+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 11:55:17 on 03-Dec-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src0184 in C2/c CELL 0.71073 15.5095 8.0208 22.5825 90.000 96.602 90.000 ZERR 4.00 0.0031 0.0016 0.0045 0.000 0.030 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H O S UNIT 112 104 16 24 V = 2790.60 F(000) = 1288.0 Mu = 0.52 mm-1 Cell Wt = 2475.39 Rho = 1.473 MERG 2 FMAP 2 PLAN 10 BOND $H OMIT -3 55 TEMP -153 SIZE 0.45 0.2 0.2 ACTA WGHT 0.07640 10.44920 L.S. 10 FVAR 0.27857 MOLE 1 C1 1 0.057365 -0.241437 0.059416 11.00000 0.03279 0.02883 = 0.02590 -0.00253 0.01117 -0.00405 C2 1 0.119493 -0.351231 0.040011 11.00000 0.03084 0.03143 = 0.02485 -0.00050 0.01023 -0.00193 C3 1 0.113816 -0.400397 -0.019398 11.00000 0.03606 0.03100 = 0.02787 -0.00152 0.01210 -0.00186 AFIX 43 H3 2 0.155718 -0.470818 -0.032001 11.00000 -1.20000 AFIX 0 C4 1 0.045516 -0.344449 -0.060111 11.00000 0.03838 0.02755 = 0.02372 -0.00116 0.00872 -0.00656 C5 1 -0.018245 -0.240989 -0.041976 11.00000 0.03468 0.03121 = 0.02970 0.00069 0.00398 -0.00227 AFIX 43 H5 2 -0.064591 -0.205836 -0.068881 11.00000 -1.20000 AFIX 0 C6 1 -0.011166 -0.191040 0.017505 11.00000 0.03373 0.03193 = 0.03201 -0.00492 0.01101 -0.00147 AFIX 43 H6 2 -0.053658 -0.121492 0.029814 11.00000 -1.20000 AFIX 0 C7 1 0.252638 -0.501295 0.063314 11.00000 0.04118 0.05689 = 0.03119 -0.00445 0.00477 0.01767 AFIX 137 H7A 2 0.231759 -0.608529 0.049270 11.00000 -1.50000 H7B 2 0.297393 -0.515615 0.095986 11.00000 -1.50000 H7C 2 0.275720 -0.442615 0.031599 11.00000 -1.50000 AFIX 0 C8 1 -0.022322 -0.351292 -0.160944 11.00000 0.06189 0.05211 = 0.02227 0.00027 0.00088 0.00994 AFIX 137 H8A 2 -0.076817 -0.382725 -0.147918 11.00000 -1.50000 H8B 2 -0.015990 -0.404904 -0.198205 11.00000 -1.50000 H8C 2 -0.020682 -0.232540 -0.166002 11.00000 -1.50000 AFIX 0 C9 1 0.062102 -0.181625 0.121833 11.00000 0.02714 0.03105 = 0.02301 0.00074 0.01074 0.00190 C10 1 0.021619 -0.105936 0.222775 11.00000 0.02822 0.02482 = 0.02424 0.00004 0.00676 -0.00061 C11 1 0.105611 -0.061035 0.215162 11.00000 0.02736 0.02540 = 0.02030 0.00264 0.00541 -0.00085 C12 1 0.129219 -0.103884 0.157372 11.00000 0.02427 0.03027 = 0.02661 0.00153 0.00839 -0.00084 C13 1 0.275290 0.043833 0.247526 11.00000 0.02814 0.04779 = 0.04871 -0.01047 0.00179 -0.00766 AFIX 23 H13A 2 0.313339 0.119955 0.271511 11.00000 -1.20000 H13B 2 0.298032 -0.067997 0.254482 11.00000 -1.20000 AFIX 0 C14 1 0.276330 0.086903 0.182588 11.00000 0.04504 0.05208 = 0.05840 -0.01364 0.02674 -0.02200 AFIX 23 H14A 2 0.335855 0.107039 0.175260 11.00000 -1.20000 H14B 2 0.244227 0.189645 0.174246 11.00000 -1.20000 AFIX 0 O1 3 0.182009 -0.406729 0.083000 11.00000 0.03623 0.04558 = 0.02355 -0.00169 0.00669 0.01073 O2 3 0.047052 -0.401557 -0.117261 11.00000 0.04544 0.04302 = 0.02267 -0.00302 0.00746 0.00155 S1 4 -0.028205 -0.201928 0.159058 11.00000 0.02743 0.03720 = 0.02761 -0.00742 0.01133 -0.00712 S2 4 0.168424 0.054410 0.271363 11.00000 0.03211 0.04349 = 0.02493 -0.00393 0.00524 -0.00828 S3 4 0.230558 -0.072161 0.131634 11.00000 0.03026 