+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src1089 started at 13:53:28 on 12-Jan-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src1089 in P2(1)2(1)2(1) CELL 0.71073 14.3658 14.5103 23.9483 90.000 90.000 90.000 ZERR 4.00 0.0007 0.0007 0.0008 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O P CE UNIT 144 324 12 48 12 4 V = 4992.07 F(000) = 2068.0 Mu = 1.06 mm-1 Cell Wt = 3924.27 Rho = 1.305 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 eadp o3 o203 anis omit 0 2 1 simu 0.01 c25 > p203 FMAP 2 PLAN 10 SIZE 0.07 0.16 0.18 ACTA BOND $H WGHT 0.00560 27.70510 L.S. 18 TEMP -153.00 FVAR 0.29718 0.49797 CE1 6 0.679994 0.941798 0.083976 11.00000 0.02283 MOLE 1 C1 1 0.389615 1.131874 0.050777 11.00000 0.03364 AFIX 23 H1A 2 0.386119 1.131436 0.092062 11.00000 -1.20000 H1B 2 0.364977 1.192048 0.038082 11.00000 -1.20000 AFIX 0 C2 1 0.325568 1.058179 0.029425 11.00000 0.03846 AFIX 13 H2 2 0.328219 1.059815 -0.012289 11.00000 -1.20000 AFIX 0 C3 1 0.223732 1.080725 0.046953 11.00000 0.06137 AFIX 137 H3A 2 0.181382 1.035335 0.030434 11.00000 -1.50000 H3B 2 0.207159 1.142494 0.033723 11.00000 -1.50000 H3C 2 0.218547 1.078538 0.087734 11.00000 -1.50000 AFIX 0 C4 1 0.351901 0.961663 0.047645 11.00000 0.05536 AFIX 137 H4A 2 0.413522 0.946164 0.032812 11.00000 -1.50000 H4B 2 0.305906 0.917682 0.033390 11.00000 -1.50000 H4C 2 0.353309 0.958705 0.088518 11.00000 -1.50000 AFIX 0 C5 1 0.517375 1.111817 -0.042977 11.00000 0.03563 AFIX 23 H5A 2 0.583464 1.117887 -0.054099 11.00000 -1.20000 H5B 2 0.498536 1.047649 -0.051320 11.00000 -1.20000 AFIX 0 C6 1 0.460277 1.175386 -0.081038 11.00000 0.04062 AFIX 13 H6 2 0.396413 1.180848 -0.064758 11.00000 -1.20000 AFIX 0 C7 1 0.500259 1.272085 -0.086456 11.00000 0.05649 AFIX 137 H7A 2 0.509187 1.298568 -0.049194 11.00000 -1.50000 H7B 2 0.457091 1.310738 -0.107799 11.00000 -1.50000 H7C 2 0.560247 1.269226 -0.105862 11.00000 -1.50000 AFIX 0 C8 1 0.450870 1.135487 -0.138882 11.00000 0.06856 AFIX 137 H8A 2 0.512781 1.128036 -0.155462 11.00000 -1.50000 H8B 2 0.413652 1.177148 -0.162098 11.00000 -1.50000 H8C 2 0.420060 1.075338 -0.136691 11.00000 -1.50000 AFIX 0 C9 1 0.569447 1.234149 0.049182 11.00000 0.04109 AFIX 23 H9A 2 0.625186 1.240413 0.025171 11.00000 -1.20000 H9B 2 0.526874 1.285465 0.039697 11.00000 -1.20000 AFIX 0 C10 1 0.599328 1.245764 0.108729 11.00000 0.05324 AFIX 13 H10 2 0.621550 1.184988 0.123218 11.00000 -1.20000 AFIX 0 C11 1 0.680229 1.315124 0.111198 11.00000 0.07447 AFIX 137 H11A 2 0.730261 1.294755 0.086268 11.00000 -1.50000 H11B 2 0.703837 1.318833 0.149525 11.00000 -1.50000 H11C 2 0.658119 1.375963 0.099373 11.00000 -1.50000 AFIX 0 C12 1 0.520477 1.279802 0.145689 11.00000 0.05789 AFIX 137 H12A 2 0.494626 1.336709 0.130029 11.00000 -1.50000 H12B 2 0.544315 1.291908 0.183322 11.00000 -1.50000 H12C 2 0.471651 1.232734 0.147544 11.00000 -1.50000 AFIX 0 O1 4 0.560838 1.048060 0.060354 11.00000 0.03395 P1 5 0.511773 1.126464 0.031330 11.00000 0.02764 MOLE 2 SAME C1 > P1 C13 1 1.013264 0.880321 0.149754 11.00000 0.03238 AFIX 23 H13A 2 0.986409 0.851018 0.183432 11.00000 -1.20000 H13B 2 1.071280 0.846665 0.140704 11.00000 -1.20000 AFIX 0 C14 1 1.039507 0.978085 0.164855 11.00000 0.03436 AFIX 13 H14 2 1.053826 1.011358 0.129311 11.00000 -1.20000 AFIX 0 C15 1 1.128800 0.979084 0.200967 11.00000 0.06375 AFIX 137 H15A 2 1.113059 0.962788 0.239541 11.00000 -1.50000 H15B 2 1.156461 1.040805 0.200131 11.00000 -1.50000 H15C 2 1.173440 0.934291 0.186104 11.00000 -1.50000 AFIX 0 C16 1 0.961884 1.030405 0.193988 11.00000 0.04979 AFIX 137 H16A 2 0.908201 1.035399 0.168920 11.00000 -1.50000 H16B 2 0.983779 1.092240 0.203905 11.00000 -1.50000 H16C 2 0.943583 0.997336 0.227938 11.00000 -1.50000 AFIX 0 C17 1 0.917715 0.741362 0.079594 11.00000 0.02480 AFIX 23 H17A 2 0.875899 0.734052 0.047035 11.00000 -1.20000 H17B 2 0.978897 0.715040 0.069221 11.00000 -1.20000 AFIX 0 C18 1 0.877475 0.684259 0.128853 11.00000 0.04009 AFIX 13 H18 2 0.839185 0.726220 0.152721 11.00000 -1.20000 AFIX 0 C19 1 0.814466 0.609875 0.105771 11.00000 0.05251 AFIX 137 H19A 2 0.850012 0.570232 0.080415 11.00000 -1.50000 H19B 2 0.762848 0.638423 0.085360 11.00000 -1.50000 H19C 2 0.789732 0.572798 0.136589 11.00000 -1.50000 AFIX 0 C20 1 0.953854 0.643136 0.164712 11.00000 0.06518 AFIX 137 H20A 2 0.925944 0.607656 0.195242 11.00000 -1.50000 H20B 2 0.992269 0.692730 0.180224 11.00000 -1.50000 H20C 2 0.992732 0.602435 0.141853 11.00000 -1.50000 AFIX 0 C21 1 0.989367 0.918198 0.033494 11.00000 0.03595 AFIX 23 H21A 2 0.992269 0.985173 0.041182 11.00000 -1.20000 H21B 2 1.054289 0.895479 0.031832 11.00000 -1.20000 AFIX 0 C22 1 0.946977 0.905562 -0.023185 11.00000 0.03214 AFIX 13 H22 2 0.877989 0.900216 -0.018655 11.00000 -1.20000 AFIX 0 C23 1 0.982513 0.817852 -0.052320 11.00000 0.04742 AFIX 137 H23A 2 0.955987 0.814155 -0.089954 11.00000 -1.50000 H23B 2 0.963615 0.763606 -0.030739 11.00000 -1.50000 H23C 2 1.050570 0.819929 -0.054823 11.00000 -1.50000 AFIX 0 C24 1 0.966914 0.987442 -0.059253 11.00000 0.05327 AFIX 137 H24A 2 0.946041 1.043577 -0.040255 11.00000 -1.50000 H24B 2 0.933762 0.981050 -0.094807 11.00000 -1.50000 H24C 2 1.033994 0.991315 -0.066316 11.00000 -1.50000 AFIX 0 O2 4 0.839497 0.906070 0.105027 11.00000 0.02719 P2 5 0.932695 0.862943 0.092817 11.00000 0.02470 MOLE 3 PART 1 SAME C1 > P1 C25 1 0.721132 1.102697 0.260308 21.00000 0.10676 AFIX 23 H25A 2 0.788373 1.096809 0.251989 21.00000 -1.20000 H25B 2 0.696768 1.145360 0.231548 21.00000 -1.20000 AFIX 0 C26 1 0.720540 1.158323 0.309768 21.00000 0.10495 AFIX 13 H26 2 0.653225 1.169814 0.317807 21.00000 -1.20000 AFIX 0 C27 1 0.757022 1.100445 0.361297 21.00000 0.10344 AFIX 137 H27A 2 0.710259 1.054365 0.371697 21.00000 -1.50000 H27B 2 0.768232 1.141758 0.392964 21.00000 -1.50000 H27C 2 0.815174 1.069359 0.351151 21.00000 -1.50000 AFIX 0 C28 1 0.764524 1.251828 0.309248 21.00000 0.06420 AFIX 137 H28A 2 0.832427 1.245353 0.309046 21.00000 -1.50000 H28B 2 0.745284 1.286040 0.342590 21.00000 -1.50000 H28C 2 0.744661 1.285315 0.275768 21.00000 -1.50000 AFIX 0 C29 1 0.749384 0.896854 0.255767 21.00000 0.04913 AFIX 23 H29A 2 0.762963 0.864811 0.220191 21.00000 -1.20000 H29B 2 0.808902 0.924259 0.268357 21.00000 -1.20000 AFIX 0 C30 1 0.725761 0.820583 0.298432 21.00000 0.04363 AFIX 13 H30 2 0.658159 0.804939 0.295386 21.00000 -1.20000 AFIX 0 C31 1 0.745362 0.858902 0.356768 21.00000 0.06318 AFIX 137 H31A 2 0.763359 0.808405 0.381705 21.00000 -1.50000 H31B 2 0.689216 0.888894 0.371260 21.00000 -1.50000 H31C 2 0.796067 0.903956 0.354709 21.00000 -1.50000 AFIX 0 C32 1 0.782594 0.735006 0.288438 21.00000 0.07180 AFIX 137 H32A 2 0.847784 0.752111 0.282278 21.00000 -1.50000 H32B 2 0.758784 0.702708 0.255459 21.00000 -1.50000 H32C 2 0.778215 0.694484 0.321070 21.00000 -1.50000 AFIX 0 C33 1 0.559852 0.970611 0.266349 21.00000 0.03865 AFIX 23 H33A 2 0.534220 0.914908 0.248090 21.00000 -1.20000 H33B 2 0.566108 0.956827 0.306662 21.00000 -1.20000 AFIX 0 C34 1 0.491000 1.047524 0.259630 21.00000 0.05025 AFIX 13 H34 2 0.516383 1.106433 0.275051 21.00000 -1.20000 AFIX 0 C35 1 0.400014 1.018750 0.290945 21.00000 0.05979 AFIX 137 H35A 2 0.371336 0.966325 0.271718 21.00000 -1.50000 H35B 2 0.356438 1.070709 0.291354 21.00000 -1.50000 H35C 2 0.415246 1.001182 0.329386 21.00000 -1.50000 AFIX 0 C36 1 0.461643 1.059366 0.201048 21.00000 0.07102 AFIX 137 H36A 2 0.512851 1.086247 0.179468 21.00000 -1.50000 H36B 2 0.407551 1.100440 0.199509 21.00000 -1.50000 H36C 2 0.445022 0.999280 0.185245 21.00000 -1.50000 AFIX 0 O3 4 