++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Version 2008/4 + + Copyright(c) 2008 Bruker Analytical X-ray Solutions All Rights Reserved + + cfc2s started at 11:42:14 on 26-Jan-2011 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL cfc1s in P1 New: P21/c CELL 1.54178 5.4215 5.0420 21.7840 90.000 98.447 90.000 ZERR 4 0.0006 0.0006 0.0030 0.000 0.008 0.000 LATT 1 SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H O UNIT 28 20 8 V = 589.01 F(000) = 252.0 Mu = 0.84 mm-1 Cell Wt = 484.44 Rho = 1.366 TEMP -173 L.S. 5 FMAP 2 PLAN -20 ACTA BOND $H CONF WGHT 0.01000 FVAR 1.00000 O1 3 0.39930 1.35243 0.06532 11.00000 0.02450 0.04380 = 0.06160 -0.00440 0.01080 0.00260 O10 3 0.71513 1.25413 0.01296 11.00000 0.04450 0.03810 = 0.04620 -0.00260 0.01330 0.00040 C5 1 0.67146 1.00782 0.10388 11.00000 0.00510 0.06210 = 0.04560 -0.00100 -0.00070 -0.01000 C8 1 0.62011 0.77470 0.19663 11.00000 0.01430 0.02330 = 0.08770 -0.00100 0.00840 0.00220 AFIX 43 H8A 2 0.53092 0.74764 0.23051 11.00000 -1.20000 AFIX 0 C11 1 0.59266 1.22051 0.05689 11.00000 0.01670 0.04350 = 0.02580 -0.00680 0.00320 -0.01420 C15 1 0.82441 0.62149 0.19069 11.00000 0.03280 0.04490 = 0.05490 -0.00520 0.00500 -0.01870 AFIX 43 H15A 2 0.87682 0.48947 0.22088 11.00000 -1.20000 AFIX 0 C21 1 0.54509 0.96815 0.15325 11.00000 0.02420 0.03310 = 0.05760 -0.00640 0.00720 -0.01900 AFIX 43 H21A 2 0.40505 1.07555 0.15763 11.00000 -1.20000 AFIX 0 C22 1 0.88347 0.85121 0.09795 11.00000 0.03010 0.02350 = 0.05140 -0.00830 0.00580 -0.00390 AFIX 43 H22A 2 0.97500 0.87889 0.06456 11.00000 -1.20000 AFIX 0 C29 1 0.95402 0.65633 0.14175 11.00000 0.01300 -0.00020 = 0.09580 -0.00280 0.01340 0.00280 AFIX 43 H29A 2 1.09272 0.54595 0.13786 11.00000 -1.20000 AFIX 0 HKLF 4 1 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 Covalent radii and connectivity table for cfc1s in P1 New: P21/c C 0.770 H 0.320 O 0.660 O1 - C11 O10 - C11 C5 - C21 C22 C11 C8 - C15 C21 C11 - O10 O1 C5 C15 - C29 C8 C21 - C5 C8 C22 - C29 C5 C29 - C15 C22 h k l Fo^2 Sigma Why rejected -1 0 1 4.00 0.42 observed but should be systematically absent -3 0 3 1.42 0.24 observed but should be systematically absent 0 3 0 5.64 0.85 observed but should be systematically absent 0 3 0 5.76 0.59 observed but should be systematically absent 0 5 0 5.75 1.26 observed but should be systematically absent 0 5 0 5.44 0.78 observed but should be systematically absent 0 5 0 4.95 1.14 observed but should be systematically absent -2 0 1 13.04 1.28 observed but should be systematically absent -2 0 1 16.26 1.33 observed but should be systematically absent -2 0 3 3.44 0.47 observed but should be systematically absent -2 0 3 4.92 0.57 observed but should be systematically absent -3 0 1 3.12 0.56 observed but should be systematically absent -3 0 1 3.59 0.44 observed but should be systematically absent -3 0 5 1.21 0.26 observed but should be systematically absent 3923 Reflections read, of which 