0.440425 -0.239978 11.00000 0.02775 0.03527 = 0.03652 -0.00333 0.00153 -0.00065 AFIX 13 H4 2 -0.389097 0.398813 -0.343944 11.00000 -1.20000 AFIX 0 C5 1 -0.433151 0.355866 -0.137718 11.00000 0.02707 0.03632 = 0.06401 0.00101 0.00667 -0.00230 C6 1 -0.283894 0.394178 -0.139692 11.00000 0.02806 0.02818 = 0.03183 0.00158 0.00992 -0.00180 AFIX 43 H6 2 -0.289620 0.313747 -0.186418 11.00000 -1.20000 AFIX 0 C7 1 -0.223401 0.422344 -0.058938 11.00000 0.02886 0.02907 = 0.03077 0.00114 0.00662 -0.00246 AFIX 43 H7 2 -0.216684 0.500172 -0.005876 11.00000 -1.20000 AFIX 0 C8 1 -0.174702 0.337459 -0.057419 11.00000 0.03050 0.02701 = 0.03017 0.00093 0.00894 -0.00313 AFIX 43 H8 2 -0.184123 0.261450 -0.112857 11.00000 -1.20000 AFIX 0 C9 1 -0.110556 0.350398 0.019010 11.00000 0.02729 0.02461 = 0.02997 0.00301 0.00820 0.00034 C10 1 -0.063150 0.261980 -0.013101 11.00000 0.03297 0.02460 = 0.03356 -0.00057 0.00654 0.00090 AFIX 43 H10 2 -0.075044 0.193541 -0.081297 11.00000 -1.20000 AFIX 0 C11 1 -0.000155 0.271588 0.051175 11.00000 0.03182 0.02493 = 0.03413 0.00122 0.00903 0.00492 AFIX 43 H11 2 0.030630 0.211116 0.024853 11.00000 -1.20000 AFIX 0 C12 1 0.019195 0.370696 0.156106 11.00000 0.02644 0.02795 = 0.02677 0.00444 0.00736 -0.00072 C13 1 -0.028544 0.460282 0.188548 11.00000 0.03172 0.02582 = 0.02916 0.00043 0.00838 -0.00066 AFIX 43 H13 2 -0.017097 0.528406 0.257657 11.00000 -1.20000 AFIX 0 C14 1 -0.090738 0.449722 0.121605 11.00000 0.02873 0.02555 = 0.02952 0.00207 0.00965 0.00388 AFIX 43 H14 2 -0.121434 0.511265 0.145095 11.00000 -1.20000 AFIX 0 C15 1 0.129731 0.289342 0.186594 11.00000 0.03076 0.03767 = 0.04540 0.00400 0.00698 0.00550 AFIX 137 H15A 2 0.115939 0.205761 0.216750 11.00000 -1.50000 H15B 2 0.170846 0.309871 0.246748 11.00000 -1.50000 H15C 2 0.135176 0.291153 0.071900 11.00000 -1.50000 AFIX 0 C16 1 0.099418 0.480185 0.335448 11.00000 0.03263 0.03742 = 0.03690 0.00159 0.00336 -0.00369 AFIX 137 H16A 2 0.090471 0.561186 0.284004 11.00000 -1.50000 H16B 2 0.145611 0.473784 0.369077 11.00000 -1.50000 H16C 2 0.074607 0.472684 0.429035 11.00000 -1.50000 AFIX 0 N1 3 -0.332489 0.471445 -0.154362 11.00000 0.02524 0.02821 = 0.02918 0.00028 0.00562 -0.00167 N2 3 0.080949 0.380513 0.222896 11.00000 0.02875 0.03178 = 0.03475 0.00169 0.00432 0.00138 F1 4 -0.443633 0.405710 0.003607 11.00000 0.04568 0.05958 = 0.05955 0.00706 0.02403 -0.00237 F2 4 -0.491303 0.330306 -0.212338 11.00000 0.03086 0.05854 = 0.10208 -0.00032 -0.00358 -0.01485 F3 4 -0.403841 0.246182 -0.108259 11.00000 0.04147 0.03484 = 0.10424 0.01568 0.01776 -0.00064 F4 4 0.274369 0.124308 0.231673 11.00000 0.09183 0.03661 = 0.04615 -0.00926 0.00127 0.00661 F5 4 0.257652 0.100114 -0.034652 11.00000 0.06148 0.05116 = 0.03979 0.01671 0.00280 -0.00293 F6 4 0.204042 -0.021302 0.131740 11.00000 0.03665 0.06551 = 0.05342 0.01277 0.01314 0.00113 F7 4 0.281101 -0.105360 -0.007628 11.00000 0.06660 0.04514 = 0.03981 -0.01006 0.01600 -0.00841 F8 4 0.298699 -0.081562 0.259030 11.00000 0.05519 0.04177 = 0.03618 0.00605 0.00728 0.00932 F9 4 0.352283 0.038551 0.093523 11.00000 0.03876 0.06612 = 0.07267 0.00916 0.00555 -0.01474 P1 5 0.278251 0.009469 0.112589 11.00000 0.03760 0.03148 = 0.02997 0.00098 0.00655 -0.00276 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 2007src1313 in P2(1)/c C 0.770 H 0.320 N 0.700 F 0.640 P 1.100 C1 - N1 C2 C2 - C1 C3 C3 - C2 C4 C4 - N1 C5 C3 C5 - F1 F3 F2 C4 C6 - N1 C7 C7 - C8 C6 C8 - C7 C9 C9 - C14 C10 C8 C10 - C11 C9 C11 - C10 C12 C12 - N2 C11 C13 C13 - C14 C12 C14 - C13 C9 C15 - N2 C16 - N2 N1 - C6 C4 C1 N2 - C12 C16 C15 F1 - C5 F2 - C5 F3 - C5 F4 - P1 F5 - P1 F6 - P1 F7 - P1 F8 - P1 F9 - P1 P1 - F4 F9 F7 F8 F6 F5 31015 Reflections read, of which 980 rejected -26 =< h =< 26, -13 =< k =< 13, -10 =< l =< 10, Max. 2-theta = 54.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -22 1 2 19.91 6.71 2 52.91 1 Inconsistent equivalents 4260 Unique reflections, of which 0 suppressed R(int) = 0.0644 R(sigma) = 0.0431 Friedel opposites merged Maximum memory for data reduction = 2303 / 41794 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 = 3002 / 317777 wR2 = 0.1421 before cycle 1 for 4260 data and 255 / 255 parameters GooF = S = 1.024; Restrained GooF = 1.024 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0676 * P )^2 + 1.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63895 0.00149 -0.102 OSF Mean shift/esd = 0.015 Maximum = -0.102 for OSF Max. shift = 0.000 A for H15C Max. dU = 0.000 for C7 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3002 / 317777 wR2 = 0.1421 before cycle 2 for 4260 data and 255 / 255 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0676 * P )^2 + 1.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63888 0.00149 -0.043 OSF Mean shift/esd = 0.005 Maximum = -0.043 for OSF Max. shift = 0.000 A for H15C Max. dU = 0.000 for C7 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3002 / 317777 wR2 = 0.1421 before cycle 3 for 4260 data and 255 / 255 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0676 * P )^2 + 1.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63888 0.00149 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.002 for y C7 Max. shift = 0.000 A for H15C Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3002 / 317777 wR2 = 0.1421 before cycle 4 for 4260 data and 255 / 255 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0676 * P )^2 + 1.