+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0837r started at 10:35:51 on 18-Jan-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0837r in P2(1) CELL 0.71073 10.4088 14.7524 18.2275 90.000 94.741 90.000 ZERR 2.00 0.0004 0.0008 0.0008 0.000 0.003 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O NA S CR UNIT 76 54 2 24 2 48 2 V = 2789.34 F(000) = 1554.0 Mu = 1.17 mm-1 Cell Wt = 3068.07 Rho = 1.826 MERG 2 OMIT -3.00 50.00 TWIN BASF 0.27450 SHEL 7 0.84 sadi c1 c2 c201 c202 c11 c12 c211 c212 c19 c20 c219 c220 sadi c1 s1 c2 s2 c201 s1 c202 s2 sadi c11 s11 c12 s12 c211 s11 c212 s12 sadi c19 s17 c20 s18 c219 s17 c220 s18 simu 0.03 isor 0.01 $c isor 0.005 c12 eqiv $1 -x, y+1/2, -z eqiv $2 x-1, y, z EQIV $3 x+1, y, z EQIV $4 -x, y-1/2, -z FREE NA1 C31 FREE NA1 C32 FREE NA1 C41_$1 FREE NA1 C42_$1 FREE NA1 C51_$2 FREE NA1 C52_$2 FREE C41 NA1_$4 FREE C42 NA1_$4 FREE C51 NA1_$3 FREE C52 NA1_$3 FMAP 2 PLAN 5 SIZE 0.01 0.06 0.08 ACTA BOND $H WGHT 0.05290 33.31150 L.S. 29 TEMP -153.00 FVAR 0.24687 0.46791 0.68259 0.47779 NA1 5 -0.201351 0.691868 0.007285 11.00000 0.02366 0.02266 = 0.00582 0.00101 0.00130 0.00523 CR1 7 0.304592 0.560121 0.004231 11.00000 0.03751 0.04075 = 0.02544 -0.00180 -0.00566 0.00014 MOLE 1 PART 1 C1 1 -0.002241 0.773639 0.208062 21.00000 0.04651 0.03867 = 0.03259 -0.00264 -0.00918 0.00932 AFIX 23 H1A 2 -0.031424 0.833705 0.224312 21.00000 -1.20000 H1B 2 0.005145 0.777448 0.154348 21.00000 -1.20000 AFIX 0 C2 1 -0.105548 0.705849 0.220965 21.00000 0.03080 0.02384 = 0.01924 -0.00623 -0.00744 -0.00140 AFIX 23 H2A 2 -0.074425 0.644582 0.209113 21.00000 -1.20000 H2B 2 -0.182311 0.719006 0.186877 21.00000 -1.20000 AFIX 0 PART 2 C201 1 0.011907 0.725987 0.196847 -21.00000 0.03008 0.01323 = 0.01317 -0.00788 -0.00681 0.00655 AFIX 23 H20A 2 0.014433 0.754037 0.147646 -21.00000 -1.20000 H20B 2 0.006716 0.659444 0.190221 -21.00000 -1.20000 AFIX 0 C202 1 -0.104869 0.758551 0.231529 -21.00000 0.04992 0.03475 = 0.04009 0.00317 -0.01016 0.00894 AFIX 23 H20C 2 -0.178738 0.754081 0.193843 -21.00000 -1.20000 H20D 2 -0.091976 0.823777 0.242589 -21.00000 -1.20000 AFIX 0 PART 0 C3 1 -0.005593 0.722778 0.365910 11.00000 0.04558 0.05490 = 0.03402 -0.00626 0.01414 0.01299 C4 1 0.112817 0.740643 0.342271 11.00000 0.04453 0.05112 = 0.03389 0.01357 -0.00592 0.00122 C5 1 0.149750 0.735543 0.483726 11.00000 0.03971 0.05723 = 0.02462 -0.00022 -0.00097 0.00749 C6 1 0.205068 0.729774 0.557363 11.00000 0.03025 0.04449 = 0.00665 0.00969 -0.00345 0.00431 C7 1 0.364755 0.731860 0.668593 11.00000 0.02332 0.03715 = 0.01288 0.00057 0.00245 0.00456 C8 1 0.246850 0.712920 0.697858 11.00000 0.02350 0.04117 = 0.03185 0.00585 -0.00156 0.01159 C9 1 0.356515 0.750628 0.832381 11.00000 0.04431 0.02855 = 0.02863 -0.00690 0.00335 0.00003 AFIX 23 H9A 2 0.355746 0.816311 0.821221 11.00000 -1.20000 H9B 2 0.353801 0.744037 0.886282 11.00000 -1.20000 AFIX 0 C10 1 0.481629 0.711493 0.811059 11.00000 0.03313 0.04551 = 0.02502 -0.00197 -0.01277 -0.01042 AFIX 23 H10A 2 0.478842 0.644720 0.816105 11.00000 -1.20000 H10B 2 0.552896 0.734285 0.845483 11.00000 -1.20000 AFIX 0 S1 6 0.154511 0.753565 0.251675 11.00000 0.04221 0.06024 = 0.03185 0.01166 -0.00920 -0.00668 S2 6 -0.152287 0.705591 0.313282 11.00000 0.02542 0.06289 = 0.03509 -0.01173 -0.01199 0.00592 S3 6 -0.015211 0.711685 0.460545 11.00000 0.03583 0.07212 = 0.02202 -0.00399 -0.00801 0.00863 S4 6 0.239858 0.749075 0.410112 11.00000 0.03425 0.05736 = 0.02415 0.00395 -0.00501 -0.00173 S5 6 0.366555 0.745257 0.575640 11.00000 0.03813 0.06343 = 0.02881 0.00539 -0.00235 0.00378 S6 6 0.114409 0.711247 0.630356 11.00000 0.03598 0.06168 = 0.02575 -0.00648 -0.00616 0.01109 S7 6 0.211490 0.700450 0.787673 11.00000 0.02863 0.05657 = 0.02412 -0.00972 -0.00005 0.00113 S8 6 0.514741 0.739511 0.718431 11.00000 0.02946 0.06861 = 0.02025 0.00010 -0.00894 0.00030 MOLE 2 PART 1 C11 1 0.597291 0.052693 0.779153 31.00000 0.04280 0.02954 = 0.02700 -0.00488 -0.00728 0.00706 AFIX 23 H11A 2 0.675231 0.042833 0.813145 31.00000 -1.20000 H11B 2 0.564623 0.114459 0.787872 31.00000 -1.20000 AFIX 0 C12 1 0.496004 -0.015856 0.794928 31.00000 0.03520 0.02143 = 0.00965 -0.00745 -0.01549 -0.00239 AFIX 23 H12A 2 0.488206 -0.016437 0.848690 31.00000 -1.20000 H12B 2 0.526973 -0.076493 0.781198 31.00000 -1.20000 AFIX 0 PART 2 C211 1 0.605070 -0.007969 0.772215 -31.00000 0.03023 0.02294 = 0.02647 0.00208 -0.00322 0.00356 AFIX 23 H21A 2 0.588306 -0.073700 0.766055 -31.00000 -1.20000 H21B 2 0.678120 0.000730 0.809899 -31.00000 -1.20000 AFIX 0 C212 1 0.487110 0.040461 0.793664 -31.00000 0.03407 0.02433 = 0.02336 -0.00099 -0.00818 0.00835 AFIX 23 H21C 2 0.496238 0.105738 0.782615 -31.00000 -1.20000 H21D 2 0.483448 0.034523 0.847551 -31.00000 -1.20000 AFIX 0 PART 0 C13 1 0.375512 0.014655 0.658527 11.00000 0.03181 0.04319 = 0.01479 -0.00653 0.00003 0.01087 C14 1 0.490256 0.033779 0.634748 11.00000 0.03898 0.04671 = 0.01077 0.00487 -0.00430 0.01301 C15 1 0.339014 0.023133 0.517908 11.00000 0.03498 0.05053 = 0.02829 0.00609 -0.00350 0.01050 C16 1 0.281370 0.019664 0.447797 11.00000 0.04481 0.05155 = 0.04043 -0.00582 -0.00114 0.00216 C17 1 0.239201 0.029830 0.307006 11.00000 0.03961 0.03686 = 0.02437 -0.00605 -0.00923 -0.00137 C18 1 0.126770 0.018416 0.327648 11.00000 0.03536 0.04147 = 0.03512 -0.00407 -0.00554 0.00347 PART 1 C19 1 0.026486 0.049433 0.189647 41.00000 0.02553 0.02154 = 0.01310 0.00749 0.00207 -0.00169 AFIX 23 H19A 2 -0.046764 0.039866 0.152245 41.00000 -1.20000 H19B 2 0.042592 0.115512 0.192789 41.00000 -1.20000 AFIX 0 C20 1 0.143254 0.005098 0.162610 41.00000 0.03024 0.02668 = 0.02468 0.00009 0.00166 -0.00033 AFIX 23 H20E 2 0.147671 0.017928 0.109565 41.00000 -1.20000 H20F 2 0.138477 -0.061391 0.169220 41.00000 -1.20000 AFIX 0 PART 2 C219 1 0.025911 -0.008657 0.186443 -41.00000 0.02773 0.02567 = 0.01921 -0.00049 0.00060 -0.00788 AFIX 23 H21E 2 0.061968 -0.070537 0.183599 -41.00000 -1.20000 H21F 2 -0.050323 -0.004363 0.150354 -41.00000 -1.20000 AFIX 0 C220 1 0.124774 0.059231 0.167756 -41.00000 0.02066 0.02206 = 0.02440 0.00166 -0.01244 0.00114 AFIX 23 H22A 2 0.091248 0.120368 0.177903 -41.00000 -1.20000 H22B 2 0.133291 0.055570 0.114142 -41.00000 -1.20000 AFIX 0 PART 0 S11 6 0.639474 0.043761 0.684890 11.00000 0.03286 0.07811 = 0.02499 0.00100 -0.00859 0.01828 S12 6 0.335540 0.000908 0.748778 11.00000 0.03529 0.15041 = 0.01084 0.00776 -0.00303 0.01181 S13 6 0.244872 0.001930 0.591497 11.00000 0.03845 0.09493 = 0.01383 0.00202 -0.00843 -0.00104 S14 6 0.499696 0.034118 0.539664 11.00000 0.02780 0.08922 = 0.02018 0.00405 -0.00165 0.01212 S15 6 0.372814 0.035868 0.371781 11.00000 0.01948 0.09472 = 0.01591 0.00713 -0.00426 0.00470 S16 6 0.119850 0.005475 0.423813 11.00000 0.02824 0.08962 = 0.01346 0.00350 -0.00147 0.00202 S17 6 -0.022420 0.011402 0.278174 11.00000 0.02863 0.06704 = 0.02415 0.00107 0.00034 -0.00090 S18 6 0.284803 0.049525 0.214720 11.00000 0.03196 0.05014 = 0.01756 0.00508 -0.00439 0.00997 MOLE 3 C21 1 1.019257 0.917872 0.798466 11.00000 0.03653 0.04259 = 0.02739 0.00489 -0.00624 -0.00524 AFIX 23 H21G 2 1.084591 0.872032 0.787727 11.00000 -1.20000 H21H 2 1.055698 0.954911 0.840451 11.00000 -1.20000 AFIX 0 C22 1 0.900922 0.870034 0.820425 11.00000 0.04278 0.06042 = 0.04391 -0.00142 0.00373 0.00692 AFIX 23 H22C 2 0.832117 0.915355 0.825616 11.00000 -1.20000 H22D 2 0.920943 0.841246 0.869091 11.00000 -1.20000 AFIX 0 C23 1 0.846693 0.844701 0.670132 11.00000 0.02974 0.03625 = 0.03614 0.00218 -0.01010 