220 rejected -5 =< h =< 6, -5 =< k =< 5, -25 =< l =< 25, Max. 2-theta = 134.07 14 Systematic absence violations 0 Inconsistent equivalents 1001 Unique reflections, of which 0 suppressed R(int) = 0.0545 R(sigma) = 0.0558 Friedel opposites merged Maximum memory for data reduction = 996 / 9978 Default effective X-H distances for T = -173.0 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 = 1216 / 109344 wR2 = 0.3632 before cycle 1 for 1001 data and 82 / 82 parameters GooF = S = 5.619; Restrained GooF = 5.619 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38233 0.00513 0.394 OSF 3 1.35608 0.00114 3.204 y O1 5 0.03379 0.00292 3.178 U11 O1 23 0.01857 0.00275 4.904 U11 C5 24 0.02858 0.00593 -5.652 U22 C5 32 0.02802 0.00345 3.978 U11 C8 34 0.05065 0.00716 -5.176 U33 C8 42 0.02596 0.00506 -3.465 U22 C11 51 0.02440 0.00577 -3.552 U22 C15 55 -0.00677 0.00356 3.353 U12 C15 64 -0.00230 0.00336 4.966 U12 C21 78 0.01255 0.00310 4.112 U22 C29 79 0.07246 0.00722 -3.234 U33 C29 Mean shift/esd = 1.503 Maximum = -5.652 for U22 C5 Max. shift = 0.021 A for O1 Max. dU =-0.009 for C5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1216 / 109344 wR2 = 0.2044 before cycle 2 for 1001 data and 82 / 82 parameters GooF = S = 3.056; Restrained GooF = 3.056 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38784 0.00275 2.001 OSF 23 0.02724 0.00177 4.895 U11 C5 32 0.03780 0.00222 4.405 U11 C8 34 0.04151 0.00280 -3.271 U33 C8 77 0.02930 0.00202 4.143 U11 C29 78 0.02183 0.00208 4.457 U22 C29 79 0.05807 0.00334 -4.306 U33 C29 Mean shift/esd = 1.048 Maximum = 4.895 for U11 C5 Max. shift = 0.008 A for C29 Max. dU = 0.001 for C11 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1216 / 109344 wR2 = 0.1788 before cycle 3 for 1001 data and 82 / 82 parameters GooF = S = 2.670; Restrained GooF = 2.670 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38856 0.00241 0.300 OSF Mean shift/esd = 0.236 Maximum = 1.019 for U11 C29 Max. shift = 0.003 A for C8 Max. dU = 0.001 for C29 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1216 / 109344 wR2 = 0.1780 before cycle 4 for 1001 data and 82 / 82 parameters GooF = S = 2.648; Restrained GooF = 2.648 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38873 0.00240 0.071 OSF Mean shift/esd = 0.048 Maximum = -0.214 for U12 O10 Max. shift = 0.001 A for C21 Max. dU = 0.000 for O10 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1216 / 109344 wR2 = 0.1780 before cycle 5 for 1001 data and 82 / 82 parameters GooF = S = 2.646; Restrained GooF = 2.646 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38877 0.00240 0.016 OSF Mean shift/esd = 0.009 Maximum = 0.030 for U11 C29 Max. shift = 0.000 A for C21 Max. dU = 0.000 for C29 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 6 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H8A 0.5320 0.7478 0.2308 43 0.950 0.000 C8 C15 C21 H15A 0.8785 0.4890 0.2208 43 0.950 0.000 C15 C29 C8 H21A 0.4025 