0.674585 0.998892 0.175196 21.00000 0.03266 P3 5 0.675038 0.992043 0.238152 21.00000 0.03193 PART 2 SAME C1 > P1 C225 1 0.725227 1.111438 0.263759 -21.00000 0.09942 AFIX 23 H22A 2 0.785793 1.081955 0.272117 -21.00000 -1.20000 H22B 2 0.735269 1.154225 0.232128 -21.00000 -1.20000 AFIX 0 C226 1 0.697595 1.165617 0.312268 -21.00000 0.10822 AFIX 13 H226 2 0.628638 1.156221 0.312654 -21.00000 -1.20000 AFIX 0 C227 1 0.727131 1.120508 0.368905 -21.00000 0.11615 AFIX 137 H22C 2 0.689673 1.065113 0.375472 -21.00000 -1.50000 H22D 2 0.717071 1.164466 0.399381 -21.00000 -1.50000 H22E 2 0.793149 1.103693 0.367335 -21.00000 -1.50000 AFIX 0 C228 1 0.704511 1.266085 0.309772 -21.00000 0.08532 AFIX 137 H22F 2 0.747428 1.287734 0.338750 -21.00000 -1.50000 H22G 2 0.642892 1.293241 0.315901 -21.00000 -1.50000 H22H 2 0.727847 1.284606 0.272993 -21.00000 -1.50000 AFIX 0 C229 1 0.657002 0.923316 0.286100 -21.00000 0.02941 AFIX 23 H22I 2 0.626703 0.939522 0.321907 -21.00000 -1.20000 H22J 2 0.620352 0.872244 0.269728 -21.00000 -1.20000 AFIX 0 C230 1 0.753768 0.883841 0.300547 -21.00000 0.03257 AFIX 13 H230 2 0.797765 0.935608 0.308500 -21.00000 -1.20000 AFIX 0 C231 1 0.748183 0.820919 0.351077 -21.00000 0.06123 AFIX 137 H23D 2 0.687829 0.789445 0.351400 -21.00000 -1.50000 H23E 2 0.754892 0.857573 0.385211 -21.00000 -1.50000 H23F 2 0.798225 0.775118 0.349241 -21.00000 -1.50000 AFIX 0 C232 1 0.789030 0.828817 0.251106 -21.00000 0.04139 AFIX 137 H23G 2 0.857247 0.828648 0.251226 -21.00000 -1.50000 H23H 2 0.766531 0.856869 0.216414 -21.00000 -1.50000 H23I 2 0.766117 0.765347 0.253702 -21.00000 -1.50000 AFIX 0 C233 1 0.527369 1.071367 0.255613 -21.00000 0.06283 AFIX 23 H23J 2 0.526855 1.092376 0.294942 -21.00000 -1.20000 H23K 2 0.519598 1.126593 0.231790 -21.00000 -1.20000 AFIX 0 C234 1 0.445182 1.009931 0.246791 -21.00000 0.07237 AFIX 13 H234 2 0.464021 0.943807 0.250067 -21.00000 -1.20000 AFIX 0 C235 1 0.370533 1.033933 0.291522 -21.00000 0.09959 AFIX 137 H23L 2 0.401012 1.060564 0.324384 -21.00000 -1.50000 H23M 2 0.337194 0.977793 0.302365 -21.00000 -1.50000 H23N 2 0.326353 1.078567 0.276003 -21.00000 -1.50000 AFIX 0 C236 1 0.400364 1.026818 0.192481 -21.00000 0.06874 AFIX 137 H23O 2 0.361067 1.081868 0.194998 -21.00000 -1.50000 H23P 2 0.361933 0.973566 0.182378 -21.00000 -1.50000 H23Q 2 0.448250 1.036264 0.163903 -21.00000 -1.50000 AFIX 0 O203 4 0.660067 1.000175 0.181551 -21.00000 0.03266 P203 5 0.643223 1.020495 0.240704 -21.00000 0.02240 MOLE 4 PART 0 N11 3 0.657896 0.810934 -0.014164 11.00000 0.03315 O11 4 0.728424 0.808156 0.017241 11.00000 0.03933 O12 4 0.598520 0.874152 -0.005111 11.00000 0.03716 O13 4 0.649903 0.754810 -0.052137 11.00000 0.05791 MOLE 5 N21 3 0.779452 1.101089 0.024991 11.00000 0.03024 O21 4 0.748663 1.030392 -0.001001 11.00000 0.03208 O22 4 0.812233 1.166103 -0.000232 11.00000 0.05926 O23 4 0.770128 1.098834 0.078970 11.00000 0.03863 MOLE 6 N31 3 0.576898 0.802924 0.152555 11.00000 0.03489 O31 4 0.662967 0.793001 0.140971 11.00000 0.04318 O32 4 0.532966 0.863712 0.125766 11.00000 0.03502 O33 4 0.539509 0.757801 0.190285 11.00000 0.05842 HKLF 4 Covalent radii and connectivity table for 2009src1089 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CE 1.830 Ce1 - O3_a O1 O2 O203_b O31 O32 O21 O11 O23 O12 N31 C1 - C2 P1 C2 - C1 C4 C3 C3 - C2 C4 - C2 C5 - C6 P1 C6 - C8 C7 C5 C7 - C6 C8 - C6 C9 - C10 P1 C10 - C9 C12 C11 C11 - C10 C12 - C10 O1 - P1 Ce1 P1 - O1 C5 C1 C9 C13 - C14 P2 C14 - C13 C16 C15 C15 - C14 C16 - C14 C17 - C18 P2 C18 - C19 C20 C17 C19 - C18 C20 - C18 C21 - C22 P2 C22 - C24 C21 C23 C23 - C22 C24 - C22 O2 - P2 Ce1 P2 - O2 C17 C13 C21 C25_a - C26_a P3_a C26_a - C25_a C28_a C27_a C27_a - C26_a C28_a - C26_a C29_a - C30_a P3_a C30_a - C32_a C31_a C29_a C31_a - C30_a C32_a - C30_a C33_a - C34_a P3_a C34_a - C36_a C33_a C35_a C35_a - C34_a C36_a - C34_a O3_a - P3_a Ce1 P3_a - O3_a C29_a C33_a C25_a C225_b - C226_b P203_b C226_b - C225_b C228_b C227_b C227_b - C226_b C228_b - C226_b C229_b - C230_b P203_b C230_b - C232_b C231_b C229_b C231_b - C230_b C232_b - C230_b C233_b - C234_b P203_b C234_b - C236_b C233_b C235_b C235_b - C234_b C236_b - C234_b O203_b - P203_b Ce1 P203_b - O203_b C229_b C225_b C233_b N11 - O13 O11 O12 O11 - N11 Ce1 O12 - N11 Ce1 O13 - N11 N21 - O22 O21 O23 O21 - N21 Ce1 O22 - N21 O23 - N21 Ce1 N31 - O33 O32 O31 Ce1 O31 - N31 Ce1 O32 - N31 Ce1 O33 - N31 h k l Fo^2 Sigma Why rejected 7 0 0 500.76 47.33 observed but should be systematically absent 7 0 0 490.44 49.87 observed but should be systematically absent 11 0 0 122.31 30.38 observed but should be systematically absent 13 0 0 145.43 27.28 observed but should be systematically absent 0 0 5 37.84 8.31 observed but should be systematically absent 0 0 5 47.04 7.99 observed but should be systematically absent 0 0 5 46.11 8.78 observed but should be systematically absent 34801 Reflections read, of which 84 rejected -18 =< h =< 18, -18 =< k =< 18, -31 =< l =< 31, Max. 2-theta = 54.96 7 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 0 4 -0.55 0.07 5 1.28 3 15 8 196.83 26.59 3 231.29 -14 5 10 66.34 30.80 2 310.05 -13 7 10 175.48 28.97 3 205.86 10 2 12 11.59 17.25 2 151.58 11 6 16 197.23 39.22 2 460.26 -7 9 18 303.55 25.68 3 150.24 -12 6 19 117.31 26.60 3 135.32 -9 10 19 51.37 41.09 2 250.98 -8 11 19 90.23 31.55 2 201.40 -4 13 19 69.02 24.91 2 317.06 0 9 22 250.63 22.30 3 155.59 0 3 26 238.29 28.27 3 143.18 13 Inconsistent equivalents 11396 Unique reflections, of which 0 suppressed R(int) = 0.0706 R(sigma) = 0.1042 Friedel opposites not merged Maximum memory for data reduction = 8557 / 113018 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 = 10671 / 887184 wR2 = 0.1700 before cycle 1 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.0783 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2064 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1324 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1517 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. 0.1219 0.0400 SAME/SADI C18 P2 C30_a P3_a Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.048 0.000 0.000 0.000 0.000 0.012 0.000 0.000 GooF = S = 1.330; Restrained GooF = 1.331 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29699 0.00044 -0.439 OSF 2 0.48877 0.00741 -1.241 FVAR 2 7 0.02148 0.00021 -6.392 U22 Ce1 10 -0.00195 0.00025 -7.851 U13 Ce1 11 0.00216 0.00025 8.530 U12 Ce1 103 -0.01867 0.00613 -3.044 U23 C10 109 0.03679 0.01059 -3.558 U11 C11 112 -0.03335 0.00739 -4.515 U23 C11 138 0.02092 0.00152 -4.431 U11 P1 140 0.03459 0.00130 5.350 U33 P1 168 -0.02077 0.00689 -3.012 U23 C15 279 0.06781 0.01215 -3.206 U11 C25_a 282 -0.03929 0.00852 -4.610 U23 C25_a 288 0.06851 0.01207 -3.020 U11 C26_a 291 -0.03182 0.00797 -3.994 U23 C26_a 412 0.13096 0.01040 3.032 U22 C225_b 414 -0.04097 0.00849 -4.827 U23 C225_b 420 0.06965 0.01212 -3.182 U11 C226_b 423 -0.03291 0.00811 -4.059 U23 C226_b 549 -0.01295 0.00340 -3.812 U23 O11 564 0.03462 0.00657 -3.545 U11 O13 565 0.07600 0.00564 3.206 U22 O13 567 -0.02864 0.00441 -6.490 U23 O13 592 0.03939 0.00537 -3.698 U22 O22 610 0.01659 0.00528 -3.469 U22 N31 641 -0.01954 0.00489 -3.999 U12 O33 Mean shift/esd = 0.883 Maximum = 8.530 for U12 Ce1 Max. shift = 0.105 A for H36C_a Max. dU =-0.020 for C235_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1553 before cycle 2 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.0671 0.0200 SAME/SADI C13 C14 C25_a C26_a 0.2101 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1495 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1521 