+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src1312 started at 22:32:49 on 10-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src1312 in P2(1)/n CELL 0.71073 9.7058 14.1810 11.9258 90.000 91.715 90.000 ZERR 4.00 0.0003 0.0005 0.0004 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H O UNIT 88 64 16 V = 1640.71 F(000) = 720.0 Mu = 0.10 mm-1 Cell Wt = 1377.39 Rho = 1.394 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 20 SIZE 0.08 0.12 0.18 WPDB ACTA BOND WGHT 0.01520 1.59780 L.S. 4 TEMP -153.00 FVAR 0.62678 MOLE 1 C1 1 -0.021575 0.682902 0.646161 11.00000 0.01577 0.02177 = 0.01917 0.00124 0.00067 0.00206 C2 1 -0.075080 0.638487 0.739284 11.00000 0.01796 0.02496 = 0.02324 0.00171 0.00223 0.00153 AFIX 43 H2 2 -0.141094 0.589449 0.729834 11.00000 -1.20000 AFIX 0 C3 1 -0.031310 0.666334 0.846270 11.00000 0.02254 0.02978 = 0.01988 0.00502 0.00485 0.00579 AFIX 43 H3 2 -0.067945 0.636267 0.910023 11.00000 -1.20000 AFIX 0 C4 1 0.065475 0.737702 0.860761 11.00000 0.02422 0.02835 = 0.01783 -0.00087 -0.00178 0.00637 AFIX 43 H4 2 0.095988 0.755473 0.934188 11.00000 -1.20000 AFIX 0 C5 1 0.117804 0.783199 0.767995 11.00000 0.01940 0.02317 = 0.02265 -0.00110 -0.00255 0.00231 AFIX 43 H5 2 0.183856 0.832145 0.778030 11.00000 -1.20000 AFIX 0 C6 1 0.073515 0.757089 0.660671 11.00000 0.01518 0.02155 = 0.01984 0.00160 -0.00047 0.00274 C7 1 -0.065428 0.653288 0.530615 11.00000 0.01954 0.01710 = 0.02130 0.00256 0.00193 -0.00238 C8 1 0.026402 0.683850 0.352226 11.00000 0.01790 0.01937 = 0.01628 0.00067 -0.00136 0.00136 AFIX 13 H8 2 -0.072260 0.677867 0.326610 11.00000 -1.20000 AFIX 0 C9 1 0.065082 0.790539 0.366217 11.00000 0.01683 0.02127 = 0.01597 -0.00056 0.00146 0.00019 AFIX 13 H9 2 0.166615 0.799179 0.358512 11.00000 -1.20000 AFIX 0 C10 1 0.125854 0.806677 0.561175 11.00000 0.01976 0.01986 = 0.01980 -0.00092 -0.00248 -0.00144 C11 1 0.117129 0.633188 0.271922 11.00000 0.02061 0.01610 = 0.01872 0.00125 0.00126 -0.00049 C12 1 0.253792 0.613094 0.303092 11.00000 0.02076 0.02159 = 0.01995 -0.00046 -0.00302 0.00091 AFIX 43 H12 2 0.288775 0.630925 0.375262 11.00000 -1.20000 AFIX 0 C13 1 0.338633 0.567249 0.229208 11.00000 0.01966 0.02015 = 0.02741 0.00332 0.00108 0.00133 AFIX 43 H13 2 0.430956 0.552642 0.251543 11.00000 -1.20000 AFIX 0 C14 1 0.289500 0.542609 0.122940 11.00000 0.02692 0.02068 = 0.02289 0.00069 0.00681 0.00184 AFIX 43 H14 2 0.347957 0.511262 0.072452 11.00000 -1.20000 AFIX 0 C15 1 0.154328 0.563941 0.090492 11.00000 0.03050 0.02531 = 0.01730 -0.00017 -0.00005 -0.00024 AFIX 43 H15 2 0.120787 0.547936 0.017295 11.00000 -1.20000 AFIX 0 C16 1 0.068000 0.608658 0.164876 11.00000 0.02105 0.02274 = 0.02046 0.00169 -0.00232 0.00128 AFIX 43 H16 2 -0.024613 0.622495 0.142647 11.00000 -1.20000 AFIX 0 C17 1 -0.012243 0.849903 0.280808 11.00000 0.01914 0.01600 = 0.01972 0.00017 -0.00128 -0.00269 C18 1 0.034279 0.853924 0.171553 11.00000 0.02395 0.01890 = 0.02224 -0.00078 0.00081 -0.00046 AFIX 43 H18 2 0.116881 0.822411 0.152920 11.00000 -1.20000 AFIX 0 C19 1 -0.039752 0.903844 0.089918 11.00000 0.03518 0.02312 = 0.01932 0.00072 -0.00021 -0.00074 AFIX 43 H19 2 -0.007728 0.906174 0.015470 11.00000 -1.20000 AFIX 0 C20 1 -0.160404 0.950456 0.116284 11.00000 0.03143 0.02236 = 0.02704 0.00451 -0.00961 0.00003 AFIX 43 H20 2 -0.211097 0.984386 0.060120 11.00000 -1.20000 AFIX 0 C21 1 -0.206294 0.947090 0.225190 11.00000 0.02124 0.02158 = 0.03337 0.00097 -0.00278 0.00115 AFIX 43 H21 2 -0.288170 0.979492 0.243807 11.00000 -1.20000 AFIX 0 C22 1 -0.133254 0.896592 0.307357 11.00000 0.02005 0.02298 = 0.02227 0.00092 0.00112 -0.00166 AFIX 43 H22 2 -0.165891 0.893938 0.381600 11.00000 -1.20000 AFIX 0 O1 3 -0.182691 0.640310 0.499279 11.00000 0.02034 0.03476 = 0.02497 -0.00051 0.00015 -0.00844 O2 3 0.045370 0.642899 0.463031 11.00000 0.01995 0.02097 = 0.01703 0.00249 0.00047 0.00167 O3 3 0.025655 0.816492 0.478082 11.00000 0.01943 0.02122 = 0.01575 -0.00017 -0.00021 0.00040 O4 3 0.240580 0.837427 0.552989 11.00000 0.02385 0.04436 = 0.02510 0.00353 -0.00270 -0.01310 HKLF 4 Covalent radii and connectivity table for 2007src1312 in P2(1)/n C 0.770 H 0.320 O 0.660 C1 - C2 C6 C7 C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - C5 C1 C10 C7 - O1 O2 C1 C8 - O2 C11 C9 C9 - O3 C17 C8 C10 - O4 O3 C6 C11 - C16 C12 C8 C12 - C13 C11 C13 - C14 C12 C14 - C13 C15 C15 - C14 C16 C16 - C15 C11 C17 - C18 C22 C9 C18 - C19 C17 C19 - C18 C20 C20 - C21 C19 C21 - C20 C22 C22 - C21 C17 O1 - C7 O2 - C7 C8 O3 - C10 C9 O4 - C10 h k l Fo^2 Sigma Why rejected 7 0 0 9.81 2.20 observed but should be systematically absent 0 13 0 19.90 3.85 observed but should be systematically absent 1 0 6 5.55 1.23 observed but should be systematically absent 1 0 6 10.23 2.51 observed but should be systematically absent -6 0 7 3.07 0.69 observed but should be systematically absent 19105 Reflections read, of which 495 rejected -12 =< h =< 12, -18 =< k =< 18, -15 =< l =< 15, Max. 2-theta = 55.00 5 Systematic absence violations 0 Inconsistent equivalents 3753 Unique reflections, of which 0 suppressed R(int) = 0.0392 R(sigma) = 0.0333 Friedel opposites merged Maximum memory for data reduction = 2053 / 37263 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 = 2696 / 290343 wR2 = 0.1064 before cycle 1 for 3753 data and 235 / 235 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0152 * P )^2 + 1.60 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62674 0.00101 -0.042 OSF Mean shift/esd = 0.006 Maximum = -0.042 for OSF Max. shift = 0.000 A for C2 Max. dU = 0.000 for O2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2696 / 290343 wR2 = 0.1064 before cycle 2 for 3753 data and 235 / 235 