0.00267 C24 1 0.896949 0.921155 0.659930 11.00000 0.03686 0.03227 = 0.03263 -0.00052 -0.00227 -0.00244 C25 1 0.779234 0.872359 0.535295 11.00000 0.03065 0.04838 = 0.03217 -0.00543 0.01549 -0.00910 C26 1 0.720027 0.874096 0.466600 11.00000 0.02855 0.05257 = 0.03819 -0.00297 0.00191 -0.00175 C27 1 0.651537 0.914802 0.327405 11.00000 0.03267 0.04617 = 0.03400 -0.00157 0.01067 0.00155 C28 1 0.588497 0.834444 0.346267 11.00000 0.03580 0.04276 = 0.03131 -0.00009 0.00395 0.00371 C29 1 0.465745 0.835031 0.204524 11.00000 0.05113 0.04818 = 0.03902 -0.00537 -0.00779 -0.00441 AFIX 23 H29A 2 0.430664 0.797177 0.162708 11.00000 -1.20000 H29B 2 0.398215 0.879200 0.215303 11.00000 -1.20000 AFIX 0 C30 1 0.580071 0.886135 0.181388 11.00000 0.03919 0.04344 = 0.03407 0.00170 0.00330 0.00809 AFIX 23 H30A 2 0.555810 0.915614 0.133444 11.00000 -1.20000 H30B 2 0.649837 0.842319 0.173909 11.00000 -1.20000 AFIX 0 S21 6 0.988546 0.991039 0.718264 11.00000 0.05153 0.04142 = 0.04071 0.00465 -0.00866 -0.01689 S22 6 0.841439 0.784351 0.755292 11.00000 0.04911 0.06138 = 0.04330 0.01199 -0.01904 -0.01511 S23 6 0.750090 0.789416 0.597742 11.00000 0.05397 0.05921 = 0.03786 -0.00331 0.00610 -0.02481 S24 6 0.882020 0.961637 0.567002 11.00000 0.05995 0.07011 = 0.02159 0.00131 0.00573 -0.02253 S25 6 0.742776 0.963611 0.401872 11.00000 0.05006 0.06463 = 0.02716 -0.00266 0.00350 -0.01148 S26 6 0.612125 0.790295 0.432982 11.00000 0.04904 0.06964 = 0.03771 0.00170 0.00390 -0.02267 S27 6 0.498332 0.763080 0.283811 11.00000 0.06600 0.06823 = 0.04710 0.01131 -0.02371 -0.01732 S28 6 0.642051 0.971627 0.245856 11.00000 0.04402 0.05117 = 0.04803 0.02415 -0.01796 -0.01518 MOLE 4 C31 1 0.089926 0.659955 -0.026373 11.00000 0.03754 0.02443 = 0.03913 -0.00239 -0.00097 0.00616 C32 1 0.064431 0.600480 0.046078 11.00000 0.04115 0.04170 = 0.03115 -0.00936 0.00452 -0.00721 O31 4 0.199351 0.658961 -0.041571 11.00000 0.06502 0.02913 = 0.04123 0.00589 0.00157 -0.00674 O32 4 0.162755 0.560439 0.073432 11.00000 0.05738 0.07473 = 0.02327 0.01374 -0.01461 -0.01228 O33 4 -0.044183 0.598612 0.067216 11.00000 0.06172 0.07050 = 0.05661 0.00370 -0.00283 -0.00877 O34 4 -0.003623 0.705173 -0.051592 11.00000 0.05439 0.04078 = 0.05133 0.00525 -0.00033 0.00406 MOLE 5 C41 1 0.211190 0.394127 -0.038388 11.00000 0.01709 0.02376 = 0.00899 0.00088 0.00225 -0.01040 C42 1 0.311414 0.375223 0.027076 11.00000 0.03955 0.04555 = 0.03233 -0.00035 0.00315 -0.00089 O41 4 0.202459 0.471396 -0.059627 11.00000 0.03528 0.05203 = 0.01670 -0.00667 -0.01326 0.00469 O42 4 0.372636 0.448822 0.051005 11.00000 0.03910 0.05922 = 0.02293 0.00378 -0.01777 0.00381 O43 4 0.323964 0.300068 0.057697 11.00000 0.06892 0.04108 = 0.03677 0.01400 -0.02528 -0.00116 O44 4 0.153849 0.326882 -0.065522 11.00000 0.05044 0.04104 = 0.03671 0.00949 -0.01655 0.00415 MOLE 6 C51 1 0.550698 0.591899 -0.026694 11.00000 0.03436 0.03633 = 0.01344 0.01013 0.00372 -0.00581 C52 1 0.539501 0.642377 0.047075 11.00000 0.04062 0.04332 = 0.03841 0.00181 0.00105 0.00422 O51 4 0.447101 0.565507 -0.060781 11.00000 0.03274 0.03621 = 0.01452 -0.00442 -0.00316 -0.01010 O52 4 0.422027 0.639159 0.067139 11.00000 0.03070 0.04639 = 0.01682 -0.01559 -0.00239 0.00826 O53 4 0.635116 0.675340 0.081397 11.00000 0.03913 0.08401 = 0.03700 -0.03062 -0.01441 0.00524 O54 4 0.661837 0.590109 -0.052445 11.00000 0.03946 0.04971 = 0.01834 0.00545 0.00939 -0.00250 MOLE 7 C61 1 0.215796 0.858768 0.037717 11.00000 0.07069 0.07973 = 0.07605 0.00398 0.00661 -0.01193 C62 1 0.229356 0.900129 -0.030565 11.00000 0.09874 0.08564 = 0.08870 -0.00275 -0.00905 -0.00198 AFIX 137 H62A 2 0.174189 0.869141 -0.068890 11.00000 -1.50000 H62B 2 0.319460 0.896166 -0.042153 11.00000 -1.50000 H62C 2 0.203885 0.963958 -0.028323 11.00000 -1.50000 AFIX 0 N61 3 0.197173 0.825836 0.092598 11.00000 0.07626 0.13391 = 0.06362 0.03213 -0.00880 -0.03844 HKLF 4 Covalent radii and connectivity table for 2009src0837r in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 NA 1.860 S 1.030 CR 1.240 Na1 - O53_$2 O54_$2 O44_$1 O43_$1 O33 O34 Cr1 - O42 O31 O51 O52 O41 O32 C1_a - C2_a S1 C2_a - C1_a S2 C201_b - C202_b S1 C202_b - C201_b S2 C3 - C4 S3 S2 C4 - C3 S4 S1 C5 - C6 S4 S3 C6 - C5 S5 S6 C7 - C8 S5 S8 C8 - C7 S7 S6 C9 - C10 S7 C10 - C9 S8 S1 - C4 C201_b C1_a S2 - C3 C202_b C2_a S3 - C3 C5 S4 - C5 C4 S5 - C6 C7 S6 - C6 C8 S7 - C8 C9 S8 - C7 C10 C11_a - C12_a S11 C12_a - C11_a S12 C211_b - C212_b S11 C212_b - C211_b S12 C13 - C14 S12 S13 C14 - C13 S11 S14 C15 - C16 S14 S13 C16 - C15 S16 S15 C17 - C18 S15 S18 C18 - C17 S17 S16 C19_a - C20_a S17 C20_a - C19_a S18 C219_b - C220_b S17 C220_b - C219_b S18 S11 - C14 C11_a C211_b S12 - C13 C212_b C12_a S13 - C15 C13 S14 - C15 C14 S15 - C17 C16 S16 - C16 C18 S17 - C18 C219_b C19_a S18 - C20_a C17 C220_b C21 - C22 S21 C22 - C21 S22 C23 - C24 S23 S22 C24 - C23 S21 S24 C25 - C26 S23 S24 C26 - C25 S26 S25 C27 - C28 S28 S25 C28 - C27 S26 S27 C29 - C30 S27 C30 - C29 S28 S21 - C24 C21 S22 - C23 C22 S23 - C25 C23 S24 - C25 C24 S25 - C27 C26 S26 - C28 C26 S27 - C28 C29 S28 - C27 C30 C31 - O31 O34 C32 C32 - O33 O32 C31 O31 - C31 Cr1 O32 - C32 Cr1 O33 - C32 Na1 O34 - C31 Na1 C41 - O41 O44 C42 C42 - O43 O42 C41 O41 - C41 Cr1 O42 - C42 Cr1 O43 - C42 Na1_$4 O44 - C41 Na1_$4 C51 - O51 O54 C52 C52 - O53 O52 C51 O51 - C51 Cr1 O52 - C52 Cr1 O53 - C52 Na1_$3 O54 - C51 Na1_$3 C61 - N61 C62 C62 - C61 N61 - C61 Operators for generating equivalent atoms: $1 -x, y+1/2, -z $2 x-1, y, z $3 x+1, y, z $4 -x, y-1/2, -z Floating origin restraints generated 25739 Reflections read, of which 4019 rejected -12 =< h =< 12, -17 =< k =< 17, -21 =< l =< 21, Max. 2-theta = 50.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -9 -9 5 1.95 3.25 2 17.36 -4 2 7 40.42 3.71 6 20.66 -7 -3 13 5.94 1.43 3 11.87 3 Inconsistent equivalents 9280 Unique reflections, of which 0 suppressed R(int) = 0.0821 R(sigma) = 0.1248 Friedel opposites not merged Maximum memory for data reduction = 6503 / 93153 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 = 8486 / 1081014 wR2 = 0.2396 before cycle 1 for 9280 data and 753 / 753 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.0174 0.0050 ISOR U13 C12_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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.009 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.089; Restrained GooF = 1.065 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.005 OSF 2 0.46748 0.03184 -0.014 FVAR 2 3 0.68130 0.02780 -0.046 FVAR 3 4 0.47810 0.02544 0.012 FVAR 4 5 0.27452 0.08191 0.000 BASF 1 Mean shift/esd = 0.022 Maximum = 1.961 for U13 C12_a Max. shift = 0.007 A for H21A_b Max. dU =-0.002 for C12_a Least-squares cycle 2 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 2 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.089; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 -0.002 OSF 2 0.46959 0.03187 0.066 FVAR 2 3 0.67811 0.02762 -0.115 FVAR 3 4 0.47789 0.02547 -0.008 FVAR 4 5 0.27505 0.08183 0.006 BASF 1 Mean shift/esd = 0.015 Maximum = 0.649 for U13 C12_a Max. shift = 0.005 A for H1B_a Max. dU = 0.001 for C12_a Least-squares cycle 3 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 3 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.089; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.002 OSF 2 0.47089 0.03193 0.041 FVAR 2 3 0.67764 0.02770 -0.017 FVAR 3 4 0.47779 0.02549 -0.004 FVAR 4 5 0.27545 0.08183 0.005 BASF 1 Mean shift/esd = 0.009 Maximum = 0.191 for U22 C12_a Max. shift = 0.002 A