1.0754 0.1572 43 0.950 0.000 C21 C5 C8 H22A 0.9733 0.8806 0.0643 43 0.950 0.000 C22 C29 C5 H29A 1.0972 0.5522 0.1381 43 0.950 0.000 C29 C15 C22 cfc1s in P1 New: P21/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O1 0.40263 1.35661 0.06538 1.00000 0.03729 0.03082 0.04829 0.00092 0.01054 0.00748 0.03837 0.00474 0.00047 0.00045 0.00012 0.00000 0.00154 0.00147 0.00163 0.00109 0.00115 0.00110 0.00072 O10 0.71656 1.25670 0.01303 1.00000 0.04256 0.03197 0.04272 0.00309 0.01414 0.00433 0.03829 0.00496 0.00048 0.00047 0.00012 0.00000 0.00151 0.00140 0.00160 0.00108 0.00113 0.00120 0.00071 C5 0.67541 1.00979 0.10401 1.00000 0.02900 0.02230 0.03571 -0.00262 0.00284 -0.00205 0.02919 0.00607 0.00063 0.00065 0.00016 0.00000 0.00179 0.00190 0.00206 0.00131 0.00142 0.00139 0.00081 C8 0.62089 0.77539 0.19684 1.00000 0.03984 0.03368 0.04064 0.00130 0.00857 -0.00331 0.03779 0.00690 0.00069 0.00072 0.00018 0.00000 0.00221 0.00218 0.00220 0.00162 0.00162 0.00168 0.00092 H8A 0.53204 0.74779 0.23077 1.00000 0.04534 0.00000 0.00000 C11 0.59595 1.22069 0.05710 1.00000 0.03196 0.01984 0.03846 -0.00433 0.00603 -0.00035 0.03000 0.00621 0.00062 0.00063 0.00016 0.00000 0.00198 0.00186 0.00208 0.00143 0.00152 0.00147 0.00084 C15 0.82616 0.62218 0.19080 1.00000 0.03816 0.02634 0.04518 0.00251 -0.00087 -0.00205 0.03726 0.00681 0.00073 0.00072 0.00018 0.00000 0.00217 0.00202 0.00226 0.00156 0.00162 0.00158 0.00092 H15A 0.87846 0.48904 0.22075 1.00000 0.04471 0.00000 0.00000 C21 0.54440 0.96968 0.15332 1.00000 0.03323 0.02429 0.04424 -0.00253 0.00727 0.00222 0.03376 0.00644 0.00066 0.00068 0.00017 0.00000 0.00206 0.00201 0.00238 0.00147 0.00162 0.00149 0.00091 H21A 0.40247 1.07537 0.15722 1.00000 0.04052 0.00000 0.00000 C22 0.88319 0.85381 0.09807 1.00000 0.03084 0.03022 0.04461 -0.00088 0.00879 -0.00098 0.03490 0.00659 0.00067 0.00068 0.00017 0.00000 0.00209 0.00211 0.00225 0.00160 0.00156 0.00151 0.00091 H22A 0.97334 0.88061 0.06434 1.00000 0.04188 0.00000 0.00000 C29 0.95641 0.65987 0.14182 1.00000 0.03175 0.02424 0.05552 -0.00027 0.00718 0.00186 0.03709 0.00692 0.00072 0.00067 0.00018 0.00000 0.00207 0.00211 0.00256 0.00161 0.00164 0.00144 0.00095 H29A 1.09719 0.55216 0.13806 1.00000 0.04451 0.00000 0.00000 Final Structure Factor Calculation for cfc1s in P1 New: P21/c Total number of l.s. parameters = 82 Maximum vector length = 511 Memory required = 1134 / 21973 wR2 = 0.1780 before cycle 6 for 1001 data and 0 / 82 parameters GooF = S = 2.646; Restrained GooF = 2.646 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0876 for 789 Fo > 4sig(Fo) and 0.1015 for all 1001 data wR2 = 0.1780, GooF = S = 2.646, Restrained GooF = 2.646 for all data Occupancy sum of asymmetric unit = 9.00 for non-hydrogen and 5.00 for hydrogen atoms Principal mean square atomic displacements U 0.0497 0.0399 0.0255 O1 0.0508 0.0337 0.0304 O10 0.0368 0.0295 0.0213 C5 0.0428 0.0393 0.0313 C8 0.0394 0.0317 0.0189 C11 0.0512 0.0348 0.0258 C15 0.0446 0.0335 0.0232 C21 0.0450 0.0306 0.0291 C22 0.0556 0.0320 0.0238 C29 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.019 0.030 0.043 0.056 0.073 0.094 0.126 0.191 1.000 Number in group 108. 