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.047 0.000 0.000 0.000 0.000 0.010 0.000 0.000 GooF = S = 1.219; Restrained GooF = 1.215 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29691 0.00040 -0.199 OSF 2 0.48641 0.00683 -0.346 FVAR 2 10 -0.00283 0.00023 -3.859 U13 Ce1 11 0.00341 0.00023 5.476 U12 Ce1 140 0.03877 0.00127 3.289 U33 P1 567 -0.04181 0.00401 -3.283 U23 O13 Mean shift/esd = 0.413 Maximum = 5.476 for U12 Ce1 Max. shift = 0.059 A for H28C_a Max. dU = 0.008 for C28_a Least-squares cycle 3 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1530 before cycle 3 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.0690 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2178 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1483 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1584 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.049 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.199; Restrained GooF = 1.197 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29724 0.00039 0.853 OSF 2 0.48531 0.00675 -0.163 FVAR 2 Mean shift/esd = 0.117 Maximum = 1.372 for U12 Ce1 Max. shift = 0.097 A for H27C_a Max. dU = 0.002 for C28_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1528 before cycle 4 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.0744 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2279 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1363 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1590 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.050 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.197 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29726 0.00039 0.045 OSF 2 0.48482 0.00674 -0.073 FVAR 2 Mean shift/esd = 0.051 Maximum = 0.372 for U12 Ce1 Max. shift = 0.094 A for H27C_a Max. dU = 0.001 for C28_a Least-squares cycle 5 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1528 before cycle 5 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.0736 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2334 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1351 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1581 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.050 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.197 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29727 0.00039 0.012 OSF 2 0.48468 0.00672 -0.021 FVAR 2 Mean shift/esd = 0.026 Maximum = 0.287 for tors H27A_a Max. shift = 0.093 A for H27C_a Max. dU = 0.000 for C28_a Least-squares cycle 6 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1528 before cycle 6 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.0738 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2372 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1334 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1572 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.050 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.197 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29727 0.00039 0.001 OSF 2 0.48458 0.00672 -0.015 FVAR 2 Mean shift/esd = 0.015 Maximum = 0.264 for tors H27A_a Max. shift = 0.085 A for H27C_a Max. dU = 0.000 for C27_a Least-squares cycle 7 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1528 before cycle 7 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.0740 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2402 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1321 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1568 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.050 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.197 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29727 0.00039 0.003 OSF 2 0.48450 0.00672 -0.011 FVAR 2 Mean shift/esd = 0.010 Maximum = 0.225 for tors H27A_a Max. shift = 0.071 A for H27C_a Max. dU = 0.000 for C27_a Least-squares cycle 8 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1528 before cycle 8 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 0.0742 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2430 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1310 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1565 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.051 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.197 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29727 0.00039 -0.002 OSF 2 0.48445 0.00672 -0.008 FVAR 2 Mean shift/esd = 0.007 Maximum = 0.151 for tors H27A_a Max. shift = 0.047 A for H27C_a Max. dU = 0.000 for C27_a Least-squares cycle 9 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1528 before cycle 9 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 0.0743 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2454 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1301 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1562 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.051 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.197 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29726 0.00039 -0.004 OSF 2 0.48441 0.00672 -0.006 FVAR 2 Mean shift/esd = 0.005 Maximum = 0.092 for z C25_a Max. shift = 0.028 A for H27C_a Max. dU = 0.000 for C27_a Least-squares cycle 10 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1528 before cycle 10 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 0.0744 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2471 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1293 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1560 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.051 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.197 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29726 0.00039 0.000 OSF 2 0.48438 0.00672 -0.003 FVAR 2 Mean shift/esd = 0.004 Maximum = 0.068 for z C25_a Max. shift = 0.015 A for H27C_a Max. dU = 0.000 for C27_a Least-squares cycle 11 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1528 before cycle 11 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 0.0744 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2484 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1287 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1558 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.051 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.197 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29726 0.00039 -0.001 OSF 2 0.48437 0.00672 -0.003 FVAR 2 Mean shift/esd = 0.002 Maximum = 0.050 for z C25_a Max. shift = 0.010 A for H27C_a Max. dU = 0.000 for C227_b Least-squares cycle 12 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1528 before cycle 12 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint 0.0744 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2493 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1283 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1557 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.051 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.197 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29726 0.00039 0.000 OSF 2 0.48436 0.00672 -0.002 FVAR 2 Mean shift/esd = 0.002 Maximum = 0.035 for z C25_a Max. shift = 0.005 A for H27C_a Max. dU = 0.000 for C227_b Least-squares cycle 13 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1528 before cycle 13 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint 0.0745 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2500 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1280 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1556 