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63888 0.00149 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H15A Max. dU = 0.000 for F3 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 H1A -0.3009 0.6526 -0.1700 23 0.990 0.000 C1 N1 C2 H1B -0.3143 0.6128 0.0090 23 0.990 0.000 C1 N1 C2 H2A -0.3996 0.7394 -0.1661 23 0.990 0.000 C2 C1 C3 H2B -0.4218 0.6405 -0.0371 23 0.990 0.000 C2 C1 C3 H3A -0.4185 0.6015 -0.3749 23 0.990 0.000 C3 C2 C4 H3B -0.4752 0.5610 -0.2663 23 0.990 0.000 C3 C2 C4 H4 -0.3891 0.3988 -0.3439 13 1.000 0.000 C4 N1 C5 C3 H6 -0.2896 0.3137 -0.1864 43 0.950 0.000 C6 N1 C7 H7 -0.2167 0.5002 -0.0059 43 0.950 0.000 C7 C8 C6 H8 -0.1841 0.2614 -0.1128 43 0.950 0.000 C8 C7 C9 H10 -0.0750 0.1935 -0.0813 43 0.950 0.000 C10 C11 C9 H11 0.0306 0.2111 0.0249 43 0.950 0.000 C11 C10 C12 H13 -0.0171 0.5284 0.2577 43 0.950 0.000 C13 C14 C12 H14 -0.1214 0.5113 0.1451 43 0.950 0.000 C14 C13 C9 H15A 0.1159 0.2058 0.2167 137 0.980 0.000 C15 N2 H15A H15B 0.1708 0.3098 0.2468 137 0.980 0.000 C15 N2 H15A H15C 0.1352 0.2912 0.0719 137 0.980 0.000 C15 N2 H15A H16A 0.0905 0.5612 0.2840 137 0.980 0.000 C16 N2 H16A H16B 0.1456 0.4738 0.3691 137 0.980 0.000 C16 N2 H16A H16C 0.0746 0.4727 0.4290 137 0.980 0.000 C16 N2 H16A 2007src1313 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.32989 0.60469 -0.10519 1.00000 0.03319 0.02840 0.04359 -0.00285 0.00490 0.00034 0.03496 0.00401 0.00011 0.00020 0.00028 0.00000 0.00117 0.00106 0.00123 0.00092 0.00094 0.00088 0.00049 H1A -0.30090 0.65264 -0.17001 1.00000 0.04196 0.00000 0.00000 H1B -0.31428 0.61279 0.00902 1.00000 0.04196 0.00000 0.00000 C2 -0.39844 0.65040 -0.13412 1.00000 0.03701 0.03474 0.06476 -0.00348 0.00136 0.00342 0.04568 0.00455 0.00012 0.00024 0.00034 0.00000 0.00131 0.00121 0.00165 0.00115 0.00115 0.00102 0.00060 H2A -0.39959 0.73938 -0.16611 1.00000 0.05481 0.00000 0.00000 H2B -0.42184 0.64047 -0.03713 1.00000 0.05481 0.00000 0.00000 C3 -0.42789 0.56762 -0.26972 1.00000 0.03167 0.03979 0.04779 0.00557 0.00060 0.00324 0.03991 0.00433 0.00012 0.00022 0.00030 0.00000 0.00120 0.00128 0.00133 0.00104 0.00097 0.00096 0.00054 H3A -0.41855 0.60153 -0.37491 1.00000 0.04790 0.00000 0.00000 H3B -0.47524 0.56102 -0.26633 1.00000 0.04790 0.00000 0.00000 C4 -0.39558 0.44042 -0.23997 1.00000 0.02770 0.03527 0.03645 -0.00333 0.00151 -0.00065 0.03321 0.00385 0.00010 0.00021 0.00027 0.00000 0.00109 0.00113 0.00112 0.00091 0.00085 0.00087 0.00047 H4 -0.38910 0.39881 -0.34394 1.00000 0.03985 0.00000 0.00000 C5 -0.43315 0.35587 -0.13772 1.00000 0.02706 0.03630 0.06396 0.00100 0.00665 -0.00230 0.04228 0.00451 0.00011 0.00023 0.00033 0.00000 0.00114 0.00121 0.00160 0.00114 0.00106 0.00094 0.00057 C6 -0.28389 0.39418 -0.13969 1.00000 0.02802 0.02815 0.03180 0.00157 0.00991 -0.00179 0.02890 0.00380 0.00010 0.00020 0.00024 0.00000 0.00106 0.00098 0.00100 0.00081 0.00081 0.00082 0.00043 H6 -0.28962 0.31375 -0.18642 1.00000 0.03468 0.00000 0.00000 C7 -0.22340 0.42234 -0.05894 1.00000 0.02881 0.02902 0.03073 0.00114 0.00661 -0.00245 0.02929 0.00377 0.00010 0.00020 0.00024 0.00000 0.00106 0.00102 0.00101 0.00081 0.00080 0.00082 0.00044 H7 -0.21668 0.50017 -0.00588 1.00000 0.03514 0.00000 0.00000 C8 -0.17470 0.33746 -0.05742 1.00000 0.03045 0.02697 0.03014 0.00093 0.00893 -0.00314 0.02882 0.00378 0.00010 0.00019 0.00024 0.00000 0.00107 