97. 96. 105. 94. 104. 96. 101. 99. 101. GooF 2.105 2.323 1.848 2.692 2.620 2.927 2.782 2.710 3.214 2.943 K 16.687 2.886 1.439 1.253 1.145 1.153 1.101 1.008 1.035 1.045 Resolution(A) 0.84 0.88 0.91 0.95 1.00 1.06 1.15 1.25 1.45 1.80 inf Number in group 104. 100. 100. 96. 103. 97. 100. 100. 100. 101. GooF 2.161 2.288 2.192 2.369 2.483 2.390 2.059 2.444 3.206 4.152 K 1.227 1.147 1.181 1.130 1.021 1.049 0.979 0.933 0.995 1.084 R1 0.166 0.144 0.158 0.144 0.123 0.105 0.088 0.098 0.073 0.067 Recommended weighting scheme: WGHT 0.0749 2.5083 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) -2 1 3 64.26 13.59 5.48 0.046 2.34 -2 3 1 41.30 6.10 5.28 0.031 1.43 2 2 0 130.85 44.29 4.46 0.084 1.84 -5 2 2 28.74 6.37 4.28 0.032 1.00 -6 2 3 48.89 1.71 4.13 0.016 0.85 1 1 1 7.85 0.02 4.12 0.002 3.56 1 5 1 83.30 0.48 4.08 0.009 0.99 -6 1 2 67.02 9.27 3.95 0.038 0.89 -1 3 3 53.57 3.45 3.91 0.023 1.58 -2 5 4 76.66 32.62 3.83 0.072 0.94 0 1 3 217.32 149.67 3.70 0.154 4.13 1 2 0 72.58 22.98 3.69 0.060 2.28 -2 5 3 125.37 69.00 3.56 0.105 0.94 -2 2 2 311.20 212.38 3.49 0.183 1.84 2 1 0 261.11 159.73 3.36 0.159 2.37 -3 1 2 29.84 1.74 3.28 0.017 1.70 -2 1 1 602.28 408.12 3.22 0.254 2.39 0 1 1 137.72 176.80 3.20 0.167 4.91 0 5 2 50.36 21.08 3.16 0.058 1.00 -4 3 4 77.87 1.74 3.02 0.017 1.05 -5 1 3 80.54 47.17 2.95 0.086 1.06 -1 3 1 323.95 187.76 2.95 0.172 1.60 3 1 3 66.59 88.14 2.93 0.118 1.59 -5 1 2 91.43 30.72 2.93 0.070 1.06 -2 4 1 57.17 0.25 2.91 0.006 1.14 -4 3 1 36.11 0.60 2.90 0.010 1.05 -3 5 3 14.24 1.33 2.87 0.015 0.88 -4 2 2 25.23 11.31 2.70 0.042 1.19 1 4 1 56.87 0.00 2.56 0.000 1.22 -3 2 2 51.28 15.66 2.54 0.050 1.47 -1 2 2 134.91 53.84 2.49 0.092 2.26 1 3 1 109.68 52.27 2.47 0.091 1.59 -1 1 4 85.73 104.83 2.44 0.129 3.19 -3 4 2 37.71 3.98 2.43 0.025 1.03 -1 5 1 341.31 209.02 2.36 0.182 0.99 -6 2 2 126.50 68.18 2.36 0.104 0.85 2 4 0 116.64 49.97 2.35 0.089 1.14 2 4 1 416.61 120.68 2.33 0.138 1.14 -1 3 2 622.63 491.27 2.31 0.279 1.60 -2 2 3 413.71 342.47 2.30 0.233 1.82 0 0 2 1226.70 811.80 2.27 0.359 10.77 -1 2 11 115.91 145.67 2.25 0.152 1.53 -4 3 5 30.38 10.90 2.23 0.042 1.05 0 3 22 42.09 26.55 2.17 0.065 0.85 2 3 11 193.63 233.16 2.16 0.192 1.11 0 1 11 91.77 74.34 2.13 0.109 1.83 -2 3 3 58.66 27.08 2.13 0.065 1.42 4 4 0 34.71 11.73 2.12 0.043 0.92 0 1 5 830.09 709.66 2.11 0.335 3.28 3 1 5 28.91 38.37 2.10 0.078 1.50 Bond lengths and angles O1 - Distance Angles C11 1.2869 (0.0038) O1 - O10 - Distance Angles C11 1.2516 (0.0037) O10 - C5 - Distance Angles C21 1.3869 (0.0045) C22 1.3953 (0.0047) 120.12 (0.33) C11 1.4937 (0.0047) 120.31 (0.30) 119.57 (0.31) C5 - C21 C22 C8 - Distance Angles C15 1.3768 (0.0050) C21 1.3837 (0.0051) 119.79 (0.33) H8A 0.9500 120.11 120.10 C8 - C15 