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.051 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.197 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29726 0.00039 0.000 OSF 2 0.48435 0.00672 -0.001 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.025 for z C25_a Max. shift = 0.004 A for H27C_a Max. dU = 0.000 for C227_b Least-squares cycle 14 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1528 before cycle 14 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint 0.0745 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2504 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1278 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1555 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.051 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.198 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29726 0.00039 0.000 OSF 2 0.48434 0.00672 -0.001 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.017 for z C25_a Max. shift = 0.002 A for H27C_a Max. dU = 0.000 for C227_b Least-squares cycle 15 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1528 before cycle 15 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint 0.0745 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2507 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1276 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1554 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.051 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.198 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29726 0.00039 0.000 OSF 2 0.48434 0.00672 -0.001 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.012 for z C25_a Max. shift = 0.002 A for H27C_a Max. dU = 0.000 for C227_b Least-squares cycle 16 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1528 before cycle 16 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint 0.0745 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2509 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1275 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1554 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.051 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.198 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29726 0.00039 -0.001 OSF 2 0.48433 0.00672 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.009 for z C25_a Max. shift = 0.001 A for H27C_a Max. dU = 0.000 for C227_b Least-squares cycle 17 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1528 before cycle 17 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 17 Observed Target Error Sigma Restraint 0.0745 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2511 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1275 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1554 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.051 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.198 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29726 0.00039 -0.001 OSF 2 0.48433 0.00672 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.006 for z C25_a Max. shift = 0.001 A for H27C_a Max. dU = 0.000 for C227_b Least-squares cycle 18 Maximum vector length = 511 Memory required = 10671 / 887184 wR2 = 0.1528 before cycle 18 for 11396 data and 641 / 641 parameters Disagreeable restraints before cycle 18 Observed Target Error Sigma Restraint 0.0745 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2512 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1274 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1553 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.051 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.198 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29726 0.00039 0.000 OSF 2 0.48433 0.00672 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.004 for z C25_a Max. shift = 0.001 A for H27C_a Max. dU = 0.000 for C227_b Largest correlation matrix elements -0.854 y O203_b / y O3_a 0.707 U11 C226_b / U11 C26_a 0.660 U23 C226_b / U23 C26_a 0.812 U22 C226_b / U22 C26_a 0.697 U12 C226_b / U12 C26_a 0.660 U33 C226_b / U33 C25_a 0.802 U22 C226_b / U22 C25_a 0.670 U12 C226_b / U12 C25_a 0.660 U33 C226_b / U33 C26_a 0.802 U22 C226_b / U22 C225_b 0.669 U12 C226_b / U12 C225_b 0.659 U33 C226_b / U33 C225_b 0.801 U22 C26_a / U22 C25_a 0.669 U12 C26_a / U12 C25_a 0.658 U33 C26_a / U33 C25_a 0.801 U22 C225_b / U22 C26_a 0.668 U12 C225_b / U12 C26_a 0.657 U11 C233_b / U11 C34_a 0.794 U22 C225_b / U22 C25_a -0.663 U12 O3_a / y O3_a 0.656 U33 C225_b / U33 C26_a 0.775 y C228_b / y C226_b -0.662 y C235_b / y C35_a 0.656 U11 C26_a / U11 C25_a Idealized hydrogen atom generation before cycle 19 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.3860 1.1314 0.0920 23 0.990 0.000 C1 C2 P1 H1B 0.3649 1.1919 0.0380 23 0.990 0.000 C1 C2 P1 H2 0.3285 1.0595 -0.0123 13 1.000 0.000 C2 C1 C4 C3 H3A 0.1813 1.0354 0.0303 137 0.980 0.000 C3 C2 H3A H3B 0.2072 1.1425 0.0333 137 0.980 0.000 C3 C2 H3A H3C 0.2183 1.0789 0.0875 137 0.980 0.000 C3 C2 H3A H4A 0.4133 0.9453 0.0325 137 0.980 0.000 C4 C2 H4A H4B 0.3056 0.9173 0.0340 137 0.980 0.000 C4 C2 H4A H4C 0.3543 0.9586 0.0886 137 0.980 0.000 C4 C2 H4A H5A 0.5833 1.1179 -0.0542 23 0.990 0.000 C5 C6 P1 H5B 0.4983 1.0477 -0.0514 23 0.990 0.000 C5 C6 P1 H6 0.3964 1.1808 -0.0649 13 1.000 0.000 C6 C8 C7 C5 H7A 0.5094 1.2982 -0.0494 137 0.980 0.000 C7 C6 H7A H7B 0.4570 1.3103 -0.1079 137 0.980 0.000 C7 C6 H7A H7C 0.5601 1.2688 -0.1062 137 0.980 0.000 C7 C6 H7A H8A 0.5131 1.1273 -0.1554 137 0.980 0.000 C8 C6 H8A H8B 0.4143 1.1769 -0.1623 137 0.980 0.000 C8 C6 H8A H8C 0.4199 1.0752 -0.1368 137 0.980 0.000 C8 C6 H8A H9A 0.6253 1.2405 0.0252 23 0.990 0.000 C9 C10 P1 H9B 0.5269 1.2856 0.0395 23 0.990 0.000 C9 C10 P1 H10 0.6214 1.1857 0.1233 13 1.000 0.000 C10 C9 C12 C11 H11A 0.7303 1.2948 0.0865 137 0.980 0.000 C11 C10 H11A H11B 0.7036 1.3192 0.1496 137 0.980 0.000 C11 C10 H11A H11C 0.6583 1.3763 0.0993 137 0.980 0.000 C11 C10 H11A H12A 0.4948 1.3377 0.1301 137 0.980 0.000 C12 C10 H12A H12B 0.5445 1.2928 0.1833 137 0.980 0.000 C12 C10 H12A H12C 0.4716 1.2338 0.1476 137 0.980 0.000 C12 C10 H12A H13A 0.9866 0.8507 0.1834 23 0.990 0.000 C13 C14 P2 H13B 1.0714 0.8465 0.1406 23 0.990 0.000 C13 C14 P2 H14 1.0540 1.0109 0.1294 13 1.000 0.000 C14 C13 C16 C15 H15A 1.1137 0.9581 0.2391 137 0.980 0.000 C15 C14 H15A H15B 1.1551 1.0403 0.2021 137 0.980 0.000 C15 C14 H15A H15C 1.1748 0.9355 0.1849 137 0.980 0.000 C15 C14 H15A H16A 0.9082 1.0354 0.1688 137 0.980 0.000 C16 C14 H16A H16B 0.9836 1.0917 0.2042 137 0.980 0.000 C16 C14 H16A H16C 0.9428 0.9967 0.2278 137 0.980 0.000 C16 C14 H16A H17A 0.8762 0.7341 0.0470 23 0.990 0.000 C17 C18 P2 H17B 0.9791 0.7152 0.0694 23 0.990 0.000 C17 C18 P2 H18 0.8391 0.7267 0.1527 13 1.000 0.000 C18 C19 C20 C17 H19A 0.8502 0.5708 0.0801 137 0.980 0.000 C19 C18 H19A H19B 0.7627 0.6384 0.0854 137 0.980 0.000 C19 C18 H19A H19C 0.7903 0.5726 0.1365 137 0.980 0.000 C19 C18 H19A H20A 0.9260 0.6079 0.1951 137 0.980 0.000 C20 C18 H20A H20B 0.9926 0.6927 0.1800 137 0.980 0.000 C20 C18 H20A H20C 0.9925 0.6024 0.1417 137 0.980 0.000 C20 C18 H20A H21A 0.9927 0.9851 0.0413 23 0.990 0.000 C21 C22 P2 H21B 1.0544 0.8952 0.0319 23 0.990 0.000 C21 C22 P2 H22 0.8781 0.9005 -0.0186 13 1.000 0.000 C22 C24 C21 C23 H23A 0.9555 0.8141 -0.0897 137 0.980 0.000 C23 C22 H23A H23B 0.9635 0.7639 -0.0304 137 0.980 0.000 C23 C22 H23A H23C 1.0503 0.8200 -0.0548 137 0.980 0.000 C23 C22 H23A H24A 0.9460 1.0439 -0.0403 137 0.980 0.000 C24 C22 H24A H24B 0.9341 0.9814 -0.0949 137 0.980 0.000 C24 