0.00099 0.00101 0.00079 0.00081 0.00082 0.00043 H8 -0.18412 0.26145 -0.11285 1.00000 0.03459 0.00000 0.00000 C9 -0.11056 0.35040 0.01900 1.00000 0.02726 0.02460 0.02994 0.00300 0.00820 0.00034 0.02693 0.00370 0.00010 0.00019 0.00024 0.00000 0.00102 0.00094 0.00098 0.00078 0.00078 0.00079 0.00042 C10 -0.06315 0.26198 -0.01310 1.00000 0.03292 0.02457 0.03354 -0.00058 0.00653 0.00089 0.03013 0.00387 0.00010 0.00019 0.00025 0.00000 0.00112 0.00096 0.00103 0.00082 0.00084 0.00083 0.00044 H10 -0.07505 0.19354 -0.08128 1.00000 0.03616 0.00000 0.00000 C11 -0.00016 0.27159 0.05118 1.00000 0.03178 0.02492 0.03410 0.00121 0.00900 0.00493 0.02991 0.00385 0.00010 0.00019 0.00025 0.00000 0.00110 0.00094 0.00103 0.00083 0.00084 0.00082 0.00044 H11 0.03063 0.21112 0.02486 1.00000 0.03589 0.00000 0.00000 C12 0.01919 0.37069 0.15610 1.00000 0.02641 0.02794 0.02674 0.00444 0.00735 -0.00072 0.02674 0.00366 0.00010 0.00019 0.00023 0.00000 0.00101 0.00098 0.00092 0.00078 0.00077 0.00078 0.00042 C13 -0.02854 0.46028 0.18855 1.00000 0.03167 0.02580 0.02915 0.00043 0.00836 -0.00066 0.02854 0.00380 0.00010 0.00019 0.00024 0.00000 0.00109 0.00096 0.00100 0.00078 0.00081 0.00082 0.00043 H13 -0.01709 0.52840 0.25766 1.00000 0.03425 0.00000 0.00000 C14 -0.09074 0.44972 0.12160 1.00000 0.02869 0.02554 0.02949 0.00207 0.00965 0.00387 0.02750 0.00369 0.00010 0.00019 0.00023 0.00000 0.00105 0.00095 0.00101 0.00078 0.00080 0.00080 0.00043 H14 -0.12143 0.51127 0.14509 1.00000 0.03299 0.00000 0.00000 C15 0.12973 0.28934 0.18659 1.00000 0.03072 0.03762 0.04537 0.00400 0.00696 0.00550 0.03769 0.00443 0.00011 0.00022 0.00029 0.00000 0.00116 0.00120 0.00127 0.00100 0.00094 0.00094 0.00051 H15A 0.11592 0.20575 0.21667 1.00000 0.05654 0.00000 0.00000 H15B 0.17084 0.30983 0.24681 1.00000 0.05654 0.00000 0.00000 H15C 0.13520 0.29120 0.07191 1.00000 0.05654 0.00000 0.00000 C16 0.09941 0.48018 0.33545 1.00000 0.03261 0.03738 0.03687 0.00159 0.00335 -0.00369 0.03560 0.00395 0.00011 0.00021 0.00027 0.00000 0.00115 0.00118 0.00115 0.00094 0.00089 0.00092 0.00049 H16A 0.09048 0.56118 0.28400 1.00000 0.05340 0.00000 0.00000 H16B 0.14560 0.47377 0.36910 1.00000 0.05340 0.00000 0.00000 H16C 0.07459 0.47269 0.42902 1.00000 0.05340 0.00000 0.00000 N1 -0.33249 0.47145 -0.15437 1.00000 0.02519 0.02820 0.02913 0.00026 0.00560 -0.00166 0.02732 0.00304 0.00008 0.00016 0.00020 0.00000 0.00086 0.00086 0.00085 0.00068 0.00066 0.00068 0.00037 N2 0.08095 0.38051 0.22290 1.00000 0.02870 0.03177 0.03472 0.00167 0.00432 0.00139 0.03164 0.00325 0.00009 0.00017 0.00021 0.00000 0.00093 0.00092 0.00092 0.00075 0.00072 0.00073 0.00040 F1 -0.44363 0.40571 0.00360 1.00000 0.04565 0.05955 0.05952 0.00704 0.02402 -0.00236 0.05378 0.00303 0.00007 0.00015 0.00019 0.00000 0.00089 0.00097 0.00094 0.00076 0.00071 0.00072 0.00041 F2 -0.49130 0.33031 -0.21234 1.00000 0.03084 0.05848 0.10206 -0.00029 -0.00359 -0.01485 0.06433 0.00288 