C21 C11 - Distance Angles O10 1.2516 (0.0037) O1 1.2869 (0.0038) 123.94 (0.32) C5 1.4937 (0.0047) 119.82 (0.30) 116.24 (0.29) C11 - O10 O1 C15 - Distance Angles C29 1.3765 (0.0050) C8 1.3768 (0.0050) 120.70 (0.36) H15A 0.9500 119.65 119.65 C15 - C29 C8 C21 - Distance Angles C5 1.3869 (0.0045) C8 1.3837 (0.0051) 119.86 (0.32) H21A 0.9500 120.07 120.07 C21 - C5 C8 C22 - Distance Angles C29 1.3822 (0.0052) C5 1.3953 (0.0047) 119.27 (0.34) H22A 0.9500 120.36 120.37 C22 - C29 C5 C29 - Distance Angles C15 1.3765 (0.0050) C22 1.3822 (0.0052) 120.26 (0.35) H29A 0.9500 119.87 119.87 C29 - C15 C22 Selected torsion angles 179.44 ( 0.34) C21 - C5 - C11 - O10 -0.28 ( 0.50) C22 - C5 - C11 - O10 -0.39 ( 0.47) C21 - C5 - C11 - O1 179.88 ( 0.30) C22 - C5 - C11 - O1 -0.07 ( 0.58) C21 - C8 - C15 - C29 0.31 ( 0.53) C22 - C5 - C21 - C8 -179.42 ( 0.33) C11 - C5 - C21 - C8 -0.25 ( 0.55) C15 - C8 - C21 - C5 -0.04 ( 0.53) C21 - C5 - C22 - C29 179.69 ( 0.32) C11 - C5 - C22 - C29 0.35 ( 0.59) C8 - C15 - C29 - C22 -0.29 ( 0.57) C5 - C22 - C29 - C15 FMAP and GRID set by program FMAP 2 1 14 GRID -4.545 -2 -1 4.545 2 1 R1 = 0.1014 for 1001 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.40 at 0.2802 0.7176 0.0334 [ 1.02 A from O10 ] Deepest hole -0.30 at 0.1961 0.4225 0.3351 [ 1.41 A from C21 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 1311 / 14797 Molecule 1 scale 0.900 inches = 2.287 cm per Angstrom O1 O10 14 C29 12 17 C15 18 C22 15 20 C8 16 C5 C21 7 2 O10 6 1 19 C11 4 5 3 10 9 O1 8 13 11 O1 3 O10 Atom Peak x y z Sof Height Distances and Angles O1 0.30 0.4026 1.3566 0.0654 1.000 0.8 0 C11 1.287 0 H21A 2.452 84.5 0 11 0.916 116.2 74.1 0 9 0.995 104.8 35.2 90.7 0 3 1.054 118.5 156.4 98.1 125.2 0 8 1.068 77.3 141.2 83.6 174.3 56.7 0 13 1.155 118.3 37.1 47.0 43.7 122.4 130.6 0 10 1.276 56.8 141.2 123.9 144.8 61.6 40.7 168.8 0 6 1.424 37.4 51.8 113.7 67.4 146.3 114.3 88.8 90.3 0 4 1.716 32.9 111.0 104.2 137.3 92.4 44.4 134.0 36.1 70.0 3 O10 2.610 115.8 159.4 98.2 128.4 3.2 53.6 124.7 58.9 145.0 89.3 6 H29A 2.644 151.3 69.6 69.3 46.6 86.8 130.9 42.8 146.1 113.9 173.3 7 3 2.810 61.2 145.7 120.8 148.4 57.4 37.2 167.4 4.9 95.1 38.5 O10 0.30 0.7166 1.2567 0.0130 1.000 0.8 0 C11 1.252 0 H22A 2.515 82.4 0 4 0.823 49.0 105.3 0 2 0.992 46.5 65.1 95.5 0 1 1.022 149.8 116.5 101.4 161.5 0 5 1.057 90.3 125.6 42.0 136.2 59.6 0 10 1.290 57.3 139.6 52.0 82.7 101.8 63.4 7 3 1.558 122.1 155.4 94.1 128.7 43.1 61.8 64.8 0 8 1.858 52.6 129.7 29.5 91.8 99.3 46.9 23.0 73.7 2 O1 2.610 120.2 157.2 93.5 126.8 45.3 62.2 62.9 2.2 72.4 5 H22A 2.642 154.8 73.9 129.6 125.8 45.3 96.3 146.3 82.1 142.4 84.1 C5 0.00 0.6754 1.0098 0.1040 1.000 1.0 0 C11 1.494 0 C21 1.387 120.3 0 C22 1.395 119.6 120.1 0 7 0.906 89.5 53.8 127.4 0 6 1.063 35.4 91.0 143.0 86.3 0 16 1.619 134.0 35.4 97.1 89.0 98.6 0 20 1.678 166.5 48.0 72.6 77.7 137.5 42.8 0 2 1.748 31.7 138.8 95.4 121.1 49.1 128.0 160.9 C8 0.00 0.6209 0.7754 0.1968 1.000 1.3 0 H8A 