for H21A_b Max. dU = 0.001 for C12_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 4 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 -0.001 OSF 2 0.47098 0.03194 0.003 FVAR 2 3 0.67775 0.02780 0.004 FVAR 3 4 0.47777 0.02550 -0.001 FVAR 4 5 0.27553 0.08183 0.001 BASF 1 Mean shift/esd = 0.004 Maximum = 0.077 for U11 C12_a Max. shift = 0.002 A for H21A_b Max. dU = 0.000 for C12_a Least-squares cycle 5 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 5 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.089; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 -0.001 OSF 2 0.47108 0.03195 0.003 FVAR 2 3 0.67794 0.02783 0.007 FVAR 3 4 0.47777 0.02550 0.000 FVAR 4 5 0.27557 0.08182 0.000 BASF 1 Mean shift/esd = 0.003 Maximum = 0.024 for U33 C12_a Max. shift = 0.001 A for C211_b Max. dU = 0.000 for C211_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 6 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.089; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 -0.002 OSF 2 0.47108 0.03195 0.000 FVAR 2 3 0.67801 0.02785 0.003 FVAR 3 4 0.47777 0.02551 0.000 FVAR 4 5 0.27557 0.08182 0.000 BASF 1 Mean shift/esd = 0.002 Maximum = -0.014 for U22 S22 Max. shift = 0.001 A for C211_b Max. dU = 0.000 for C12_a Least-squares cycle 7 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 7 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47106 0.03195 -0.001 FVAR 2 3 0.67807 0.02786 0.002 FVAR 3 4 0.47777 0.02551 0.000 FVAR 4 5 0.27558 0.08182 0.000 BASF 1 Mean shift/esd = 0.001 Maximum = -0.011 for U22 S22 Max. shift = 0.001 A for H21A_b Max. dU = 0.000 for C211_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 8 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47103 0.03194 -0.001 FVAR 2 3 0.67811 0.02787 0.001 FVAR 3 4 0.47777 0.02551 0.000 FVAR 4 5 0.27558 0.08182 0.000 BASF 1 Mean shift/esd = 0.001 Maximum = -0.008 for U22 S22 Max. shift = 0.000 A for H21A_b Max. dU = 0.000 for C211_b Least-squares cycle 9 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 9 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 -0.001 OSF 2 0.47100 0.03194 -0.001 FVAR 2 3 0.67815 0.02788 0.001 FVAR 3 4 0.47777 0.02551 0.000 FVAR 4 5 0.27558 0.08183 0.000 BASF 1 Mean shift/esd = 0.001 Maximum = -0.006 for U22 S22 Max. shift = 0.000 A for H21A_b Max. dU = 0.000 for C211_b Least-squares cycle 10 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 10 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47098 0.03194 -0.001 FVAR 2 3 0.67817 0.02788 0.001 FVAR 3 4 0.47778 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.001 Maximum = -0.004 for y C11_a Max. shift = 0.000 A for H21A_b Max. dU = 0.000 for C211_b Least-squares cycle 11 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 11 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 -0.001 OSF 2 0.47096 0.03194 -0.001 FVAR 2 3 0.67819 0.02788 0.001 FVAR 3 4 0.47778 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.003 for y C11_a Max. shift = 0.000 A for C211_b Max. dU = 0.000 for C211_b Least-squares cycle 12 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 12 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47095 0.03194 0.000 FVAR 2 3 0.67821 0.02788 0.001 FVAR 3 4 0.47778 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.002 for U22 S22 Max. shift = 0.000 A for C211_b Max. dU = 0.000 for C211_b Least-squares cycle 13 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 13 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47094 0.03194 0.000 FVAR 2 3 0.67822 0.02789 0.000 FVAR 3 4 0.47778 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.002 for y C11_a Max. shift = 0.000 A for H21A_b Max. dU = 0.000 for C211_b Least-squares cycle 14 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 14 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47093 0.03194 0.000 FVAR 2 3 0.67823 0.02789 0.000 FVAR 3 4 0.47778 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.001 for U22 S22 Max. shift = 0.000 A for H21A_b Max. dU = 0.000 for C211_b Least-squares cycle 15 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 15 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47092 0.03194 0.000 FVAR 2 3 0.67823 0.02789 0.000 FVAR 3 4 0.47778 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.001 for y C11_a Max. shift = 0.000 A for C211_b Max. dU = 0.000 for C211_b Least-squares cycle 16 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 16 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47092 0.03194 0.000 FVAR 2 3 0.67824 0.02789 0.000 FVAR 3 4 0.47779 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.001 for y C11_a Max. shift = 0.000 A for C211_b Max. dU = 0.000 for C211_b Least-squares cycle 17 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 17 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.001 OSF 2 0.47091 0.03194 0.000 FVAR 2 3 0.67824 0.02789 0.000 FVAR 3 4 0.47779 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.001 for y C11_a Max. shift = 0.000 A for H21A_b Max. dU = 0.000 for C211_b Least-squares cycle 18 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 18 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47091 0.03194 0.000 FVAR 2 3 0.67825 0.02789 0.000 FVAR 3 4 0.47779 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for U22 S22 Max. shift = 0.000 A for H21A_b Max. dU = 0.000 for C211_b Least-squares cycle 19 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 19 for 9280 data and 753 / 753 parameters 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. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47091 0.03194 0.000 FVAR 2 3 0.67825 0.02789 0.000 FVAR 3 4 0.47779 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H21A_b Max. dU = 0.000 for C62 Least-squares cycle 20 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 20 for 9280 data and 753 / 753 parameters Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47090 0.03194 0.000 FVAR 2 3 0.67825 0.02789 0.000 FVAR 3 4 0.47779 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for y C11_a Max. shift = 0.000 A for H21A_b Max. dU = 0.000 for C211_b Least-squares cycle 21 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 21 for 9280 data and 753 / 753 parameters Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47090 0.03194 0.000 FVAR 2 3 0.67826 0.02789 0.000 FVAR 3 4 0.47779 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for y C11_a Max. shift = 0.000 A for H21A_b Max. dU = 0.000 for C62 Least-squares cycle 22 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 22 for 9280 data and 753 / 753 parameters Summary of restraints applied in cycle 22 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47090 0.03194 0.000 FVAR 2 3 0.67826 0.02789 0.000 FVAR 3 4 0.47779 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for U22 Cr1 Max. shift = 0.000 A for H21A_b Max. dU = 0.000 for C211_b Least-squares cycle 23 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 23 for 9280 data and 753 / 753 parameters Summary of restraints applied in cycle 23 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47090 0.03194 0.000 FVAR 2 3 0.67826 0.02789 0.000 FVAR 3 4 0.47779 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for U33 S5 Max. shift = 0.000 A for C211_b Max. dU = 0.000 for C62 Least-squares cycle 24 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 24 for 9280 data and 753 / 753 parameters Summary of restraints applied in cycle 24 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47090 