+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s93 started at 14:51:20 on 31-Mar-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s93 in Pna2(1) CELL 0.71073 25.8077 11.9889 17.3842 90.000 90.000 90.000 ZERR 4.00 0.0052 0.0008 0.0032 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H N O CL CO UNIT 176 184 64 84 16 8 V = 5378.77 F(000) = 2848.0 Mu = 0.91 mm-1 Cell Wt = 5578.51 Rho = 1.722 MERG 2 OMIT -3.00 55.00 TWIN BASF 0.48101 SHEL 7 0.77 DFIX 21 0.01 CL1 O1 CL1 O2 CL1 O3 CL1 O4 DANG 21.6333 O1 O2 O1 O3 O1 O4 O2 O3 O2 O4 O3 O4 FMAP 2 PLAN 10 SIZE 0.16 0.24 0.36 ACTA BOND $H WGHT 0.07240 11.89580 L.S. 10 TEMP -153.00 FVAR 0.10979 1.42068 MOLE 1 C1 1 0.352452 0.391141 0.145044 11.00000 0.03674 0.03320 = 0.02364 0.00060 -0.01115 -0.00427 AFIX 43 H1 2 0.342887 0.350881 0.189919 11.00000 -1.20000 AFIX 0 C2 1 0.390318 0.470838 0.151571 11.00000 0.02577 0.02724 = 0.03434 -0.00081 -0.00229 -0.00259 AFIX 43 H2 2 0.406144 0.485255 0.199898 11.00000 -1.20000 AFIX 0 C3 1 0.404864 0.528727 0.088260 11.00000 0.02068 0.03044 = 0.04585 -0.00101 -0.00346 -0.00935 AFIX 43 H3 2 0.431210 0.583901 0.091222 11.00000 -1.20000 AFIX 0 C4 1 0.380325 0.505554 0.018677 11.00000 0.03006 0.02880 = 0.02919 -0.00384 0.00367 -0.00728 AFIX 43 H4 2 0.389560 0.545542 -0.026465 11.00000 -1.20000 AFIX 0 C5 1 0.343337 0.425945 0.015729 11.00000 0.01989 0.01870 = 0.02513 -0.00043 0.00654 0.00292 C6 1 0.314430 0.395087 -0.054175 11.00000 0.01939 0.01740 = 0.02210 0.00244 0.00038 0.00155 C7 1 0.325297 0.439302 -0.126471 11.00000 0.02421 0.02685 = 0.02452 0.00986 0.00782 -0.00114 AFIX 43 H7 2 0.352785 0.490928 -0.133793 11.00000 -1.20000 AFIX 0 C8 1 0.294614 0.405248 -0.187035 11.00000 0.03992 0.03316 = 0.00987 0.00206 0.00218 -0.00589 AFIX 43 H8 2 0.300912 0.434014 -0.237088 11.00000 -1.20000 AFIX 0 C9 1 0.254924 0.330011 -0.175882 11.00000 0.02755 0.02623 = 0.01946 0.00509 0.00275 -0.00242 AFIX 43 H9 2 0.234263 0.304866 -0.217653 11.00000 -1.20000 AFIX 0 C10 1 0.246156 0.292121 -0.101254 11.00000 0.02522 0.02540 = 0.01010 -0.00027 0.00395 0.00292 C11 1 0.204378 0.217365 -0.077641 11.00000 0.02205 0.01462 = 0.02063 -0.00522 0.00327 0.00426 C12 1 0.167371 0.041335 0.058962 11.00000 0.02464 0.02124 = 0.01607 -0.00002 -0.00408 -0.00106 C13 1 0.121505 0.012327 0.104273 11.00000 0.01943 0.02313 = 0.01572 -0.00121 -0.00082 0.00020 C14 1 0.107422 -0.092210 0.128257 11.00000 0.02695 0.01714 = 0.03363 0.00445 0.00186 0.00079 AFIX 43 H14 2 0.127717 -0.155917 0.116080 11.00000 -1.20000 AFIX 0 C15 1 0.062037 -0.101094 0.171294 11.00000 0.02997 0.02453 = 0.02507 0.01353 0.00370 0.00096 AFIX 43 H15 2 0.049814 -0.172500 0.186526 11.00000 -1.20000 AFIX 0 C16 1 0.035383 -0.008814 0.191423 11.00000 0.02843 0.02805 = 0.01825 0.00775 0.00158 -0.00853 AFIX 43 H16 2 0.005922 -0.015291 0.223881 11.00000 -1.20000 AFIX 0 C17 1 0.050428 0.094433 0.165442 11.00000 0.01645 0.03062 = 0.01584 0.00963 -0.00023 -0.00325 C18 1 0.025062 0.202824 0.179542 11.00000 0.01643 0.03922 = 0.02198 0.00159 -0.00048 -0.00415 C19 1 -0.016444 0.214363 0.227020 11.00000 0.02499 0.03735 = 0.02214 -0.00304 -0.00218 -0.00192 AFIX 43 H19 2 -0.032226 0.151277 0.250356 11.00000 -1.20000 AFIX 0 C20 1 -0.034788 0.319921 0.240136 11.00000 0.02017 0.04622 = 0.01908 -0.00294 0.00169 0.00399 AFIX 43 H20 2 -0.063485 0.331187 0.273469 11.00000 -1.20000 AFIX 0 C21 1 -0.011924 0.407772 0.205517 11.00000 0.02777 0.03401 = 0.02520 -0.00615 0.00070 0.00836 AFIX 43 H21 2 -0.023869 0.481439 0.215051 11.00000 -1.20000 AFIX 0 C22 1 0.028516 0.389561 0.156701 11.00000 0.03137 0.02648 = 0.02831 -0.00455 0.00049 0.00247 AFIX 43 H22 2 0.044512 0.451598 0.132370 11.00000 -1.20000 AFIX 0 C31 1 0.347796 0.096155 -0.030585 11.00000 0.02304 0.02693 = 0.03209 0.00866 0.00166 0.00448 AFIX 43 H31 2 0.333797 0.129975 -0.075423 11.00000 -1.20000 AFIX 0 C32 1 0.389042 0.022894 -0.038087 11.00000 0.02214 0.02539 = 0.03254 -0.00451 0.00533 -0.00086 AFIX 43 H32 2 0.403114 0.005988 -0.087220 11.00000 -1.20000 AFIX 0 C33 1 0.408575 -0.023534 0.025935 11.00000 0.02788 0.02240 = 0.04388 -0.00473 -0.00073 0.00607 AFIX 43 H33 2 0.436637 -0.074588 0.022585 11.00000 -1.20000 AFIX 0 C34 1 0.387884 0.003023 0.095948 11.00000 0.02723 0.03018 = 0.03604 0.00427 -0.00529 0.01084 AFIX 43 H34 2 0.402258 -0.026888 0.141834 11.00000 -1.20000 AFIX 0 C35 1 0.345772 0.073982 0.099020 11.00000 0.01508 0.02115 = 0.02355 0.00025 0.00012 -0.00196 C36 1 0.318586 0.098803 0.171331 11.00000 0.01634 0.01512 = 0.03164 0.00027 -0.00853 0.00079 C37 1 0.329753 0.058377 0.243750 11.00000 0.03051 0.02416 = 0.02952 -0.00207 -0.00938 0.00561 AFIX 43 H37 2 0.357138 0.006474 0.250986 11.00000 -1.20000 AFIX 0 C38 1 0.301360 0.093404 0.304014 11.00000 0.02255 0.02707 = 0.03558 0.00582 -0.01140 -0.00156 AFIX 43 H38 2 0.309932 0.068734 0.354362 11.00000 -1.20000 AFIX 0 C39 1 0.259754 0.165032 0.293606 11.00000 0.03017 0.02677 = 0.01913 0.00098 -0.00952 -0.00059 AFIX 43 H39 2 0.238774 0.187914 0.335644 11.00000 -1.20000 AFIX 0 C40 1 0.250210 0.201082 0.221127 11.00000 0.01598 0.01518 = 0.02700 0.00083 -0.00475 -0.00304 C41 1 0.206296 0.272242 0.195666 11.00000 0.01641 0.01663 = 0.01689 0.00446 -0.00246 0.00142 C42 1 0.167898 0.447629 0.061035 11.00000 0.01724 0.01370 = 0.01894 -0.00415 0.00038 -0.00067 C43 1 0.121819 0.474358 0.012057 11.00000 0.01748 0.01821 = 0.02213 0.00339 0.00457 -0.00005 C44 1 0.108800 0.578193 -0.013180 11.00000 0.03216 0.02301 = 0.02143 0.00559 -0.00260 -0.00015 AFIX 43 H44 2 0.129370 0.641425 -0.000843 11.00000 -1.20000 AFIX 0 C45 1 0.064736 0.588068 -0.057213 11.00000 0.03468 0.03320 = 0.03112 0.00645 0.00038 0.01919 AFIX 43 H45 2 0.054266 0.659213 -0.075582 11.00000 -1.20000 AFIX 0 C46 1 0.035665 0.494546 -0.074769 11.00000 0.01961 0.04049 = 0.03142 0.01043 -0.00443 0.00026 AFIX 43 H46 2 0.005650 0.499741 -0.106202 11.00000 -1.20000 AFIX 0 C47 1 0.051458 0.394740 -0.045537 11.00000 0.02314 0.02916 = 0.01773 -0.00052 0.00230 0.00441 C48 1 0.025360 0.288361 -0.060112 11.00000 0.01968 0.02826 = 0.01506 -0.00139 0.00380 0.00176 C49 1 -0.016495 0.274234 -0.108381 11.00000 0.01997 0.04069 = 0.02269 0.00167 -0.00534 0.00189 AFIX 43 H49 2 -0.031781 0.336536 -0.133386 11.00000 -1.20000 AFIX 0 C50 1 -0.035830 0.168445 -0.119829 11.00000 0.02311 0.05442 = 0.02625 -0.00938 -0.00264 -0.00409 AFIX 43 H50 2 -0.065202 0.158407 -0.152033 11.00000 -1.20000 AFIX 0 C51 1 -0.013686 0.078273 -0.085938 11.00000 0.02326 0.04366 = 0.03404 -0.00648 0.00086 -0.00653 AFIX 43 H51 2 -0.026182 0.004915 -0.095036 11.00000 -1.20000 AFIX 0 C52 1 0.027771 0.097873 -0.037693 11.00000 0.02233 0.02587 = 0.03038 -0.00384 -0.00005 -0.00274 AFIX 43 H52 2 0.043392 0.035819 -0.012850 11.00000 -1.20000 AFIX 0 N1 3 0.328298 0.366914 0.079369 11.00000 0.01809 0.02903 = 0.02717 0.00366 -0.00826 -0.00392 N2 3 0.276386 0.324905 -0.044522 11.00000 0.02064 0.01588 = 0.02186 0.00309 0.00722 0.00288 N3 3 0.163921 0.205277 -0.123482 11.00000 0.02285 0.03437 = 0.01719 0.00150 -0.00371 -0.00399 AFIX 93 H3A 2 0.137108 0.165614 -0.108325 11.00000 -1.20000 H3B 2 0.163793 0.236889 -0.169167 11.00000 -1.20000 AFIX 0 N4 3 0.209812 0.175925 -0.009523 11.00000 0.01879 0.01527 = 0.01975 0.00157 0.00275 -0.00118 N5 3 0.163668 0.135964 0.021660 11.00000 0.02293 0.01760 = 0.02114 -0.00222 0.00573 -0.00115 N6 3 0.208611 -0.023415 0.059107 11.00000 0.02524 0.01891 = 0.02305 0.00418 -0.00232 0.00245 AFIX 93 H6A 2 0.236319 -0.004042 0.032803 11.00000 -1.20000 H6B 2 0.208450 -0.086043 0.085506 11.00000 -1.20000 AFIX 0 N7 3 0.093641 0.102137 0.122184 11.00000 0.02328 