0.00007 0.00016 0.00024 0.00000 0.00079 0.00103 0.00139 0.00094 0.00080 0.00070 0.00050 F3 -0.40384 0.24618 -0.10825 1.00000 0.04144 0.03481 0.10417 0.01567 0.01773 -0.00064 0.05948 0.00317 0.00007 0.00014 0.00023 0.00000 0.00086 0.00078 0.00138 0.00082 0.00084 0.00064 0.00047 F4 0.27437 0.12431 0.23167 1.00000 0.09186 0.03658 0.04610 -0.00926 0.00128 0.00662 0.05845 0.00287 0.00009 0.00014 0.00018 0.00000 0.00131 0.00080 0.00085 0.00066 0.00082 0.00080 0.00046 F5 0.25765 0.10012 -0.03465 1.00000 0.06146 0.05115 0.03974 0.01672 0.00281 -0.00291 0.05087 0.00280 0.00008 0.00014 0.00017 0.00000 0.00099 0.00088 0.00077 0.00066 0.00067 0.00073 0.00039 F6 0.20404 -0.02130 0.13173 1.00000 0.03661 0.06552 0.05336 0.01277 0.01314 0.00112 0.05130 0.00297 0.00007 0.00016 0.00019 0.00000 0.00080 0.00099 0.00089 0.00074 0.00064 0.00069 0.00040 F7 0.28110 -0.10536 -0.00763 1.00000 0.06658 0.04509 0.03978 -0.01007 0.01598 -0.00841 0.04983 0.00264 0.00008 0.00014 0.00017 0.00000 0.00102 0.00082 0.00076 0.00063 0.00068 0.00071 0.00039 F8 0.29870 -0.08156 0.25902 1.00000 0.05516 0.04174 0.03616 0.00606 0.00728 0.00934 0.04416 0.00265 0.00007 0.00013 0.00016 0.00000 0.00090 0.00078 0.00072 0.00058 0.00061 0.00064 0.00036 F9 0.35228 0.03856 0.09353 1.00000 0.03872 0.06610 0.07264 0.00914 0.00554 -0.01476 0.05911 0.00298 0.00008 0.00017 0.00021 0.00000 0.00085 0.00105 0.00109 0.00088 0.00073 0.00075 0.00044 P1 0.27825 0.00947 0.11259 1.00000 0.03757 0.03146 0.02994 0.00098 0.00655 -0.00276 0.03278 0.00101 0.00003 0.00005 0.00006 0.00000 0.00033 0.00030 0.00030 0.00022 0.00023 0.00023 0.00017 Final Structure Factor Calculation for 2007src1313 in P2(1)/c Total number of l.s. parameters = 255 Maximum vector length = 511 Memory required = 2747 / 24017 wR2 = 0.1421 before cycle 5 for 4260 data and 0 / 255 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0676 * P )^2 + 1.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0520 for 3329 Fo > 4sig(Fo) and 0.0690 for all 4260 data wR2 = 0.1421, GooF = S = 1.025, Restrained GooF = 1.025 for all data Occupancy sum of asymmetric unit = 28.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0442 0.0329 0.0278 C1 0.0659 0.0390 0.0321 C2 0.0508 0.0392 0.0297 C3 0.0393 0.0328 0.0275 C4 0.0640 0.0368 0.0260 C5 0.0369 0.0290 0.0208 C6 0.0337 0.0304 0.0238 C7 0.0364 0.0284 0.0216 C8 0.0347 0.0250 0.0212 C9 0.0366 0.0294 0.0243 C10 0.0398 0.0282 0.0218 C11 0.0330 0.0280 0.0193 C12 0.0359 0.0261 0.0237 C13 0.0371 0.0247 0.0207 C14 0.0484 0.0373 0.0274 C15 0.0400 0.0365 0.0303 C16 0.0308 0.0285 0.0226 N1 0.0359 0.0311 0.0279 N2 0.0732 0.0594 0.0287 F1 0.1043 0.0647 0.0240 F2 0.1085 0.0401 0.0298 F3 0.0940 0.0509 0.0305 F4 0.0664 0.0585 0.0277 F5 0.0742 0.0489 0.0309 F6 0.0741 0.0445 0.0309 F7 0.0608 0.0395 0.0322 F8 0.0816 0.0644 0.0313 F9 0.0394 0.0319 0.0271 P1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.016 0.026 0.036 0.047 0.061 0.079 0.109 0.168 1.000 Number in group 447. 