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0152 * P )^2 + 1.60 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62673 0.00101 -0.010 OSF Mean shift/esd = 0.002 Maximum = -0.010 for OSF Max. shift = 0.000 A for H2 Max. dU = 0.000 for O2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2696 / 290343 wR2 = 0.1064 before cycle 3 for 3753 data and 235 / 235 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0152 * P )^2 + 1.60 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62673 0.00101 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U33 C17 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2696 / 290343 wR2 = 0.1064 before cycle 4 for 3753 data and 235 / 235 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0152 * P )^2 + 1.60 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62673 0.00101 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C2 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 -0.1411 0.5894 0.7298 43 0.950 0.000 C2 C3 C1 H3 -0.0679 0.6363 0.9100 43 0.950 0.000 C3 C4 C2 H4 0.0960 0.7555 0.9342 43 0.950 0.000 C4 C3 C5 H5 0.1839 0.8321 0.7780 43 0.950 0.000 C5 C6 C4 H8 -0.0723 0.6779 0.3266 13 1.000 0.000 C8 O2 C11 C9 H9 0.1666 0.7992 0.3585 13 1.000 0.000 C9 O3 C17 C8 H12 0.2888 0.6309 0.3753 43 0.950 0.000 C12 C13 C11 H13 0.4310 0.5526 0.2515 43 0.950 0.000 C13 C14 C12 H14 0.3480 0.5113 0.0725 43 0.950 0.000 C14 C13 C15 H15 0.1208 0.5479 0.0173 43 0.950 0.000 C15 C14 C16 H16 -0.0246 0.6225 0.1427 43 0.950 0.000 C16 C15 C11 H18 0.1169 0.8224 0.1529 43 0.950 0.000 C18 C19 C17 H19 -0.0077 0.9062 0.0155 43 0.950 0.000 C19 C18 C20 H20 -0.2111 0.9844 0.0601 43 0.950 0.000 C20 C21 C19 H21 -0.2882 0.9795 0.2438 43 0.950 0.000 C21 C20 C22 H22 -0.1659 0.8939 0.3816 43 0.950 0.000 C22 C21 C17 2007src1312 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.02158 0.68290 0.64616 1.00000 0.01576 0.02177 0.01916 0.00123 0.00068 0.00206 0.01889 0.00298 0.00017 0.00012 0.00014 0.00000 0.00076 0.00085 0.00083 0.00067 0.00064 0.00065 0.00035 C2 -0.07507 0.63849 0.73928 1.00000 0.01795 0.02494 0.02324 0.00171 0.00222 0.00152 0.02201 0.00320 0.00018 0.00013 0.00015 0.00000 0.00080 0.00092 0.00087 0.00071 0.00068 0.00069 0.00037 H2 -0.14109 0.58945 0.72983 1.00000 0.02642 0.00000 0.00000 C3 -0.03131 0.66634 0.84627 1.00000 0.02254 0.02977 0.01987 0.00501 0.00485 0.00579 0.02398 0.00334 0.00018 0.00013 0.00015 0.00000 0.00087 0.00099 0.00085 0.00073 0.00070 0.00073 0.00039 H3 -0.06794 0.63627 0.91002 1.00000 0.02877 0.00000 0.00000 C4 0.06547 0.73770 0.86076 1.00000 0.02421 0.02835 0.01782 -0.00087 -0.00177 0.00638 0.02351 0.00324 0.00018 0.00013 0.00015 0.00000 0.00087 0.00097 0.00084 0.00071 0.00069 0.00073 0.00038 H4 0.09599 0.75547 0.93419 1.00000 0.02821 0.00000 0.00000 C5 0.11780 0.78320 0.76799 1.00000 0.01937 0.02317 0.02266 -0.00111 -0.00255 0.00231 0.02180 0.00310 