0.01868 = 0.02189 0.00056 -0.00390 -0.00545 N8 3 0.046163 0.288279 0.142172 11.00000 0.01878 0.02040 = 0.02864 -0.00344 -0.00030 0.00816 N31 3 0.327529 0.120152 0.036580 11.00000 0.02750 0.01525 = 0.02392 0.00368 -0.00278 0.00397 N32 3 0.279204 0.169737 0.160376 11.00000 0.01290 0.02107 = 0.01896 -0.00312 0.00260 -0.00171 N33 3 0.166675 0.289338 0.242145 11.00000 0.02241 0.03383 = 0.02767 0.00680 0.00139 0.00807 AFIX 93 H33A 2 0.140307 0.330201 0.226784 11.00000 -1.20000 H33B 2 0.166615 0.259878 0.288510 11.00000 -1.20000 AFIX 0 N34 3 0.210353 0.311156 0.127062 11.00000 0.01046 0.01993 = 0.02327 -0.00033 -0.00371 -0.00064 N35 3 0.163643 0.353209 0.097068 11.00000 0.01142 0.02751 = 0.01831 0.00842 0.00076 0.00055 N36 3 0.208609 0.513082 0.059179 11.00000 0.01823 0.02163 = 0.03287 0.00335 -0.00644 0.00111 AFIX 93 H36A 2 0.236931 0.494293 0.084212 11.00000 -1.20000 H36B 2 0.207597 0.575781 0.032902 11.00000 -1.20000 AFIX 0 N37 3 0.093303 0.385982 -0.003187 11.00000 0.00930 0.02541 = 0.01478 0.00301 0.00138 0.00217 N38 3 0.047167 0.199184 -0.023968 11.00000 0.01827 0.02807 = 0.01545 0.00232 -0.00533 0.00466 CO1 6 0.269734 0.245706 0.058161 11.00000 0.01523 0.01809 = 0.01831 0.00319 -0.00045 -0.00056 CO2 6 0.104090 0.244260 0.059391 11.00000 0.01542 0.01798 = 0.01833 0.00136 -0.00064 -0.00063 MOLE 2 O1 4 0.434272 0.671299 0.265554 11.00000 0.03126 0.02758 = 0.04027 0.00796 -0.00551 -0.00086 O2 4 0.424493 0.864235 0.271149 11.00000 0.03890 0.02560 = 0.03186 -0.00927 -0.01118 -0.00210 O3 4 0.445379 0.779242 0.155452 11.00000 0.04776 0.05074 = 0.03958 -0.00435 0.01188 0.00201 O4 4 0.363582 0.758902 0.207590 11.00000 0.03392 0.04545 = 0.04768 -0.00120 -0.01733 -0.00459 CL1 5 0.418540 0.767806 0.225013 11.00000 0.02742 0.02306 = 0.03221 -0.00177 0.00060 -0.00061 MOLE 3 SAME O1 > CL1 O11 4 0.077405 0.135025 0.342292 11.00000 0.04264 0.02869 = 0.02942 0.00400 0.00417 0.00889 O12 4 0.065178 0.328304 0.344721 11.00000 0.05681 0.01850 = 0.04457 -0.00146 -0.02246 0.00343 O13 4 0.136913 0.245365 0.403573 11.00000 0.02032 0.05831 = 0.04275 -0.00029 -0.00053 -0.00236 O14 4 0.055737 0.223682 0.457512 11.00000 0.06441 0.05892 = 0.03298 0.00584 0.01782 0.02571 CL11 5 0.081890 0.232956 0.387112 11.00000 0.03798 0.02636 = 0.02363 0.00056 -0.00197 -0.00108 MOLE 4 SAME O1 > CL1 O21 4 0.309776 0.398054 0.388620 11.00000 0.03606 0.07353 = 0.06338 -0.00207 0.00759 0.01113 O22 4 0.386693 0.352437 0.451586 11.00000 0.08884 0.06524 = 0.03633 0.00780 -0.00037 0.02382 O23 4 0.386687 0.482042 0.354243 11.00000 0.08834 0.02532 = 0.09085 0.00697 0.00906 -0.00665 O24 4 0.374457 0.297418 0.325112 11.00000 0.05650 0.05484 = 0.04343 -0.02431 0.00658 0.01279 CL21 5 0.363969 0.382062 0.378890 11.00000 0.06330 0.02311 = 0.02198 -0.00221 0.00757 -0.00279 MOLE 5 SAME O1 > CL1 O31 4 0.131697 0.703936 0.283577 11.00000 0.06406 0.02957 = 0.08274 -0.01973 -0.02597 0.00085 O32 4 0.122360 0.639483 0.161420 11.00000 0.13897 0.05164 = 0.04134 0.01271 0.02724 0.01793 O33 4 0.140048 0.516323 0.257331 11.00000 0.10350 0.03763 = 0.10451 -0.00252 -0.04632 0.01637 O34 4 0.059965 0.600639 0.251708 11.00000 0.03590 0.12445 = 0.11137 -0.06914 0.02953 -0.01591 CL31 5 0.115185 0.614570 0.237994 11.00000 0.08088 0.02612 = 0.03066 -0.00106 0.00581 0.00049 MOLE 6 O51 4 0.269634 0.204134 0.471973 11.00000 0.06733 0.03443 = 0.02503 0.00242 -0.00019 0.01401 O52 4 0.242726 0.539840 0.310576 11.00000 0.06913 0.06824 = 0.08509 0.02422 -0.01560 0.00435 O53 4 0.280459 0.601580 0.172400 11.00000 0.04292 0.05444 = 0.06606 -0.00924 -0.00515 0.00188 O54 4 0.217081 0.781291 0.151305 11.00000 0.07497 0.04800 = 0.03826 0.00709 -0.00182 0.02189 O55 4 0.316701 0.791769 0.046588 11.00000 0.06174 0.09091 = 0.05573 -0.01880 0.02217 -0.03165 HKLF 4 Covalent radii and connectivity table for s93 in Pna2(1) C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 CO 1.250 C1 - N1 C2 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - C4 N1 C6 C6 - N2 C7 C5 C7 - C8 C6 C8 - C9 C7 C9 - C8 C10 C10 - N2 C9 C11 C11 - N4 N3 C10 C12 - N5 N6 C13 C13 - N7 C14 C12 C14 - C13 C15 C15 - C16 C14 C16 - C15 C17 C17 - N7 C16 C18 C18 - N8 C19 C17 C19 - C18 C20 C20 - C21 C19 C21 - C20 C22 C22 - N8 C21 C31 - N31 C32 C32 - C33 C31 C33 - C32 C34 C34 - C33 C35 C35 - N31 C34 C36 C36 - N32 C37 C35 C37 - C38 C36 C38 - C37 C39 C39 - C40 C38 C40 - N32 C39 C41 C41 - N34 N33 C40 C42 - N35 N36 C43 C43 - N37 C44 C42 C44 - C43 C45 C45 - C44 C46 C46 - C47 C45 C47 - N37 C46 C48 C48 - N38 C49 C47 C49 - C50 C48 C50 - C51 C49 C51 - C50 C52 C52 - N38 C51 N1 - C1 C5 Co1 N2 - C6 C10 Co1 N3 - C11 N4 - C11 N5 Co1 N5 - C12 N4 Co2 N6 - C12 N7 - C13 C17 Co2 N8 - C22 C18 Co2 N31 - C35 C31 Co1 N32 - C36 C40 Co1 N33 - C41 N34 - C41 N35 Co1 N35 - C42 N34 Co2 N36 - C42 N37 - C47 C43 Co2 N38 - C52 C48 Co2 Co1 - N32 N2 N34 N4 N1 N31 Co2 - N37 N7 N5 N35 N38 N8 O1 - Cl1 O2 - Cl1 O3 - Cl1 O4 - Cl1 Cl1 - O3 O1 O2 O4 O11 - Cl11 O12 - Cl11 O13 - Cl11 O14 - Cl11 Cl11 - O14 O11 O12 O13 O21 - Cl21 O22 - Cl21 O23 - Cl21 O24 - Cl21 Cl21 - O23 O24 O21 O22 O31 - Cl31 O32 - Cl31 O33 - Cl31 O34 - Cl31 Cl31 - O32 O33 O31 O34 O51 - no bonds found O52 - no bonds found O53 - no bonds found O54 - no bonds found O55 - no bonds found Floating origin restraints generated h k l Fo^2 Sigma Why rejected 0 7 -4 4.58 1.14 observed but should be systematically absent 19 0 6 4.48 1.12 observed but should be systematically absent 19 0 -5 4.56 1.14 observed but should be systematically absent 19 0 -5 4.54 1.13 observed but should be systematically absent 9 0 -9 4.50 1.12 observed but should be systematically absent 9 0 -9 4.54 1.13 observed but should be systematically absent 5 0 0 4.56 1.14 observed but should be systematically absent 5 0 0 4.56 1.14 observed but should be systematically absent 9 0 9 4.50 1.12 observed but should be systematically absent 9 0 9 5.66 1.13 observed but should be systematically absent 0 3 4 4.62 1.15 observed but should be systematically absent 0 7 -4 5.69 1.14 observed but should be systematically absent 0 7 -4 4.53 1.13 observed but should be systematically absent 76314 Reflections read, of which 3602 rejected -32 =< h =< 33, -15 =< k =< 15, -22 =< l =< 22, Max. 2-theta = 54.96 13 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 9 -4 110.83 0.95 10 6.09 5 10 -4 59.80 0.93 7 6.03 6 10 -3 58.10 0.88 8 4.79 7 11 -3 5.49 0.51 6 6.17 9 13 -2 3.68 1.12 2 6.31 3 1 -1 28.89 0.34 11 2.36 0 3 -1 20.95 0.53 6 2.87 4 0 0 656.01 6.90 6 132.76 6 9 2 182.13 1.08 7 18.22 0 12 12 4.93 0.92 4 6.39 10 Inconsistent equivalents 12146 Unique reflections, of which 0 suppressed R(int) = 0.0606 R(sigma) = 0.0525 Friedel opposites not merged Maximum memory for data reduction = 6050 / 121210 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. ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 176.00 176.00 H 184.00 144.00 N 64.00 64.00 O 84.00 84.00 CL 16.00 16.00 CO 8.00 8.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 8096 / 1139194 wR2 = 0.1512 before cycle 1 for 12146 data and 786 / 786 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 1.4542 1.4207 0.0336 0.0100 DFIX Cl1 O4 0.0734 0.0200 SAME/SADI O33 Cl31 O13 Cl11 0.0610 0.0200 SAME/SADI O32 Cl31 O22 Cl21 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.020 0.012 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.023 for 71 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0724 * P )^2 + 11.