410. 431. 419. 444. 428. 418. 418. 418. 427. GooF 1.000 1.033 1.039 0.996 1.004 1.052 1.031 1.007 0.978 1.101 K 3.259 1.357 1.019 0.986 0.967 1.002 0.992 1.011 1.019 0.965 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.64 inf Number in group 435. 424. 431. 425. 424. 423. 419. 429. 422. 428. GooF 0.972 0.912 0.928 0.880 0.968 1.065 0.922 0.814 0.949 1.611 K 0.984 1.006 1.004 1.011 1.037 1.009 1.033 1.030 1.014 0.936 R1 0.183 0.150 0.136 0.102 0.096 0.066 0.051 0.036 0.034 0.052 ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** Recommended weighting scheme: WGHT 0.0671 1.3230 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) 6 0 8 773.29 1497.79 6.79 0.229 0.98 5 0 8 112.80 298.51 6.62 0.102 0.99 -8 2 2 51.47 11.33 6.30 0.020 2.11 4 6 0 30.48 3.68 5.78 0.011 1.69 3 5 1 42.37 9.59 5.69 0.018 1.98 -1 4 3 22.22 0.53 5.63 0.004 1.93 4 0 8 120.90 255.34 5.57 0.095 1.01 -7 2 1 27.44 3.43 5.52 0.011 2.53 2 2 0 10214.19 21029.81 5.25 0.858 4.76 -7 3 2 175.94 95.41 5.14 0.058 2.06 0 1 1 52.90 126.31 4.77 0.066 6.60 -2 0 8 255.97 519.63 4.40 0.135 1.05 -2 4 1 29.45 8.18 4.20 0.017 2.49 -1 2 8 95.26 183.84 4.18 0.080 1.03 8 1 1 186.15 115.77 3.98 0.064 2.36 1 1 3 71.00 36.37 3.96 0.036 2.65 -9 3 1 26.67 7.11 3.94 0.016 1.92 0 0 4 76.27 37.29 3.87 0.036 2.09 0 3 4 98.25 56.69 3.73 0.045 1.81 11 4 0 225.84 150.98 3.72 0.073 1.54 4 7 0 55.20 26.97 3.61 0.031 1.47 4 5 1 31.96 9.97 3.59 0.019 1.91 -1 2 2 42.41 19.01 3.57 0.026 3.29 8 1 2 476.60 350.22 3.48 0.111 2.08 -5 0 2 837.17 1118.81 3.43 0.198 3.08 -13 10 5 227.88 140.08 3.36 0.070 0.80 2 0 8 241.77 393.46 3.32 0.117 1.03 -6 1 2 245.65 174.34 3.31 0.078 2.69 -17 1 9 6.71 40.52 3.31 0.038 0.77 5 4 8 1.97 16.44 3.18 0.024 0.93 2 5 4 7.34 0.39 2.98 0.004 1.47 -4 0 2 104.15 67.26 2.96 0.049 3.40 5 4 2 9.30 1.28 2.95 0.007 1.94 -8 3 2 787.67 621.83 2.93 0.148 1.93 3 0 8 122.21 69.58 2.92 0.049 1.02 2 6 0 12.84 3.09 2.91 0.010 1.76 4 5 0 808.12 639.31 2.90 0.150 1.98 0 0 6 13.42 1.19 2.90 0.006 1.40 0 0 2 187.84 123.95 2.90 0.066 4.19 7 1 3 1281.49 1024.37 2.89 0.189 1.92 -10 3 2 58.80 33.81 2.88 0.034 1.69 -5 2 3 6.44 0.38 2.85 0.004 2.20 12 0 0 246.82 182.86 2.82 0.080 1.73 -1 2 7 9.29 25.55 2.81 0.030 1.17 -8 4 2 70.15 106.75 2.81 0.061 1.74 9 2 0 1541.52 1249.75 2.81 0.209 2.11 15 7 6 29.87 0.00 2.80 0.000 0.80 -3 4 4 40.86 22.53 2.77 0.028 1.63 -23 6 3 -15.51 35.78 2.72 0.035 0.79 7 0 8 10.20 29.75 2.71 0.032 0.96 Bond lengths and angles C1 - Distance Angles N1 1.4855 (0.0027) C2 1.5069 (0.0033) 104.83 (0.18) C1 - N1 C2 - Distance Angles C1 1.5069 (0.0033) C3 1.5294 (0.0035) 104.15 (0.20) C2 - C1 C3 - Distance Angles C2 1.5294 (0.0035) C4 1.5300 (0.0032) 104.63 (0.19) C3 - C2 C4 - Distance Angles N1 1.4788 (0.0027) C5 1.5111 (0.0033) 109.78 (0.18) C3 1.5300 (0.0032) 103.77 (0.17) 112.67 (0.19) C4 - N1 C5 C5 - Distance Angles F1 1.3367 (0.0030) F3 1.3369 (0.0028) 107.04 (0.22) F2 1.3415 (0.0028) 106.71 (0.20) 106.58 (0.20) C4 1.5111 (0.0033) 113.40 (0.20) 112.48 (0.20) 110.23 (0.22) C5 - F1 F3 F2 C6 - Distance Angles N1 1.3038 (0.0027) C7 1.4096 (0.0030) 124.19 (0.20) C6 - N1 C7 - Distance Angles C8 1.3601 (0.0030) C6 1.4096 (0.0030) 119.62 (0.20) C7 - C8 C8 - Distance Angles C7 1.3601 (0.0030) C9 1.4364 (0.0030) 126.99 (0.20) C8 - C7 C9 - Distance Angles C14 1.4084 (0.0028) C10 1.4096 (0.0028) 116.87 (0.19) C8 1.4364 (0.0030) 123.93 (0.18) 119.17 (0.19) C9 - C14 C10 C10 - Distance Angles C11 1.3771 (0.0031) C9 1.4096 (0.0028) 122.13 (0.20) C10 - C11 C11 - Distance Angles C10 1.3771 (0.0031) C12 1.4159 (0.0029) 120.67 (0.19) C11 - C10 C12 - Distance Angles N2 1.3605 (0.0027) C11 1.4159 (0.0029) 121.50 (0.19) C13 1.4236 (0.0028) 121.18 (0.19) 117.32 (0.19) C12 - N2 C11 C13 - Distance Angles C14 1.3699 (0.0029) C12 1.4236 (0.0028) 120.99 (0.19) C13 - C14 C14 - Distance Angles C13 1.3699 (0.0029) C9 1.4084 (0.0028) 122.00 (0.19) C14 - C13 C15 - Distance Angles N2 1.4590 (0.0028) C15 - C16 - Distance Angles N2 1.4557 (0.0028) C16 - N1 - Distance Angles C6 1.3038 (0.0027) C4 1.4788 (0.0027) 123.46 (0.18) C1 1.4855 (0.0027) 125.05 (0.18) 111.14 (0.16) N1 - C6 C4 N2 - Distance Angles C12 1.3605 (0.0027) C16 1.4557 (0.0028) 120.77 (0.18) C15 1.4590 (0.0028) 120.69 (0.19) 118.51 (0.18) N2 - C12 C16 F1 - Distance Angles C5 1.3367 (0.0030) F1 - F2 - Distance Angles C5 1.3415 (0.0028) F2 - F3 - Distance Angles C5 1.3369 (0.0028) F3 - F4 - Distance Angles P1 1.5920 (0.0015) F4 - F5 - Distance Angles P1 1.6017 (0.0014) F5 - F6 - Distance Angles P1 1.5994 (0.0015) F6 - F7 - Distance Angles P1 1.5958 (0.0015) F7 - F8 - Distance Angles P1 1.5985 (0.0014) F8 - F9 - Distance Angles P1 1.5919 (0.0016) F9 - P1 - Distance Angles F4 1.5920 (0.0015) F9 1.5919 (0.0016) 90.78 (0.10) F7 1.5958 (0.0015) 179.19 (0.10) 89.91 (0.09) F8 1.5985 (0.0014) 90.70 (0.08) 90.07 (0.09) 89.72 (0.08) F6 1.5994 (0.0015) 89.69 (0.10) 179.39 (0.10) 89.62 (0.09) 89.55 (0.08) F5 1.6017 (0.0014) 89.56 (0.09) 90.03 (0.09) 90.03 (0.08) 179.73 (0.10) 90.36 (0.08) P1 - F4 F9 F7 F8 F6 FMAP and GRID set by program FMAP 2 3 21 GRID -2.778 -1 -2 2.778 1 2 R1 = 0.0686 for 4260 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.53 at 0.3786 0.3423 0.2464 [ 1.06 A from C2 ] Deepest hole -0.49 at 0.2505 0.0048 0.0482 [ 0.76 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 3041 / 33183 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.3786 0.6577 -0.2464 1.00000 0.05 0.53 1.06 C2 1.21 H2A 1.41 C3 1.44 H3A Q2 1 -0.4091 0.4969 -0.2520 1.00000 0.05 0.29 0.67 C4 0.86 C3 1.39 H4 1.52 H3A Q3 1 0.3379 0.0616 0.1886 1.00000 0.05 0.27 0.91 F9 1.46 P1 1.55 F4 1.86 F8 Q4 1 0.2250 0.0618 0.1934 1.00000 0.05 0.27 1.10 F6 1.24 F4 1.46 P1 2.13 F5 Q5 1 -0.0178 0.4610 0.3881 1.00000 0.05 0.25 1.31 H13 1.67 C13 1.93 H16C 2.07 H10 Q6 1 -0.0058 