0.00018 0.00013 0.00015 0.00000 0.00081 0.00090 0.00089 0.00069 0.00069 0.00068 0.00037 H5 0.18385 0.83215 0.77803 1.00000 0.02616 0.00000 0.00000 C6 0.07351 0.75709 0.66067 1.00000 0.01517 0.02154 0.01983 0.00160 -0.00047 0.00274 0.01887 0.00298 0.00017 0.00012 0.00014 0.00000 0.00075 0.00086 0.00083 0.00067 0.00063 0.00064 0.00035 C7 -0.06543 0.65329 0.53062 1.00000 0.01955 0.01709 0.02131 0.00257 0.00193 -0.00237 0.01929 0.00298 0.00017 0.00012 0.00014 0.00000 0.00080 0.00082 0.00084 0.00066 0.00066 0.00064 0.00035 C8 0.02640 0.68385 0.35223 1.00000 0.01789 0.01938 0.01627 0.00068 -0.00136 0.00136 0.01789 0.00291 0.00017 0.00012 0.00013 0.00000 0.00077 0.00083 0.00079 0.00064 0.00063 0.00064 0.00034 H8 -0.07226 0.67787 0.32661 1.00000 0.02146 0.00000 0.00000 C9 0.06508 0.79054 0.36621 1.00000 0.01683 0.02128 0.01595 -0.00055 0.00147 0.00019 0.01800 0.00290 0.00017 0.00012 0.00014 0.00000 0.00076 0.00085 0.00078 0.00064 0.00063 0.00064 0.00034 H9 0.16662 0.79918 0.35851 1.00000 0.02160 0.00000 0.00000 C10 0.12585 0.80668 0.56118 1.00000 0.01976 0.01986 0.01980 -0.00093 -0.00249 -0.00143 0.01987 0.00293 0.00017 0.00012 0.00014 0.00000 0.00081 0.00084 0.00082 0.00067 0.00066 0.00066 0.00035 C11 0.11713 0.63319 0.27192 1.00000 0.02061 0.01609 0.01872 0.00125 0.00126 -0.00049 0.01846 0.00293 0.00017 0.00012 0.00014 0.00000 0.00080 0.00081 0.00082 0.00063 0.00066 0.00063 0.00035 C12 0.25379 0.61309 0.30309 1.00000 0.02076 0.02158 0.01994 -0.00046 -0.00302 0.00090 0.02083 0.00303 0.00018 0.00012 0.00015 0.00000 0.00082 0.00086 0.00083 0.00069 0.00066 0.00068 0.00035 H12 0.28877 0.63092 0.37526 1.00000 0.02500 0.00000 0.00000 C13 0.33863 0.56725 0.22921 1.00000 0.01965 0.02014 0.02741 0.00331 0.00108 0.00133 0.02239 0.00317 0.00018 0.00012 0.00015 0.00000 0.00082 0.00086 0.00092 0.00071 0.00070 0.00068 0.00037 H13 0.43095 0.55264 0.25154 1.00000 0.02687 0.00000 0.00000 C14 0.28950 0.54261 0.12294 1.00000 0.02691 0.02068 0.02288 0.00070 0.00682 0.00183 0.02337 0.00325 0.00019 0.00013 0.00015 0.00000 0.00090 0.00089 0.00088 0.00070 0.00073 0.00071 0.00038 H14 0.34796 0.51126 0.07245 1.00000 0.02804 0.00000 0.00000 C15 0.15433 0.56394 0.09049 1.00000 0.03050 0.02531 0.01730 -0.00018 -0.00006 -0.00025 0.02438 0.00323 0.00019 0.00013 0.00015 0.00000 0.00095 0.00093 0.00083 0.00070 0.00072 0.00075 0.00038 H15 0.12079 0.54793 0.01730 1.00000 0.02926 0.00000 0.00000 C16 0.06800 0.60866 0.16488 1.00000 0.02104 0.02274 0.02046 0.00170 -0.00232 0.00127 0.02147 0.00308 0.00018 0.00013 0.00014 0.00000 0.00082 0.00089 0.00084 0.00069 0.00067 0.00069 0.00036 H16 -0.02461 0.62250 0.14265 1.00000 0.02577 0.00000 0.00000 C17 -0.01224 0.84990 0.28081 1.00000 0.01913 0.01600 0.01972 0.00017 -0.00128 -0.00269 0.01832 0.00284 0.00017 0.00012 0.00014 0.00000 0.00079 0.00079 0.00081 0.00064 0.00065 0.00064 0.00034 