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10979 0.00017 0.015 OSF 2 1.42067 0.00516 -0.001 FVAR 2 3 0.48086 0.02310 -0.006 BASF 1 Mean shift/esd = 0.017 Maximum = 0.768 for x O4 Max. shift = 0.004 A for O4 Max. dU = 0.000 for O14 Least-squares cycle 2 Maximum vector length = 511 Memory required = 8096 / 1139194 wR2 = 0.1512 before cycle 2 for 12146 data and 786 / 786 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.0758 0.0200 SAME/SADI O33 Cl31 O13 Cl11 0.0609 0.0200 SAME/SADI O32 Cl31 O22 Cl21 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.013 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.023 for 71 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0724 * P )^2 + 11.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10979 0.00017 -0.002 OSF 2 1.42067 0.00516 0.000 FVAR 2 3 0.48071 0.02309 -0.007 BASF 1 Mean shift/esd = 0.009 Maximum = 0.255 for x O4 Max. shift = 0.001 A for O4 Max. dU = 0.000 for O13 Least-squares cycle 3 Maximum vector length = 511 Memory required = 8096 / 1139194 wR2 = 0.1512 before cycle 3 for 12146 data and 786 / 786 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.0767 0.0200 SAME/SADI O33 Cl31 O13 Cl11 0.0609 0.0200 SAME/SADI O32 Cl31 O22 Cl21 Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.013 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.024 for 71 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0724 * P )^2 + 11.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10979 0.00017 -0.002 OSF 2 1.42067 0.00516 0.000 FVAR 2 3 0.48069 0.02310 -0.001 BASF 1 Mean shift/esd = 0.005 Maximum = -0.031 for x Cl11 Max. shift = 0.000 A for O54 Max. dU = 0.000 for O13 Least-squares cycle 4 Maximum vector length = 511 Memory required = 8096 / 1139194 wR2 = 0.1512 before cycle 4 for 12146 data and 786 / 786 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.0769 0.0200 SAME/SADI O33 Cl31 O13 Cl11 0.0610 0.0200 SAME/SADI O32 Cl31 O22 Cl21 Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.013 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.023 for 71 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0724 * P )^2 + 11.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10979 0.00017 0.001 OSF 2 1.42067 0.00516 0.000 FVAR 2 3 0.48070 0.02310 0.000 BASF 1 Mean shift/esd = 0.003 Maximum = -0.015 for x Cl11 Max. shift = 0.000 A for C4 Max. dU = 0.000 for O13 Least-squares cycle 5 Maximum vector length = 511 Memory required = 8096 / 1139194 wR2 = 0.1512 before cycle 5 for 12146 data and 786 / 786 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.0770 0.0200 SAME/SADI O33 Cl31 O13 Cl11 0.0611 0.0200 SAME/SADI O32 Cl31 O22 Cl21 Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.016 0.013 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.024 for 71 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0724 * P )^2 + 11.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10979 0.00017 0.001 OSF 2 1.42067 0.00516 0.000 FVAR 2 3 0.48071 0.02310 0.001 BASF 1 Mean shift/esd = 0.001 Maximum = -0.007 for x Cl11 Max. shift = 0.000 A for C4 Max. dU = 0.000 for O13 Least-squares cycle 6 Maximum vector length = 511 Memory required = 8096 / 1139194 wR2 = 0.1512 before cycle 6 for 12146 data and 786 / 786 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.0770 0.0200 SAME/SADI O33 Cl31 O13 Cl11 0.0612 0.0200 SAME/SADI O32 Cl31 O22 Cl21 Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.016 0.013 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.024 for 71 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0724 * P )^2 + 11.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10979 0.00017 -0.001 OSF 2 1.42068 0.00516 0.001 FVAR 2 3 0.48072 0.02310 0.000 BASF 1 Mean shift/esd = 0.001 Maximum = -0.005 for U33 O23 Max. shift = 0.000 A for C4 Max. dU = 0.000 for O13 Least-squares cycle 7 Maximum vector length = 511 Memory required = 8096 / 1139194 wR2 = 0.1512 before cycle 7 for 12146 data and 786 / 786 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.0770 0.0200 SAME/SADI O33 Cl31 O13 Cl11 0.0612 0.0200 SAME/SADI O32 Cl31 O22 Cl21 Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.016 0.013 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.024 for 71 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0724 * P )^2 + 11.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10979 0.00017 -0.001 OSF 2 1.42068 0.00516 0.000 FVAR 2 3 0.48072 0.02310 0.000 BASF 1 Mean shift/esd = 0.001 Maximum = -0.003 for U33 O23 Max. shift = 0.000 A for C4 Max. dU = 0.000 for O23 Least-squares cycle 8 Maximum vector length = 511 Memory required = 8096 / 1139194 wR2 = 0.1512 before cycle 8 for 12146 data and 786 / 786 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 0.0770 0.0200 SAME/SADI O33 Cl31 O13 Cl11 0.0612 0.0200 SAME/SADI O32 Cl31 O22 Cl21 Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.016 0.013 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.024 for 71 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0724 * P )^2 + 11.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10979 0.00017 -0.001 OSF 2 1.42068 0.00516 0.000 FVAR 2 3 0.48072 0.02310 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.003 for U33 O23 Max. shift = 0.000 A for C4 Max. dU = 0.000 for O23 Least-squares cycle 9 Maximum vector length = 511 Memory required = 8096 / 1139194 wR2 = 0.1512 before cycle 9 for 12146 data and 786 / 786 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 0.0770 0.0200 SAME/SADI O33 Cl31 O13 Cl11 0.0613 0.0200 SAME/SADI O32 Cl31 O22 Cl21 Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.016 0.013 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.024 for 71 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0724 * P )^2 + 11.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10979 0.00017 -0.001 OSF 2 1.42068 0.00516 0.000 FVAR 2 3 0.48072 0.02310 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.002 for U33 O23 Max. shift = 0.000 A for H34 Max. dU = 0.000 for O23 Least-squares cycle 10 Maximum vector length = 511 Memory required = 8096 / 1139194 wR2 = 0.1512 before cycle 10 for 12146 data and 786 / 786 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 0.0770 0.0200 SAME/SADI O33 Cl31 O13 Cl11 0.0613 0.0200 SAME/SADI O32 Cl31 O22 Cl21 Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.016 0.013 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.024 for 71 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0724 * P )^2 + 11.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10979 0.00017 0.000 OSF 2 1.42068 0.00516 0.000 FVAR 2 3 0.48072 0.02310 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.001 for U33 O23 Max. shift = 0.000 A for C4 Max. dU = 0.000 for O23 Largest correlation matrix elements -0.697 U11 Cl11 / U11 Cl1 -0.631 U13 Cl11 / U13 Cl1 -0.626 U11 O13 / U11 O4 -0.684 U13 O13 / U13 O4 0.631 x Cl11 / x Cl1 -0.625 U33 C49 / U33 C19 -0.683 U33 O13 / U33 O4 -0.630 U22 O13 / U22 O4 -0.625 U11 C48 / U11 C18 -0.654 U23 Cl11 / U23 Cl1 0.630 z O13 / z O4 0.624 U13 C42 / U13 C12 -0.653 U23 O14 / U23 O3 -0.628 U33 C39 / U33 C9 0.623 z N36 / z N6 -0.640 U23 C49 / U23 C19 -0.627 U33 C36 / U33 C6 -0.622 U33 C37 / U33 C7 0.638 U13 N36 / U13 N6 0.627 x O13 / x O4 -0.617 U33 N31 / U33 N1 -0.635 U33 O14 / U33 O3 -0.627 U33 C43 / U33 C13 0.616 z C35 / z C5 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.3429 0.3508 0.1899 43 0.950 0.000 C1 N1 C2 H2 0.4061 0.4853 0.1999 43 0.950 0.000 C2 C3 C1 H3 0.4312 0.5840 0.0912 43 0.950 0.000 C3 C2 C4 H4 0.3896 0.5454 -0.0265 43 0.950 0.000 C4 C5 C3 H7 0.3528 0.4909 -0.1338 43 0.950 0.000 C7 C8 C6 H8 0.3009 0.4340 -0.2371 43 0.950 0.000 C8 C9 C7 H9 0.2343 0.3049 -0.2177 43 0.950 0.000 C9 C8 C10 H14 0.1277 -0.1559 0.1161 43 0.950 0.000 C14 C13 C15 H15 0.0498 -0.1725 0.1865 43 0.950 0.000 C15 C16 C14 H16 0.0059 -0.0153 0.2239 43 0.950 0.000 C16 C15 C17 H19 -0.0322 0.1512 0.2503 43 0.950 0.000 C19 C18 C20 H20 -0.0635 0.3312 0.2735 43 0.950 0.000 C20 C21 C19 H21 -0.0239 0.4815 0.2150 43 0.950 0.000 C21 C20 C22 H22 0.0445 0.4516 0.1324 43 0.950 0.000 C22 N8 C21 H31 0.3338 0.1299 -0.0755 43 0.950 0.000 C31 N31 C32 H32 0.4031 0.0060 -0.0872 43 0.950 0.000 C32 C33 C31 H33 0.4367 -0.0745 0.0225 43 0.950 0.000 C33 C32 C34 H34 0.4022 -0.0270 0.1419 43 0.950 0.000 C34 C33 C35 H37 0.3571 0.0065 0.2510 43 0.950 0.000 C37 C38 C36 H38 0.3099 0.0687 0.3544 43 0.950 0.000 C38 C37 C39 H39 0.2388 0.1879 0.3356 43 0.950 0.000 C39 C40 C38 H44 0.1294 0.6414 -0.0008 43 0.950 0.000 C44 C43 C45 H45 0.0543 0.6592 -0.0756 43 0.950 0.000 C45 C44 C46 H46 0.0057 0.4997 -0.1063 43 0.950 0.000 C46 C47 C45 H49 -0.0318 0.3365 -0.1334 43 0.950 0.000 C49 C50 C48 H50 -0.0652 0.1584 -0.1520 43 0.950 0.000 C50 C51 C49 H51 -0.0262 0.0050 -0.0950 43 0.950 0.000 C51 C50 C52 H52 0.0434 0.0358 -0.0128 43 0.950 0.000 C52 N38 C51 H3A 0.1371 0.1656 -0.1083 93 0.880 0.000 N3 C11 N4 H3B 0.1638 0.2369 -0.1692 93 0.880 0.000 N3 C11 N4 H6A 0.2363 -0.0040 0.0327 93 0.880 0.000 N6 C12 N5 H6B 0.2085 -0.0860 0.0855 93 0.880 0.000 N6 C12 N5 H33A 0.1403 0.3302 0.2268 93 0.880 0.000 N33 C41 N34 H33B 0.1666 0.2599 0.2885 93 0.880 0.000 N33 C41 N34 H36A 0.2369 0.4943 0.0842 93 0.880 0.000 N36 C42 N35 H36B 0.2076 0.5758 0.0329 93 0.880 0.000 N36 C42 N35 s93 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.35247 0.39112 0.14502 1.00000 0.03670 0.03305 0.02373 0.00059 -0.01110 -0.00409 0.03116 0.01091 0.00026 0.00056 0.00040 0.00000 0.00373 0.00348 0.00348 0.00274 0.00267 0.00282 0.00151 H1 0.34294 0.35079 0.18988 1.00000 0.03739 0.00000 0.00000 C2 0.39032 0.47085 0.15157 1.00000 0.02571 0.02735 0.03426 -0.00085 -0.00234 -0.00255 0.02911 0.01158 0.00025 0.00053 0.00042 0.00000 0.00350 0.00318 0.00410 0.00273 0.00281 0.00268 0.00146 H2 0.40614 0.48529 0.19990 1.00000 0.03493 0.00000 0.00000 C3 0.40485 0.52874 0.08825 1.00000 0.02071 0.03044 0.04579 -0.00102 -0.00356 -0.00939 0.03231 0.01110 0.00025 0.00056 0.00041 0.00000 0.00321 0.00335 0.00449 0.00288 0.00287 0.00256 0.00160 H3 0.43118 0.58395 0.09121 1.00000 0.03878 0.00000 0.00000 C4 0.38034 0.50552 0.01869 1.00000 0.03015 0.02882 0.02922 -0.00383 0.00375 -0.00734 0.02940 0.01125 0.00026 0.00054 0.00041 0.00000 0.00340 0.00322 0.00372 0.00264 0.00272 0.00263 0.00145 H4 0.38960 0.54545 -0.02646 1.00000 0.03528 0.00000 0.00000 C5 0.34333 0.42597 0.01573 1.00000 0.01989 0.01864 0.02534 -0.00045 0.00667 0.00303 0.02129 0.01084 0.00023 0.00047 0.00038 0.00000 0.00307 0.00287 0.00349 0.00241 0.00244 0.00222 0.00128 C6 0.31443 0.39507 -0.05418 1.00000 0.01955 0.01739 0.02200 0.00246 0.00048 0.00155 0.01965 0.01011 0.00022 0.00045 0.00035 0.00000 0.00288 0.00259 0.00325 0.00226 0.00229 0.00224 0.00119 C7 0.32529 0.43929 -0.12648 1.00000 0.02405 0.02680 0.02463 0.00985 0.00785 -0.00119 0.02516 0.01152 0.00023 0.00049 0.00038 0.00000 0.00304 0.00310 0.00338 0.00258 0.00258 0.00233 0.00133 H7 0.35278 0.49093 -0.13381 1.00000 0.03019 0.00000 0.00000 C8 0.29463 0.40523 -0.18702 1.00000 0.03996 0.03317 0.00981 0.00198 0.00224 -0.00576 0.02765 0.01092 0.00026 0.00051 0.00035 0.00000 0.00370 0.00325 0.00279 0.00234 0.00250 0.00277 0.00139 H8 0.30095 0.43397 -0.23708 1.00000 0.03318 0.00000 0.00000 C9 0.25493 0.33003 -0.17588 1.00000 0.02759 0.02625 0.01928 0.00513 0.00274 -0.00243 0.02438 0.01119 0.00024 0.00049 0.00036 0.00000 0.00324 0.00305 0.00326 0.00245 0.00246 0.00243 0.00132 H9 0.23426 0.30491 -0.21765 1.00000 0.02925 0.00000 0.00000 C10 0.24616 0.29211 -0.10123 1.00000 0.02527 0.02541 0.00995 -0.00031 0.00403 0.00300 0.02021 0.01030 0.00023 0.00049 0.00032 0.00000 0.00313 0.00302 0.00283 0.00222 0.00218 0.00235 0.00124 C11 0.20438 0.21736 -0.07764 1.00000 0.02213 0.01462 0.02058 -0.00521 0.00317 0.00427 0.01911 0.01036 0.00024 0.00049 0.00034 0.00000 0.00321 0.00240 0.00319 0.00238 0.00238 0.00252 0.00122 C12 0.16737 0.04133 0.05900 1.00000 0.02459 0.02127 0.01609 -0.00003 -0.00410 -0.00100 0.02065 0.00966 0.00021 0.00041 0.00039 0.00000 0.00278 0.00239 0.00277 0.00276 0.00282 0.00205 0.00107 C13 0.12151 0.01234 0.10427 1.00000 0.01933 0.02319 0.01573 -0.00118 -0.00080 0.00021 0.01942 0.00999 0.00022 0.00048 0.00035 0.00000 0.00292 0.00279 0.00297 0.00224 0.00220 0.00218 0.00122 C14 0.10743 -0.09224 0.12826 1.00000 0.02709 0.01705 0.03350 0.00436 0.00189 0.00075 0.02588 0.01086 0.00024 0.00048 0.00037 0.00000 0.00334 0.00263 0.00384 0.00238 0.00271 0.00227 0.00138 H14 0.12772 -0.15595 0.11608 1.00000 0.03106 0.00000 0.00000 C15 0.06203 -0.10110 0.17129 1.00000 0.02991 0.02453 0.02508 0.01354 0.00359 0.00089 0.02651 0.01200 0.00023 0.00056 0.00038 0.00000 0.00342 0.00308 0.00353 0.00252 0.00258 0.00242 0.00142 H15 0.04980 -0.17250 0.18652 1.00000 0.03181 0.00000 0.00000 C16 0.03538 -0.00883 0.19141 1.00000 0.02842 0.02811 0.01835 0.00773 0.00167 -0.00863 0.02496 0.01060 0.00024 0.00049 0.00036 0.00000 0.00341 0.00307 0.00311 0.00230 0.00245 0.00256 0.00134 H16 0.00592 -0.01531 0.22385 1.00000 0.02995 0.00000 0.00000 C17 0.05043 0.09445 0.16544 1.00000 0.01642 0.03066 0.01589 0.00965 -0.00025 -0.00324 0.02099 0.01077 0.00023 0.00053 0.00035 0.00000 0.00286 0.00325 0.00305 0.00240 0.00228 0.00244 0.00129 C18 0.02505 0.20282 0.17957 1.00000 0.01643 0.03924 0.02196 0.00165 -0.00045 -0.00420 0.02588 0.01104 0.00024 0.00058 0.00038 0.00000 0.00325 0.00394 0.00345 0.00281 0.00243 0.00273 0.00140 C19 -0.01643 0.21432 0.22700 1.00000 0.02507 0.03723 0.02211 -0.00308 -0.00228 -0.00172 0.02814 0.01174 0.00024 0.00063 0.00040 0.00000 0.00350 0.00329 0.00343 0.00313 0.00264 0.00295 0.00138 H19 -0.03221 0.15122 0.25031 1.00000 0.03377 0.00000 0.00000 C20 -0.03479 0.31993 0.24015 1.00000 0.02003 0.04609 0.01921 -0.00297 0.00168 0.00396 0.02844 0.01106 0.00024 0.00056 0.00038 0.00000 0.00314 0.00372 0.00315 0.00278 0.00261 0.00265 0.00139 H20 -0.06348 0.33119 0.27350 1.00000 0.03413 0.00000 0.00000 C21 -0.01192 0.40780 0.20550 1.00000 0.02753 0.03407 0.02534 -0.00611 0.00071 0.00837 0.02898 0.01136 0.00024 0.00055 0.00038 0.00000 0.00338 0.00326 0.00364 0.00258 0.00267 0.00259 0.00145 H21 -0.02386 0.48147 0.21502 1.00000 0.03478 0.00000 0.00000 C22 0.02850 0.38956 0.15671 1.00000 0.03141 0.02649 0.02831 -0.00458 0.00048 0.00240 0.02873 0.01163 0.00025 0.00057 0.00039 0.00000 0.00357 0.00325 0.00364 0.00265 0.00274 0.00270 0.00146 H22 0.04449 0.45160 0.13237 1.00000 0.03448 0.00000 0.00000 C31 0.34778 0.09612 -0.03061 1.00000 0.02305 0.02694 0.03194 0.00860 0.00163 0.00450 0.02731 0.01205 0.00024 0.00052 0.00042 0.00000 0.00307 0.00310 0.00379 0.00262 0.00256 0.00244 0.00141 H31 0.33377 0.12989 -0.07546 1.00000 0.03277 0.00000 0.00000 C32 0.38903 0.02291 -0.03809 1.00000 0.02224 0.02530 0.03255 -0.00447 0.00528 -0.00079 0.02670 0.01097 0.00024 0.00050 0.00040 0.00000 0.00331 0.00307 0.00390 0.00263 0.00274 0.00248 0.00140 H32 0.40310 0.00601 -0.08722 1.00000 0.03204 0.00000 0.00000 C33 0.40858 -0.02353 0.02591 1.00000 0.02757 0.02243 0.04398 -0.00479 -0.00079 0.00597 0.03133 0.01152 0.00026 0.00053 0.00041 0.00000 0.00354 0.00301 0.00426 0.00271 0.00305 0.00255 0.00155 H33 0.43665 -0.07455 0.02255 1.00000 0.03760 0.00000 0.00000 C34 0.38787 0.00300 0.09598 1.00000 0.02718 0.03026 0.03604 0.00424 -0.00530 0.01088 0.03116 0.01238 0.00026 0.00055 0.00044 0.00000 