C22 H24A H24C 1.0342 0.9918 -0.0662 137 0.980 0.000 C24 C22 H24A H25A 0.7902 1.0915 0.2575 23 0.990 0.000 C25_a C26_a P3_a H25B 0.7034 1.1432 0.2332 23 0.990 0.000 C25_a C26_a P3_a H26 0.6540 1.1714 0.3195 13 1.000 0.000 C26_a C25_a C28_a C27_a H27A 0.7371 1.0400 0.3619 137 0.980 0.000 C27_a C26_a H27A_a H27B 0.7405 1.1329 0.3979 137 0.980 0.000 C27_a C26_a H27A_a H27C 0.8289 1.1025 0.3616 137 0.980 0.000 C27_a C26_a H27A_a H28A 0.8349 1.2451 0.3084 137 0.980 0.000 C28_a C26_a H28A_a H28B 0.7482 1.2898 0.3405 137 0.980 0.000 C28_a C26_a H28A_a H28C 0.7481 1.2840 0.2738 137 0.980 0.000 C28_a C26_a H28A_a H29A 0.7625 0.8635 0.2202 23 0.990 0.000 C29_a C30_a P3_a H29B 0.8098 0.9230 0.2680 23 0.990 0.000 C29_a C30_a P3_a H30 0.6574 0.8057 0.2955 13 1.000 0.000 C30_a C32_a C31_a C29_a H31A 0.7592 0.8100 0.3826 137 0.980 0.000 C31_a C30_a H31A_a H31B 0.6901 0.8941 0.3703 137 0.980 0.000 C31_a C30_a H31A_a H31C 0.7981 0.9027 0.3548 137 0.980 0.000 C31_a C30_a H31A_a H32A 0.8484 0.7533 0.2868 137 0.980 0.000 C32_a C30_a H32A_a H32B 0.7635 0.7075 0.2537 137 0.980 0.000 C32_a C30_a H32A_a H32C 0.7730 0.6929 0.3197 137 0.980 0.000 C32_a C30_a H32A_a H33A 0.5354 0.9131 0.2477 23 0.990 0.000 C33_a C34_a P3_a H33B 0.5662 0.9552 0.3064 23 0.990 0.000 C33_a C34_a P3_a H34 0.5160 1.1048 0.2744 13 1.000 0.000 C34_a C36_a C33_a C35_a H35A 0.3699 0.9673 0.2698 137 0.980 0.000 C35_a C34_a H35A_a H35B 0.3593 1.0698 0.2935 137 0.980 0.000 C35_a C34_a H35A_a H35C 0.4174 0.9948 0.3279 137 0.980 0.000 C35_a C34_a H35A_a H36A 0.5118 1.0874 0.1794 137 0.980 0.000 C36_a C34_a H36A_a H36B 0.4056 1.0956 0.1990 137 0.980 0.000 C36_a C34_a H36A_a H36C 0.4486 0.9969 0.1841 137 0.980 0.000 C36_a C34_a H36A_a H22A 0.7858 1.0854 0.2686 23 0.990 0.000 C225_b C226_b P203_b H22B 0.7308 1.1561 0.2297 23 0.990 0.000 C225_b C226_b P203_b H226 0.6277 1.1585 0.3108 13 1.000 0.000 C226_b C225_b C228_b C227_b H22C 0.6809 1.0660 0.3741 137 0.980 0.000 C227_b C226_b H22C_b H22D 0.7261 1.1593 0.3971 137 0.980 0.000 C227_b C226_b H22C_b H22E 0.7880 1.0887 0.3618 137 0.980 0.000 C227_b C226_b H22C_b H22F 0.7543 1.2851 0.3373 137 0.980 0.000 C228_b C226_b H22F_b H22G 0.6473 1.2953 0.3198 137 0.980 0.000 C228_b C226_b H22F_b H22H 0.7259 1.2867 0.2727 137 0.980 0.000 C228_b C226_b H22F_b H22I 0.6265 0.9393 0.3215 23 0.990 0.000 C229_b C230_b P203_b H22J 0.6205 0.8720 0.2693 23 0.990 0.000 C229_b C230_b P203_b H230 0.7968 0.9358 0.3085 13 1.000 0.000 C230_b C232_b C231_b C229_b H23D 0.6876 0.7912 0.3523 137 0.980 0.000 C231_b C230_b H23D_b H23E 0.7570 0.8586 0.3850 137 0.980 0.000 C231_b C230_b H23D_b H23F 0.7976 0.7750 0.3488 137 0.980 0.000 C231_b C230_b H23D_b H23G 0.8572 0.8251 0.2535 137 0.980 0.000 C232_b C230_b H23G_b H23H 0.7722 0.8618 0.2165 137 0.980 0.000 C232_b C230_b H23G_b H23I 0.7619 0.7681 0.2512 137 0.980 0.000 C232_b C230_b H23G_b H23J 0.5265 1.0895 0.2965 23 0.990 0.000 C233_b C234_b P203_b H23K 0.5185 1.1266 0.2339 23 0.990 0.000 C233_b C234_b P203_b H234 0.4663 0.9418 0.2492 13 1.000 0.000 C234_b C236_b C233_b C235_b H23L 0.4022 1.0534 0.3253 137 0.980 0.000 C235_b C234_b H23L_b H23M 0.3397 0.9706 0.3021 137 0.980 0.000 C235_b C234_b H23L_b H23N 0.3266 1.0723 0.2776 137 0.980 0.000 C235_b C234_b H23L_b H23O 0.3610 1.0799 0.1958 137 0.980 0.000 C236_b C234_b H23O_b H23P 0.3621 0.9717 0.1826 137 0.980 0.000 C236_b C234_b H23O_b H23Q 0.4480 1.0350 0.1641 137 0.980 0.000 C236_b C234_b H23O_b 2009src1089 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Ce1 0.67999 0.94180 0.08398 1.00000 0.02377 0.02132 0.02344 -0.00024 -0.00296 0.00383 0.02284 0.00079 0.00003 0.00003 0.00002 0.00000 0.00021 0.00018 0.00019 0.00021 0.00023 0.00022 0.00011 C1 0.38956 1.13180 0.05074 1.00000 0.01845 0.03430 0.04763 0.01156 0.01037 0.00612 0.03346 0.01552 0.00053 0.00060 0.00039 0.00000 0.00484 0.00529 0.00572 0.00433 0.00418 0.00401 0.00222 H1A 0.38602 1.13142 0.09202 1.00000 0.04015 0.00000 0.00000 H1B 0.36487 1.19193 0.03799 1.00000 0.04015 0.00000 0.00000 C2 0.32565 1.05796 0.02937 1.00000 0.02407 0.03925 0.05233 0.00661 -0.00338 -0.00251 0.03855 0.01505 0.00059 0.00062 0.00036 0.00000 0.00448 0.00456 0.00496 0.00478 0.00460 0.00573 0.00191 H2 0.32848 1.05951 -0.01234 1.00000 0.04626 0.00000 0.00000 C3 0.22364 1.08080 0.04672 1.00000 0.02409 0.06688 0.09207 0.01311 0.00825 -0.00621 0.06101 0.02079 0.00065 0.00081 0.00053 0.00000 0.00587 0.00900 0.00914 0.00675 0.00584 0.00544 0.00355 H3A 0.18129 1.03536 0.03025 1.00000 0.09152 0.00000 0.00000 H3B 0.20721 1.14250 0.03331 1.00000 0.09152 0.00000 0.00000 H3C 0.21829 1.07890 0.08750 1.00000 0.09152 0.00000 0.00000 C4 0.35205 0.96121 0.04772 1.00000 0.04696 0.03662 0.08258 0.00985 -0.00303 -0.01351 0.05539 0.01854 0.00076 0.00064 0.00048 0.00000 0.00721 0.00673 0.00804 0.00541 0.00591 0.00493 0.00319 H4A 0.41328 0.94534 0.03245 1.00000 0.08308 0.00000 0.00000 H4B 0.30557 0.91731 0.03395 1.00000 0.08308 0.00000 0.00000 H4C 0.35433 0.95857 0.08859 1.00000 0.08308 0.00000 0.00000 C5 0.51717 1.11188 -0.04305 1.00000 0.02061 0.03395 0.05138 0.01328 -0.01524 -0.01088 0.03532 0.01421 0.00062 0.00059 0.00033 0.00000 0.00499 0.00530 0.00593 0.00437 0.00445 0.00400 0.00232 H5A 0.58326 1.11786 -0.05419 1.00000 0.04238 0.00000 0.00000 H5B 0.49827 1.04772 -0.05137 1.00000 0.04238 0.00000 0.00000 C6 0.46034 1.17523 -0.08109 1.00000 0.02382 0.05942 0.03871 0.01475 0.00652 0.00134 0.04065 0.01623 0.00062 0.00061 0.00039 0.00000 0.00479 0.00613 0.00519 0.00553 0.00500 0.00436 0.00224 H6 0.39644 1.18076 -0.06487 1.00000 0.04878 0.00000 0.00000 C7 0.50027 1.27169 -0.08663 1.00000 0.07664 0.03097 0.06262 0.01722 0.00420 0.00356 0.05674 0.01961 0.00083 0.00058 0.00052 0.00000 0.00854 0.00529 0.00691 0.00590 0.00772 0.00517 0.00296 H7A 0.50944 1.29822 -0.04940 1.00000 0.08512 0.00000 0.00000 H7B 0.45699 1.31034 -0.10790 1.00000 0.08512 0.00000 0.00000 H7C 0.56013 1.26877 -0.10617 1.00000 0.08512 0.00000 0.00000 C8 0.45107 1.13513 -0.13896 1.00000 0.07833 0.06324 0.06237 0.01925 -0.02528 -0.01219 0.06798 0.01919 0.00098 0.00082 0.00044 0.00000 0.01011 0.00827 0.00803 0.00644 0.00721 0.00751 0.00382 H8A 0.51305 1.12725 -0.15538 1.00000 0.10197 0.00000 0.00000 H8B 0.41427 1.17693 -0.16232 1.00000 0.10197 0.00000 0.00000 H8C 0.41989 1.07517 -0.13676 1.00000 0.10197 0.00000 0.00000 C9 0.56948 1.23436 0.04915 1.00000 0.02434 0.03939 0.05908 -0.00037 0.01407 -0.00204 0.04093 0.01483 0.00066 0.00062 0.00039 0.00000 0.00568 0.00597 0.00677 0.00488 0.00493 0.00445 0.00257 H9A 0.62526 1.24051 0.02517 1.00000 0.04912 0.00000 0.00000 H9B 0.52693 1.28562 0.03953 1.00000 0.04912 0.00000 0.00000 C10 0.59930 1.24644 0.10870 1.00000 0.03957 0.04681 0.07284 -0.02890 0.00004 0.01955 0.05307 0.01726 0.00071 0.00076 0.00044 0.00000 0.00708 0.00675 0.00778 0.00570 0.00578 0.00541 0.00322 H10 0.62139 1.18569 0.12331 1.00000 0.06369 0.00000 0.00000 C11 0.68020 1.31540 0.11125 1.00000 0.03157 0.08407 0.10655 -0.05243 0.00393 -0.01318 0.07406 0.01740 0.00085 0.00085 0.00052 0.00000 0.00625 0.00888 0.00973 0.00747 0.00800 0.00769 0.00398 H11A 0.73033 1.29481 0.08646 1.00000 0.11110 0.00000 0.00000 H11B 0.70359 1.31917 0.14962 1.00000 0.11110 0.00000 0.00000 H11C 0.65835 1.37627 0.09930 1.00000 0.11110 0.00000 0.00000 C12 0.52053 1.28074 0.14571 1.00000 0.05267 0.06490 0.05795 -0.00966 0.02002 0.01805 0.05850 0.02175 0.00080 0.00084 0.00045 0.00000 0.00812 0.00813 0.00745 0.00604 0.00617 0.00637 0.00337 H12A 0.49482 1.33771 0.13006 1.00000 0.08775 0.00000 0.00000 H12B 0.54446 1.29280 0.18333 1.00000 0.08775 