0.05415 = 0.03490 -0.00682 0.01582 -0.01005 HKLF 4 Covalent radii and connectivity table for 04src0184 in C2/c C 0.770 H 0.320 O 0.660 S 1.030 C1 - C6 C2 C9 C2 - O1 C3 C1 C3 - C2 C4 C4 - O2 C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - O1 C8 - O2 C9 - C12 C1 S1 C10 - C11 C10_$1 S1 C11 - C10 C12 S2 C12 - C9 C11 S3 C13 - C14 S2 C14 - C13 S3 O1 - C2 C7 O2 - C4 C8 S1 - C9 C10 S2 - C11 C13 S3 - C12 C14 Operators for generating equivalent atoms: $1 -x, y, -z+1/2 h k l Fo^2 Sigma Why rejected -14 0 21 21.96 5.23 observed but should be systematically absent 6 0 17 20.06 2.36 observed but should be systematically absent 6 0 15 4.89 1.22 observed but should be systematically absent -6 0 19 62.57 14.18 observed but should be systematically absent -6 0 19 67.63 13.53 observed but should be systematically absent 4 0 17 78.70 7.50 observed but should be systematically absent 4 0 17 303.37 12.32 observed but should be systematically absent -4 0 25 23.24 5.81 observed but should be systematically absent -4 0 27 36.04 8.14 observed but should be systematically absent 2 0 23 17.74 2.10 observed but should be systematically absent 2 0 21 10.21 2.27 observed but should be systematically absent 2 0 21 51.61 4.52 observed but should be systematically absent 2 0 19 218.84 17.00 observed but should be systematically absent 2 0 19 551.40 22.14 observed but should be systematically absent -2 0 15 30.10 6.03 observed but should be systematically absent -2 0 17 20.62 3.44 observed but should be systematically absent -2 0 19 48.39 4.74 observed but should be systematically absent -2 0 19 19.56 4.12 observed but should be systematically absent -2 0 19 20.58 4.58 observed but should be systematically absent -2 0 21 15.94 3.68 observed but should be systematically absent -2 0 23 225.65 20.71 observed but should be systematically absent -2 0 23 125.83 11.44 observed but should be systematically absent 0 0 21 84.61 6.56 observed but should be systematically absent 0 0 19 116.87 8.43 observed but should be systematically absent 0 0 17 35.81 3.72 observed but should be systematically absent 0 0 15 16.40 3.79 observed but should be systematically absent 0 0 17 22.53 3.76 observed but should be systematically absent 0 0 19 121.43 7.75 observed but should be systematically absent 0 0 19 71.70 8.47 observed but should be systematically absent 0 0 19 82.36 9.17 observed but should be systematically absent 0 0 21 93.72 7.86 observed but should be systematically absent 0 0 21 75.42 7.28 observed but should be systematically absent 0 0 21 59.06 9.10 observed but should be systematically absent -2 0 27 14.78 2.69 observed but should be systematically absent -2 0 23 205.29 14.16 observed but should be systematically absent -2 0 19 20.20 4.76 observed but should be systematically absent -2 0 15 42.30 9.96 observed but should be systematically absent 2 0 15 11.00 2.45 observed but should be systematically absent 2 0 17 266.65 19.34 observed but should be systematically absent 2 0 19 301.89 21.38 observed but should be systematically