0.00328 0.00329 0.00398 0.00281 0.00280 0.00268 0.00149 H34 0.40222 -0.02696 0.14186 1.00000 0.03739 0.00000 0.00000 C35 0.34578 0.07402 0.09902 1.00000 0.01503 0.02119 0.02344 0.00024 0.00025 -0.00189 0.01989 0.01040 0.00022 0.00049 0.00038 0.00000 0.00282 0.00290 0.00339 0.00239 0.00238 0.00219 0.00124 C36 0.31857 0.09880 0.17134 1.00000 0.01626 0.01511 0.03166 0.00027 -0.00847 0.00080 0.02101 0.00980 0.00022 0.00047 0.00037 0.00000 0.00287 0.00260 0.00364 0.00229 0.00238 0.00215 0.00128 C37 0.32976 0.05837 0.24375 1.00000 0.03067 0.02418 0.02938 -0.00204 -0.00927 0.00557 0.02808 0.01058 0.00025 0.00048 0.00039 0.00000 0.00329 0.00298 0.00374 0.00262 0.00289 0.00245 0.00138 H37 0.35714 0.00647 0.25097 1.00000 0.03369 0.00000 0.00000 C38 0.30135 0.09340 0.30404 1.00000 0.02270 0.02707 0.03563 0.00588 -0.01139 -0.00144 0.02847 0.01112 0.00025 0.00050 0.00043 0.00000 0.00307 0.00310 0.00382 0.00270 0.00260 0.00241 0.00143 H38 0.30991 0.06873 0.35439 1.00000 0.03416 0.00000 0.00000 C39 0.25975 0.16503 0.29360 1.00000 0.03024 0.02676 0.01926 0.00098 -0.00955 -0.00055 0.02542 0.01023 0.00025 0.00050 0.00036 0.00000 0.00344 0.00313 0.00330 0.00248 0.00244 0.00252 0.00136 H39 0.23878 0.18793 0.33564 1.00000 0.03050 0.00000 0.00000 C40 0.25020 0.20107 0.22115 1.00000 0.01599 0.01516 0.02708 0.00088 -0.00472 -0.00302 0.01941 0.00961 0.00021 0.00042 0.00037 0.00000 0.00277 0.00263 0.00333 0.00237 0.00236 0.00211 0.00123 C41 0.20629 0.27224 0.19567 1.00000 0.01634 0.01663 0.01691 0.00448 -0.00254 0.00143 0.01663 0.01032 0.00023 0.00047 0.00034 0.00000 0.00294 0.00242 0.00290 0.00225 0.00224 0.00234 0.00117 C42 0.16789 0.44763 0.06106 1.00000 0.01720 0.01377 0.01888 -0.00409 0.00032 -0.00064 0.01662 0.00919 0.00019 0.00037 0.00038 0.00000 0.00248 0.00214 0.00277 0.00259 0.00262 0.00182 0.00101 C43 0.12181 0.47436 0.01206 1.00000 0.01755 0.01819 0.02207 0.00336 0.00453 -0.00008 0.01927 0.01043 0.00022 0.00046 0.00036 0.00000 0.00292 0.00264 0.00327 0.00227 0.00223 0.00208 0.00124 C44 0.10880 0.57816 -0.01318 1.00000 0.03201 0.02301 0.02151 0.00562 -0.00257 -0.00017 0.02551 0.01116 0.00025 0.00050 0.00036 0.00000 0.00350 0.00292 0.00319 0.00227 0.00262 0.00239 0.00133 H44 0.12937 0.64138 -0.00084 1.00000 0.03061 0.00000 0.00000 C45 0.06474 0.58806 -0.05722 1.00000 0.03470 0.03318 0.03107 0.00644 0.00039 0.01919 0.03298 0.01308 0.00026 0.00059 0.00042 0.00000 0.00373 0.00358 0.00398 0.00288 0.00284 0.00271 0.00165 H45 0.05427 0.65921 -0.07558 1.00000 0.03958 0.00000 0.00000 C46 0.03568 0.49454 -0.07480 1.00000 0.01963 0.04041 0.03128 0.01047 -0.00429 0.00020 0.03044 0.01198 0.00025 0.00055 0.00041 0.00000 0.00322 0.00369 0.00387 0.00280 0.00263 0.00268 0.00151 H46 0.00568 0.49973 -0.10626 1.00000 0.03653 0.00000 0.00000 C47 0.05146 0.39475 -0.04555 1.00000 0.02315 0.02917 0.01767 -0.00056 0.00227 0.00447 0.02333 0.01083 0.00023 0.00054 0.00036 0.00000 0.00318 0.00316 0.00315 0.00245 0.00245 0.00258 0.00131 C48 0.02538 0.28836 -0.06010 1.00000 0.01972 0.02829 0.01494 -0.00145 0.00376 0.00173 0.02098 0.01118 0.00023 0.00055 0.00035 0.00000 0.00327 0.00319 0.00300 0.00248 0.00233 0.00240 0.00125 C49 -0.01652 0.27419 -0.10840 1.00000 0.01986 0.04069 0.02275 0.00167 -0.00544 0.00205 0.02777 0.01188 0.00025 0.00064 0.00040 0.00000 0.00330 0.00345 0.00359 0.00296 0.00252 0.00287 0.00144 H49 -0.03181 0.33648 -0.13341 1.00000 0.03332 0.00000 0.00000 C50 -0.03582 0.16845 -0.11982 1.00000 0.02325 0.05459 0.02608 -0.00936 -0.00271 -0.00411 0.03464 0.01196 0.00025 0.00062 0.00043 0.00000 0.00341 0.00434 0.00343 0.00327 0.00297 0.00303 0.00156 H50 -0.06519 0.15841 -0.15202 1.00000 0.04157 0.00000 0.00000 C51 -0.01370 0.07831 -0.08595 1.00000 0.02351 0.04364 0.03395 -0.00661 0.00082 -0.00652 0.03370 0.01188 0.00025 0.00061 0.00042 0.00000 0.00342 0.00384 0.00406 0.00299 0.00278 0.00273 0.00161 H51 -0.02620 0.00496 -0.09504 1.00000 0.04044 0.00000 0.00000 C52 0.02779 0.09789 -0.03769 1.00000 0.02231 0.02586 0.03038 -0.00379 -0.00010 -0.00273 0.02618 0.01094 0.00024 0.00055 0.00039 0.00000 0.00312 0.00317 0.00366 0.00251 0.00259 0.00247 0.00140 H52 0.04341 0.03583 -0.01284 1.00000 0.03142 0.00000 0.00000 N1 0.32831 0.36693 0.07937 1.00000 0.01815 0.02905 0.02718 0.00367 -0.00828 -0.00385 0.02479 0.00818 0.00018 0.00042 0.00028 0.00000 0.00235 0.00254 0.00307 0.00204 0.00195 0.00198 0.00116 N2 0.27639 0.32489 -0.04452 1.00000 0.02080 0.01578 0.02189 0.00310 0.00722 0.00292 0.01949 0.00858 0.00018 0.00037 0.00029 0.00000 0.00253 0.00218 0.00271 0.00194 0.00204 0.00184 0.00103 N3 0.16393 0.20527 -0.12347 1.00000 0.02293 0.03430 0.01723 0.00153 -0.00372 -0.00402 0.02482 0.00877 0.00019 0.00044 0.00031 0.00000 0.00273 0.00290 0.00257 0.00235 0.00225 0.00222 0.00107 H3A 0.13711 0.16561 -0.10830 1.00000 0.02978 0.00000 0.00000 H3B 0.16379 0.23689 -0.16915 1.00000 0.02978 0.00000 0.00000 N4 0.20982 0.17592 -0.00952 1.00000 0.01878 0.01533 0.01973 0.00159 0.00285 -0.00116 0.01795 0.00808 0.00018 0.00036 0.00028 0.00000 0.00245 0.00205 0.00263 0.00179 0.00192 0.00174 0.00098 N5 0.16367 0.13596 0.02166 1.00000 0.02298 0.01753 0.02112 -0.00226 0.00580 -0.00112 0.02054 0.00813 0.00018 0.00038 0.00027 0.00000 0.00254 0.00225 0.00262 0.00192 0.00199 0.00191 0.00102 N6 0.20861 -0.02341 0.05910 1.00000 0.02534 0.01889 0.02298 0.00408 -0.00241 0.00245 0.02240 0.00839 0.00017 0.00034 0.00034 0.00000 0.00244 0.00209 0.00257 0.00240 0.00262 0.00175 0.00097 H6A 0.23630 -0.00405 0.03275 1.00000 0.02688 0.00000 0.00000 H6B 0.20847 -0.08602 0.08551 1.00000 0.02688 0.00000 0.00000 N7 0.09363 0.10216 0.12219 1.00000 0.02320 0.01872 0.02186 0.00058 -0.00390 -0.00547 0.02126 0.00821 0.00019 0.00039 0.00029 0.00000 0.00256 0.00225 0.00271 0.00192 0.00201 0.00197 0.00105 N8 0.04616 0.28829 0.14216 1.00000 0.01875 0.02051 0.02854 -0.00339 -0.00030 0.00809 0.02260 0.00913 0.00020 0.00042 0.00032 0.00000 0.00262 0.00248 0.00289 0.00207 0.00216 0.00206 0.00108 N31 0.32753 0.12016 0.03659 1.00000 0.02755 0.01525 0.02384 0.00370 -0.00277 0.00399 0.02221 0.00824 0.00019 0.00038 0.00027 0.00000 0.00254 0.00212 0.00292 0.00180 0.00198 0.00190 0.00110 N32 0.27920 0.16973 0.16038 1.00000 0.01278 0.02117 0.01890 -0.00309 0.00261 -0.00170 0.01762 0.00778 0.00017 0.00038 0.00027 0.00000 0.00235 0.00236 0.00261 0.00193 0.00188 0.00181 0.00100 N33 0.16668 0.28934 0.24216 1.00000 0.02238 0.03394 0.02763 0.00678 0.00141 0.00802 0.02798 0.00960 0.00020 0.00045 0.00032 0.00000 0.00273 0.00282 0.00306 0.00246 0.00239 0.00226 0.00114 H33A 0.14031 0.33021 0.22682 1.00000 0.03358 0.00000 0.00000 H33B 0.16662 0.25987 0.28853 1.00000 0.03358 0.00000 0.00000 N34 0.21035 0.31116 0.12706 1.00000 0.01049 0.01989 0.02337 -0.00036 -0.00361 -0.00063 0.01792 0.00773 0.00017 0.00037 0.00028 0.00000 0.00233 0.00225 0.00275 0.00187 0.00189 0.00173 0.00101 N35 0.16364 0.35320 0.09706 1.00000 0.01135 0.02751 0.01834 0.00843 0.00082 0.00057 0.01907 0.00815 0.00017 0.00040 0.00026 0.00000 0.00222 0.00249 0.00253 0.00197 0.00188 0.00184 0.00101 N36 0.20860 0.51308 0.05917 1.00000 0.01822 0.02169 0.03297 0.00343 -0.00657 0.00112 0.02429 0.00878 0.00017 0.00035 0.00037 0.00000 0.00229 0.00216 0.00291 0.00254 0.00268 0.00171 0.00101 H36A 0.23694 0.49427 0.08415 1.00000 0.02915 0.00000 0.00000 H36B 0.20758 0.57579 0.03291 1.00000 0.02915 0.00000 0.00000 N37 0.09331 0.38600 -0.00318 1.00000 0.00940 0.02543 0.01478 0.00301 0.00139 0.00217 0.01654 0.00805 0.00017 0.00039 0.00027 0.00000 0.00210 0.00236 0.00230 0.00187 0.00171 0.00180 0.00093 N38 0.04717 0.19920 -0.02399 1.00000 