0.0825 -0.0063 1.00000 0.05 0.25 1.58 H11 1.90 H16C 1.93 H10 2.00 H16C Q7 1 0.0681 0.5766 0.4640 1.00000 0.05 0.23 1.16 H16C 1.59 H10 1.63 H16A 1.67 C16 Q8 1 0.0855 0.5865 0.3242 1.00000 0.05 0.23 0.45 H16A 1.18 C16 1.53 H16C 1.76 H16B Q9 1 -0.0189 0.5358 0.3112 1.00000 0.05 0.23 0.46 H13 1.31 C13 2.21 H16C 2.28 C14 Q10 1 0.3022 -0.1855 0.1586 1.00000 0.05 0.21 1.40 F8 1.42 H6 1.67 F7 2.17 P1 Q11 1 0.0141 0.5553 0.2424 1.00000 0.05 0.21 0.73 H13 1.40 C13 1.60 H16A 2.04 C16 Q12 1 0.0278 0.5146 0.3819 1.00000 0.05 0.21 1.11 H16C 1.35 H13 1.61 C16 1.68 H16A Q13 1 0.0309 0.4331 0.5043 1.00000 0.05 0.21 1.23 H16C 1.55 H11 2.09 H13 2.16 C16 Q14 1 0.2976 0.2073 0.0876 1.00000 0.05 0.20 1.61 F4 1.65 H1A 1.71 F5 2.12 C1 Q15 1 -0.0113 0.5590 0.3934 1.00000 0.05 0.20 1.18 H13 1.83 H11 2.01 H16C 2.03 C13 Q16 1 0.0010 0.4854 0.4425 1.00000 0.05 0.20 1.55 H16C 1.63 H13 2.03 H16C 2.19 C13 Q17 1 0.1949 0.2003 0.3333 1.00000 0.05 0.20 1.45 H15B 1.84 H15A 2.00 C15 2.09 F4 Q18 1 -0.1878 0.2472 -0.2192 1.00000 0.05 0.20 0.90 H8 1.67 C8 2.27 H6 2.46 C7 Q19 1 0.2917 0.1239 -0.0087 1.00000 0.05 0.20 0.77 F5 1.63 P1 1.72 F9 2.08 F4 Q20 1 -0.1856 0.3355 -0.2274 1.00000 0.05 0.20 1.25 H8 1.43 C8 1.92 C7 2.23 H6 Shortest distances between peaks (including symmetry equivalents) 5 16 0.63 9 15 0.74 6 13 0.78 12 16 0.85 6 16 0.86 15 16 0.92 18 20 0.95 12 15 0.95 13 16 0.96 9 11 0.96 13 15 0.98 5 6 1.01 6 15 1.02 16 16 1.02 5 9 1.03 5 15 1.06 5 12 1.11 9 12 1.12 6 16 1.17 13 16 1.20 14 19 1.20 7 12 1.23 11 12 1.26 7 8 1.26 9 16 1.26 12 13 1.35 6 7 1.37 5 13 1.38 6 12 1.38 11 15 1.42 15 16 1.46 5 13 1.49 8 12 1.54 5 16 1.55 6 12 1.60 8 11 1.62 9 13 1.62 12 16 1.64 6 13 1.68 5 6 1.68 7 16 1.70 12 13 1.71 7 15 1.72 6 15 1.73 5 7 1.74 6 9 1.75 5 11 1.76 7 13 1.77 6 6 1.78 7 16 1.82 13 15 1.82 1 2 1.83 11 16 1.88 5 15 1.89 13 13 1.92 3 14 1.93 3 19 1.96 5 12 1.98 6 9 1.99 4 17 2.02 9 16 2.08 7 13 2.10 12 15 2.10 7 11 2.10 5 5 2.13 9 13 2.15 8 15 2.16 7 9 2.17 15 15 2.21 5 7 2.22 8 9 2.23 6 11 2.26 7 15 2.28 6 7 2.32 6 8 2.35 3 4 2.35 8 16 2.35 4 19 2.38 4 14 2.39 11 13 2.40 12 12 2.40 8 20 2.45 1 14 2.51 7 9 2.53 11 13 2.56 10 18 2.56 8 13 2.56 5 9 2.58 5 8 2.63 6 11 2.64 7 12 2.66 9 12 2.66 9 15 2.70 11 16 2.73 3 10 2.76 1 19 2.87 8 16 2.88 8 13 2.93 5 8 2.94 8 18 2.97 17 19 2.98 Time profile in seconds ----------------------- 0.05: 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 0.00: Analyse other restraints etc. 4.88: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.84: Structure factors and derivatives 2.98: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.42: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.10: Analysis of variance 0.07: Merge reflections for Fourier and .fcf 0.04: Fourier summations 0.10: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src1313 finished at 15:31:33 Total CPU time: 10.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++