absent 2 0 19 339.91 25.39 observed but should be systematically absent 2 0 21 31.24 4.64 observed but should be systematically absent 2 0 21 50.92 6.80 observed but should be systematically absent 2 0 23 19.30 4.55 observed but should be systematically absent 2 0 23 33.54 5.60 observed but should be systematically absent -4 0 27 16.86 3.90 observed but should be systematically absent -4 0 25 9.96 2.49 observed but should be systematically absent -4 0 1 5.44 1.09 observed but should be systematically absent 4 0 1 4.81 1.20 observed but should be systematically absent 4 0 17 113.19 12.99 observed but should be systematically absent ** etc. ** 13634 Reflections read, of which 562 rejected -20 =< h =< 20, -10 =< k =< 9, -29 =< l =< 29, Max. 2-theta = 54.67 53 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 12 0 0 59.26 3.38 2 27.38 6 6 0 129.73 3.90 5 29.09 7 7 0 87.38 5.78 2 50.58 7 7 2 100.31 4.62 2 24.06 4 4 4 230.81 7.55 2 60.85 2 4 11 115.53 1.13 6 17.46 4 0 12 156.76 3.21 2 89.74 6 0 12 329.08 8.69 2 144.98 1 1 12 332.89 8.15 3 46.73 13 1 12 247.82 6.38 4 34.91 -9 5 12 237.71 6.24 4 31.65 3 5 12 24.86 0.89 5 5.99 6 6 12 61.76 3.37 2 27.53 1 1 13 62.48 2.44 3 15.60 2 2 13 754.57 11.80 5 64.59 0 4 13 310.75 4.39 8 24.22 6 0 14 96.81 3.04 3 16.43 2 2 14 20.03 0.70 5 3.89 1 1 15 547.35 17.23 2 154.84 -1 1 17 50.42 1.02 4 11.53 1 1 17 140.88 4.44 5 25.81 -6 0 18 956.14 18.76 4 108.44 6 0 18 49.33 1.74 4 11.20 12 0 18 22.33 2.05 2 13.36 -4 6 18 71.53 3.44 4 19.91 -1 1 19 107.33 1.05 8 11.31 -2 2 19 209.80 1.91 9 17.25 -2 2 20 67.43 0.96 9 7.51 28 Inconsistent equivalents 3113 Unique reflections, of which 0 suppressed R(int) = 0.0938 R(sigma) = 0.0574 Friedel opposites merged Maximum memory for data reduction = 1770 / 37722 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 = 2250 / 216396 wR2 = 0.1754 before cycle 1 for 3113 data and 174 / 174 parameters GooF = S = 1.079; Restrained GooF = 1.079 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0764 * P )^2 + 10.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27916 0.00094 0.625 OSF Mean shift/su = 0.134 Maximum = 0.680 for U22 S3 Max. shift = 0.006 A for H7C Max. dU = 0.000 for C14 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2250 / 216396 wR2 = 0.1752 before cycle 2 for 3113 data and 174 / 174 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0764 * P )^2 + 10.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27946 0.00094 0.323 OSF Mean shift/su = 0.054 Maximum = 0.323 for OSF Max. shift = 0.001 A for H7C Max. dU = 0.000 for C14 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2250 / 216396 wR2 = 0.1752 before cycle 3 for 3113 data and 174 / 174 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0764 * P )^2 + 10.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27948 0.00094 0.022 OSF Mean shift/su = 0.005 Maximum = 0.025 for U22 S3 Max. shift = 0.000 A for H7B Max. dU = 0.000 for C14 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2250 / 216396 wR2 = 0.1752 before cycle 4 for 3113 data and 174 / 174 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0764 * P )^2 + 10.