0.01822 0.02798 0.01549 0.00221 -0.00532 0.00464 0.02056 0.00885 0.00019 0.00042 0.00029 0.00000 0.00253 0.00277 0.00247 0.00196 0.00197 0.00202 0.00105 Co1 0.26973 0.24571 0.05817 1.00000 0.01523 0.01809 0.01832 0.00319 -0.00046 -0.00056 0.01721 0.00159 0.00002 0.00006 0.00007 0.00000 0.00025 0.00026 0.00025 0.00023 0.00045 0.00030 0.00013 Co2 0.10409 0.24426 0.05939 1.00000 0.01543 0.01797 0.01834 0.00136 -0.00064 -0.00064 0.01724 0.00158 0.00002 0.00006 0.00007 0.00000 0.00025 0.00027 0.00026 0.00024 0.00045 0.00030 0.00013 O1 0.43429 0.67126 0.26558 1.00000 0.03125 0.02754 0.04040 0.00798 -0.00562 -0.00089 0.03306 0.00846 0.00017 0.00038 0.00029 0.00000 0.00256 0.00264 0.00296 0.00217 0.00201 0.00182 0.00116 O2 0.42450 0.86427 0.27116 1.00000 0.03902 0.02559 0.03176 -0.00932 -0.01111 -0.00211 0.03212 0.00682 0.00018 0.00036 0.00026 0.00000 0.00261 0.00255 0.00270 0.00206 0.00207 0.00201 0.00112 O3 0.44545 0.77932 0.15530 1.00000 0.04767 0.05074 0.03983 -0.00431 0.01211 0.00157 0.04608 0.01078 0.00022 0.00052 0.00029 0.00000 0.00346 0.00311 0.00364 0.00285 0.00264 0.00272 0.00139 O4 0.36380 0.75887 0.20761 1.00000 0.03412 0.04508 0.04742 -0.00106 -0.01772 -0.00491 0.04220 0.00833 0.00020 0.00040 0.00037 0.00000 0.00310 0.00328 0.00404 0.00222 0.00287 0.00205 0.00153 Cl1 0.41851 0.76780 0.22501 1.00000 0.02732 0.02307 0.03226 -0.00176 0.00060 -0.00053 0.02755 0.00288 0.00007 0.00013 0.00010 0.00000 0.00092 0.00064 0.00089 0.00069 0.00071 0.00062 0.00036 O11 0.07741 0.13504 0.34230 1.00000 0.04248 0.02871 0.02954 0.00407 0.00411 0.00885 0.03358 0.00815 0.00019 0.00038 0.00026 0.00000 0.00273 0.00261 0.00271 0.00207 0.00207 0.00212 0.00113 O12 0.06519 0.32828 0.34475 1.00000 0.05673 0.01853 0.04456 -0.00148 -0.02236 0.00349 0.03994 0.00833 0.00020 0.00039 0.00030 0.00000 0.00338 0.00249 0.00319 0.00218 0.00242 0.00204 0.00135 O13 0.13705 0.24535 0.40359 1.00000 0.02013 0.05881 0.04306 -0.00044 0.00007 -0.00222 0.04066 0.00917 0.00020 0.00041 0.00036 0.00000 0.00267 0.00390 0.00377 0.00224 0.00253 0.00195 0.00152 O14 0.05579 0.22377 0.45742 1.00000 0.06454 0.05886 0.03249 0.00591 0.01785 0.02601 0.05196 0.01252 0.00024 0.00055 0.00032 0.00000 0.00412 0.00330 0.00332 0.00286 0.00285 0.00295 0.00159 Cl11 0.08187 0.23295 0.38711 1.00000 0.03811 0.02634 0.02358 0.00054 -0.00200 -0.00117 0.02934 0.00298 0.00007 0.00013 0.00010 0.00000 0.00108 0.00072 0.00081 0.00068 0.00073 0.00067 0.00038 O21 0.30977 0.39803 0.38863 1.00000 0.03613 0.07346 0.06341 -0.00207 0.00759 0.01113 0.05767 0.00948 0.00017 0.00049 0.00031 0.00000 0.00269 0.00362 0.00347 0.00274 0.00242 0.00243 0.00138 O22 0.38671 0.35242 0.45160 1.00000 0.08892 0.06524 0.03629 0.00775 -0.00031 0.02378 0.06348 0.01117 0.00025 0.00051 0.00031 0.00000 0.00444 0.00386 0.00330 0.00286 0.00298 0.00330 0.00168 O23 0.38667 0.48204 0.35423 1.00000 0.08854 0.02530 0.09068 0.00702 0.00887 -0.00664 0.06817 0.01064 0.00024 0.00041 0.00038 0.00000 0.00432 0.00262 0.00477 0.00261 0.00360 0.00268 0.00177 O24 0.37444 0.29745 0.32512 1.00000 0.05677 0.05489 0.04329 -0.02437 0.00652 0.01289 0.05165 0.00966 0.00022 0.00049 0.00033 0.00000 0.00342 0.00341 0.00313 0.00271 0.00256 0.00270 0.00144 Cl21 0.36397 0.38207 0.37889 1.00000 0.06326 0.02309 0.02197 -0.00220 0.00759 -0.00278 0.03611 0.00285 0.00007 0.00012 0.00009 0.00000 0.00101 0.00068 0.00070 0.00058 0.00071 0.00067 0.00036 O31 0.13169 0.70396 0.28357 1.00000 0.06389 0.02958 0.08294 -0.01966 -0.02602 0.00077 0.05880 0.00864 0.00022 0.00044 0.00038 0.00000 0.00370 0.00282 0.00461 0.00287 0.00315 0.00252 0.00169 O32 0.12238 0.63948 0.16142 1.00000 0.13864 0.05165 0.04137 0.01284 0.02724 0.01799 0.07722 0.01348 0.00031 0.00053 0.00034 0.00000 0.00631 0.00364 0.00360 0.00285 0.00367 0.00387 0.00216 O33 0.14006 0.51631 0.25733 1.00000 0.10379 0.03763 0.10474 -0.00260 -0.04636 0.01654 0.08205 0.01079 0.00026 0.00045 0.00044 0.00000 0.00489 0.00308 0.00540 0.00321 0.00430 0.00315 0.00216 O34 0.05997 0.60061 0.25171 1.00000 0.03597 0.12453 0.11140 -0.06925 0.02957 -0.01605 0.09063 0.00981 0.00019 0.00060 0.00042 0.00000 0.00288 0.00561 0.00543 0.00468 0.00317 0.00309 0.00244 Cl31 0.11518 0.61458 0.23800 1.00000 0.08077 0.02615 0.03070 -0.00107 0.00583 0.00050 0.04588 0.00318 0.00008 0.00013 0.00010 0.00000 0.00127 0.00074 0.00089 0.00062 0.00086 0.00078 0.00044 O51 0.26965 0.20413 0.47199 1.00000 0.06732 0.03445 0.02499 0.00247 -0.00037 0.01401 0.04225 0.00913 0.00021 0.00041 0.00027 0.00000 0.00332 0.00251 0.00244 0.00197 0.00216 0.00234 0.00123 O52 0.24273 0.53984 0.31056 1.00000 0.06889 0.06820 0.08515 0.02421 -0.01561 0.00446 0.07408 0.01139 0.00024 0.00048 0.00040 0.00000 0.00383 0.00384 0.00415 0.00365 0.00322 0.00314 0.00173 O53 0.28045 0.60157 0.17241 1.00000 0.04288 0.05447 0.06610 -0.00925 -0.00506 0.00183 0.05448 0.00850 0.00019 0.00043 0.00031 0.00000 0.00278 0.00301 0.00339 0.00251 0.00241 0.00230 0.00129 O54 0.21710 0.78128 0.15132 1.00000 0.07528 0.04794 0.03820 0.00706 -0.00166 0.02186 0.05381 0.01099 0.00024 0.00049 0.00031 0.00000 0.00400 0.00287 0.00311 0.00241 0.00268 0.00286 0.00148 O55 0.31673 0.79178 0.04659 1.00000 0.06184 0.09096 0.05589 -0.01881 0.02217 -0.03176 0.06956 0.00983 0.00020 0.00051 0.00035 0.00000 0.00327 0.00422 0.00379 0.00343 0.00296 0.00284 0.00172 Final Structure Factor Calculation for s93 in Pna2(1) Total number of l.s. parameters = 786 Maximum vector length = 511 Memory required = 7312 / 27090 wR2 = 0.1512 before cycle 11 for 12146 data and 2 / 786 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 0.0770 0.0200 SAME/SADI O33 Cl31 O13 Cl11 0.0613 0.0200 SAME/SADI O32 Cl31 O22 Cl21 Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.016 0.013 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.024 for 71 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0724 * P )^2 + 11.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0568 for 9321 Fo > 4sig(Fo) and 0.0827 for all 12146 data wR2 = 0.1512, GooF = S = 1.022, Restrained GooF = 1.024 for all data Occupancy sum of asymmetric unit = 87.00 for non-hydrogen and 36.00 for hydrogen atoms Principal mean square atomic displacements U 0.0444 0.0319 0.0172 C1 0.0349 0.0291 0.0233 C2 0.0463 0.0361 0.0146 C3 0.0396 0.0265 0.0221 C4 0.0300 0.0201 0.0138 C5 0.0234 0.0197 0.0159 C6 0.0373 0.0263 0.0119 C7 0.0433 0.0303 0.0094 C8 0.0297 0.0280 0.0155 C9 0.0287 0.0230 0.0089 C10 0.0246 0.0233 0.0094 C11 0.0264 0.0211 0.0144 C12 0.0234 0.0194 0.0154 C13 0.0351 0.0266 0.0160 C14 0.0394 0.0290 0.0111 C15 0.0379 0.0251 0.0119 C16 0.0359 0.0162 0.0108 C17 0.0401 0.0218 0.0157 C18 0.0380 0.0263 0.0201 C19 0.0469 0.0213 0.0171 C20 0.0412 0.0269 0.0188 C21 0.0331 0.0309 0.0222 C22 0.0394 0.0239 0.0186 C31 0.0365 0.0238 0.0198 C32 0.0453 0.0307 0.0180 C33 0.0397 0.0382 0.0155 C34 0.0235 0.0217 0.0145 C35 0.0354 0.0154 0.0123 C36 0.0411 0.0239 0.0192 C37 0.0442 0.0254 0.0158 C38 0.0359 0.0267 0.0137 C39 0.0291 0.0171 0.0121 C40 0.0214 0.0176 0.0108 C41 0.0212 0.0171 0.0115 C42 0.0259 0.0181 0.0138 C43 0.0329 0.0273 0.0164 C44 0.0541 0.0312 0.0136 C45 0.0474 0.0264 0.0175 C46 0.0316 0.0220 0.0165 C47 0.0287 0.0217 0.0126 C48 0.0410 0.0269 0.0154 C49 0.0577 0.0269 0.0194 C50 0.0485 0.0311 0.0215 C51 0.0327 0.0255 0.0204 C52 0.0360 0.0253 0.0131 N1 0.0299 0.0145 0.0141 N2 0.0359 0.0231 0.0154 N3 0.0222 0.0178 0.0138 N4 0.0284 0.0177 0.0155 N5 0.0268 0.0251 0.0153 N6 0.0288 0.0204 0.0146 N7 0.0310 0.0255 0.0112 N8 0.0293 0.0249 0.0124 N31 0.0241 0.0170 0.0118 N32 0.0413 0.0248 0.0178 N33 0.0243 0.0199 0.0095 N34 0.0326 0.0134 0.0112 N35 0.0360 0.0219 0.0149 N36 0.0266 0.0141 0.0089 N37 0.0298 0.0217 0.0101 N38 0.0215 0.0152 0.0150 Co1 0.0197 0.0168 0.0152 Co2 0.0462 0.0296 0.0233 O1 0.0478 0.0329 0.0156 O2 0.0568 0.0514 0.0301 O3 0.0600 0.0457 0.0209 O4 0.0327 0.0273 0.0227 Cl1 0.0484 0.0287 0.0236 O11 0.0741 0.0276 0.0182 O12 0.0589 0.0430 0.0200 O13 0.0929 0.0397 0.0233 O14 0.0385 0.0263 0.0233 Cl11 0.0765 0.0653 0.0311 O21 0.1039 0.0532 0.0334 O22 0.0986 0.0823 0.0237 O23 0.0764 0.0592 0.0194 O24 0.0648 0.0238 0.0197 Cl21 0.1049 0.0501 0.0215 O31 0.1501 0.0509 0.0307 O32 0.1522 0.0617 0.0322 O33 0.1939 0.0533 0.0246 O34 0.0814 0.0303 0.0259 Cl31 0.0725 0.0304 0.0239 O51 0.1054 0.0728 0.0441 O52 0.0722 0.0495 0.0418 O53 0.0875 0.0440 0.0299 O54 0.1230 0.0508 0.0349 O55 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 0.030 0.039 0.048 0.060 0.076 0.100 0.138 1.000 Number in group 1240. 