0.03194 0.000 FVAR 2 3 0.67826 0.02789 0.000 FVAR 3 4 0.47779 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for U11 Cr1 Max. shift = 0.000 A for C211_b Max. dU = 0.000 for C62 Least-squares cycle 25 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 25 for 9280 data and 753 / 753 parameters Summary of restraints applied in cycle 25 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47090 0.03194 0.000 FVAR 2 3 0.67826 0.02789 0.000 FVAR 3 4 0.47779 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C211_b Max. dU = 0.000 for C1_a Least-squares cycle 26 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 26 for 9280 data and 753 / 753 parameters Summary of restraints applied in cycle 26 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47090 0.03194 0.000 FVAR 2 3 0.67826 0.02789 0.000 FVAR 3 4 0.47779 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H21A_b Max. dU = 0.000 for C61 Least-squares cycle 27 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 27 for 9280 data and 753 / 753 parameters Summary of restraints applied in cycle 27 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47090 0.03194 0.000 FVAR 2 3 0.67826 0.02789 0.000 FVAR 3 4 0.47779 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C211_b Max. dU = 0.000 for O42 Least-squares cycle 28 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 28 for 9280 data and 753 / 753 parameters Summary of restraints applied in cycle 28 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47090 0.03194 0.000 FVAR 2 3 0.67826 0.02789 0.000 FVAR 3 4 0.47779 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H62A Max. dU = 0.000 for C61 Least-squares cycle 29 Maximum vector length = 511 Memory required = 8486 / 1081014 wR2 = 0.2397 before cycle 29 for 9280 data and 753 / 753 parameters Summary of restraints applied in cycle 29 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24687 0.00064 0.000 OSF 2 0.47090 0.03194 0.000 FVAR 2 3 0.67826 0.02789 0.000 FVAR 3 4 0.47779 0.02551 0.000 FVAR 4 5 0.27559 0.08183 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for U33 S15 Max. shift = 0.000 A for H62A Max. dU = 0.000 for C22 Largest correlation matrix elements -0.722 U23 S26 / U23 S24 0.687 z C211_b / y C211_b -0.673 U22 S17 / U22 S8 -0.710 U23 S25 / U23 S23 -0.685 U22 S26 / U22 S24 -0.671 U23 S15 / U23 S6 0.710 U23 Cr1 / U23 Na1 -0.684 U23 S11 / U23 S2 -0.664 U22 S18 / U22 S7 0.702 z C26 / z C25 -0.682 U23 S27 / U23 S21 -0.664 U22 Cr1 / U22 Na1 -0.693 U23 S18 / U23 S7 -0.680 U23 S14 / U23 S3 -0.660 U22 S25 / U22 S23 -0.692 U23 S16 / U23 S5 -0.677 U23 S17 / U23 S8 0.659 z S26 / z S24 -0.692 U33 S26 / U33 S24 -0.677 U33 S27 / U33 S21 -0.659 U33 S28 / U33 S22 -0.688 U33 S25 / U33 S23 0.676 y S18 / y S7 0.659 y C18 / y C7 Idealized hydrogen atom generation before cycle 30 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A -0.0313 0.8335 0.2232 23 0.990 0.000 C1_a C2_a S1 H1B 0.0056 0.7762 0.1539 23 0.990 0.000 C1_a C2_a S1 H2A -0.0744 0.6443 0.2094 23 0.990 0.000 C2_a C1_a S2 H2B -0.1822 0.7187 0.1870 23 0.990 0.000 C2_a C1_a S2 H20A 0.0146 0.7535 0.1478 23 0.990 0.000 C201_b C202_b S1 H20B 0.0071 0.6591 0.1907 23 0.990 0.000 C201_b C202_b S1 H20C -0.1788 0.7532 0.1936 23 0.990 0.000 C202_b C201_b S2 H20D -0.0928 0.8236 0.2421 23 0.990 0.000 C202_b C201_b S2 H9A 0.3559 0.8164 0.8210 23 0.990 0.000 C9 C10 S7 H9B 0.3539 0.7443 0.8862 23 0.990 0.000 C9 C10 S7 H10A 0.4786 0.6447 0.8161 23 0.990 0.000 C10 C9 S8 H10B 0.5529 0.7341 0.8455 23 0.990 0.000 C10 C9 S8 H11A 0.6754 0.0424 0.8131 23 0.990 0.000 C11_a C12_a S11 H11B 0.5650 0.1143 0.7881 23 0.990 0.000 C11_a C12_a S11 H12A 0.4882 -0.0166 0.8487 23 0.990 0.000 C12_a C11_a S12 H12B 0.5268 -0.0766 0.7811 23 0.990 0.000 C12_a C11_a S12 H21A 0.5861 -0.0741 0.7651 23 0.990 0.000 C211_b C212_b S11 H21B 0.6772 -0.0010 0.8096 23 0.990 0.000 C211_b C212_b S11 H21C 0.4965 0.1057 0.7825 23 0.990 0.000 C212_b C211_b S12 H21D 0.4836 0.0346 0.8475 23 0.990 0.000 C212_b C211_b S12 H19A -0.0467 0.0396 0.1522 23 0.990 0.000 C19_a C20_a S17 H19B 0.0424 0.1154 0.1927 23 0.990 0.000 C19_a C20_a S17 H20E 0.1478 0.0186 0.1094 23 0.990 0.000 C20_a C19_a S18 H20F 0.1387 -0.0612 0.1686 23 0.990 0.000 C20_a C19_a S18 H21E 0.0619 -0.0705 0.1836 23 0.990 0.000 C219_b C220_b S17 H21F -0.0503 -0.0043 0.1503 23 0.990 0.000 C219_b C220_b S17 H22A 0.0913 0.1204 0.1778 23 0.990 0.000 C220_b C219_b S18 H22B 0.1334 0.0555 0.1141 23 0.990 0.000 C220_b C219_b S18 H21G 1.0847 0.8723 0.7880 23 0.990 0.000 C21 C22 S21 H21H 1.0552 0.9552 0.8406 23 0.990 0.000 C21 C22 S21 H22C 0.8319 0.9153 0.8256 23 0.990 0.000 C22 C21 S22 H22D 0.9207 0.8412 0.8691 23 0.990 0.000 C22 C21 S22 H29A 0.4303 0.7975 0.1628 23 0.990 0.000 C29 C30 S27 H29B 0.3984 0.8795 0.2156 23 0.990 0.000 C29 C30 S27 H30A 0.5556 0.9157 0.1334 23 0.990 0.000 C30 C29 S28 H30B 0.6497 0.8423 0.1739 23 0.990 0.000 C30 C29 S28 H62A 0.1741 0.8692 -0.0689 137 0.980 0.000 C62 C61 H62A H62B 0.3194 0.8960 -0.0422 137 0.980 0.000 C62 C61 H62A H62C 0.2040 0.9639 -0.0283 137 0.980 0.000 C62 C61 H62A 2009src0837r in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Na1 -0.20137 0.69187 0.00728 1.00000 0.02360 0.02266 0.00591 0.00096 0.00137 0.00506 0.01738 0.01096 0.00055 0.00045 0.00031 0.00000 0.00306 0.00382 0.00277 0.00289 0.00228 0.00298 0.00140 Cr1 0.30460 0.56013 0.00424 1.00000 0.03750 0.04074 0.02542 -0.00182 -0.00566 0.00004 0.03501 0.00569 0.00029 0.00025 0.00017 0.00000 0.00160 0.00208 0.00157 0.00169 0.00124 0.00165 0.00079 C1_a -0.00207 0.77319 0.20762 0.47090 0.04588 0.03694 0.02851 -0.00363 -0.01255 0.00905 0.03798 0.06041 0.00216 0.00267 0.00229 0.03194 0.01052 0.01093 0.01020 0.00812 0.00778 0.00814 0.00809 H1A_a -0.03131 0.83352 0.22323 0.47090 0.04558 0.03194 0.00000 H1B_a 0.00555 0.77616 0.15389 0.47090 0.04558 0.03194 0.00000 C2_a -0.10536 0.70569 0.22108 0.47090 0.03117 0.02395 0.01949 -0.00638 -0.00760 -0.00140 0.02541 0.05215 0.00313 0.00278 0.00114 0.03194 0.00957 0.01033 0.00943 0.00776 0.00738 0.00791 0.00720 H2A_a -0.07437 0.64433 0.20938 0.47090 0.03049 0.03194 0.00000 H2B_a -0.18216 0.71871 0.18698 0.47090 0.03049 0.03194 0.00000 C201_b 0.01203 0.72571 0.19710 0.52910 0.03016 0.01295 0.01220 -0.00663 -0.00813 0.00781 0.01898 0.03502 0.00175 0.00212 0.00131 0.03194 0.00879 0.00938 0.00833 0.00711 0.00676 0.00715 0.00614 H20A_b 0.01462 0.75346 0.14779 0.52910 0.02278 0.03194 0.00000 H20B_b 0.00705 0.65913 0.19071 0.52910 0.02278 0.03194 0.00000 C202_b -0.10516 0.75820 0.23133 0.52910 0.04964 0.03373 0.03873 0.00308 -0.01119 0.00923 0.04152 0.08095 0.00308 0.00262 0.00156 0.03194 0.01004 0.01044 0.00982 0.00791 0.00763 0.00803 0.00754 H20C_b -0.17884 0.75315 0.19357 0.52910 0.04983 0.03194 0.00000 H20D_b -0.09284 0.82355 0.24205 0.52910 0.04983 0.03194 0.00000 C3 -0.00553 0.72269 0.36588 1.00000 0.04514 0.05473 0.03307 -0.00599 0.01378 0.01276 0.04373 0.03847 0.00183 0.00159 0.00108 0.00000 0.00772 0.00888 0.00757 0.00680 0.00629 0.00689 0.00505 C4 0.11284 0.74066 0.34237 1.00000 0.04437 0.05111 0.03381 0.01355 -0.00578 0.00148 0.04360 0.03842 0.00188 0.00159 0.00111 0.00000 0.00792 0.00868 0.00775 0.00691 0.00644 0.00697 0.00517 C5 0.14965 0.73551 0.48372 1.00000 0.03952 0.05726 0.02460 -0.00018 -0.00101 0.00743 0.04066 0.03585 0.00175 0.00155 0.00100 0.00000 0.00744 0.00874 0.00703 0.00659 0.00600 0.00677 0.00482 C6 0.20502 0.72975 0.55731 1.00000 0.03011 0.04439 0.00698 0.00952 -0.00356 0.00434 0.02744 