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27948 0.00094 0.002 OSF Mean shift/su = 0.001 Maximum = 0.004 for y C3 Max. shift = 0.000 A for H7B Max. dU = 0.000 for C7 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2250 / 216396 wR2 = 0.1752 before cycle 5 for 3113 data and 174 / 174 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0764 * P )^2 + 10.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27948 0.00094 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for U33 C10 Max. shift = 0.000 A for H7C Max. dU = 0.000 for C7 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2250 / 216396 wR2 = 0.1752 before cycle 6 for 3113 data and 174 / 174 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0764 * P )^2 + 10.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27948 0.00094 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z S2 Max. shift = 0.000 A for H7C Max. dU = 0.000 for C7 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2250 / 216396 wR2 = 0.1752 before cycle 7 for 3113 data and 174 / 174 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0764 * P )^2 + 10.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27948 0.00094 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z S2 Max. shift = 0.000 A for H8C Max. dU = 0.000 for O1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2250 / 216396 wR2 = 0.1752 before cycle 8 for 3113 data and 174 / 174 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0764 * P )^2 + 10.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27948 0.00094 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z S2 Max. shift = 0.000 A for C14 Max. dU = 0.000 for O1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2250 / 216396 wR2 = 0.1752 before cycle 9 for 3113 data and 174 / 174 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0764 * P )^2 + 10.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27948 0.00094 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z S2 Max. shift = 0.000 A for H7B Max. dU = 0.000 for C3 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2250 / 216396 wR2 = 0.1752 before cycle 10 for 3113 data and 174 / 174 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0764 * P )^2 + 10.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27948 0.00094 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z S2 Max. shift = 0.000 A for H5 Max. dU = 0.000 for C3 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.1565 -0.4724 -0.0323 43 0.950 0.000 C3 C2 C4 H5 -0.0655 -0.2048 -0.0695 43 0.950 0.000 C5 C4 C6 H6 -0.0546 -0.1200 0.0301 43 0.950 0.000 C6 C5 C1 H7A 0.2314 -0.6111 0.0492 137 0.980 0.000 C7 O1 H7A H7B 0.2986 -0.5154 0.0965 137 0.980 0.000 C7 O1 H7A H7C 0.2759 -0.4419 0.0307 137 0.980 0.000 C7 O1 H7A H8A -0.0780 -0.3833 -0.1477 137 0.980 0.000 C8 O2 H8A H8B -0.0158 -0.4058 -0.1990 137 0.980 0.000 C8 O2 H8A H8C -0.0206 -0.2299 -0.1661 137 0.980 0.000 C8 O2 H8A H13A 0.3140 0.1217 0.2719 23 0.990 0.000 C13 C14 