0.950 0 C15 1.377 120.1 0 C21 1.384 120.1 119.8 0 15 0.792 113.8 42.3 109.5 0 20 0.973 168.4 58.4 62.7 73.4 0 16 1.265 126.7 98.7 41.3 70.9 63.5 0 17 1.824 142.0 30.5 94.1 63.1 31.7 89.5 0 14 1.957 126.4 18.3 110.7 26.2 56.4 82.2 37.9 H8A 0.00 0.5320 0.7478 0.2308 1.000 1.3 0 C8 0.950 0 15 1.462 29.7 C11 0.00 0.5959 1.2207 0.0571 1.000 0.9 0 O1 1.287 0 O10 1.252 123.9 0 C5 1.494 116.2 119.8 0 6 0.879 79.8 146.2 44.5 0 2 0.918 130.2 51.7 89.6 94.9 0 4 0.944 99.4 41.1 130.2 170.5 92.8 0 10 1.220 61.1 62.9 175.6 131.2 89.8 54.2 0 8 1.481 44.7 85.3 146.4 124.0 123.9 54.7 34.5 0 5 1.643 96.5 40.0 135.3 173.7 91.4 5.3 49.1 51.9 0 7 1.740 93.1 137.7 31.4 49.8 121.0 121.0 149.0 115.1 125.8 0 9 1.816 32.0 149.0 87.7 47.8 120.8 131.1 88.8 76.6 128.5 73.4 0 11 1.881 25.9 129.2 105.0 83.1 156.0 92.0 74.1 44.6 91.3 75.6 0 3 2.015 27.4 96.7 143.4 103.1 113.5 78.7 33.8 28.6 74.6 119.2 C15 0.12 0.8262 0.6222 0.1908 1.000 1.3 0 C8 1.377 0 H15A 0.950 119.6 0 C29 1.376 120.7 119.6 0 14 0.781 128.0 89.5 52.7 0 17 0.946 101.9 126.0 38.1 90.7 0 15 0.954 34.0 115.9 113.4 95.9 117.8 0 20 1.200 43.7 160.4 77.9 109.2 61.5 58.0 0 16 2.006 38.6 144.4 88.7 92.3 89.5 28.6 33.5 H15A 0.00 0.8785 0.4890 0.2208 1.000 1.4 0 C15 0.950 0 14 1.225 39.6 C21 0.15 0.5444 0.9697 0.1533 1.000 1.1 0 C5 1.387 0 C8 1.384 119.9 0 H21A 0.950 120.1 120.1 0 16 0.941 85.9 62.6 122.1 0 7 1.123 40.6 129.2 97.3 126.1 0 20 1.275 78.1 42.7 160.0 63.8 92.1 0 6 1.762 37.1 152.1 85.0 94.8 50.1 114.3 0 15 1.810 101.6 24.4 135.0 40.5 126.7 35.3 128.4 H21A 0.00 0.4025 1.0754 0.1572 1.000 1.1 0 O1 2.452 0 C21 0.950 98.9 0 7 1.560 62.6 45.6 C22 0.15 0.8832 0.8538 0.0981 1.000 1.1 0 C5 1.395 0 H22A 0.950 120.4 0 C29 1.382 119.3 120.4 0 12 1.021 136.2 86.1 49.2 0 18 1.238 125.3 19.7 112.0 91.9 0 17 1.739 95.6 140.0 29.3 54.3 138.9 0 20 1.833 60.9 173.9 58.8 89.4 165.2 36.4 H22A 0.00 0.9733 0.8806 0.0643 1.000 1.0 0 O10 2.515 0 C22 0.950 97.9 0 18 0.470 103.8 117.4 0 12 1.347 133.7 49.1 119.5 4 O10 2.642 106.1 154.7 65.0 106.5 C29 0.11 0.9564 0.6599 0.1418 1.000 1.2 0 C15 1.376 0 C22 1.382 120.3 0 H29A 0.950 119.9 119.9 0 17 0.860 42.7 99.0 125.5 0 12 1.052 137.0 47.2 87.0 94.7 0 14 1.096 34.5 129.2 101.1 77.2 170.8 0 20 1.626 46.2 74.6 164.1 40.4 100.3 70.7 0 15 1.962 26.5 98.2 139.0 54.9 133.0 38.3 32.9 H29A 0.00 1.0972 0.5522 0.1381 1.000 1.3 0 C29 0.950 0 12 1.381 49.6 0 14 1.583 42.8 92.3 1 O1 2.644 147.8 98.9 167.9 1 0.40 0.7198 1.2824 -0.0334 1.000 0.4 0 O10 1.022 0 5 1.033 61.9 7 3 1.071 96.2 84.1 0 4 1.434 34.3 27.7 91.6 0 10 1.802 44.5 42.3 58.5 34.3 0 19 1.980 119.9 155.0 70.9 148.8 118.9 0 2 1.988 9.1 70.0 93.3 42.7 47.1 110.8 2 0.39 0.7593 1.2719 0.0588 1.000 1.5 0 O10 0.992 0 C5 1.748 117.8 0 C11 0.918 81.8 58.7 0 6 1.324 122.9 37.4 41.4 0 4 1.349 37.4 90.8 44.4 85.6 0 10 1.525 57.1 111.7 53.1 84.2 40.9 0 5 1.901 22.6 105.3 59.8 101.1 15.9 41.0 0 1 1.988 9.4 126.2 90.4 131.8 46.1 60.0 30.7 3 0.33 0.3507 1.5187 0.0357 1.000 