0.03077 0.00154 0.00132 0.00081 0.00000 0.00667 0.00800 0.00564 0.00555 0.00510 0.00600 0.00398 C7 0.36484 0.73179 0.66863 1.00000 0.02310 0.03709 0.01241 0.00060 0.00241 0.00452 0.02415 0.03114 0.00152 0.00130 0.00088 0.00000 0.00644 0.00784 0.00598 0.00566 0.00519 0.00589 0.00396 C8 0.24684 0.71293 0.69783 1.00000 0.02373 0.04117 0.03220 0.00590 -0.00133 0.01174 0.03257 0.03427 0.00153 0.00143 0.00101 0.00000 0.00649 0.00782 0.00705 0.00638 0.00562 0.00621 0.00421 C9 0.35658 0.75075 0.83230 1.00000 0.04407 0.02820 0.02817 -0.00699 0.00279 -0.00016 0.03349 0.02821 0.00149 0.00135 0.00095 0.00000 0.00730 0.00724 0.00663 0.00603 0.00575 0.00617 0.00415 H9A 0.35587 0.81640 0.82100 1.00000 0.04019 0.00000 0.00000 H9B 0.35387 0.74434 0.88622 1.00000 0.04019 0.00000 0.00000 C10 0.48157 0.71145 0.81104 1.00000 0.03309 0.04549 0.02476 -0.00183 -0.01299 -0.01043 0.03530 0.03166 0.00156 0.00150 0.00087 0.00000 0.00682 0.00816 0.00663 0.00624 0.00555 0.00651 0.00433 H10A 0.47858 0.64468 0.81605 1.00000 0.04236 0.00000 0.00000 H10B 0.55287 0.73413 0.84549 1.00000 0.04236 0.00000 0.00000 S1 0.15448 0.75357 0.25168 1.00000 0.04243 0.06000 0.03170 0.01155 -0.00944 -0.00661 0.04540 0.00964 0.00049 0.00043 0.00029 0.00000 0.00285 0.00375 0.00282 0.00284 0.00217 0.00272 0.00143 S2 -0.15230 0.70559 0.31328 1.00000 0.02559 0.06286 0.03510 -0.01178 -0.01199 0.00607 0.04199 0.00911 0.00042 0.00045 0.00028 0.00000 0.00232 0.00393 0.00280 0.00288 0.00200 0.00254 0.00141 S3 -0.01519 0.71168 0.46055 1.00000 0.03579 0.07195 0.02194 -0.00404 -0.00802 0.00860 0.04381 0.00968 0.00045 0.00046 0.00027 0.00000 0.00252 0.00416 0.00243 0.00267 0.00190 0.00267 0.00142 S4 0.23986 0.74906 0.41009 1.00000 0.03427 0.05766 0.02410 0.00381 -0.00505 -0.00186 0.03909 0.00948 0.00046 0.00043 0.00027 0.00000 0.00254 0.00368 0.00251 0.00257 0.00197 0.00249 0.00133 S5 0.36656 0.74524 0.57564 1.00000 0.03804 0.06385 0.02854 0.00554 -0.00238 0.00379 0.04376 0.01025 0.00048 0.00045 0.00029 0.00000 0.00274 0.00403 0.00273 0.00289 0.00213 0.00264 0.00144 S6 0.11441 0.71124 0.63036 1.00000 0.03594 0.06162 0.02579 -0.00628 -0.00610 0.01097 0.04160 0.00948 0.00045 0.00044 0.00027 0.00000 0.00256 0.00380 0.00253 0.00265 0.00199 0.00269 0.00137 S7 0.21149 0.70043 0.78766 1.00000 0.02867 0.05654 0.02413 -0.00983 -0.00004 0.00125 0.03657 0.00867 0.00042 0.00042 0.00025 0.00000 0.00236 0.00377 0.00251 0.00264 0.00189 0.00258 0.00130 S8 0.51475 0.73953 0.71838 1.00000 0.02941 0.06881 0.01999 0.00035 -0.00887 0.00021 0.04001 0.00914 0.00044 0.00042 0.00026 0.00000 0.00241 0.00433 0.00244 0.00263 0.00189 0.00261 0.00145 C11_a 0.59745 0.05246 0.77921 0.67826 0.04212 0.03006 0.02736 -0.00458 -0.00669 0.00720 0.03371 0.03989 0.00231 0.00196 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0.03845 0.09453 0.01395 0.00208 -0.00843 -0.00100 0.04956 0.01013 0.00049 0.00051 0.00026 0.00000 0.00269 0.00520 0.00228 0.00281 0.00193 0.00297 0.00173 S14 0.49970 0.03411 0.53966 1.00000 0.02785 0.08942 0.02031 0.00418 -0.00163 0.01215 0.04606 0.00991 0.00043 0.00048 0.00025 0.00000 0.00229 0.00495 0.00232 0.00282 0.00179 0.00269 0.00162 S15 0.37280 0.03586 0.37178 1.00000 0.01948 0.09476 0.01586 0.00685 -0.00427 0.00467 0.04369 0.00944 0.00039 0.00047 0.00024 0.00000 0.00207 0.00499 0.00214 0.00272 0.00167 0.00271 0.00162 S16 0.11984 0.00546 0.42381 1.00000 0.02838 0.08919 0.01354 0.00336 -0.00143 0.00194 0.04388 0.00995 0.00045 0.00049 0.00025 0.00000 0.00234 0.00473 0.00223 0.00274 0.00179 0.00268 0.00155 S17 -0.02242 0.01143 0.27811 1.00000 0.02873 0.06677 0.02422 0.00090 0.00011 -0.00083 0.04002 0.00952 0.00044 0.00043 0.00027 0.00000 0.00239 0.00417 0.00251 0.00270 0.00189 0.00264 0.00142 S18 0.28479 0.04950 0.21470 1.00000 0.03192 0.05018 0.01759 0.00521 -0.00447 0.00985 0.03359 0.00878 0.00041 0.00040 0.00023 0.00000 0.00231 0.00354 0.00219 0.00243 0.00176 0.00252 0.00123 C21 1.01915 0.91807 0.79861 1.00000 0.03708 0.04352 0.02843 0.00477 -0.00547 -0.00494 0.03680 0.03612 0.00173 0.00151 0.00105 0.00000 0.00743 0.00809 0.00711 0.00641 0.00595 0.00651 0.00465 H21G 1.08472 0.87232 0.78804 1.00000 0.04416 0.00000 0.00000 H21H 1.05523 0.95524 0.84060 1.00000 0.04416 0.00000 0.00000 C22 0.90077 0.87005 0.82041 1.00000 0.04241 0.06046 0.04431 -0.00146 0.00376 0.00716 0.04905 0.03928 0.00192 0.00165 0.00124 0.00000 0.00803 0.00917 0.00811 0.00709 0.00666 0.00708 0.00547 H22C 0.83188 0.91532 0.82557 1.00000 0.05886 0.00000 0.00000 H22D 0.92072 0.84125 0.86907 1.00000 0.05886 0.00000 0.00000 C23 0.84678 0.84471 0.67025 1.00000 0.03004 0.03646 0.03641 0.00196 -0.01003 0.00264 0.03501 0.03531 0.00176 0.00147 0.00112 0.00000 0.00715 0.00789 0.00753 0.00652 0.00601 0.00634 0.00461 C24 0.89689 0.92118 0.65997 1.00000 0.03683 0.03229 0.03269 -0.00059 -0.00214 -0.00252 0.03422 0.03445 0.00177 0.00144 0.00106 0.00000 0.00741 0.00762 0.00736 0.00630 0.00605 0.00644 0.00450 C25 0.77927 0.87248 0.53530 1.00000 0.03062 0.04839 0.03182 -0.00528 0.01543 -0.00907 0.03623 0.03651 0.00176 0.00147 0.00112 0.00000 0.00710 0.00813 0.00702 0.00633 0.00602 0.00637 0.00450 C26 0.72002 0.87422 0.46661 1.00000 0.02860 0.05285 0.03860 -0.00291 0.00206 -0.00193 0.04006 0.03784 0.00176 0.00154 0.00120 0.00000 0.00699 0.00841 0.00750 0.00671 0.00606 0.00653 0.00471 C27 0.65163 0.91479 0.32752 1.00000 0.03236 0.04615 0.03397 -0.00153 0.01082 0.00140 0.03704 0.03767 0.00181 0.00155 0.00110 0.00000 0.00738 0.00840 0.00748 0.00671 0.00615 0.00656 0.00477 C28 0.58848 0.83444 0.34631 1.00000 0.03579 0.04260 0.03138 -0.00013 0.00402 0.00388 0.03652 0.03700 0.00181 0.00152 0.00108 0.00000 0.00738 0.00813 0.00729 0.00643 0.00609 0.00651 0.00462 C29 0.46570 0.83523 0.20464 1.00000 0.05039 0.04713 0.03746 -0.00540 -0.00820 -0.00429 0.04565 0.03734 0.00193 0.00159 0.00115 0.00000 0.00822 0.00851 0.00794 0.00688 0.00662 0.00698 0.00527 H29A 0.43029 0.79750 0.16283 1.00000 0.05478 0.00000 0.00000 H29B 0.39838 0.87949 0.21558 1.00000 0.05478 0.00000 0.00000 C30 0.57996 0.88618 0.18136 1.00000 0.03899 0.04309 0.03353 0.00175 0.00313 0.00794 0.03853 0.03581 0.00180 0.00145 0.00109 0.00000 0.00748 0.00804 0.00731 0.00636 0.00617 0.00654 0.00466 H30A 0.55564 0.91565 0.13342 1.00000 0.04624 0.00000 0.00000 H30B 0.64966 0.84232 0.17386 1.00000 0.04624 0.00000 0.00000 S21 0.98854 0.99106 0.71826 1.00000 0.05149 0.04155 0.04067 0.00451 -0.00862 -0.01692 0.04526 0.00941 0.00051 0.00041 0.00030 0.00000 0.00312 0.00355 0.00317 0.00271 0.00242 0.00270 0.00145 S22 0.84141 0.78437 0.75529 1.00000 0.04913 0.06080 0.04344 0.01203 -0.01899 -0.01497 0.05239 0.01005 0.00053 0.00045 0.00033 0.00000 0.00313 0.00428 0.00335 0.00307 0.00254 0.00297 0.00167 S23 0.75008 0.78942 0.59775 1.00000 0.05389 0.05906 0.03794 -0.00337 0.00613 -0.02467 0.05017 0.01000 0.00054 0.00045 0.00031 0.00000 0.00346 0.00422 0.00333 0.00307 0.00269 0.00315 0.00163 S24 0.88199 0.96166 0.56697 1.00000 0.05974 0.07038 0.02135 0.00119 0.00563 -0.02240 0.05036 0.01020 0.00056 0.00047 0.00028 0.00000 0.00361 0.00463 0.00274 0.00296 0.00249 0.00328 0.00168 S25 0.74276 0.96361 0.40188 1.00000 0.05013 0.06477 0.02717 -0.00260 0.00350 -0.01165 0.04734 0.01016 0.00053 0.00046 0.00029 0.00000 0.00324 0.00430 0.00290 0.00293 0.00243 0.00306 0.00155 S26 0.61209 0.79033 0.43296 1.00000 0.04928 0.06933 0.03788 0.00190 0.00397 -0.02283 0.05214 0.01058 0.00054 0.00048 0.00033 0.00000 0.00339 0.00470 0.00332 0.00329 0.00264 0.00320 0.00171 S27 0.49833 0.76310 0.28382 1.00000 0.06614 