S2 H13B 0.2984 -0.0702 0.2546 23 0.990 0.000 C13 C14 S2 H14A 0.3370 0.1075 0.1751 23 0.990 0.000 C14 C13 S3 H14B 0.2435 0.1918 0.1740 23 0.990 0.000 C14 C13 S3 04src0184 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.05737 -0.24144 0.05943 1.00000 0.03278 0.02898 0.02590 -0.00231 0.01109 -0.00429 0.02862 0.00618 0.00023 0.00043 0.00015 0.00000 0.00182 0.00172 0.00159 0.00134 0.00131 0.00141 0.00072 C2 0.11949 -0.35122 0.04001 1.00000 0.03087 0.03101 0.02554 -0.00068 0.00996 -0.00216 0.02862 0.00626 0.00022 0.00044 0.00015 0.00000 0.00178 0.00177 0.00162 0.00135 0.00130 0.00142 0.00072 C3 0.11377 -0.40043 -0.01940 1.00000 0.03663 0.03118 0.02813 -0.00129 0.01273 -0.00139 0.03128 0.00645 0.00024 0.00045 0.00015 0.00000 0.00197 0.00183 0.00171 0.00141 0.00140 0.00150 0.00077 H3 0.15654 -0.47244 -0.03228 1.00000 0.03754 0.00000 0.00000 C4 0.04552 -0.34448 -0.06010 1.00000 0.03859 0.02757 0.02423 -0.00117 0.00923 -0.00638 0.02969 0.00628 0.00024 0.00044 0.00015 0.00000 0.00195 0.00172 0.00159 0.00132 0.00133 0.00147 0.00074 C5 -0.01824 -0.24087 -0.04202 1.00000 0.03494 0.03202 0.02960 0.00087 0.00426 -0.00221 0.03214 0.00651 0.00024 0.00045 0.00016 0.00000 0.00193 0.00185 0.00173 0.00144 0.00137 0.00150 0.00077 H5 -0.06552 -0.20483 -0.06953 1.00000 0.03857 0.00000 0.00000 C6 -0.01120 -0.19100 0.01750 1.00000 0.03384 0.03171 0.03194 -0.00478 0.01082 -0.00125 0.03195 0.00649 0.00024 0.00046 0.00015 0.00000 0.00189 0.00183 0.00179 0.00143 0.00140 0.00150 0.00077 H6 -0.05463 -0.12002 0.03008 1.00000 0.03834 0.00000 0.00000 C7 0.25266 -0.50137 0.06327 1.00000 0.04073 0.05781 0.03186 -0.00412 0.00476 0.01786 0.04342 0.00806 0.00027 0.00059 0.00017 0.00000 0.00224 0.00262 0.00192 0.00181 0.00156 0.00196 0.00098 H7A 0.23137 -0.61111 0.04921 1.00000 0.06513 0.00000 0.00000 H7B 0.29856 -0.51538 0.09653 1.00000 0.06513 0.00000 0.00000 H7C 0.27594 -0.44191 0.03069 1.00000 0.06513 0.00000 0.00000 C8 -0.02231 -0.35115 -0.16098 1.00000 0.06291 0.05146 0.02211 0.00013 0.00044 0.00985 0.04584 0.00791 0.00030 0.00058 0.00016 0.00000 0.00277 0.00249 0.00172 0.00166 0.00166 0.00214 0.00102 H8A -0.07796 -0.38325 -0.14773 1.00000 0.06876 0.00000 0.00000 H8B -0.01579 -0.40581 -0.19903 1.00000 0.06876 0.00000 0.00000 H8C -0.02062 -0.22991 -0.16612 1.00000 0.06876 0.00000 0.00000 C9 0.06215 -0.18161 0.12182 1.00000 0.02714 0.03079 0.02385 0.00074 0.01097 0.00225 0.02664 0.00622 0.00022 0.00043 0.00014 0.00000 0.00167 0.00175 0.00155 0.00131 0.00123 0.00135 0.00070 C10 0.02165 -0.10592 0.22275 1.00000 0.02857 0.02474 0.02422 -0.00005 0.00679 -0.00058 0.02555 0.00601 0.00022 0.00040 0.00014 0.00000 0.00166 0.00161 0.00156 0.00127 0.00126 0.00133 0.00068 C11 0.10557 -0.06095 0.21517 1.00000 0.02752 0.02547 0.02075 0.00258 0.00554 -0.00094 0.02437 0.00591 0.00021 0.00041 0.00014 0.00000 0.00168 0.00160 0.00147 0.00120 0.00118 0.00127 0.00066 C12 0.12917 -0.10399 0.15739 1.00000 0.02412 0.03023 0.02719 0.00160 0.00881 -0.00082 0.02673 0.00617 0.00021 0.00043 0.00015 0.00000 0.00160 0.00172 0.00161 0.00135 0.00123 0.00134 