C18 0.03428 0.85392 0.17155 1.00000 0.02394 0.01891 0.02224 -0.00078 0.00082 -0.00045 0.02169 0.00303 0.00018 0.00012 0.00015 0.00000 0.00086 0.00085 0.00087 0.00068 0.00070 0.00068 0.00036 H18 0.11688 0.82241 0.15292 1.00000 0.02603 0.00000 0.00000 C19 -0.03975 0.90384 0.08992 1.00000 0.03517 0.02311 0.01931 0.00072 -0.00020 -0.00075 0.02588 0.00324 0.00020 0.00013 0.00015 0.00000 0.00101 0.00093 0.00086 0.00071 0.00076 0.00077 0.00040 H19 -0.00773 0.90617 0.01547 1.00000 0.03106 0.00000 0.00000 C20 -0.16041 0.95045 0.11628 1.00000 0.03142 0.02235 0.02703 0.00452 -0.00960 0.00003 0.02714 0.00323 0.00020 0.00013 0.00016 0.00000 0.00098 0.00094 0.00095 0.00075 0.00078 0.00076 0.00041 H20 -0.21110 0.98438 0.06012 1.00000 0.03257 0.00000 0.00000 C21 -0.20629 0.94709 0.22519 1.00000 0.02122 0.02157 0.03339 0.00097 -0.00277 0.00115 0.02546 0.00321 0.00019 0.00013 0.00016 0.00000 0.00086 0.00092 0.00101 0.00076 0.00076 0.00070 0.00040 H21 -0.28817 0.97949 0.24381 1.00000 0.03056 0.00000 0.00000 C22 -0.13325 0.89659 0.30736 1.00000 0.02005 0.02297 0.02226 0.00092 0.00112 -0.00167 0.02175 0.00306 0.00018 0.00013 0.00015 0.00000 0.00081 0.00090 0.00086 0.00070 0.00068 0.00068 0.00036 H22 -0.16589 0.89394 0.38160 1.00000 0.02610 0.00000 0.00000 O1 -0.18269 0.64031 0.49928 1.00000 0.02033 0.03476 0.02497 -0.00051 0.00015 -0.00844 0.02670 0.00217 0.00013 0.00010 0.00011 0.00000 0.00062 0.00076 0.00067 0.00056 0.00052 0.00055 0.00030 O2 0.04537 0.64290 0.46303 1.00000 0.01993 0.02097 0.01701 0.00249 0.00048 0.00167 0.01931 0.00206 0.00012 0.00008 0.00010 0.00000 0.00058 0.00061 0.00058 0.00047 0.00046 0.00047 0.00026 O3 0.02565 0.81649 0.47808 1.00000 0.01942 0.02122 0.01574 -0.00017 -0.00021 0.00040 0.01881 0.00202 0.00012 0.00008 0.00009 0.00000 0.00058 0.00062 0.00058 0.00047 0.00046 0.00047 0.00026 O4 0.24058 0.83743 0.55299 1.00000 0.02384 0.04436 0.02510 0.00353 -0.00270 -0.01310 0.03117 0.00229 0.00013 0.00011 0.00011 0.00000 0.00067 0.00086 0.00068 0.00061 0.00054 0.00061 0.00033 Final Structure Factor Calculation for 2007src1312 in P2(1)/n Total number of l.s. parameters = 235 Maximum vector length = 511 Memory required = 2461 / 21973 wR2 = 0.1064 before cycle 5 for 3753 data and 0 / 235 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0152 * P )^2 + 1.60 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0507 for 3196 Fo > 4sig(Fo) and 0.0623 for all 3753 data wR2 = 0.1064, GooF = S = 1.121, Restrained GooF = 1.121 for all data Occupancy sum of asymmetric unit = 26.