1289. 1129. 1322. 1127. 1177. 1218. 1235. 1185. 1224. GooF 0.989 0.992 1.024 0.994 0.994 1.004 1.110 1.044 1.074 0.989 K 1.630 1.160 1.023 1.010 0.977 0.986 0.986 0.996 1.010 1.010 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 1251. 1176. 1227. 1216. 1227. 1207. 1202. 1213. 1204. 1223. GooF 0.952 0.946 0.903 0.936 0.903 0.955 0.922 0.911 1.042 1.564 K 0.970 0.998 1.017 1.022 1.022 1.004 1.023 1.029 1.025 0.991 R1 0.205 0.190 0.134 0.116 0.085 0.072 0.054 0.045 0.043 0.049 Recommended weighting scheme: WGHT 0.0724 11.9187 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) 4 3 0 581.18 127.44 6.59 0.022 3.40 3 1 7 379.26 48.48 6.29 0.013 2.34 3 1 -7 376.91 48.23 6.17 0.013 2.34 5 2 0 2768.54 5152.03 6.10 0.139 3.91 5 4 -5 1983.84 1055.10 5.68 0.063 2.08 5 4 5 1946.08 1058.42 5.45 0.063 2.08 6 2 -4 5002.00 3157.58 5.29 0.109 2.72 6 2 4 4898.10 3146.45 5.11 0.108 2.72 7 2 0 2604.18 4369.16 5.10 0.128 3.14 8 4 7 1442.78 2524.56 4.83 0.097 1.64 4 4 0 2170.95 1249.15 4.83 0.068 2.72 8 4 -7 1425.90 2522.69 4.81 0.097 1.64 5 5 0 4554.43 7064.28 4.77 0.163 2.17 6 0 -3 3344.25 2109.96 4.71 0.089 3.45 2 2 6 485.47 181.65 4.53 0.026 2.56 5 3 -6 264.75 50.08 4.49 0.014 2.14 0 2 2 4129.62 6268.40 4.48 0.153 4.93 6 0 3 3284.62 2122.51 4.44 0.089 3.45 3 5 0 1634.16 2647.53 4.32 0.100 2.31 1 3 0 248.38 3.47 4.32 0.004 3.95 0 2 -2 4196.25 6258.87 4.31 0.153 4.93 7 2 5 769.21 1402.74 4.29 0.072 2.33 7 2 -5 771.44 1404.25 4.27 0.072 2.33 1 6 -5 2004.38 1265.89 4.23 0.069 1.73 5 3 7 3514.45 2357.81 4.22 0.094 1.95 2 2 -6 452.85 180.69 4.17 0.026 2.56 1 4 6 5969.00 4180.63 4.15 0.125 2.08 1 6 5 1988.90 1263.34 4.11 0.069 1.73 1 4 -6 5900.71 4185.72 4.06 0.125 2.08 17 3 5 618.48 289.02 4.03 0.033 1.31 5 3 -2 1812.57 2805.39 4.02 0.102 2.97 30 1 0 688.94 1542.76 3.96 0.076 0.86 4 1 -2 2824.50 4165.37 3.95 0.125 4.76 5 3 2 1835.92 2806.40 3.93 0.102 2.97 4 1 2 2824.16 4150.83 3.91 0.125 4.76 2 1 -7 2115.25 3174.21 3.83 0.109 2.39 7 4 0 363.14 114.59 3.82 0.021 2.33 5 3 -7 3374.97 2356.59 3.81 0.094 1.95 12 1 -5 4205.53 2986.51 3.80 0.106 1.81 17 3 -5 599.88 289.25 3.79 0.033 1.31 2 2 12 250.36 58.52 3.79 0.015 1.40 32 0 -4 93.74 883.87 3.79 0.057 0.79 3 1 1 2484.00 3734.94 3.77 0.118 6.48 5 1 -7 2137.35 1420.92 3.76 0.073 2.20 5 3 6 227.04 50.61 3.76 0.014 2.14 30 0 -3 2437.31 4313.00 3.75 0.127 0.85 21 2 10 224.49 600.87 3.73 0.047 0.99 17 4 -2 499.75 217.01 3.70 0.028 1.34 3 1 -1 2396.36 3734.53 3.70 0.118 6.48 25 5 -5 938.41 345.65 3.67 0.036 0.91 Bond lengths and angles C1 - Distance Angles N1 1.3325 (0.0079) C2 1.3714 (0.0092) 123.79 (0.67) H1 0.9500 118.10 118.10 C1 - N1 C2 C2 - Distance Angles C3 1.3543 (0.0093) C1 1.3714 (0.0091) 119.14 (0.66) H2 0.9500 120.43 120.43 C2 - C3 C1 C3 - Distance Angles C2 1.3543 (0.0093) C4 1.3928 (0.0094) 118.51 (0.58) H3 0.9500 120.74 120.74 C3 - C2 C4 C4 - Distance Angles C5 1.3507 (0.0088) C3 1.3928 (0.0094) 119.70 (0.64) H4 0.9500 120.15 120.15 C4 - C5 C3 C5 - Distance Angles C4 1.3507 (0.0089) N1 1.3693 (0.0077) 122.30 (0.61) C6 1.4733 (0.0087) 124.54 (0.60) 113.15 (0.49) C5 - C4 N1 C6 - Distance Angles N2 1.3038 (0.0072) C7 1.3927 (0.0082) 120.90 (0.56) C5 1.4733 (0.0087) 115.92 (0.53) 123.16 (0.53) C6 - N2 C7 C7 - Distance Angles C8 1.3785 (0.0092) C6 1.3927 (0.0082) 117.43 (0.54) H7 0.9500 121.28 121.28 C7 - C8 C6 C8 - Distance Angles C9 1.3785 (0.0085) C7 1.3785 (0.0092) 120.88 (0.58) H8 0.9500 119.56 119.56 C8 - C9 C7 C9 - Distance Angles C8 1.3785 (0.0085) C10 1.3935 (0.0083) 117.70 (0.60) H9 0.9500 121.15 121.15 C9 - C8 C10 C10 - Distance Angles N2 1.3172 (0.0077) C9 1.3935 (0.0083) 120.24 (0.56) C11 1.4609 (0.0086) 114.21 (0.50) 125.55 (0.56) C10 - N2 C9 C11 - Distance Angles N4 1.2919 (0.0074) N3 1.3212 (0.0079) 126.61 (0.58) C10 1.4609 (0.0086) 114.39 (0.53) 118.77 (0.54) C11 - N4 N3 C12 - Distance Angles N5 1.3105 (0.0071) N6 1.3172 (0.0067) 124.72 (0.56) C13 1.4631 (0.0083) 114.40 (0.48) 120.85 (0.52) C12 - N5 N6 C13 - Distance Angles N7 1.3321 (0.0073) C14 1.3704 (0.0080) 121.67 (0.56) C12 1.4631 (0.0083) 111.76 (0.49) 126.56 (0.52) C13 - N7 C14 C14 - Distance Angles C13 1.3704 (0.0080) C15 1.3942 (0.0086) 117.13 (0.56) H14 0.9500 121.44 121.44 C14 - C13 C15 C15 - Distance Angles C16 1.3486 (0.0091) C14 1.3942 (0.0086) 120.34 (0.58) H15 0.9500 119.83 119.83 C15 - C16 C14 C16 - Distance Angles C15 1.3486 (0.0091) C17 1.3739 (0.0081) 120.66 (0.58) H16 0.9500 119.67 119.67 C16 - C15 C17 C17 - Distance Angles N7 1.3479 (0.0076) C16 1.3739 (0.0081) 118.61 (0.56) C18 1.4757 (0.0092) 113.55 (0.51) 127.83 (0.55) C17 - N7 C16 C18 - Distance Angles N8 1.3304 (0.0085) C19 1.3582 (0.0091) 122.78 (0.67) C17 1.4757 (0.0092) 114.52 (0.56) 122.70 (0.62) C18 - N8 C19 C19 - Distance Angles C18 1.3582 (0.0091) C20 1.3711 (0.0093) 117.87 (0.71) H19 0.9500 121.07 121.07 C19 - C18 C20 C20 - Distance Angles C21 1.3494 (0.0091) C19 1.3711 (0.0093) 119.68 (0.64) H20 0.9500 120.16 120.16 C20 - C21 C19 C21 - Distance Angles C20 1.3494 (0.0091) C22 1.3622 (0.0089) 119.19 (0.62) H21 0.9500 120.41 120.41 C21 - C20 C22 C22 - Distance Angles N8 1.3213 (0.0082) C21 1.3622 (0.0089) 122.07 (0.64) H22 0.9500 118.97 118.97 C22 - N8 C21 C31 - Distance Angles N31 1.3119 (0.0082) C32 1.3858 (0.0088) 121.92 (0.62) H31 0.9500 119.04 119.04 C31 - N31 C32 C32 - Distance Angles C33 1.3425 (0.0093) C31 1.3858 (0.0088) 118.27 (0.63) H32 0.9500 120.86 120.86 C32 - C33 C31 C33 - Distance Angles C32 1.3425 (0.0093) C34 1.3676 (0.0097) 119.65 (0.59) H33 0.9500 120.17 120.17 C33 - C32 C34 C34 - Distance Angles C33 1.3676 (0.0097) C35 1.3812 (0.0086) 119.00 (0.63) H34 0.9500 120.50 120.50 C34 - C33 C35 C35 - Distance Angles N31 1.3061 (0.0077) C34 1.3812 (0.0086) 120.86 (0.60) C36 1.4703 (0.0090) 116.92 (0.50) 122.20 (0.60) C35 - N31 C34 C36 - Distance Angles N32 1.3388 (0.0072) C37 1.3794 (0.0088) 120.79 (0.58) C35 1.4703 (0.0090) 111.66 (0.53) 127.55 (0.55) C36 - N32 C37 C37 - Distance Angles C38 1.3463 (0.0097) C36 1.3794 (0.0088) 119.14 (0.57) H37 0.9500 120.43 120.43 C37 - C38 C36 C38 - Distance Angles C37 1.3463 (0.0097) C39 1.3866 (0.0087) 120.86 (0.63) H38 0.9500 119.57 119.57 C38 - C37 C39 C39 - Distance Angles C40 1.3542 (0.0088) C38 1.3866 (0.0087) 117.40 (0.63) H39 0.9500 121.30 121.30 C39 - C40 C38 C40 - Distance Angles N32 1.3481 (0.0077) C39 1.3542 (0.0088) 122.61 (0.53) C41 1.4860 (0.0079) 110.47 (0.51) 126.82 (0.58) C40 - N32 C39 C41 - Distance Angles N34 1.2850 (0.0073) N33 1.3193 (0.0079) 125.12 (0.54) C40 1.4860 (0.0079) 115.03 (0.52) 119.83 (0.52) C41 - N34 N33 C42 - Distance Angles N35 1.2982 (0.0068) N36 1.3118 (0.0064) 126.98 (0.53) C43 1.4977 (0.0081) 113.18 (0.43) 119.59 (0.51) C42 - N35 N36 C43 - Distance Angles N37 1.3164 (0.0074) C44 1.3615 (0.0079) 122.20 (0.56) C42 1.4977 (0.0081) 112.69 (0.47) 125.08 (0.52) C43 - N37 C44 C44 - Distance Angles C43 1.3615 (0.0079) C45 1.3759 (0.0092) 117.51 (0.60) H44 0.9500 121.24 121.24 C44 - C43 C45 C45 - Distance Angles C44 1.3759 (0.0092) C46 1.3830 (0.0098) 120.07 (0.61) H45 0.9500 119.96 119.96 C45 - C44 C46 C46 - Distance Angles C47 1.3622 (0.0088) C45 1.3830 (0.0098) 117.86 (0.60) H46 0.9500 121.07 121.07 C46 - C47 C45 C47 - Distance Angles N37 1.3116 (0.0075) C46 1.3622 (0.0088) 121.74 (0.59) C48 1.4642 (0.0090) 113.94 (0.54) 124.28 (0.57) C47 - N37 C46 C48 - Distance Angles N38 1.3612 (0.0080) C49 1.3796 (0.0089) 120.52 (0.64) C47 1.4642 (0.0091) 114.49 (0.55) 124.93 (0.62) C48 - N38 C49 C49 - Distance Angles C50 1.3765 (0.0097) C48 1.3796 (0.0089) 119.01 (0.69) H49 0.9500 120.50 120.50 C49 - C50 C48 C50 - Distance Angles C51 1.3567 (0.0100) C49 1.3765 (0.0097) 121.24 (0.66) H50 0.9500 119.38 119.38 C50 - C51 C49 C51 - Distance Angles C50 1.3567 (0.0100) C52 1.3803 (0.0091) 117.05 (0.65) H51 0.9500 121.47 121.47 C51 - C50 C52 C52 - Distance Angles N38 1.3351 (0.0080) C51 1.3803 (0.0091) 123.63 (0.63) H52 0.9500 118.19 118.19 C52 - N38 C51 N1 - Distance Angles C1 1.3325 (0.0079) C5 1.3693 (0.0077) 116.55 (0.53) Co1 2.1291 (0.0048) 128.98 (0.44) 114.46 (0.38) N1 - C1 C5 N2 - Distance Angles C6 1.3038 (0.0072) C10 1.3172 (0.0077) 122.82 (0.53) Co1 2.0291 (0.0049) 118.62 (0.42) 117.95 (0.38) N2 - C6 C10 N3 - Distance Angles C11 1.3212 (0.0079) H3A 0.8800 120.00 H3B 0.8800 120.00 120.00 N3 - C11 H3A N4 - Distance Angles C11 1.2919 (0.0074) N5 1.3935 (0.0066) 113.32 (0.48) Co1 2.1155 (0.0048) 115.93 (0.39) 122.98 (0.35) N4 - C11 N5 N5 - Distance Angles C12 1.3105 (0.0071) N4 1.3935 (0.0066) 115.34 (0.46) Co2 2.1167 (0.0046) 115.49 (0.39) 122.04 (0.32) N5 - C12 N4 N6 - Distance Angles C12 1.3172 (0.0067) H6A 0.8800 120.00 H6B 0.8800 120.00 120.00 N6 - C12 H6A N7 - Distance Angles C13 1.3321 (0.0073) C17 1.3479 (0.0076) 121.46 (0.50) Co2 2.0414 (0.0048) 118.56 (0.41) 117.71 (0.39) N7 - C13 C17 N8 - Distance Angles C22 1.3213 (0.0082) C18 1.3304 (0.0085) 118.22 (0.59) Co2 2.1410 (0.0054) 126.59 (0.46) 115.13 (0.44) N8 - C22 C18 N31 - Distance Angles C35 1.3061 (0.0077) C31 1.3119 (0.0082) 120.21 (0.52) Co1 2.1519 (0.0047) 113.67 (0.38) 125.81 (0.40) N31 - C35 C31 N32 - Distance Angles C36 1.3388 (0.0072) C40 1.3481 (0.0077) 119.14 (0.52) Co1 2.0116 (0.0050) 120.36 (0.41) 119.91 (0.37) N32 - C36 C40 N33 - Distance Angles C41 1.3193 (0.0079) H33A 0.8800 120.00 H33B 0.8800 120.00 120.00 N33 - C41 H33A N34 - Distance Angles C41 1.2850 (0.0073) N35 1.4068 (0.0063) 113.86 (0.46) Co1 2.0975 (0.0048) 116.98 (0.38) 123.26 (0.35) N34 - C41 N35 N35 - Distance Angles C42 1.2982 (0.0068) N34 1.4068 (0.0063) 114.75 (0.43) Co2 2.1205 (0.0047) 116.71 (0.37) 120.99 (0.34) N35 - C42 N34 N36 - Distance Angles C42 1.3118 (0.0064) H36A 0.8800 120.00 H36B 0.8800 120.00 120.00 N36 - C42 H36A N37 - Distance Angles C47 1.3116 (0.0075) C43 1.3164 (0.0074) 120.57 (0.52) Co2 2.0367 (0.0047) 118.63 (0.40) 119.19 (0.39) N37 - C47 C43 N38 - Distance Angles C52 1.3351 (0.0080) C48 1.3612 (0.0080) 118.51 (0.57) Co2 2.1332 (0.0051) 127.56 (0.42) 113.51 (0.42) N38 - C52 C48 Co1 - Distance Angles N32 2.0116 (0.0050) N2 2.0291 (0.0049) 168.14 (0.14) N34 2.0975 (0.0047) 75.74 (0.19) 112.90 (0.18) N4 2.1155 (0.0048) 113.64 (0.18) 75.97 (0.19) 86.07 (0.13) N1 2.1291 (0.0048) 94.01 (0.19) 76.87 (0.19) 99.47 (0.19) 152.27 (0.19) N31 2.1519 (0.0047) 75.71 (0.18) 96.62 (0.18) 150.19 (0.19) 97.64 (0.18) 90.89 (0.15) Co1 - N32 N2 N34 N4 N1 Co2 - Distance Angles N37 2.0367 (0.0047) N7 2.0414 (0.0048) 164.55 (0.14) N5 2.1167 (0.0046) 116.46 (0.19) 75.51 (0.19) N35 2.1205 (0.0047) 75.52 (0.18) 116.40 (0.19) 86.97 (0.13) N38 2.1332 (0.0051) 75.78 (0.19) 93.50 (0.20) 97.72 (0.19) 149.87 (0.19) N8 2.1410 (0.0054) 93.31 (0.19) 75.76 (0.20) 150.08 (0.20) 98.43 (0.19) 92.19 (0.14) Co2 - N37 N7 N5 N35 N38 O1 - Distance Angles Cl1 1.4152 (0.0043) O1 - O2 - Distance Angles Cl1 1.4161 (0.0041) O2 - O3 - Distance Angles Cl1 1.4040 (0.0048) O3 - O4 - Distance Angles Cl1 1.4480 (0.0050) O4 - Cl1 - Distance Angles O3 1.4040 (0.0048) O1 1.4152 (0.0043) 111.60 (0.34) O2 1.4161 (0.0041) 110.77 (0.35) 110.74 (0.33) O4 1.4480 (0.0050) 108.05 (0.39) 108.92 (0.29) 106.57 (0.30) Cl1 - O3 O1 O2 O11 - Distance Angles Cl11 1.4136 (0.0047) O11 - O12 - Distance Angles Cl11 1.4261 (0.0048) O12 - O13 - Distance Angles Cl11 1.4602 (0.0053) O13 - O14 - Distance Angles Cl11 1.3997 (0.0054) O14 - Cl11 - Distance Angles O14 1.3997 (0.0054) O11 1.4136 (0.0047) 112.14 (0.37) O12 1.4261 (0.0048) 111.65 (0.35) 110.87 (0.31) O13 1.4602 (0.0053) 107.80 (0.39) 105.78 (0.30) 108.31 (0.32) Cl11 - O14 O11 O12 O21 - Distance Angles Cl21 1.4219 (0.0046) O21 - O22 - Distance Angles Cl21 1.4381 (0.0054) O22 - O23 - Distance Angles Cl21 1.4012 (0.0051) O23 - O24 - Distance Angles Cl21 1.4057 (0.0049) O24 - Cl21 - Distance Angles O23 1.4012 (0.0051) O24 1.4057 (0.0049) 109.48 (0.39) O21 1.4219 (0.0046) 109.43 (0.36) 111.44 (0.35) O22 1.4381 (0.0054) 108.04 (0.40) 109.12 (0.36) 109.26 (0.35) Cl21 - O23 O24 O21 O31 - Distance Angles Cl31 1.3990 (0.0050) O31 - O32 - Distance Angles Cl31 1.3768 (0.0058) O32 - O33 - Distance Angles Cl31 1.3832 (0.0053) O33 - O34 - Distance Angles Cl31 1.4541 (0.0051) O34 - Cl31 - Distance Angles O32 1.3768 (0.0058) O33 1.3832 (0.0053) 110.91 (0.44) O31 1.3990 (0.0051) 109.89 (0.44) 111.92 (0.38) O34 1.4541 (0.0051) 108.40 (0.47) 108.48 (0.46) 107.09 (0.36) Cl31 - O32 O33 O31 FMAP and GRID set by program FMAP 2 3 39 GRID -1.389 -1 -2 1.389 1 2 R1 = 0.0705 for 6361 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.41 at 0.1483 0.6141 0.2435 [ 0.86 A from CL31 ] Deepest hole -1.27 at 0.0875 0.6159 0.2368 [ 0.72 A from CL31 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 7123 / 71196 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1483 0.6141 0.2435 1.00000 0.05 1.41 0.86 CL31 1.22 O33 1.35 O31 1.61 O32 Q2 1 0.2640 0.2509 0.5594 1.00000 0.05 0.94 1.63 O51 1.71 O54 2.13 H6B 2.15 O55 Q3 1 0.4508 0.7561 0.2333 1.00000 0.05 0.87 0.86 CL1 1.24 O1 1.39 O3 1.60 O2 Q4 1 0.0495 0.2523 0.3831 1.00000 0.05 0.83 0.87 CL11 1.20 O12 1.35 O14 1.73 O11 Q5 1 0.4914 0.8012 0.2198 1.00000 0.05 0.82 1.65 O3 1.93 CL1 2.09 O2 2.20 O34 Q6 1 0.3848 0.4784 0.4150 1.00000 0.05 0.77 1.06 O23 1.42 CL21 1.64 O22 2.21 O21 Q7 1 0.0098 0.2027 0.3940 1.00000 0.05 0.76 1.64 O14 1.90 CL11 2.12 O11 2.24 O12 Q8 1 0.3929 0.3817 0.3805 1.00000 0.05 0.69 0.75 CL21 1.29 O22 1.30 O23 1.47 O24 Q9 1 0.2301 0.4809 0.3889 1.00000 0.05 0.67 1.57 O52 2.28 O21 2.51 H31 2.65 H6A Q10 1 0.1694 0.6875 0.1942 1.00000 0.05 0.65 1.46 O32 1.82 CL31 1.83 O54 1.84 O31 Shortest distances between peaks (including symmetry equivalents) 4 7 1.20 3 5 1.20 6 8 1.32 1 10 1.34 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 6.13: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.08: Set up l.s. refinement 0.02: Generate idealized H-atoms 118.09: Structure factors and derivatives 161.80: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.39: Apply other restraints 17.48: Solve l.s. equations 0.00: Generate HTAB table 0.13: Other dependent quantities, CIF, tables 0.47: Analysis of variance 0.17: Merge reflections for Fourier and .fcf 0.27: Fourier summations 0.25: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s93 finished at 14:56:40 Total CPU time: 305.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++