0.00069 C13 0.27520 0.04394 0.24747 1.00000 0.02817 0.04822 0.04871 -0.01032 0.00171 -0.00802 0.04191 0.00700 0.00024 0.00057 0.00019 0.00000 0.00200 0.00239 0.00231 0.00184 0.00162 0.00169 0.00094 H13A 0.31402 0.12167 0.27194 1.00000 0.05029 0.00000 0.00000 H13B 0.29844 -0.07017 0.25458 1.00000 0.05029 0.00000 0.00000 C14 0.27628 0.08696 0.18253 1.00000 0.04512 0.05340 0.05929 -0.01355 0.02731 -0.02234 0.05095 0.00804 0.00030 0.00058 0.00021 0.00000 0.00248 0.00265 0.00269 0.00218 0.00206 0.00208 0.00115 H14A 0.33704 0.10747 0.17506 1.00000 0.06114 0.00000 0.00000 H14B 0.24352 0.19182 0.17400 1.00000 0.06114 0.00000 0.00000 O1 0.18204 -0.40658 0.08301 1.00000 0.03615 0.04617 0.02359 -0.00192 0.00682 0.01097 0.03504 0.00471 0.00017 0.00033 0.00010 0.00000 0.00141 0.00155 0.00118 0.00107 0.00098 0.00116 0.00060 O2 0.04703 -0.40151 -0.11726 1.00000 0.04562 0.04349 0.02289 -0.00326 0.00738 0.00184 0.03707 0.00471 0.00018 0.00033 0.00011 0.00000 0.00156 0.00154 0.00118 0.00109 0.00103 0.00124 0.00062 S1 -0.02819 -0.20195 0.15906 1.00000 0.02779 0.03756 0.02791 -0.00752 0.01147 -0.00707 0.03044 0.00155 0.00006 0.00012 0.00004 0.00000 0.00045 0.00050 0.00042 0.00035 0.00031 0.00036 0.00025 S2 0.16842 0.05437 0.27136 1.00000 0.03238 0.04387 0.02506 -0.00394 0.00527 -0.00843 0.03362 0.00158 0.00006 0.00012 0.00004 0.00000 0.00050 0.00055 0.00043 0.00036 0.00033 0.00039 0.00026 S3 0.23053 -0.07210 0.13162 1.00000 0.03054 0.05479 0.03520 -0.00696 0.01598 -0.01019 0.03923 0.00177 0.00006 0.00014 0.00004 0.00000 0.00051 0.00064 0.00051 0.00042 0.00037 0.00042 0.00029 Final Structure Factor Calculation for 04src0184 in C2/c Total number of l.s. parameters = 174 Maximum vector length = 511 Memory required = 2076 / 22995 wR2 = 0.1752 before cycle 11 for 3113 data and 0 / 174 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0764 * P )^2 + 10.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0654 for 2511 Fo > 4sig(Fo) and 0.0812 for all 3113 data wR2 = 0.1752, GooF = S = 1.075, Restrained GooF = 1.075 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0391 0.0269 0.0198 C1 0.0357 0.0301 0.0201 C2 0.0417 0.0309 0.0212 C3 0.0426 0.0253 0.0211 C4 0.0361 0.0314 0.0288 C5 0.0410 0.0312 0.0237 C6 0.0698 0.0337 0.0268 C7 0.0695 0.0461 0.0220 C8 0.0342 0.0295 0.0162 C9 0.0304 0.0247 0.0215 C10 0.0282 0.0266 0.0183 C11 0.0316 0.0300 0.0186 C12 0.0589 0.0424 0.0244 C13 0.0881 0.0428 0.0220 C14 0.0533 0.0310 0.0208 O1 0.0467 0.0432 0.0213 O2 0.0463 0.0266 0.0185 S1 0.0488 0.0279 0.0241 S2 0.0620 0.0372 0.0185 S3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.029 0.044 0.061 0.079 0.101 0.127 0.170 0.247 1.000 Number in group 333. 292. 324. 296. 311. 312. 310. 317. 308. 310. GooF 1.209 1.110 1.083 0.975 1.094 1.061 0.946 1.109 0.986 1.136 K 5.221 1.526 1.156 1.071 1.073 1.024 1.019 1.011 0.998 1.035 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.32 1.66 inf Number in group 312. 312. 313. 307. 311. 311. 312. 313. 310. 