0.00000 0.00000 H12C 0.47158 1.23380 0.14760 1.00000 0.08775 0.00000 0.00000 O1 0.56090 1.04793 0.06027 1.00000 0.03095 0.02455 0.04558 0.00136 -0.00152 0.00209 0.03369 0.01038 0.00041 0.00041 0.00023 0.00000 0.00351 0.00333 0.00339 0.00280 0.00271 0.00294 0.00142 P1 0.51175 1.12645 0.03132 1.00000 0.01731 0.02547 0.03978 0.00391 0.00326 0.00405 0.02752 0.00421 0.00016 0.00016 0.00010 0.00000 0.00121 0.00119 0.00132 0.00098 0.00100 0.00093 0.00051 C13 1.01335 0.88014 0.14973 1.00000 0.00750 0.04837 0.04023 -0.00145 0.00340 -0.00697 0.03203 0.01291 0.00056 0.00061 0.00035 0.00000 0.00427 0.00599 0.00539 0.00444 0.00381 0.00397 0.00218 H13A 0.98656 0.85073 0.18339 1.00000 0.03844 0.00000 0.00000 H13B 1.07135 0.84652 0.14060 1.00000 0.03844 0.00000 0.00000 C14 1.03953 0.97759 0.16487 1.00000 0.02926 0.03835 0.03467 -0.00881 0.00292 -0.00708 0.03409 0.01421 0.00062 0.00061 0.00037 0.00000 0.00554 0.00529 0.00502 0.00397 0.00430 0.00425 0.00222 H14 1.05404 1.01092 0.12938 1.00000 0.04091 0.00000 0.00000 C15 1.12900 0.97790 0.20109 1.00000 0.04540 0.07599 0.06961 -0.02898 -0.00791 -0.01888 0.06367 0.01663 0.00075 0.00085 0.00049 0.00000 0.00758 0.00894 0.00800 0.00657 0.00627 0.00628 0.00363 H15A 1.11371 0.95812 0.23912 1.00000 0.09550 0.00000 0.00000 H15B 1.15507 1.04029 0.20209 1.00000 0.09550 0.00000 0.00000 H15C 1.17475 0.93550 0.18493 1.00000 0.09550 0.00000 0.00000 C16 0.96157 1.03000 0.19400 1.00000 0.06356 0.03188 0.05247 -0.00711 -0.00966 0.00528 0.04931 0.01861 0.00078 0.00067 0.00044 0.00000 0.00825 0.00597 0.00651 0.00468 0.00598 0.00529 0.00298 H16A 0.90815 1.03540 0.16876 1.00000 0.07396 0.00000 0.00000 H16B 0.98356 1.09168 0.20421 1.00000 0.07396 0.00000 0.00000 H16C 0.94285 0.99667 0.22777 1.00000 0.07396 0.00000 0.00000 C17 0.91783 0.74150 0.07964 1.00000 0.02204 0.02445 0.02817 0.00046 0.00247 0.00432 0.02489 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0.00890 0.04023 0.01099 0.00048 0.00046 0.00028 0.00000 0.00423 0.00409 0.00401 0.00316 0.00327 0.00330 0.00171 O12 0.59852 0.87423 -0.00509 1.00000 0.02732 0.04245 0.04224 -0.00348 -0.00485 -0.00241 0.03734 0.01080 0.00047 0.00045 0.00027 0.00000 0.00381 0.00398 0.00384 0.00315 0.00305 0.00313 0.00157 O13 0.64983 0.75482 -0.05215 1.00000 0.02990 0.09048 0.05285 -0.04365 0.00125 -0.00073 0.05774 0.01161 0.00049 0.00059 0.00030 0.00000 0.00438 0.00602 0.00446 0.00423 0.00334 0.00391 0.00227 N21 0.77948 1.10107 0.02488 1.00000 0.01728 0.02601 0.04779 0.00604 -0.00579 0.00386 0.03036 0.01352 0.00052 0.00051 0.00034 0.00000 0.00401 0.00412 0.00500 0.00354 0.00357 0.00321 0.00179 O21 0.74867 1.03033 -0.00104 1.00000 0.03050 0.02600 0.03935 0.00182 -0.00279 -0.00281 0.03195 0.01058 0.00044 0.00039 0.00026 0.00000 0.00369 0.00341 0.00355 0.00262 0.00294 0.00267 0.00148 O22 0.81210 1.16607 -0.00026 1.00000 0.07010 0.03696 0.07055 0.00878 0.01174 -0.01758 0.05920 0.01375 0.00066 0.00046 0.00031 0.00000 0.00579 0.00389 0.00487 0.00354 0.00504 0.00449 0.00209 O23 0.77018 1.09872 0.07880 1.00000 0.03598 0.03025 0.04910 0.00510 0.00194 -0.00278 0.03844 0.01153 0.00044 0.00039 0.00032 0.00000 0.00379 0.00323 0.00411 0.00325 0.00366 0.00267 0.00154 N31 0.57684 0.80310 0.15261 1.00000 0.05928 0.01409 0.03139 0.00219 -0.00050 -0.01753 0.03492 0.01295 0.00067 0.00048 0.00031 0.00000 0.00623 0.00370 0.00417 0.00304 0.00412 0.00382 0.00201 O31 0.66302 0.79316 0.14103 1.00000 0.04143 0.02714 0.06074 0.00320 -0.00995 -0.00255 0.04311 0.01148 0.00053 0.00042 0.00029 0.00000 0.00514 0.00342 0.00440 0.00295 0.00382 0.00320 0.00179 O32 0.53292 0.86370 0.12586 1.00000 0.02706 0.03080 0.04652 0.01419 0.00273 0.00047 0.03479 0.01147 0.00045 0.00043 0.00027 0.00000 0.00375 0.00357 0.00393 0.00300 0.00309 0.00292 0.00154 O33 0.53954 0.75817 0.19036 1.00000 0.08268 0.04387 0.04828 0.01210 0.00189 -0.02958 0.05828 0.01291 0.00062 0.00050 0.00030 0.00000 0.00657 0.00450 0.00438 0.00351 0.00424 0.00439 0.00229 Final Structure Factor Calculation for 2009src1089 in P2(1)2(1)2(1) Total number of l.s. parameters = 641 Maximum vector length = 511 Memory required = 10032 / 27090 wR2 = 0.1528 before cycle 19 for 11396 data and 2 / 641 parameters Disagreeable restraints before cycle 19 Observed Target Error Sigma Restraint 0.0745 0.0200 SAME/SADI C13 C14 C25_a C26_a etc. 0.2512 0.0400 SAME/SADI C26_a P3_a C226_b P203_b etc. 0.1274 0.0400 SAME/SADI C1 O1 C25_a O3_a 0.1553 0.0400 SAME/SADI C13 C21 C25_a C33_a etc. Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 186. 0. 0. 0. 0. 318. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.000 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.051 0.000 0.000 0.000 0.000 0.011 0.000 0.000 GooF = S = 1.197; Restrained GooF = 1.198 for 504 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0056 * P )^2 + 27.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0830 for 9563 Fo > 4sig(Fo) and 0.1026 for all 11396 data wR2 = 0.1528, GooF = S = 1.197, Restrained GooF = 1.198 for all data Flack x parameter = 0.0408 with esd 0.0212 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 55.00 for non-hydrogen and 81.00 for hydrogen atoms Principal mean square atomic displacements U 0.0280 0.0225 0.0180 Ce1 0.0580 0.0276 0.0148 C1 0.0556 0.0366 0.0235 C2 0.0980 0.0633 0.0217 C3 0.0855 0.0541 0.0266 C4 0.0662 0.0271 0.0127 C5 0.0675 0.0336 0.0208 C6 0.0796 0.0672 0.0234 C7 0.1073 0.0571 0.0395 C8 0.0641 0.0395 0.0192 C9 0.0938 0.0495 0.0159 C10 0.1500 0.0456 0.0265 C11 0.0794 0.0711 0.0250 C12 0.0458 0.0315 0.0238 O1 0.0415 0.0255 0.0155 P1 0.0499 0.0401 0.0061 C13 0.0484 0.0291 0.0248 C14 0.1034 0.0620 0.0255 C15 0.0709 0.0475 0.0295 C16 0.0300 0.0262 0.0185 C17 0.0604 0.0343 0.0252 C18 0.0832 0.0513 0.0264 C19 0.1180 0.0441 0.0337 C20 0.0552 0.0342 0.0195 C21 0.0470 0.0325 0.0176 C22 0.0823 0.0379 0.0232 C23 0.0726 0.0531 0.0330 C24 0.0388 0.0267 0.0156 O2 0.0279 0.0260 0.0202 P2 0.1952 0.0808 0.0285 C25_a 0.1849 0.0877 0.0319 C26_a 0.1655 0.0979 0.0561 C27_a 0.1535 0.0736 0.0213 C28_a 0.0579 0.0458 0.0252 C29_a 0.0533 0.0510 0.0247 C30_a 0.0718 0.0509 0.0401 C31_a 0.0909 0.0575 0.0343 C32_a 0.0569 0.0463 0.0145 C33_a 0.0770 0.0576 0.0179 C34_a 0.1042 0.0631 0.0225 C35_a 0.0962 0.0695 0.0251 C36_a 0.0362 0.0293 0.0165 O3_a 0.0518 0.0260 0.0129 P3_a 0.1953 0.0815 0.0250 C225_b 0.1865 0.0862 0.0368 C226_b 0.1730 0.1035 0.0443 C227_b 0.1658 0.0616 0.0460 C228_b 0.0448 0.0352 0.0240 C229_b 0.0508 0.0381 0.0250 C230_b 0.0647 0.0504 0.0443 C231_b 0.0621 0.0551 0.0031 C232_b 0.0865 0.0674 0.0141 C233_b 0.0883 0.0719 0.0285 C234_b 0.1115 0.0746 0.0412 C235_b 0.0803 0.0659 0.0569 C236_b 0.0362 0.0293 0.0165 O203_b 0.0356 0.0225 0.0108 P203_b 0.0620 0.0269 0.0103 N11 0.0689 0.0286 0.0231 O11 0.0460 0.0408 0.0252 O12 0.1192 0.0300 0.0241 O13 0.0500 0.0270 0.0141 N21 0.0406 0.0306 0.0246 O21 0.0832 0.0687 0.0257 O22 0.0505 0.0371 0.0277 O23 0.0653 0.0315 0.0079 N31 0.0654 0.0373 0.0266 O31 0.0551 0.0270 0.0222 O32 0.0990 0.0532 0.0227 O33 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.040 0.059 0.075 0.092 0.110 0.128 0.150 0.184 0.242 1.000 Number in group 1144. 1160. 1113. 1146. 1200. 1097. 1115. 1147. 1135. 1139. GooF 1.690 1.388 1.260 1.182 1.114 0.979 1.050 0.945 0.940 1.205 K 4.615 1.845 1.380 1.213 1.111 1.073 1.043 0.995 0.985 0.988 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 1163. 1133. 1122. 1158. 1127. 1140. 1150. 1128. 1126. 