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0228 0.0188 0.0151 C1 0.0265 0.0222 0.0173 C2 0.0355 0.0199 0.0166 C3 0.0333 0.0203 0.0169 C4 0.0263 0.0219 0.0172 C5 0.0230 0.0198 0.0138 C6 0.0225 0.0210 0.0144 C7 0.0203 0.0187 0.0147 C8 0.0213 0.0174 0.0152 C9 0.0230 0.0205 0.0161 C10 0.0208 0.0191 0.0155 C11 0.0245 0.0213 0.0168 C12 0.0287 0.0203 0.0181 C13 0.0314 0.0205 0.0182 C14 0.0306 0.0253 0.0173 C15 0.0239 0.0234 0.0171 C16 0.0221 0.0185 0.0144 C17 0.0240 0.0224 0.0187 C18 0.0353 0.0232 0.0192 C19 0.0407 0.0241 0.0166 C20 0.0345 0.0224 0.0195 C21 0.0240 0.0222 0.0190 C22 0.0387 0.0250 0.0164 O1 0.0229 0.0194 0.0157 O2 0.0213 0.0195 0.0156 O3 0.0517 0.0246 0.0172 O4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.018 0.029 0.039 0.051 0.066 0.084 0.108 0.154 1.000 Number in group 409. 351. 398. 366. 354. 395. 375. 359. 371. 375. GooF 1.373 1.282 1.174 1.120 0.983 1.054 0.979 1.030 0.932 1.175 K 4.281 1.498 1.096 1.031 1.000 0.984 0.995 1.003 1.004 0.998 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 378. 372. 386. 370. 375. 371. 376. 384. 364. 377. GooF 1.221 1.173 1.134 1.072 0.998 1.045 1.041 0.956 1.173 1.346 K 1.062 1.052 1.053 1.019 1.000 0.976 1.002 0.991 1.015 0.995 R1 0.151 0.134 0.115 0.097 0.073 0.058 0.042 0.036 0.042 0.030 Recommended weighting scheme: WGHT 0.0151 1.5991 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 1 9 121.34 254.19 6.32 0.099 1.04 6 0 0 46.55 0.00 6.26 0.000 1.62 -3 6 8 118.35 207.09 4.72 0.089 1.18 3 9 3 30.19 2.79 4.56 0.010 1.33 -4 1 4 22.13 1.20 4.40 0.007 1.89 2 2 1 614.73 440.27 4.27 0.130 3.77 6 9 0 32.30 5.49 4.26 0.014 1.13 -3 0 3 14.44 0.06 4.26 0.002 2.55 0 1 6 70.48 34.14 3.77 0.036 1.97 -6 6 3 40.64 12.95 3.72 0.022 1.27 -4 12 1 19.96 0.98 3.68 0.006 1.06 -6 0 6 20.93 0.56 3.54 0.005 1.27 3 12 0 24.15 1.75 3.51 0.008 1.11 -4 9 9 61.35 110.67 3.45 0.065 0.94 2 0 6 3692.40 3212.76 3.40 0.351 1.82 -10 1 8 -4.38 34.50 3.36 0.036 0.82 -9 1 10 36.46 0.76 3.26 0.005 0.81 -3 6 6 8.90 0.04 3.18 0.001 1.39 0 9 10 18.41 0.63 3.17 0.005 0.95 9 1 9 54.91 21.99 3.13 0.029 0.82 3 9 6 18.40 2.68 3.13 0.010 1.15 5 14 6 307.98 226.17 3.11 0.093 0.81 6 15 0 18.68 0.27 3.05 0.003 0.82 -4 0 6 712.30 583.74 3.05 0.149 1.56 -1 2 1 9142.39 10000.10 2.99 0.618 5.20 12 5 0 30.34 8.30 2.96 0.018 0.78 -1 13 3 16.15 1.05 2.91 0.006 1.05 8 13 4 20.62 50.63 2.90 0.044 0.78 4 16 4 -4.97 10.80 2.89 0.020 0.80 6 13 7 15.04 43.22 2.85 0.041 0.79 -5 13 9 31.49 1.85 2.80 0.008 0.78 0 0 2 2231.00 2496.98 2.79 0.309 5.96 4 7 11 355.55 277.46 2.77 0.103 0.88 5 1 0 1385.01 1225.86 2.77 0.217 1.92 9 12 3 0.10 17.59 2.77 0.026 0.78 -7 11 8 203.27 136.08 2.76 0.072 0.80 6 14 6 16.46 0.65 2.76 0.005 0.78 -2 0 6 2606.71 2343.30 2.73 0.299 1.86 -3 4 13 352.63 263.92 2.71 0.100 0.86 9 1 2 23.88 7.71 2.70 0.017 1.05 2 2 9 15.97 3.29 2.70 0.011 1.25 8 12 0 16.95 0.00 2.68 0.000 0.85 1 2 14 -5.53 8.19 2.68 0.018 0.84 6 8 10 49.81 20.70 2.64 0.028 0.83 1 18 2 52.15 24.59 2.62 0.031 0.78 3 5 14 178.61 114.56 2.61 0.066 0.79 -6 8 7 65.98 101.81 2.61 0.062 0.99 2 5 12 63.95 102.36 2.60 0.063 0.92 11 2 5 -5.98 9.45 2.59 0.019 0.81 -8 13 1 27.67 7.31 2.58 0.017 0.81 Bond