312. GooF 0.890 1.004 0.986 1.100 0.978 0.943 1.001 0.961 1.086 1.620 K 1.013 1.081 1.095 1.086 1.068 0.990 0.968 0.963 0.964 1.082 R1 0.146 0.129 0.113 0.118 0.091 0.078 0.065 0.056 0.054 0.061 Recommended weighting scheme: WGHT 0.0770 10.1322 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)/su Fc/Fc(max) Resolution(A) 3 3 12 863.16 245.91 5.73 0.062 1.43 -3 9 3 259.48 0.49 5.38 0.003 0.87 -3 1 11 114.64 1.48 4.77 0.005 1.92 3 1 3 2213.72 1279.44 4.74 0.141 3.60 -3 3 24 483.78 14.03 4.74 0.015 0.89 1 1 25 163.37 6.07 4.48 0.010 0.88 6 0 2 2168.19 1302.44 4.42 0.142 2.44 -6 6 3 1191.80 568.90 4.38 0.094 1.18 2 2 2 179.80 17.53 4.38 0.017 3.34 -3 3 2 153.58 459.72 4.29 0.085 2.35 3 3 18 583.76 225.72 4.27 0.059 1.08 6 0 6 582.61 252.99 4.22 0.063 2.01 -4 2 5 315.41 106.96 4.21 0.041 2.45 1 1 17 1803.57 289.03 4.16 0.067 1.29 6 6 0 1660.81 4.36 4.15 0.008 1.19 -12 0 12 967.49 460.79 4.09 0.085 1.12 0 2 7 1623.22 903.81 4.07 0.118 2.50 6 0 18 631.54 3.58 3.96 0.007 1.07 -4 2 3 1047.16 594.17 3.93 0.096 2.68 -1 1 24 206.19 35.04 3.86 0.023 0.93 -1 1 20 320.79 112.80 3.65 0.042 1.12 -5 1 21 656.44 235.91 3.50 0.061 1.04 -4 2 7 595.22 317.88 3.47 0.070 2.19 0 6 15 427.84 51.78 3.40 0.028 1.00 -2 2 7 1175.64 1821.70 3.40 0.168 2.45 -12 6 12 376.79 97.67 3.38 0.039 0.86 -3 1 1 1588.32 1060.54 3.33 0.128 4.33 -3 1 21 2084.49 1330.05 3.09 0.144 1.06 8 8 0 324.98 38.31 3.07 0.024 0.89 -6 2 3 5765.74 4299.63 3.06 0.258 2.13 -1 1 16 136.38 2.93 3.05 0.007 1.39 -1 1 22 72.09 5.43 3.03 0.009 1.02 4 0 0 84036.61 64380.93 3.02 1.000 3.85 3 1 23 107.09 13.96 3.02 0.015 0.93 4 4 8 95.92 0.14 3.00 0.001 1.47 -1 1 4 3105.24 2265.87 2.98 0.188 4.52 -3 1 4 18278.25 14313.23 2.95 0.472 3.60 -3 1 27 159.42 39.72 2.95 0.025 0.83 5 1 23 195.49 64.68 2.94 0.032 0.89 10 4 17 2246.49 1567.46 2.91 0.156 0.86 1 1 23 224.78 38.26 2.91 0.024 0.96 -5 1 6 122.52 36.81 2.90 0.024 2.41 8 0 0 2166.55 1548.34 2.90 0.155 1.93 0 6 18 405.50 58.08 2.89 0.030 0.91 -14 0 14 14439.43 10905.90 2.88 0.412 0.96 0 6 9 192.33 3.35 2.86 0.007 1.18 10 4 14 144.24 0.03 2.84 0.001 0.93 0 2 2 33172.05 26333.36 2.83 0.640 3.78 1 9 7 1097.56 683.78 2.79 0.103 0.86 0 8 2 1548.04 2187.76 2.76 0.184 1.00 Bond lengths and angles C1 - Distance Angles C6 1.3998 (0.0050) C2 1.4118 (0.0048) 117.56 (0.31) C9 1.4823 (0.0044) 120.03 (0.31) 122.40 (0.32) C1 - C6 C2 C2 - Distance Angles O1 1.3656 (0.0042) C3 1.3915 (0.0047) 123.70 (0.32) C1 1.4118 (0.0048) 115.87 (0.29) 120.41 (0.33) C2 - O1 C3 C3 - Distance Angles C2 1.3915 (0.0047) C4 1.3938 (0.0052) 120.26 (0.33) H3 0.9500 119.87 119.87 C3 - C2 C4 C4 - Distance Angles O2 1.3721 (0.0040) C5 1.3886 (0.0051) 124.47 (0.33) C3 1.3938 (0.0052) 114.78 (0.31) 120.74 (0.32) C4 - O2 C5 C5 - Distance Angles C4 1.3886 (0.0051) C6 1.3944 (0.0049) 118.40 (0.34) H5 0.9500 120.80 120.80 C5 - C4 C6 C6 - Distance Angles C5 1.3944 (0.0049) C1 1.3998 (0.0050) 122.56 (0.33) H6 0.9500 118.72 118.72 C6 - C5 C1 C7 - Distance Angles O1 1.4453 (0.0044) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - O1 H7A H7B C8 - Distance Angles O2 1.4319 (0.0046) 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 C12 