1149. GooF 1.084 1.067 1.100 1.111 1.148 1.163 1.204 1.211 1.156 1.622 K 1.134 1.156 1.121 1.170 1.100 1.065 1.019 1.001 0.990 1.012 R1 0.231 0.199 0.164 0.157 0.129 0.105 0.079 0.063 0.049 0.039 Recommended weighting scheme: WGHT 0.0000 28.3812 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 0 2556.72 144.40 10.51 0.036 2.36 0 4 10 2068.31 407.85 8.12 0.061 2.00 0 1 3 6015.94 12665.92 7.16 0.339 6.99 0 3 6 4416.73 2084.57 6.84 0.138 3.08 0 8 0 2377.73 667.28 6.47 0.078 1.81 -1 3 10 2484.39 888.05 6.34 0.090 2.12 12 4 0 1817.43 9.14 6.31 0.009 1.14 2 4 0 1152.14 224.29 5.93 0.045 3.24 1 3 10 2635.16 1143.60 5.70 0.102 2.12 5 11 0 1359.00 72.19 5.37 0.026 1.20 -11 1 9 1764.55 274.91 5.33 0.050 1.17 14 1 0 2100.35 44.91 5.22 0.020 1.02 8 9 0 1454.72 260.31 5.18 0.049 1.20 1 3 1 15705.11 11760.71 4.89 0.327 4.50 2 0 4 4017.09 2339.39 4.86 0.146 4.60 11 1 9 1659.64 289.05 4.77 0.051 1.17 -1 3 1 13850.78 10317.97 4.73 0.306 4.50 -8 1 12 1238.72 223.55 4.69 0.045 1.33 14 5 9 1318.06 34.08 4.59 0.018 0.91 3 0 5 481.38 53.89 4.51 0.022 3.39 7 2 0 4393.41 2605.03 4.50 0.154 1.97 8 1 0 3460.95 1855.33 4.45 0.130 1.78 3 0 10 542.45 46.39 4.39 0.021 2.14 0 12 6 969.06 46.70 4.32 0.021 1.16 6 1 6 948.20 233.37 4.32 0.046 2.03 -4 7 16 803.94 117.86 4.27 0.033 1.15 5 1 0 1910.18 926.79 4.20 0.092 2.82 0 0 4 -6.17 430.23 4.16 0.063 5.99 0 1 5 2417.65 1347.65 4.12 0.111 4.55 -11 5 12 917.36 91.49 4.08 0.029 1.02 0 7 12 489.70 32.82 4.00 0.017 1.44 -7 6 9 1032.86 104.94 3.99 0.031 1.35 10 8 3 1391.38 414.67 3.94 0.061 1.12 -6 1 6 1150.81 330.90 3.94 0.055 2.03 0 6 7 912.05 268.10 3.92 0.049 1.97 2 0 5 1401.88 649.82 3.91 0.077 3.98 17 5 0 1547.31 36.67 3.91 0.018 0.81 -2 3 1 1826.29 935.14 3.87 0.092 3.96 -13 4 3 971.20 39.29 3.82 0.019 1.05 12 0 3 2285.22 421.10 3.81 0.062 1.18 2 1 0 3590.61 2257.72 3.80 0.143 6.44 -3 1 3 537.83 106.46 3.79 0.031 3.95 0 2 3 24850.88 20531.67 3.77 0.432 5.37 -10 3 4 1379.31 367.20 3.73 0.058 1.34 5 13 6 1388.37 464.88 3.72 0.065 1.01 14 5 3 1665.43 259.73 3.71 0.049 0.96 -1 8 18 629.96 54.68 3.71 0.022 1.07 3 1 3 568.06 112.24 3.66 0.032 3.95 10 8 0 1028.81 122.96 3.65 0.033 1.13 11 13 6 1285.88 192.69 3.60 0.042 0.83 Bond lengths and angles Ce1 - Distance Angles O3_a 2.3531 (0.0132) O1 2.3708 (0.0056) 89.04 (0.50) O2 2.4019 (0.0053) 83.62 (0.47) 151.47 (0.20) O203_b 2.4891 (0.0118) 7.64 (0.72) 84.91 (0.44) 90.27 (0.39) O31 2.5648 (0.0063) 78.88 (0.52) 127.24 (0.22) 78.31 (0.21) 76.51 (0.49) O32 2.5989 (0.0062) 78.03 (0.48) 77.82 (0.20) 126.88 (0.20) 70.89 (0.42) 49.49 (0.21) O21 2.6018 (0.0060) 123.60 (0.50) 76.44 (0.19) 84.79 (0.19) 128.32 (0.47) 150.24 (0.21) 145.65 (0.20) O11 2.6068 (0.0061) 147.37 (0.51) 121.95 (0.20) 73.34 (0.19) 148.65 (0.48) 74.13 (0.22) 97.45 (0.22) 77.65 (0.22) O23 2.6227 (0.0058) 74.53 (0.51) 77.37 (0.21) 74.10 (0.19) 79.94 (0.47) 143.35 (0.22) 142.99 (0.21) 49.23 (0.21) O12 2.6233 (0.0062) 152.90 (0.46) 74.10 (0.21) 121.04 (0.20) 145.30 (0.39) 94.38 (0.21) 77.76 (0.21) 73.58 (0.20) N31 2.9913 (0.0073) 74.21 (0.50) 102.19 (0.23) 102.23 (0.22) 68.96 (0.47) 25.10 (0.23) 24.75 (0.22) 161.81 (0.19) Ce1 - O3_a O1 O2 O203_b O31 O32 O21 C1 - Distance Angles C2 1.5010 (0.0108) P1 1.8175 (0.0077) 118.23 (0.62) H1A 0.9900 107.75 107.75 H1B 0.9900 107.75 107.75 107.12 C1 - C2 P1 H1A C2 - Distance Angles C1 1.5010 (0.0108) C4 1.5191 (0.0112) 114.11 (0.76) C3 1.5588 (0.0112) 109.42 (0.77) 110.74 (0.81) H2 1.0000 107.43 107.43 107.43 C2 - C1 C4 C3 C3 - Distance Angles C2 1.5588 (0.0112) H3A 0.9800 109.47 H3B 0.9800 109.47 109.47 H3C 0.9800 109.47 109.47 109.47 C3 - C2 H3A H3B C4 - Distance Angles C2 1.5191 (0.0112) H4A 0.9800 109.47 H4B 0.9800 109.47 109.47 H4C 0.9800 109.47 109.47 109.47 C4 - C2 H4A H4B C5 - Distance Angles C6 1.5302 (0.0103) P1 1.7952 (0.0082) 119.78 (0.68) H5A 0.9900 107.38 107.38 H5B 0.9900 107.38 107.38 106.93 C5 - C6 P1 H5A C6 - Distance Angles C8 1.5090 (0.0120) C7 1.5185 (0.0108) 107.97 (0.84) C5 1.5302 (0.0103) 111.24 (0.80) 113.85 (0.79) H6 1.0000 107.86 107.86 107.86 C6 - C8 C7 C5 C7 - Distance Angles C6 1.5185 (0.0108) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C6 H7A H7B C8 - Distance Angles C6 1.5090 (0.0120) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C6 H8A H8B C9 - Distance Angles C10 1.4992 (0.0114) P1 1.8226 (0.0085) 116.96 (0.73) H9A 0.9900 108.06 108.06 H9B 0.9900 108.06 108.06 107.28 C9 - C10 P1 H9A C10 - Distance Angles C9 1.4992 (0.0114) C12 1.5212 (0.0112) 112.33 (0.89) C11 1.5349 (0.0127) 109.30 (0.90) 109.07 (0.85) H10 1.0000 108.69 108.69 108.69 C10 - C9 C12 C11 C11 - Distance Angles C10 1.5349 (0.0127) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C10 H11A H11B C12 - Distance Angles C10 1.5212 (0.0113) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C10 H12A H12B O1 - Distance Angles P1 1.5091 (0.0058) Ce1 2.3708 (0.0056) 159.73 (0.37) O1 - P1 P1 - Distance Angles O1 1.5091 (0.0058) C5 1.7952 (0.0082) 110.28 (0.38) C1 1.8175 (0.0077) 111.51 (0.38) 107.50 (0.43) C9 1.8226 (0.0085) 109.15 (0.41) 108.29 (0.42) 110.05 (0.43) P1 - O1 C5 C1 C13 - Distance Angles C14 1.5074 (0.0104) P2 1.8062 (0.0078) 118.12 (0.65) H13A 0.9900 107.78 107.78 H13B 0.9900 107.78 107.78 107.13 C13 - C14 P2 H13A C14 - Distance Angles C13 1.5074 (0.0104) C16 1.5228 (0.0115) 113.28 (0.78) C15 1.5505 (0.0116) 110.13 (0.77) 110.60 (0.78) H14 1.0000 107.53 107.53 107.53 C14 - C13 C16 C15 C15 - Distance Angles C14 1.5505 (0.0116) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - C14 H15A H15B C16 - Distance Angles C14 1.5228 (0.0115) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - C14 H16A H16B C17 - Distance Angles C18 1.5496 (0.0100) P2 1.8028 (0.0070) 115.52 (0.58) H17A 0.9900 108.40 108.40 H17B 0.9900 108.40 108.40 107.46 C17 - C18 P2 H17A C18 - Distance Angles C19 1.5151 (0.0112) C20 1.5180 (0.0118) 110.71 (0.82) C17 1.5496 (0.0100) 109.00 (0.73) 111.63 (0.80) H18 1.0000 108.47 108.47 108.47 C18 - C19 C20 C17 C19 - Distance Angles C18 1.5151 (0.0112) H19A 0.9800 109.47 H19B 0.9800 109.47 109.47 H19C 0.9800 109.47 109.47 109.47 C19 - C18 H19A H19B C20 - Distance Angles C18 1.5180 (0.0118) H20A 0.9800 109.47 H20B 0.9800 109.47 109.47 H20C 0.9800 109.47 109.47 109.47 C20 - C18 H20A H20B C21 - Distance Angles C22 1.5001 (0.0105) P2 1.8235 (0.0076) 118.03 (0.65) H21A 0.9900 107.80 107.80 H21B 0.9900 107.80 107.80 107.14 C21 - C22 P2 H21A C22 - Distance Angles C24 1.4991 (0.0107) C21 1.5001 (0.0105) 110.44 (0.75) C23 1.5358 (0.0105) 109.58 (0.75) 112.02 (0.73) H22 1.0000 108.23 108.23 108.23 C22 - C24 C21 C23 C23 - Distance Angles C22 1.5358 (0.0105) H23A 0.9800 109.47 H23B 0.9800 109.47 109.47 H23C 0.9800 109.47 109.47 109.47 C23 - C22 H23A H23B C24 - Distance Angles C22 1.4991 (0.0107) H24A 0.9800 109.47 H24B 0.9800 109.47 109.47 H24C 0.9800 109.47 109.47 109.47 C24 - C22 H24A H24B O2 - Distance Angles P2 1.5074 (0.0055) Ce1 2.4019 (0.0053) 153.67 (0.33) O2 - P2 P2 - Distance Angles O2 1.5074 (0.0055) C17 1.8028 (0.0070) 109.57 (0.34) C13 1.8062 (0.0078) 111.49 (0.36) 110.07 (0.40) C21 1.8235 (0.0076) 111.54 (0.39) 110.24 (0.38) 103.81 (0.41) P2 - O2 C17 C13 C25_a - Distance Angles C26_a 1.4329 (0.0158) P3_a 1.8156 (0.0128) 141.15 (1.95) H25A_a 0.9900 101.73 101.73 H25B_a 0.9900 101.72 101.72 104.67 C25_a - C26_a P3_a H25A_a C26_a - Distance Angles C25_a 1.4329 (0.0158) C28_a 1.5073 (0.0170) 119.57 (1.97) C27_a 1.5929 (0.0172) 108.26 (1.87) 109.92 (1.80) H26_a 1.0000 106.08 106.08 106.07 C26_a - C25_a C28_a C27_a C27_a - Distance Angles C26_a 1.5929 (0.0172) H27A_a 0.9800 109.47 H27B_a 0.9800 109.47 109.47 H27C_a 0.9800 109.47 109.47 109.47 C27_a - C26_a H27A_a H27B_a C28_a - Distance Angles C26_a 1.5073 (0.0170) H28A_a 