0.8 0 O1 1.054 0 C11 2.015 34.2 0 8 1.007 62.3 44.7 0 10 1.209 68.2 34.1 43.3 0 11 1.491 37.5 62.8 60.6 91.4 3 O10 1.558 174.6 141.2 112.5 107.1 142.5 0 9 1.820 26.5 56.3 88.7 88.9 47.3 158.8 0 13 1.937 30.2 64.1 79.9 97.9 24.8 153.4 24.8 4 0.32 0.5705 1.2127 0.0133 1.000 0.3 0 O1 1.716 0 O10 0.823 119.7 0 C11 0.944 47.7 89.9 0 5 0.708 124.8 86.9 167.6 0 10 1.016 47.7 88.4 76.8 91.1 0 8 1.211 38.1 131.0 85.8 87.3 43.1 0 2 1.349 80.8 47.1 42.8 132.6 78.9 112.8 0 1 1.434 140.8 44.3 133.8 42.8 93.1 117.2 91.1 7 3 1.814 105.5 59.0 123.4 45.4 58.2 83.5 92.7 36.2 0 6 1.817 47.4 93.6 4.6 170.7 79.7 85.4 46.6 137.7 127.8 5 0.32 0.5514 1.2369 -0.0190 1.000 0.0 0 O10 1.057 0 C11 1.643 49.6 0 4 0.708 51.1 7.1 0 1 1.033 58.5 108.1 109.4 0 10 1.249 67.4 47.5 54.4 103.9 0 8 1.374 98.9 58.0 61.8 139.4 36.9 7 3 1.410 76.9 107.4 113.7 49.1 70.6 95.7 0 2 1.901 21.2 28.9 31.5 79.3 53.1 79.5 87.3 6 0.32 0.6029 1.2053 0.0975 1.000 1.3 0 O1 1.424 0 C5 1.063 143.4 0 C11 0.879 62.8 100.1 0 C21 1.762 119.9 51.9 139.9 0 2 1.324 93.7 93.5 43.7 143.9 0 7 1.352 106.1 42.0 100.4 39.6 122.7 0 9 1.389 41.4 139.8 104.2 89.8 126.1 101.7 0 13 1.815 39.5 121.4 96.0 80.9 133.1 79.8 25.2 0 4 1.817 62.6 97.6 4.9 135.2 47.8 95.6 104.0 93.8 0 10 1.916 41.8 128.7 28.6 155.7 52.3 120.8 80.2 80.8 31.5 0 11 1.978 25.1 121.1 70.7 98.0 110.9 81.3 43.4 25.6 68.3 59.8 7 0.30 0.5147 0.9560 0.1013 1.000 0.5 0 C5 0.906 0 C11 1.740 59.1 0 C21 1.123 85.5 120.1 0 H21A 1.560 108.4 107.2 37.2 0 6 1.352 51.7 29.8 90.3 82.6 0 20 1.729 71.5 130.5 47.5 83.4 112.1 0 16 1.841 61.6 106.3 24.4 57.5 79.0 39.3 8 0.30 0.3857 1.3447 0.0160 1.000 0.2 0 O1 1.068 0 O10 1.858 96.2 0 C11 1.481 58.0 42.2 0 10 0.839 83.1 36.9 55.5 0 3 1.007 61.0 117.8 106.7 81.3 0 4 1.211 97.5 19.6 39.5 55.9 135.1 0 11 1.327 43.3 125.5 83.9 126.0 78.1 114.4 0 5 1.374 128.0 34.2 70.2 63.5 139.6 31.0 138.4 0 13 2.020 25.7 113.8 71.8 108.4 70.7 107.7 17.6 137.2 9 0.29 0.4035 1.3561 0.1111 1.000 1.3 0 O1 0.995 0 C11 1.816 43.2 0 13 0.814 78.7 98.6 0 11 1.361 42.3 71.0 36.4 0 6 1.389 71.2 28.0 108.1 92.0 0 3 1.820 28.2 67.3 85.7 53.6 94.5 10 0.29 0.5314 1.4049 0.0221 1.000 0.8 0 O1 1.276 0 O10 1.290 121.7 0 C11 1.220 62.0 59.7 0 8 0.839 56.2 120.1 90.0 0 4 1.016 96.2 39.7 48.9 80.9 0 3 1.209 50.1 171.6 112.1 55.4 134.2 0 5 1.249 121.0 49.1 83.4 79.6 34.5 131.0 0 2 1.525 91.0 40.2 37.0 126.6 60.2 134.7 85.9 7 3 1.542 171.1 66.1 125.8 117.1 87.8 122.0 59.6 97.8 0 1 1.802 148.8 33.7 91.1 112.5 52.6 152.4 33.8 72.8 36.3 0 6 1.916 48.0 76.3 20.2 90.7 68.8 96.2 103.3 43.4 140.8 109.4 0 11 1.942 23.0 121.9 68.7 33.6 86.4 50.1 102.4 104.1 150.6 135.3 11 0.27 0.2534 1.2682 0.0595 1.000 0.2 0 O1 0.916 0 C11 1.881 37.9 0 13 0.855 81.3 92.3 0 8 1.327 53.1 51.5 134.4 0 9 1.361 47.0 65.9 34.4 100.1 0 3 1.491 44.4 72.4 108.2 41.4 79.2 0 10 1.942 33.1 37.2 114.0 20.5 79.9 38.5 0 6 1.978 41.2 26.2 66.5 76.1 44.5 85.1 58.5 12 0.26 0.9176 0.6566 0.0930 1.000 0.6 0 C22 1.021 0 H22A 1.347 44.7 