1.3861 (0.0048) C1 1.4823 (0.0044) 130.43 (0.30) S1 1.7228 (0.0032) 110.95 (0.24) 118.60 (0.25) C9 - C12 C1 C10 - Distance Angles C11 1.3802 (0.0046) C10_$1 1.4683 (0.0061) 129.25 (0.37) S1 1.7332 (0.0034) 110.50 (0.23) 119.49 (0.29) C10 - C11 C10_$1 C11 - Distance Angles C10 1.3802 (0.0046) C12 1.4372 (0.0043) 113.08 (0.29) S2 1.7697 (0.0034) 119.82 (0.24) 126.86 (0.25) C11 - C10 C12 C12 - Distance Angles C9 1.3861 (0.0048) C11 1.4372 (0.0043) 112.44 (0.29) S3 1.7565 (0.0033) 120.90 (0.25) 126.64 (0.26) C12 - C9 C11 C13 - Distance Angles C14 1.5085 (0.0062) S2 1.8017 (0.0040) 113.19 (0.29) H13A 0.9900 108.94 108.94 H13B 0.9900 108.94 108.94 107.75 C13 - C14 S2 H13A C14 - Distance Angles C13 1.5085 (0.0062) S3 1.8070 (0.0045) 114.18 (0.30) H14A 0.9900 108.71 108.71 H14B 0.9900 108.71 108.71 107.63 C14 - C13 S3 H14A O1 - Distance Angles C2 1.3656 (0.0042) C7 1.4453 (0.0044) 116.95 (0.26) O1 - C2 O2 - Distance Angles C4 1.3721 (0.0040) C8 1.4319 (0.0046) 117.52 (0.29) O2 - C4 S1 - Distance Angles C9 1.7228 (0.0032) C10 1.7332 (0.0034) 93.03 (0.16) S1 - C9 S2 - Distance Angles C11 1.7697 (0.0034) C13 1.8017 (0.0040) 102.15 (0.17) S2 - C11 S3 - Distance Angles C12 1.7565 (0.0033) C14 1.8070 (0.0045) 101.12 (0.18) S3 - C12 FMAP and GRID set by program FMAP 2 2 12 GRID -2.778 24 -2 2.778 1 2 R1 = 0.0808 for 3113 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.70 at 0.7471 0.1661 0.5566 [ 0.52 A from H7A ] Deepest hole -0.38 at 0.8962 0.1642 0.6797 [ 1.34 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 3014 / 30027 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2471 -0.6661 0.0566 1.00000 0.05 0.70 0.52 H7A 1.33 C7 1.66 H7B 1.96 H7C Q2 1 0.2176 -0.3026 0.0859 1.00000 0.05 0.60 1.00 O1 1.78 C7 1.78 C2 1.97 H7C Q3 1 0.2226 0.0525 0.1309 1.00000 0.05 0.57 1.01 S3 1.38 C14 1.49 H14B 1.98 H14A Q4 1 0.2063 0.0266 0.1217 1.00000 0.05 0.56 0.89 S3 1.72 C14 1.82 H14B 1.84 C12 Q5 1 0.0031 -0.3102 0.1628 1.00000 0.05 0.42 0.99 S1 1.72 C9 2.12 C10 2.42 H8B Q6 1 0.2221 0.0396 0.2597 1.00000 0.05 0.40 0.90 C13 0.91 S2 1.49 H13B 1.57 H13A Q7 1 -0.0163 -0.1172 0.1942 1.00000 0.05 0.38 0.83 C10 1.05 S1 1.89 C10 1.95 C11 Q8 1 -0.0671 -0.3004 0.1534 1.00000 0.05 0.37 0.99 S1 1.78 H14A 2.40 C9 2.51 C10 Q9 1 -0.0005 -0.2474 0.1908 1.00000 0.05 0.37 0.87 S1 1.37 C10 2.00 C9 2.24 C11 Q10 1 0.1321 0.0242 0.2337 1.00000 0.05 0.36 0.88 C11 0.99 S2 2.00 C10 2.00 C12 Shortest distances between peaks (including symmetry equivalents) 3 4 0.37 5 9 0.82 7 9 1.08 5 8 1.09 8 9 1.33 6 10 1.46 5 7 1.74 7 8 1.86 7 7 2.51 7 10 2.63 9 9 2.67 2 4 2.77 7 9 2.78 7 10 2.80 3 10 2.86 1 3 2.86 4 10 2.90 1 1 2.90 3 6 2.91 1 4 2.98 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: 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. 0.67: 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 1.02: Structure factors and derivatives 1.33: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.19: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 11:55:21 Total CPU time: 3.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++