lengths and angles C1 - Distance Angles C2 1.3907 (0.0024) C6 1.4067 (0.0024) 119.98 (0.16) C7 1.4904 (0.0024) 120.50 (0.16) 119.51 (0.15) C1 - C2 C6 C2 - Distance Angles C3 1.3899 (0.0025) C1 1.3907 (0.0024) 119.55 (0.17) C2 - C3 C3 - Distance Angles C4 1.3881 (0.0027) C2 1.3899 (0.0025) 120.57 (0.17) C3 - C4 C4 - Distance Angles C3 1.3881 (0.0027) C5 1.3899 (0.0025) 120.09 (0.17) C4 - C3 C5 - Distance Angles C6 1.3882 (0.0024) C4 1.3899 (0.0025) 119.97 (0.17) C5 - C6 C6 - Distance Angles C5 1.3882 (0.0024) C1 1.4067 (0.0024) 119.79 (0.16) C10 1.4821 (0.0024) 120.50 (0.16) 119.71 (0.15) C6 - C5 C1 C7 - Distance Angles O1 1.2014 (0.0020) O2 1.3711 (0.0020) 123.58 (0.16) C1 1.4904 (0.0024) 124.92 (0.16) 111.50 (0.14) C7 - O1 O2 C8 - Distance Angles O2 1.4501 (0.0019) C11 1.5031 (0.0023) 109.17 (0.13) C9 1.5665 (0.0024) 105.44 (0.13) 112.73 (0.14) C8 - O2 C11 C9 - Distance Angles O3 1.4465 (0.0019) C17 1.5045 (0.0023) 109.98 (0.13) C8 1.5665 (0.0024) 105.95 (0.13) 110.81 (0.13) C9 - O3 C17 C10 - Distance Angles O4 1.2025 (0.0021) O3 1.3746 (0.0020) 122.79 (0.16) C6 1.4821 (0.0024) 125.27 (0.16) 111.91 (0.14) C10 - O4 O3 C11 - Distance Angles C16 1.3934 (0.0023) C12 1.3961 (0.0023) 119.30 (0.16) C8 1.5031 (0.0023) 120.81 (0.15) 119.86 (0.15) C11 - C16 C12 C12 - Distance Angles C13 1.3858 (0.0025) C11 1.3961 (0.0023) 120.28 (0.16) C12 - C13 C13 - Distance Angles C14 1.3854 (0.0025) C12 1.3858 (0.0025) 120.34 (0.16) C13 - C14 C14 - Distance Angles C13 1.3854 (0.0025) C15 1.3900 (0.0025) 119.73 (0.17) C14 - C13 C15 - Distance Angles C14 1.3900 (0.0025) C16 1.3913 (0.0025) 120.21 (0.17) C15 - C14 C16 - Distance Angles C15 1.3913 (0.0025) C11 1.3934 (0.0023) 120.12 (0.16) C16 - C15 C17 - Distance Angles C18 1.3929 (0.0024) C22 1.3930 (0.0024) 119.49 (0.16) C9 1.5045 (0.0023) 119.15 (0.15) 121.26 (0.15) C17 - C18 C22 C18 - Distance Angles C19 1.3869 (0.0025) C17 1.3929 (0.0024) 120.13 (0.17) C18 - C19 C19 - Distance Angles C18 1.3869 (0.0025) C20 1.3889 (0.0027) 120.44 (0.17) C19 - C18 C20 - Distance Angles C21 1.3864 (0.0027) C19 1.3889 (0.0027) 119.49 (0.17) C20 - C21 C21 - Distance Angles C20 1.3864 (0.0027) C22 1.3906 (0.0025) 120.43 (0.17) C21 - C20 C22 - Distance Angles C21 1.3906 (0.0025) C17 1.3930 (0.0024) 120.01 (0.17) C22 - C21 O1 - Distance Angles C7 1.2014 (0.0021) O1 - O2 - Distance Angles C7 1.3711 (0.0020) C8 1.4501 (0.0019) 114.35 (0.12) O2 - C7 O3 - Distance Angles C10 1.3746 (0.0020) C9 1.4465 (0.0019) 115.99 (0.13) O3 - C10 O4 - Distance Angles C10 1.2025 (0.0021) O4 - FMAP and GRID set by program FMAP 2 1 14 GRID -2.273 -2 -2 2.273 2 2 R1 = 0.0623 for 3753 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.0578 0.7380 0.3594 [ 0.75 A from C9 ] Deepest hole -0.24 at 0.1365 0.8012 0.8206 [ 0.70 A from C5 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2661 / 21097 