0 C29 1.052 83.6 115.5 0 H29A 1.381 114.6 117.8 43.4 0 17 1.413 89.7 134.1 37.4 70.4 0 18 1.630 49.4 14.5 106.3 103.3 133.1 13 0.24 0.2755 1.2752 0.0992 1.000 0.7 0 O1 1.155 0 9 0.814 57.6 0 11 0.855 51.6 109.3 0 6 1.815 51.6 46.6 88.0 0 3 1.937 27.4 69.6 47.0 78.5 0 8 2.020 23.7 81.3 28.0 66.2 29.4 14 0.24 0.9646 0.6679 0.1923 1.000 1.8 0 C8 1.957 0 C15 0.781 33.7 0 H15A 1.225 75.0 50.9 0 C29 1.096 99.3 92.8 121.2 0 H29A 1.583 132.8 113.5 110.8 36.1 0 17 1.234 65.2 50.1 86.8 42.8 68.4 0 15 1.294 15.7 47.2 79.7 110.1 145.7 80.1 0 20 1.633 29.8 43.9 94.6 70.0 105.1 43.2 40.7 15 0.23 0.7673 0.7833 0.2065 1.000 1.8 0 C8 0.792 0 H8A 1.462 36.5 0 C15 0.954 103.7 112.4 0 C21 1.810 46.1 76.0 116.1 0 C29 1.962 113.7 142.8 40.1 94.3 0 20 1.066 61.1 97.2 72.7 43.8 56.0 0 16 1.254 72.4 93.6 130.0 29.2 94.3 61.9 0 14 1.294 138.2 145.8 36.9 125.3 31.6 87.1 117.8 0 17 1.627 91.1 117.2 31.0 86.9 25.6 43.1 99.4 48.3 16 0.22 0.6983 0.9947 0.1789 1.000 1.9 0 C5 1.619 0 C8 1.265 111.9 0 C15 2.006 98.5 42.7 0 C21 0.941 58.7 76.1 102.2 0 20 1.204 71.2 46.4 33.4 71.7 0 15 1.254 119.8 36.7 21.4 110.3 51.3 0 7 1.841 29.5 91.8 98.6 29.5 65.3 115.7 17 0.22 0.8117 0.6026 0.1472 1.000 0.8 0 C8 1.824 0 C15 0.946 47.6 0 C22 1.739 102.4 123.3 0 C29 0.860 121.9 99.2 51.7 0 20 1.119 27.2 70.5 76.4 109.7 0 14 1.234 76.9 39.3 96.4 60.0 87.8 0 12 1.413 137.6 146.5 35.9 47.9 110.7 107.8 0 15 1.627 25.7 31.3 98.8 99.5 40.6 51.6 132.9 18 0.21 1.0538 0.9167 0.0689 1.000 1.4 0 C22 1.238 0 H22A 0.470 42.9 0 12 1.630 38.7 46.0 19 0.21 0.9703 1.5211 -0.0618 1.000 1.3 7 3 1.918 0 1 1.980 31.9 20 0.20 0.6932 0.7724 0.1585 1.000 1.0 0 C5 1.678 0 C8 0.973 127.4 0 C15 1.200 146.3 77.8 0 C21 1.275 53.9 74.6 149.5 0 C22 1.833 46.6 162.2 102.1 100.2 0 C29 1.626 93.0 132.4 55.9 144.8 46.6 0 15 1.066 129.2 45.4 49.4 100.9 121.5 91.2 0 17 1.119 111.4 121.1 48.0 162.5 67.2 29.9 96.2 0 16 1.204 66.0 70.1 113.1 44.5 94.1 115.7 66.7 144.1 0 14 1.633 120.2 93.9 26.8 143.9 80.3 39.3 52.3 49.0 99.4 0 7 1.729 30.8 110.9 170.0 40.5 71.2 116.3 140.4 122.0 75.4 150.4 Code Atom x y z Height Symmetry Transformation 1 O1 1.4026 0.3566 0.0654 0.7 1.0000+X -1.0000+Y 0.0000+Z 2 O1 0.5974 1.6434 -0.0654 0.7 1.0000-X 3.0000-Y 0.0000-Z 3 O10 0.2834 1.7433 -0.0130 0.7 1.0000-X 3.0000-Y 0.0000-Z 4 O10 1.2834 0.7433 -0.0130 0.6 2.0000-X 2.0000-Y 0.0000-Z 5 H22A 1.0267 1.1194 -0.0643 0.4 2.0000-X 2.0000-Y 0.0000-Z 6 H29A 0.0972 1.5522 0.1381 1.4 -1.0000+X 1.0000+Y 0.0000+Z 7 3 0.6493 1.4813 -0.0357 0.7 1.0000-X 3.0000-Y 0.0000-Z 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. 0.02: 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 0.00: Structure factors and derivatives 0.02: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.00: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.00: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + cfc2s finished at 11:42:14 Total CPU time: 0.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++