0.06802 0.04712 0.01147 -0.02377 -0.01723 0.06201 0.01094 0.00058 0.00051 0.00034 0.00000 0.00385 0.00467 0.00374 0.00349 0.00294 0.00351 0.00188 S28 0.64203 0.97166 0.24586 1.00000 0.04392 0.05163 0.04791 0.02406 -0.01804 -0.01520 0.04903 0.01021 0.00052 0.00043 0.00033 0.00000 0.00292 0.00386 0.00343 0.00299 0.00242 0.00268 0.00159 C31 0.09001 0.66000 -0.02635 1.00000 0.03718 0.02431 0.03873 -0.00240 -0.00104 0.00625 0.03364 0.03192 0.00177 0.00125 0.00102 0.00000 0.00702 0.00679 0.00694 0.00593 0.00611 0.00622 0.00396 C32 0.06433 0.60053 0.04606 1.00000 0.04120 0.04184 0.03102 -0.00943 0.00423 -0.00731 0.03795 0.03401 0.00188 0.00143 0.00105 0.00000 0.00725 0.00757 0.00685 0.00610 0.00607 0.00642 0.00431 O31 0.19936 0.65892 -0.04166 1.00000 0.06447 0.02926 0.04201 0.00591 0.00179 -0.00674 0.04539 0.02438 0.00138 0.00094 0.00075 0.00000 0.00862 0.00717 0.00739 0.00587 0.00641 0.00630 0.00351 O32 0.16269 0.56045 0.07339 1.00000 0.05778 0.07433 0.02327 0.01360 -0.01479 -0.01228 0.05280 0.02472 0.00126 0.00121 0.00065 0.00000 0.00780 0.00958 0.00603 0.00683 0.00544 0.00791 0.00370 O33 -0.04423 0.59862 0.06719 1.00000 0.06177 0.07082 0.05681 0.00337 -0.00296 -0.00875 0.06357 0.02814 0.00142 0.00119 0.00086 0.00000 0.00929 0.01052 0.00925 0.00794 0.00732 0.00807 0.00440 O34 -0.00364 0.70519 -0.05159 1.00000 0.05421 0.04078 0.05134 0.00521 -0.00046 0.00406 0.04904 0.02308 0.00120 0.00096 0.00073 0.00000 0.00793 0.00777 0.00769 0.00643 0.00626 0.00683 0.00342 C41 0.21118 0.39415 -0.03840 1.00000 0.01713 0.02353 0.00914 0.00088 0.00253 -0.01033 0.01652 0.02516 0.00135 0.00113 0.00074 0.00000 0.00574 0.00658 0.00537 0.00519 0.00461 0.00529 0.00310 C42 0.31140 0.37528 0.02708 1.00000 0.03962 0.04559 0.03230 -0.00034 0.00316 -0.00095 0.03916 0.03525 0.00177 0.00142 0.00100 0.00000 0.00709 0.00784 0.00698 0.00632 0.00591 0.00633 0.00436 O41 0.20241 0.47141 -0.05959 1.00000 0.03534 0.05180 0.01672 -0.00684 -0.01308 0.00454 0.03546 0.02113 0.00110 0.00096 0.00064 0.00000 0.00634 0.00859 0.00549 0.00557 0.00466 0.00594 0.00318 O42 0.37260 0.44885 0.05101 1.00000 0.03909 0.05962 0.02263 0.00383 -0.01796 0.00357 0.04158 0.02172 0.00113 0.00094 0.00062 0.00000 0.00672 0.00898 0.00593 0.00587 0.00491 0.00593 0.00346 O43 0.32394 0.30011 0.05774 1.00000 0.06881 0.04100 0.03675 0.01399 -0.02551 -0.00116 0.05051 0.02409 0.00133 0.00100 0.00077 0.00000 0.00871 0.00822 0.00726 0.00641 0.00643 0.00700 0.00389 O44 0.15386 0.32688 -0.06554 1.00000 0.05054 0.04079 0.03659 0.00916 -0.01658 0.00435 0.04376 0.02330 0.00122 0.00090 0.00069 0.00000 0.00732 0.00786 0.00691 0.00603 0.00568 0.00613 0.00340 C51 0.55063 0.59190 -0.02670 1.00000 0.03437 0.03639 0.01384 0.01044 0.00379 -0.00555 0.02810 0.03062 0.00153 0.00125 0.00084 0.00000 0.00675 0.00710 0.00559 0.00539 0.00533 0.00596 0.00365 C52 0.53951 0.64245 0.04713 1.00000 0.04069 0.04325 0.03855 0.00184 0.00102 0.00418 0.04096 0.03651 0.00182 0.00150 0.00111 0.00000 0.00729 0.00770 0.00721 0.00630 0.00625 0.00648 0.00449 O51 0.44709 0.56552 -0.06080 1.00000 0.03272 0.03614 0.01457 -0.00455 -0.00326 -0.00998 0.02810 0.01793 0.00092 0.00083 0.00051 0.00000 0.00575 0.00668 0.00458 0.00476 0.00421 0.00528 0.00258 O52 0.42202 0.63915 0.06717 1.00000 0.03083 0.04606 0.01683 -0.01565 -0.00244 0.00834 0.03148 0.01991 0.00104 0.00089 0.00060 0.00000 0.00597 0.00770 0.00539 0.00510 0.00451 0.00534 0.00292 O53 0.63518 0.67533 0.08140 1.00000 0.03901 0.08403 0.03704 -0.03055 -0.01428 0.00541 0.05432 0.02338 0.00118 0.00117 0.00073 0.00000 0.00707 0.01083 0.00713 0.00730 0.00569 0.00703 0.00410 O54 0.66183 0.59010 -0.05237 1.00000 0.03973 0.04937 0.01855 0.00537 0.00986 -0.00265 0.03547 0.02220 0.00110 0.00093 0.00061 0.00000 0.00686 0.00812 0.00552 0.00533 0.00491 0.00588 0.00312 C61 0.21580 0.85871 0.03771 1.00000 0.07074 0.07976 0.07607 0.00416 0.00654 -0.01206 0.07550 0.04518 0.00237 0.00193 0.00155 0.00000 0.00958 0.01014 0.00981 0.00810 0.00807 0.00805 0.00666 C62 0.22936 0.90008 -0.03057 1.00000 0.09897 0.08574 0.08895 -0.00295 -0.00911 -0.00211 0.09216 0.04920 0.00261 0.00197 0.00150 0.00000 0.01144 0.01121 0.01108 0.00844 0.00848 0.00867 0.00841 H62A 0.17409 0.86916 -0.06888 1.00000 0.13823 0.00000 0.00000 H62B 0.31944 0.89604 -0.04219 1.00000 0.13823 0.00000 0.00000 H62C 0.20402 0.96394 -0.02830 1.00000 0.13823 0.00000 0.00000 N61 0.19721 0.82590 0.09259 1.00000 0.07616 0.13420 0.06233 0.03195 -0.00837 -0.03856 0.09168 0.03440 0.00183 0.00154 0.00104 0.00000 0.01290 0.01816 0.01182 0.01213 0.00997 0.01236 0.00668 Final Structure Factor Calculation for 2009src0837r in P2(1) Total number of l.s. parameters = 753 Maximum vector length = 511 Memory required = 7735 / 28112 wR2 = 0.2397 before cycle 30 for 9280 data and 2 / 753 parameters Summary of restraints applied in cycle 30 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 0. 288. 270. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.032 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.000 0.012 0.007 0.000 GooF = S = 1.090; Restrained GooF = 1.064 for 592 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 33.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0976 for 5564 Fo > 4sig(Fo) and 0.1731 for all 9280 data wR2 = 0.2397, GooF = S = 1.090, Restrained GooF = 1.064 for all data Occupancy sum of asymmetric unit = 77.00 for non-hydrogen and 27.00 for hydrogen atoms Principal mean square atomic displacements U 0.0282 0.0181 0.0058 Na1 0.0429 0.0404 0.0217 Cr1 0.0607 0.0328 0.0204 C1_a 0.0379 0.0266 0.0117 C2_a 0.0394 0.0116 0.0059 C201_b 0.0626 0.0384 0.0235 C202_b 0.0636 0.0464 0.0212 C3 0.0597 0.0474 0.0236 C4 0.0601 0.0379 0.0240 C5 0.0471 0.0314 0.0038 C6 0.0384 0.0218 0.0122 C7 0.0477 0.0338 0.0162 C8 0.0441 0.0352 0.0212 C9 0.0540 0.0395 0.0124 C10 0.0695 0.0434 0.0233 S1 0.0707 0.0391 0.0161 S2 0.0749 0.0393 0.0172 S3 0.0585 0.0382 0.0205 S4 0.0650 0.0407 0.0256 S5 0.0681 0.0352 0.0215 S6 0.0595 0.0291 0.0211 S7 0.0688 0.0376 0.0136 S8 0.0513 0.0267 0.0231 C11_a 0.0316 0.0233 0.0150 C12_a 0.0362 0.0292 0.0206 C211_b 0.0454 0.0250 0.0162 C212_b 0.0516 0.0255 0.0135 C13 0.0568 0.0329 0.0093 C14 0.0561 0.0372 0.0213 C15 0.0559 0.0456 0.0366 C16 0.0477 0.0384 0.0166 C17 0.0491 0.0372 0.0274 C18 0.0274 0.0249 0.0087 C19_a 0.0307 0.0271 0.0250 C20_a 0.0349 0.0204 0.0180 C219_b 0.0386 0.0224 0.0089 C220_b 0.0848 0.0369 0.0160 S11 0.1522 0.0356 0.0098 S12 0.0946 0.0433 0.0108 S13 0.0918 0.0282 0.0181 S14 0.0955 0.0242 0.0113 S15 0.0894 0.0293 0.0130 S16 0.0668 0.0297 0.0236 S17 0.0545 0.0326 0.0137 S18 0.0502 0.0362 0.0240 C21 0.0631 0.0443 0.0397 C22 0.0475 0.0371 0.0204 C23 0.0410 0.0329 0.0287 C24 0.0559 0.0359 0.0169 C25 0.0535 0.0382 0.0284 C26 0.0464 0.0407 0.0241 C27 0.0444 0.0344 0.0308 C28 0.0585 0.0495 0.0290 C29 0.0493 0.0340 0.0323 C30 0.0710 0.0368 0.0279 S21 0.0868 0.0454 0.0250 S22 0.0814 0.0375 0.0317 S23 0.0881 0.0423 0.0206 S24 0.0712 0.0438 0.0270 S25 0.0845 0.0385 0.0334 S26 0.1026 0.0546 0.0288 S27 0.0914 0.0322 0.0234 S28 0.0445 0.0347 0.0217 C31 0.0514 0.0371 0.0253 C32 0.0666 0.0436 0.0260 O31 0.0891 0.0536 0.0157 O32 0.0791 0.0603 0.0513 O33 0.0582 0.0518 0.0371 O34 0.0312 0.0112 0.0072 C41 0.0457 0.0395 0.0323 C42 0.0571 0.0403 0.0090 O41 0.0602 0.0547 0.0098 O42 0.0910 0.0446 0.0160 O43 0.0669 0.0450 0.0194 O44 0.0434 0.0321 0.0088 C51 0.0463 0.0411 0.0354 C52 0.0446 0.0281 0.0116 O51 0.0571 0.0273 0.0100 O52 0.1028 0.0444 0.0158 O53 0.0506 0.0414 0.0144 O54 0.0893 0.0757 0.0615 C61 0.1131 0.0870 0.0763 C62 0.1676 0.0577 0.0497 N61 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.023 0.031 0.038 0.047 0.058 0.072 0.096 0.135 1.000 Number in group 931. 