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0578 0.7380 0.3594 1.00000 0.05 0.24 0.75 C9 0.83 C8 1.37 H9 1.56 H8 Q2 1 0.0029 0.7344 0.6555 1.00000 0.05 0.24 0.76 C6 0.77 C1 1.85 C5 1.86 C2 Q3 1 0.1815 0.6322 0.2815 1.00000 0.05 0.22 0.63 C11 0.79 C12 1.50 H12 1.78 C16 Q4 1 0.0659 0.7792 0.8187 1.00000 0.05 0.21 0.77 C4 0.80 C5 1.44 H4 1.46 H5 Q5 1 0.0626 0.6479 0.3133 1.00000 0.05 0.21 0.76 C11 0.78 C8 1.39 H8 1.80 O2 Q6 1 0.0261 0.8316 0.3377 1.00000 0.05 0.21 0.77 C9 0.81 C17 1.45 H9 1.69 O3 Q7 1 0.0967 0.5574 0.1458 1.00000 0.05 0.20 0.81 C16 0.88 C15 1.50 H16 1.56 H15 Q8 1 -0.0680 0.6808 0.6922 1.00000 0.05 0.20 0.72 C1 0.83 C2 1.55 H2 1.80 C6 Q9 1 0.0927 0.7829 0.6163 1.00000 0.05 0.20 0.67 C6 0.81 C10 1.81 O4 1.82 O3 Q10 1 0.0746 0.7845 0.7172 1.00000 0.05 0.19 0.73 C5 0.78 C6 1.44 H5 1.84 C4 Q11 1 -0.0130 0.6443 0.6911 1.00000 0.05 0.19 0.77 C1 0.85 C2 1.55 H2 1.85 C6 Q12 1 -0.0750 0.9554 0.1024 1.00000 0.05 0.19 0.82 C19 0.85 C20 1.42 H19 1.46 H20 Q13 1 0.0574 0.6999 0.6580 1.00000 0.05 0.18 0.81 C1 0.83 C6 1.85 C5 1.85 C2 Q14 1 0.0970 0.6204 0.2225 1.00000 0.05 0.18 0.64 C11 0.75 C16 1.49 H16 1.78 C12 Q15 1 -0.0211 0.6410 0.7916 1.00000 0.05 0.18 0.75 C3 0.80 C2 1.50 H3 1.54 H2 Q16 1 0.3283 0.5790 0.1638 1.00000 0.05 0.18 0.80 C14 0.80 C13 1.47 H14 1.47 H13 Q17 1 0.0194 0.6995 0.8413 1.00000 0.05 0.18 0.68 C3 0.74 C4 1.50 H3 1.54 H4 Q18 1 -0.0348 0.6685 0.5986 1.00000 0.05 0.18 0.61 C1 0.88 C7 1.78 C6 1.79 C2 Q19 1 0.0017 0.8954 0.4632 1.00000 0.05 0.17 1.16 O3 1.87 H22 1.99 C9 2.08 C10 Q20 1 0.1528 0.8805 0.8982 1.00000 0.05 0.17 1.63 H5 1.91 H4 1.99 O1 2.05 H20 Shortest distances between peaks (including symmetry equivalents) 2 13 0.72 8 11 0.74 3 14 1.08 15 17 1.09 2 8 1.12 11 13 1.12 11 18 1.17 8 18 1.18 11 15 1.20 2 18 1.20 5 14 1.21 13 18 1.21 2 9 1.21 4 10 1.22 9 10 1.22 2 10 1.22 3 5 1.25 4 17 1.25 7 14 1.28 8 13 1.32 9 13 1.33 2 11 1.36 8 15 1.38 1 6 1.38 1 5 1.39 10 13 1.40 6 19 1.77 4 20 1.90 8 17 1.96 11 17 1.97 13 15 1.97 10 17 1.99 8 10 2.04 9 18 2.05 3 7 2.08 2 15 2.11 2 4 2.12 1 3 2.15 4 15 2.15 3 16 2.17 10 11 2.18 4 13 2.22 13 17 2.23 2 17 2.27 7 16 2.27 8 9 2.33 15 18 2.33 1 14 2.37 10 18 2.40 9 11 2.40 5 7 2.41 4 8 2.41 10 15 2.42 4 9 2.44 14 16 2.44 12 20 2.45 4 11 2.55 9 19 2.56 1 19 2.62 10 20 2.64 5 6 2.64 17 20 2.94 17 18 2.96 16 19 2.99 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: 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 0.02: Analyse other restraints etc. 5.20: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.61: Structure factors and derivatives 2.41: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.70: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.04: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src1312 finished at 22:33:01 Total CPU time: 10.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++