0.9800 109.47 H28B_a 0.9800 109.47 109.47 H28C_a 0.9800 109.47 109.47 109.47 C28_a - C26_a H28A_a H28B_a C29_a - Distance Angles C30_a 1.5384 (0.0152) P3_a 1.7925 (0.0129) 124.22 (1.22) H29A_a 0.9900 106.27 106.27 H29B_a 0.9900 106.27 106.27 106.40 C29_a - C30_a P3_a H29A_a C30_a - Distance Angles C32_a 1.5040 (0.0160) C31_a 1.5299 (0.0159) 110.14 (1.60) C29_a 1.5384 (0.0153) 110.25 (1.44) 107.70 (1.51) H30_a 1.0000 109.57 109.57 109.57 C30_a - C32_a C31_a C29_a C31_a - Distance Angles C30_a 1.5299 (0.0158) H31A_a 0.9800 109.47 H31B_a 0.9800 109.47 109.47 H31C_a 0.9800 109.47 109.47 109.47 C31_a - C30_a H31A_a H31B_a C32_a - Distance Angles C30_a 1.5040 (0.0160) H32A_a 0.9800 109.47 H32B_a 0.9800 109.47 109.47 H32C_a 0.9800 109.47 109.47 109.47 C32_a - C30_a H32A_a H32B_a C33_a - Distance Angles C34_a 1.5047 (0.0157) P3_a 1.8192 (0.0122) 115.51 (1.13) H33A_a 0.9900 108.40 108.40 H33B_a 0.9900 108.40 108.40 107.46 C33_a - C34_a P3_a H33A_a C34_a - Distance Angles C36_a 1.4725 (0.0166) C33_a 1.5047 (0.0157) 112.37 (1.61) C35_a 1.5515 (0.0171) 104.90 (1.70) 107.19 (1.55) H34_a 1.0000 110.73 110.73 110.73 C34_a - C36_a C33_a C35_a C35_a - Distance Angles C34_a 1.5515 (0.0171) H35A_a 0.9800 109.47 H35B_a 0.9800 109.47 109.47 H35C_a 0.9800 109.47 109.47 109.47 C35_a - C34_a H35A_a H35B_a C36_a - Distance Angles C34_a 1.4725 (0.0166) H36A_a 0.9800 109.47 H36B_a 0.9800 109.47 109.47 H36C_a 0.9800 109.47 109.47 109.47 C36_a - C34_a H36A_a H36B_a O3_a - Distance Angles P3_a 1.5094 (0.0106) Ce1 2.3531 (0.0132) 153.85 (1.32) O3_a - P3_a P3_a - Distance Angles O3_a 1.5094 (0.0106) C29_a 1.7925 (0.0129) 106.28 (0.95) C33_a 1.8192 (0.0123) 113.87 (0.91) 108.45 (0.77) C25_a 1.8156 (0.0128) 104.06 (1.11) 112.15 (1.17) 111.92 (1.05) P3_a - O3_a C29_a C33_a C225_b - Distance Angles C226_b 1.4607 (0.0161) P203_b 1.8490 (0.0133) 116.04 (1.57) H22A_b 0.9900 108.27 108.27 H22B_b 0.9900 108.28 108.28 107.39 C225_b - C226_b P203_b H22A_b C226_b - Distance Angles C225_b 1.4607 (0.0161) C228_b 1.4654 (0.0164) 119.34 (1.92) C227_b 1.5745 (0.0167) 111.29 (1.81) 116.75 (1.76) H226_b 1.0000 101.98 101.98 101.98 C226_b - C225_b C228_b C227_b C227_b - Distance Angles C226_b 1.5745 (0.0167) H22C_b 0.9800 109.47 H22D_b 0.9800 109.47 109.47 H22E_b 0.9800 109.47 109.47 109.47 C227_b - C226_b H22C_b H22D_b C228_b - Distance Angles C226_b 1.4654 (0.0164) H22F_b 0.9800 109.47 H22G_b 0.9800 109.47 109.47 H22H_b 0.9800 109.47 109.47 109.47 C228_b - C226_b H22F_b H22G_b C229_b - Distance Angles C230_b 1.5363 (0.0146) P203_b 1.7872 (0.0117) 122.09 (1.05) H22I_b 0.9900 106.81 106.81 H22J_b 0.9900 106.81 106.81 106.65 C229_b - C230_b P203_b H22I_b C230_b - Distance Angles C232_b 1.5094 (0.0155) C231_b 1.5104 (0.0154) 109.69 (1.47) C229_b 1.5363 (0.0146) 108.74 (1.24) 111.43 (1.52) H230_b 1.0000 108.98 108.98 108.98 C230_b - C232_b C231_b C229_b C231_b - Distance Angles C230_b 1.5104 (0.0155) H23D_b 0.9800 109.47 H23E_b 0.9800 109.47 109.47 H23F_b 0.9800 109.47 109.47 109.47 C231_b - C230_b H23D_b H23E_b C232_b - Distance Angles C230_b 1.5094 (0.0155) H23G_b 0.9800 109.47 H23H_b 0.9800 109.47 109.47 H23I_b 0.9800 109.47 109.47 109.47 C232_b - C230_b H23G_b H23H_b C233_b - Distance Angles C234_b 1.4993 (0.0163) P203_b 1.8668 (0.0126) 115.07 (1.23) H23J_b 0.9900 108.50 108.50 H23K_b 0.9900 108.50 108.50 107.51 C233_b - C234_b P203_b H23J_b C234_b - Distance Angles C236_b 1.4709 (0.0162) C233_b 1.4993 (0.0162) 112.31 (1.73) C235_b 1.5480 (0.0166) 106.17 (1.62) 107.88 (1.77) H234_b 1.0000 110.12 110.12 110.12 C234_b - C236_b C233_b C235_b C235_b - Distance Angles C234_b 1.5480 (0.0166) H23L_b 0.9800 109.47 H23M_b 0.9800 109.47 109.47 H23N_b 0.9800 109.47 109.47 109.47 C235_b - C234_b H23L_b H23M_b C236_b - Distance Angles C234_b 1.4709 (0.0162) H23O_b 0.9800 109.47 H23P_b 0.9800 109.47 109.47 H23Q_b 0.9800 109.47 109.47 109.47 C236_b - C234_b H23O_b H23P_b O203_b - Distance Angles P203_b 1.4671 (0.0103) Ce1 2.4891 (0.0118) 173.05 (1.28) O203_b - P203_b P203_b - Distance Angles O203_b 1.4671 (0.0103) C229_b 1.7872 (0.0117) 113.98 (0.95) C225_b 1.8490 (0.0133) 109.93 (0.98) 109.85 (1.09) C233_b 1.8668 (0.0126) 113.67 (0.91) 106.22 (0.81) 102.53 (0.97) P203_b - O203_b C229_b C225_b N11 - Distance Angles O13 1.2279 (0.0091) O11 1.2631 (0.0092) 119.77 (0.80) O12 1.2716 (0.0095) 122.78 (0.78) 117.44 (0.69) N11 - O13 O11 O11 - Distance Angles N11 1.2631 (0.0092) Ce1 2.6068 (0.0061) 97.25 (0.50) O11 - N11 O12 - Distance Angles N11 1.2716 (0.0096) Ce1 2.6233 (0.0062) 96.22 (0.48) O12 - N11 O13 - Distance Angles N11 1.2279 (0.0091) O13 - N21 - Distance Angles O22 1.2132 (0.0094) O21 1.2786 (0.0089) 121.13 (0.81) O23 1.2986 (0.0105) 123.62 (0.78) 115.21 (0.71) N21 - O22 O21 O21 - Distance Angles N21 1.2786 (0.0089) Ce1 2.6018 (0.0060) 98.50 (0.50) O21 - N21 O22 - Distance Angles N21 1.2132 (0.0094) O22 - O23 - Distance Angles N21 1.2986 (0.0105) Ce1 2.6227 (0.0058) 96.94 (0.47) O23 - N21 N31 - Distance Angles O33 1.2366 (0.0095) O32 1.2577 (0.0096) 121.57 (0.95) O31 1.2769 (0.0110) 121.28 (0.88) 117.05 (0.71) Ce1 2.9913 (0.0073) 166.16 (0.58) 59.88 (0.42) 58.42 (0.40) N31 - O33 O32 O31 O31 - Distance Angles N31 1.2769 (0.0110) Ce1 2.5648 (0.0063) 96.48 (0.48) O31 - N31 O32 - Distance Angles N31 1.2577 (0.0097) Ce1 2.5989 (0.0062) 95.37 (0.52) O32 - N31 O33 - Distance Angles N31 1.2366 (0.0095) O33 - FMAP and GRID set by program FMAP 2 3 28 GRID -1.000 -2 -2 1.000 2 2 R1 = 0.0963 for 6284 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.56 at 0.6797 0.9468 0.0456 [ 0.92 A from CE1 ] Deepest hole -2.53 at 0.8189 0.0593 0.2481 [ 0.66 A from H25A ] Mean = 0.00, Rms deviation from mean = 0.14 e/A^3, Highest memory used = 9273 / 39814 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6797 0.9468 0.0456 1.00000 0.05 1.56 0.92 CE1 1.92 O21 1.99 O12 2.23 O11 Q2 1 0.7835 1.2048 0.2198 1.00000 0.05 1.21 1.06 H22B 1.49 H25B 1.80 H28C 1.87 C225 Q3 1 0.6758 0.9417 0.1242 1.00000 0.05 1.16 0.96 CE1 1.50 O3 1.62 O203 2.20 O31 Q4 1 0.7100 1.1810 0.2619 1.00000 0.05 1.08 0.88 H25B 0.90 H22B 1.01 C225 1.18 C25 Q5 1 0.8619 1.0564 0.2432 1.00000 0.05 0.99 1.20 H25A 1.32 H22A 1.50 H16C 1.89 C16 Q6 1 0.5374 0.8222 0.2488 1.00000 0.05 0.98 1.32 H33A 1.48 H22J 1.68 O33 2.01 H234 Q7 1 0.7737 1.0505 0.2488 1.00000 0.05 0.83 0.67 H25A 0.72 H22A 1.09 C25 1.19 C225 Q8 1 0.5998 0.9408 0.0823 1.00000 0.05 0.82 1.15 CE1 1.73 O1 1.81 O32 2.31 O12 Q9 1 0.6842 0.9435 0.4266 1.00000 0.05 0.81 1.53 H31B 1.90 H23E 2.02 O21 2.04 H24A Q10 1 0.4220 0.9403 0.2404 1.00000 0.05 0.79 0.67 H234 1.05 C234 1.10 H35A 1.62 H36C Shortest distances between peaks (including symmetry equivalents) 5 7 1.28 1 8 1.45 3 8 1.48 2 4 1.50 1 3 1.88 4 7 2.13 2 7 2.35 6 10 2.39 2 5 2.49 4 5 2.87 Time profile in seconds ----------------------- 0.17: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.03: Generate connectivity array 0.03: 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 0.03: Analyse other restraints etc. 8.77: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.08: Set up l.s. refinement 0.02: Generate idealized H-atoms 57.49: Structure factors and derivatives 97.97: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.80: Apply other restraints 10.36: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.20: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.22: Fourier summations 0.09: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src1089 finished at 13:57:15 Total CPU time: 176.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++