963. 993. 838. 976. 885. 941. 933. 890. 930. GooF 1.213 1.118 1.165 1.132 1.068 1.083 1.024 0.990 0.966 1.106 K 4.009 1.432 1.222 1.129 1.064 1.082 1.006 1.035 1.001 1.023 Resolution(A) 0.84 0.87 0.91 0.95 1.01 1.07 1.15 1.27 1.46 1.82 inf Number in group 975. 900. 925. 947. 894. 945. 910. 941. 909. 934. GooF 1.223 1.160 1.146 1.098 1.047 0.994 0.997 1.039 1.002 1.156 K 1.179 1.149 1.088 1.065 1.059 0.988 1.005 1.020 0.982 1.036 R1 0.315 0.280 0.275 0.231 0.210 0.150 0.114 0.095 0.078 0.062 Recommended weighting scheme: WGHT 0.0523 33.7302 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 0 4 48650.32 30531.55 6.61 0.431 3.28 -4 1 9 2937.20 798.39 6.24 0.070 1.65 0 0 13 968.49 0.96 5.78 0.002 1.40 -2 1 20 1702.33 139.38 5.77 0.029 0.91 4 0 6 10720.29 6410.60 5.60 0.197 1.89 -8 -1 1 3475.54 1303.81 5.38 0.089 1.30 -6 1 5 6707.91 2323.95 5.06 0.119 1.60 8 1 0 3755.49 1776.84 4.78 0.104 1.29 2 0 17 4290.79 2124.32 4.70 0.114 1.03 -4 -1 9 2531.76 806.06 4.53 0.070 1.65 -6 -1 5 5906.87 2358.76 4.24 0.120 1.60 -1 -1 14 4815.56 1310.47 3.89 0.089 1.30 -2 -1 20 1322.03 140.90 3.86 0.029 0.91 3 2 4 74946.17 56650.18 3.86 0.586 2.49 -2 -1 14 532.58 9.47 3.85 0.008 1.28 -2 0 8 6587.26 4394.23 3.84 0.163 2.15 -8 -1 4 2838.31 1625.61 3.75 0.099 1.27 0 0 18 635.17 26.46 3.75 0.013 1.01 8 -1 0 4035.10 1790.46 3.71 0.104 1.29 4 1 6 14670.57 10574.80 3.70 0.253 1.88 3 -3 5 8616.61 5843.88 3.67 0.188 2.16 -7 0 7 909.40 182.95 3.63 0.033 1.34 -3 -15 9 2082.58 1035.32 3.56 0.079 0.86 2 0 3 7520.11 5302.00 3.56 0.179 3.79 4 -1 4 6172.44 4233.75 3.52 0.160 2.15 -3 9 18 766.52 58.70 3.49 0.019 0.85 -1 1 14 4269.06 1349.47 3.49 0.091 1.30 6 0 6 362.79 37.66 3.34 0.015 1.45 -4 1 13 459.77 71.06 3.32 0.021 1.27 8 -1 2 1210.48 519.41 3.30 0.056 1.26 -9 0 11 805.12 2.61 3.28 0.004 0.98 3 -1 4 25599.86 19661.49 3.28 0.346 2.61 4 1 4 6002.36 4188.32 3.28 0.159 2.15 8 1 2 1226.06 519.99 3.28 0.056 1.26 3 -2 4 75235.20 56908.87 3.28 0.588 2.49 2 0 6 36692.58 29100.18 3.26 0.420 2.53 -3 0 13 304.83 3.02 3.22 0.004 1.33 -8 1 1 3120.78 1320.85 3.21 0.090 1.30 4 3 14 -112.53 283.21 3.16 0.041 1.10 -5 11 14 803.03 6.77 3.16 0.006 0.87 -3 -14 9 597.04 121.01 3.15 0.027 0.91 -10 1 11 1270.76 453.20 3.13 0.052 0.91 -1 -15 6 778.39 200.48 3.11 0.035 0.93 1 12 13 621.81 31.31 3.07 0.014 0.91 -4 -1 13 459.46 72.15 3.06 0.021 1.27 -2 -13 10 587.96 1.34 3.06 0.003 0.95 -2 1 14 453.07 10.48 3.05 0.008 1.28 -5 -1 5 318.43 62.87 3.05 0.020 1.85 4 -15 5 600.43 52.08 3.04 0.018 0.89 4 -1 6 13899.73 10501.75 3.02 0.253 1.88 Bond lengths and angles Na1 - Distance Angles O53_$2 2.2715 (0.0149) O54_$2 2.2821 (0.0140) 75.18 (0.47) O44_$1 2.2918 (0.0139) 87.78 (0.56) 153.48 (0.52) O43_$1 2.3091 (0.0151) 88.30 (0.59) 85.06 (0.47) 74.08 (0.51) O33 2.3378 (0.0170) 100.86 (0.59) 102.73 (0.58) 100.32 (0.58) 169.19 (0.63) O34 2.4064 (0.0138) 169.81 (0.53) 111.36 (0.49) 88.62 (0.51) 99.87 (0.57) 70.44 (0.52) Na1 - O53_$2 O54_$2 O44_$1 O43_$1 O33 Cr1 - Distance Angles O42 1.9552 (0.0130) O31 1.9678 (0.0140) 167.40 (0.57) O51 1.9753 (0.0102) 91.88 (0.51) 97.72 (0.56) O52 1.9842 (0.0117) 93.31 (0.54) 96.04 (0.56) 82.31 (0.46) O41 1.9983 (0.0126) 81.95 (0.52) 89.24 (0.52) 93.83 (0.49) 173.82 (0.53) O32 2.0195 (0.0137) 89.25 (0.61) 81.57 (0.62) 177.03 (0.61) 94.89 (0.54) 89.04 (0.57) Cr1 - O42 O31 O51 O52 O41 C1_a - Distance Angles C2_a 1.5004 (0.0174) S1 1.7799 (0.0180) 117.39 (2.31) H1A_a 0.9900 107.96 107.96 H1B_a 0.9900 107.96 107.96 107.22 C1_a - C2_a S1 H1A_a C2_a - Distance Angles C1_a 1.5004 (0.0175) S2 1.7886 (0.0178) 114.16 (2.53) H2A_a 0.9900 108.72 108.72 H2B_a 0.9900 108.72 108.72 107.63 C2_a - C1_a S2 H2A_a C201_b - Distance Angles C202_b 1.4942 (0.0170) S1 1.7645 (0.0165) 111.52 (2.11) H20A_b 0.9900 109.32 109.32 H20B_b 0.9900 109.32 109.32 107.97 C201_b - C202_b S1 H20A_b C202_b - Distance Angles C201_b 1.4942 (0.0170) S2 1.7876 (0.0178) 119.97 (2.04) H20C_b 0.9900 107.33 107.33 H20D_b 0.9900 107.33 107.33 106.91 C202_b - C201_b S2 H20C_b C3 - Distance Angles C4 1.3635 (0.0271) S3 1.7444 (0.0201) 117.16 (1.56) S2 1.7534 (0.0206) 128.70 (1.58) 114.11 (1.09) C3 - C4 S3 C4 - Distance Angles C3 1.3635 (0.0270) S4 1.7370 (0.0196) 116.42 (1.57) S1 1.7536 (0.0204) 128.13 (1.58) 115.42 (1.14) C4 - C3 S4 C5 - Distance Angles C6 1.4180 (0.0231) S4 1.7121 (0.0190) 122.83 (1.36) S3 1.7681 (0.0190) 121.64 (1.39) 114.85 (1.04) C5 - C6 S4 C6 - Distance Angles C5 1.4180 (0.0231) S5 1.7024 (0.0166) 119.69 (1.28) S6 1.7160 (0.0162) 122.48 (1.30) 117.80 (0.88) C6 - C5 S5 C7 - Distance Angles C8 1.4062 (0.0234) S5 1.7082 (0.0164) 118.66 (1.28) S8 1.7425 (0.0166) 126.06 (1.29) 115.24 (0.92) C7 - C8 S5 C8 - Distance Angles C7 1.4062 (0.0234) S7 1.7174 (0.0188) 130.15 (1.34) S6 1.7701 (0.0173) 113.22 (1.32) 116.42 (0.96) C8 - C7 S7 C9 - Distance Angles C10 1.5040 (0.0216) S7 1.8141 (0.0159) 115.62 (1.23) H9A 0.9900 108.37 108.37 H9B 0.9900 108.37 108.37 107.44 C9 - C10 S7 H9A C10 - Distance Angles C9 1.5040 (0.0216) S8 1.8001 (0.0165) 112.97 (1.26) H10A 0.9900 108.99 108.99 H10B 0.9900 108.99 108.99 107.78 C10 - C9 S8 H10A S1 - Distance Angles C4 1.7536 (0.0204) C201_b 1.7645 (0.0166) 104.15 (1.10) C1_a 1.7799 (0.0181) 98.89 (1.55) 24.23 (1.36) S1 - C4 C201_b S2 - Distance Angles C3 1.7534 (0.0207) C202_b 1.7876 (0.0178) 96.17 (1.46) C2_a 1.7886 (0.0178) 102.72 (1.21) 25.75 (1.46) S2 - C3 C202_b S3 - Distance Angles C3 1.7444 (0.0201) C5 1.7681 (0.0192) 94.80 (0.91) S3 - C3 S4 - Distance Angles C5 1.7121 (0.0190) C4 1.7370 (0.0197) 96.56 (0.97) S4 - C5 S5 - Distance Angles C6 1.7024 (0.0167) C7 1.7082 (0.0164) 95.05 (0.78) S5 - C6 S6 - Distance Angles C6 1.7160 (0.0162) C8 1.7701 (0.0174) 95.19 (0.83) S6 - C6 S7 - Distance Angles C8 1.7174 (0.0188) C9 1.8141 (0.0161) 98.49 (0.86) S7 - C8 S8 - Distance Angles C7 1.7425 (0.0167) C10 1.8001 (0.0165) 103.90 (0.77) S8 - C7 C11_a - Distance Angles C12_a 1.5056 (0.0160) S11 1.8132 (0.0159) 111.14 (1.64) H11A_a 0.9900 109.41 109.41 H11B_a 0.9900 109.41 109.41 108.02 C11_a - C12_a S11 H11A_a C12_a - Distance Angles C11_a 1.5056 (0.0160) S12 1.8237 (0.0155) 116.81 (1.61) H12A_a 0.9900 108.09 108.09 H12B_a 0.9900 108.09 108.09 107.29 C12_a - C11_a S12 H12A_a C211_b - Distance Angles C212_b 1.4990 (0.0181) S11 1.8273 (0.0193) 104.62 (2.78) H21A_b 0.9900 110.83 110.83 H21B_b 0.9900 110.83 110.83 108.88 C211_b - C212_b S11 H21A_b C212_b - Distance Angles C211_b 1.4990 (0.0182) S12 1.8116 (0.0191) 114.87 (3.11) H21C_b 0.9900 108.55 108.55 H21D_b 0.9900 108.55 108.55 107.54 C212_b - C211_b S12 H21C_b C13 - Distance Angles C14 1.3342 (0.0243) S12 1.7407 (0.0172) 128.56 (1.33) S13 1.7626 (0.0168) 117.10 (1.30) 114.34 (1.00) C13 - C14 S12 C14 - Distance Angles C13 1.3342 (0.0243) S11 1.7427 (0.0169) 129.00 (1.31) S14 1.7432 (0.0162) 116.80 (1.30) 113.59 (0.97) C14 - C13 S11 C15 - Distance Angles C16 1.3674 (0.0261) S14 1.6961 (0.0176) 124.79 (1.52) S13 1.7525 (0.0192) 118.67 (1.45) 116.12 (1.01) C15 - C16 S14 C16 - Distance Angles C15 1.3674 (0.0261) S16 1.7135 (0.0195) 125.97 (1.58) S15 1.7604 (0.0207) 120.41 (1.50) 113.55 (1.10) C16 - C15 S16 C17 - Distance Angles C18 1.2701 (0.0252) S15 1.7503 (0.0166) 120.42 (1.48) S18 1.8088 (0.0184) 128.06 (1.43) 111.39 (0.99) C17 - C18 S15 C18 - Distance Angles C17 1.2701 (0.0252) S17 1.7345 (0.0183) 131.33 (1.62) S16 1.7694 (0.0202) 115.00 (1.42) 113.67 (1.09) C18 - C17 S17 C19_a - Distance Angles C20_a 1.4986 (0.0179) S17 1.8197 (0.0167) 117.06 (2.13) H19A_a 0.9900 108.03 108.03 H19B_a 0.9900 108.03 108.03 107.26 C19_a - C20_a S17 H19A_a C20_a - Distance Angles C19_a 1.4986 (0.0179) S18 1.8081 (0.0173) 108.47 (2.01) H20E_a 0.9900 110.00 110.00 H20F_a 0.9900 110.00 110.00 108.37 C20_a - C19_a S18 H20E_a C219_b - Distance Angles C220_b 1.4951 (0.0174) S17 1.8091 (0.0161) 110.50 (1.70) H21E_b 0.9900 109.55 109.55 H21F_b 0.9900 109.55 109.55 108.10 C219_b - C220_b S17 H21E_b C220_b - Distance Angles C219_b 1.4951 (0.0174) S18 1.8140 (0.0151) 117.53 (1.76) H22A_b 0.9900 107.92 107.92 H22B_b 0.9900 107.92 107.92 107.20 C220_b - C219_b S18 H22A_b S11 - Distance Angles C14 1.7427 (0.0170) C11_a 1.8132 (0.0159) 103.26 (0.96) C211_b 1.8273 (0.0193) 100.60 (1.81) 29.10 (1.66) S11 - C14 C11_a S12 - Distance Angles C13 1.7407 (0.0172) C212_b 1.8116 (0.0193) 96.96 (1.74) C12_a 1.8237 (0.0156) 99.77 (0.97) 26.66 (1.54) S12 - C13 C212_b S13 - Distance Angles C15 1.7525 (0.0193) C13 1.7626 (0.0169) 93.73 (0.86) S13 - C15 S14 - Distance Angles C15 1.6961 (0.0176) C14 1.7432 (0.0162) 95.55 (0.85) S14 - C15 S15 - Distance Angles C17 1.7503 (0.0166) C16 1.7604 (0.0207) 94.14 (0.90) S15 - C17 S16 - Distance Angles C16 1.7135 (0.0196) C18 1.7694 (0.0202) 96.84 (0.93) S16 - C16 S17 - Distance Angles C18 1.7345 (0.0183) C219_b 1.8091 (0.0161) 100.70 (1.10) C19_a 1.8197 (0.0167) 98.04 (1.24) 27.31 (1.24) S17 - C18 C219_b S18 - Distance Angles C20_a 1.8081 (0.0173) C17 1.8088 (0.0184) 99.70 (1.27) C220_b 1.8140 (0.0151) 26.34 (1.26) 98.67 (0.99) S18 - C20_a C17 C21 - Distance Angles C22 1.5030 (0.0268) S21 1.8245 (0.0199) 113.44 (1.42) H21G 0.9900 108.88 108.88 H21H 0.9900 108.88 108.88 107.72 C21 - C22 S21 H21G C22 - Distance Angles C21 1.5030 (0.0268) S22 1.8074 (0.0234) 113.53 (1.47) H22C 0.9900 108.86 108.86 H22D 0.9900 108.86 108.86 107.71 C22 - C21 S22 H22C C23 - Distance Angles C24 1.2633 (0.0282) S23 1.7903 (0.0202) 120.75 (1.62) S22 1.7924 (0.0212) 127.92 (1.66) 110.87 (1.15) C23 - C24 S23 C24 - Distance Angles C23 1.2633 (0.0282) S21 1.7130 (0.0200) 131.38 (1.68) S24 1.7918 (0.0202) 115.69 (1.56) 112.73 (1.17) C24 - C23 S21 C25 - Distance Angles C26 1.3493 (0.0167) S23 1.7166 (0.0214) 122.44 (1.16) S24 1.7622 (0.0209) 120.54 (1.17) 116.84 (1.22) C25 - C26 S23 C26 - Distance Angles C25 1.3493 (0.0167) S26 1.7482 (0.0217) 122.90 (1.24) S25 1.7982 (0.0230) 123.22 (1.18) 113.86 (1.21) C26 - C25 S26 C27 - Distance Angles C28 1.4113 (0.0293) S28 1.7043 (0.0216) 129.09 (1.61) S25 1.7444 (0.0213) 113.11 (1.51) 117.66 (1.28) C27 - C28 S28 C28 - Distance Angles C27 1.4113 (0.0293) S26 1.7071 (0.0206) 120.69 (1.55) S27 1.7632 (0.0214) 125.33 (1.54) 113.48 (1.26) C28 - C27 S26 C29 - Distance Angles C30 1.4977 (0.0267) S27 1.8027 (0.0221) 114.93 (1.47) H29A 0.9900 108.53 108.53 H29B 0.9900 108.53 108.53 107.53 C29 - C30 S27 H29A C30 - Distance Angles C29 1.4977 (0.0267) S28 1.8067 (0.0212) 114.55 (1.40) H30A 0.9900 108.62 108.62 H30B 0.9900 108.62 108.62 107.58 C30 - C29 S28 H30A S21 - Distance Angles C24 1.7130 (0.0201) C21 1.8245 (0.0199) 101.19 (1.02) S21 - C24 S22 - Distance Angles C23 1.7924 (0.0213) C22 1.8074 (0.0236) 100.79 (1.07) S22 - C23 S23 - Distance Angles C25 1.7166 (0.0215) C23 1.7903 (0.0203) 92.56 (1.02) S23 - C25 S24 - Distance Angles C25 1.7622 (0.0211) C24 1.7918 (0.0202) 93.66 (0.98) S24 - C25 S25 - Distance Angles C27 1.7444 (0.0213) C26 1.7982 (0.0230) 96.57 (1.03) S25 - C27 S26 - Distance Angles C28 1.7071 (0.0206) C26 1.7482 (0.0219) 95.39 (1.07) S26 - C28 S27 - Distance Angles C28 1.7632 (0.0215) C29 1.8027 (0.0221) 102.70 (1.05) S27 - C28 S28 - Distance Angles C27 1.7043 (0.0216) C30 1.8067 (0.0212) 102.52 (1.04) S28 - C27 C31 - Distance Angles O31 1.1942 (0.0209) O34 1.2377 (0.0208) 131.07 (1.89) C32 1.6253 (0.0270) 113.98 (1.58) 114.53 (1.68) C31 - O31 O34 C32 - Distance Angles O33 1.2239 (0.0209) O32 1.2496 (0.0227) 127.66 (2.00) C31 1.6253 (0.0271) 119.08 (1.80) 113.25 (1.60) C32 - O33 O32 O31 - Distance Angles C31 1.1942 (0.0210) Cr1 1.9678 (0.0140) 114.74 (1.24) O31 - C31 O32 - Distance Angles C32 1.2496 (0.0227) Cr1 2.0195 (0.0137) 111.70 (1.24) O32 - C32 O33 - Distance Angles C32 1.2239 (0.0209) Na1 2.3378 (0.0169) 117.90 (1.42) O33 - C32 O34 - Distance Angles C31 1.2377 (0.0208) Na1 2.4064 (0.0138) 117.82 (1.29) O34 - C31 C41 - Distance Angles O41 1.2046 (0.0192) O44 1.2397 (0.0191) 127.46 (1.45) C42 1.5442 (0.0182) 116.54 (1.28) 115.87 (1.41) C41 - O41 O44 C42 - Distance Angles O43 1.2436 (0.0224) O42 1.3146 (0.0230) 123.86 (1.70) C41 1.5442 (0.0182) 123.17 (1.62) 112.67 (1.47) C42 - O43 O42 O41 - Distance Angles C41 1.2046 (0.0192) Cr1 1.9983 (0.0126) 114.24 (0.99) O41 - C41 O42 - Distance Angles C42 1.3146 (0.0230) Cr1 1.9552 (0.0130) 113.61 (1.07) O42 - C42 O43 - Distance Angles C42 1.2436 (0.0224) Na1_$4 2.3091 (0.0151) 110.67 (1.18) O43 - C42 O44 - Distance Angles C41 1.2397 (0.0191) Na1_$4 2.2918 (0.0139) 115.62 (1.04) O44 - C41 C51 - Distance Angles O51 1.2604 (0.0181) O54 1.2842 (0.0179) 125.00 (1.49) C52 1.5511 (0.0261) 117.01 (1.43) 117.40 (1.48) C51 - O51 O54 C52 - Distance Angles O53 1.2306 (0.0217) O52 1.3058 (0.0209) 127.58 (1.88) C51 1.5511 (0.0261) 120.98 (1.69) 111.32 (1.55) C52 - O53 O52 O51 - Distance Angles C51 1.2604 (0.0181) Cr1 1.9753 (0.0102) 111.73 (0.96) O51 - C51 O52 - Distance Angles C52 1.3058 (0.0209) Cr1 1.9842 (0.0117) 113.98 (1.13) O52 - C52 O53 - Distance Angles C52 1.2306 (0.0217) Na1_$3 2.2715 (0.0149) 110.78 (1.30) O53 - C52 O54 - Distance Angles C51 1.2842 (0.0179) Na1_$3 2.2821 (0.0140) 111.01 (1.06) O54 - C51 C61 - Distance Angles N61 1.1421 (0.0295) C62 1.4037 (0.0267) 176.00 (2.96) C61 - N61 C62 - Distance Angles C61 1.4037 (0.0267) H62A 0.9800 109.47 H62B 0.9800 109.47 109.47 H62C 0.9800 109.47 109.47 109.47 C62 - C61 H62A H62B N61 - Distance Angles C61 1.1421 (0.0295) N61 - FMAP and GRID set by program FMAP 2 3 38 GRID -1.429 -2 -2 1.429 2 2 R1 = 0.1620 for 5100 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.11 at 0.1996 0.2069 0.4184 [ 1.37 A from S23 ] Deepest hole -0.60 at 0.9273 0.0549 0.4119 [ 2.13 A from S16 ] Mean = 0.00, Rms deviation from mean = 0.16 e/A^3, Highest memory used = 6975 / 35241 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8004 0.7069 0.5816 1.00000 0.05 1.11 1.37 S23 2.59 C25 2.62 C23 2.93 C16 Q2 1 0.7088 1.0480 0.4157 1.00000 0.05 1.04 1.32 S25 2.58 C27 2.73 C26 2.86 C6 Q3 1 0.6982 0.7090 0.4427 1.00000 0.05 0.89 1.50 S26 2.48 C26 2.74 C28 2.87 C15 Q4 1 0.3045 0.6390 0.0020 1.00000 0.05 0.88 1.16 CR1 1.33 O31 1.63 O52 2.23 O51 Q5 1 0.8015 1.0517 0.5581 1.00000 0.05 0.86 1.57 S24 2.68 C25 2.80 C24 2.87 C5 Shortest distances between peaks (including symmetry equivalents) 1 3 2.66 2 5 2.69 Time profile in seconds ----------------------- 0.06: 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 0.00: Analyse other restraints etc. 8.02: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.17: Set up l.s. refinement 0.00: Generate idealized H-atoms 92.91: Structure factors and derivatives 184.56: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 1.30: Apply other restraints 24.13: Solve l.s. equations 0.00: Generate HTAB table 0.20: Other dependent quantities, CIF, tables 0.20: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0837r finished at 10:43:16 Total CPU time: 311.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++