+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0927 started at 14:30:52 on 02-Aug-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0927 in P2(1) CELL 0.71073 9.6827 22.3776 16.0124 90.000 91.846 90.000 ZERR 8.00 0.0001 0.0002 0.0002 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O P CL UNIT 80 120 40 8 24 24 V = 3467.70 F(000) = 1712.0 Mu = 0.81 mm-1 Cell Wt = 3364.24 Rho = 1.611 MERG 2 OMIT -3.00 55.00 OMIT 0 4 0 OMIT 0 -4 14 TWIN BASF 0.43599 FMAP 2 PLAN 20 SIZE 0.04 0.06 0.20 ACTA BOND WGHT 0.01970 2.31060 L.S. 4 TEMP -153.00 FVAR 0.38088 C1 1 1.039593 0.238004 0.232284 11.00000 0.04462 0.01917 = 0.03780 0.00078 0.00094 -0.00166 AFIX 137 H1A 2 0.944639 0.252748 0.225166 11.00000 -1.50000 H1B 2 1.082695 0.236439 0.177785 11.00000 -1.50000 H1C 2 1.092483 0.264960 0.269436 11.00000 -1.50000 AFIX 0 C2 1 0.976305 0.175935 0.351961 11.00000 0.02777 0.03439 = 0.02095 -0.00726 0.00104 0.00327 AFIX 23 H2A 2 0.875265 0.182053 0.345489 11.00000 -1.20000 H2B 2 1.014639 0.208921 0.386777 11.00000 -1.20000 AFIX 0 C3 1 1.003770 0.117519 0.395715 11.00000 0.02895 0.03782 = 0.01430 -0.00115 0.00194 0.00314 AFIX 23 H3A 2 1.104648 0.112399 0.405035 11.00000 -1.20000 H3B 2 0.960818 0.118218 0.450983 11.00000 -1.20000 AFIX 0 C4 1 0.947460 0.065551 0.346049 11.00000 0.03193 0.03112 = 0.01959 0.00240 0.00318 -0.00603 AFIX 23 H4A 2 0.969404 0.027804 0.375868 11.00000 -1.20000 H4B 2 0.845711 0.068969 0.339818 11.00000 -1.20000 AFIX 0 C5 1 0.658579 0.124399 -0.063399 11.00000 0.01864 0.03590 = 0.01754 0.00547 -0.00351 -0.01023 C6 1 0.726954 0.106119 -0.131984 11.00000 0.02746 0.03092 = 0.03106 -0.00284 -0.00347 0.00483 AFIX 43 H6 2 0.815206 0.087738 -0.126385 11.00000 -1.20000 AFIX 0 C7 1 0.663708 0.115137 -0.211043 11.00000 0.03757 0.04152 = 0.02270 -0.00504 0.00152 0.00076 AFIX 43 H7 2 0.710007 0.103151 -0.259703 11.00000 -1.20000 AFIX 0 C8 1 0.536226 0.140982 -0.218655 11.00000 0.03100 0.04118 = 0.01915 0.00298 -0.00656 -0.00365 AFIX 43 H8 2 0.493273 0.146343 -0.272310 11.00000 -1.20000 AFIX 0 C9 1 0.470390 0.159191 -0.148363 11.00000 0.02406 0.08202 = 0.03275 -0.00542 -0.00748 0.01265 AFIX 43 H9 2 0.382106 0.177548 -0.153921 11.00000 -1.20000 AFIX 0 C10 1 0.531041 0.151175 -0.068842 11.00000 0.02449 0.09507 = 0.02250 -0.00343 0.00066 0.00455 AFIX 43 H10 2 0.485610 0.163816 -0.020190 11.00000 -1.20000 AFIX 0 C11 1 0.592657 0.287736 0.381738 11.00000 0.03968 0.02832 = 0.02808 -0.00168 0.00153 -0.01583 AFIX 137 H11A 2 0.685349 0.271138 0.391863 11.00000 -1.50000 H11B 2 0.544894 0.290189 0.434665 11.00000 -1.50000 H11C 2 0.600108 0.327791 0.357552 11.00000 -1.50000 AFIX 0 C12 1 0.579021 0.244672 0.241091 11.00000 0.02335 0.03157 = 0.01941 0.00422 0.00539 -0.00393 AFIX 23 H12A 2 0.670401 0.225157 0.248212 11.00000 -1.20000 H12B 2 0.593885 0.285444 0.219126 11.00000 -1.20000 AFIX 0 C13 1 0.490683 0.209449 0.178552 11.00000 0.02288 0.03758 = 0.01115 0.00474 0.00134 -0.00130 AFIX 23 H13A 2 0.401746 0.230433 0.168261 11.00000 -1.20000 H13B 2 0.538404 0.207021 0.124899 11.00000 -1.20000 AFIX 0 C14 1 0.463200 0.147003 0.210247 11.00000 0.02751 0.03091 = 0.01433 -0.00574 0.00097 0.00189 AFIX 23 H14A 2 0.409825 0.124360 0.167010 11.00000 -1.20000 H14B 2 0.552194 0.126108 0.220744 11.00000 -1.20000 AFIX 0 C15 1 0.157753 0.156888 0.632252 11.00000 0.01434 0.03037 = 0.01403 0.00113 0.00085 -0.00317 C16 1 0.182967 0.100364 0.663436 11.00000 0.02945 0.02737 = 0.02284 0.00173 0.00624 -0.00023 AFIX 43 H16 2 0.226808 0.071019 0.630587 11.00000 -1.20000 AFIX 0 C17 1 0.143016 0.087286 0.743664 11.00000 0.03251 0.03789 = 0.03188 0.01049 0.00866 -0.00050 AFIX 43 H17 2 0.160623 0.048818 0.766738 11.00000 -1.20000 AFIX 0 C18 1 0.077851 0.130008 0.789908 11.00000 0.02814 0.04926 = 0.01933 0.00473 0.00492 -0.00372 AFIX 43 H18 2 0.050248 0.120815 0.844837 11.00000 -1.20000 AFIX 0 C19 1 0.052133 0.186271 0.757131 11.00000 0.02595 0.04612 = 0.02443 -0.00854 0.00716 0.00210 AFIX 43 H19 2 0.006169 0.215266 0.789496 11.00000 -1.20000 AFIX 0 C20 1 0.092980 0.200656 0.677338 11.00000 0.02035 0.03090 = 0.02912 -0.00009 0.00322 0.00380 AFIX 43 H20 2 0.076894 0.239320 0.654536 11.00000 -1.20000 AFIX 0 C21 1 -0.257901 0.278935 0.723514 11.00000 0.03269 0.03164 = 0.04866 -0.00359 -0.00011 -0.00847 AFIX 137 H21A 2 -0.268155 0.242899 0.757536 11.00000 -1.50000 H21B 2 -0.202502 0.269632 0.675038 11.00000 -1.50000 H21C 2 -0.349319 0.293112 0.704399 11.00000 -1.50000 AFIX 0 C22 1 -0.265915 0.340196 0.849434 11.00000 0.02558 0.04705 = 0.02100 0.00941 0.00228 -0.00520 AFIX 23 H22A 2 -0.283881 0.302905 0.880527 11.00000 -1.20000 H22B 2 -0.356272 0.357801 0.832344 11.00000 -1.20000 AFIX 0 C23 1 -0.188534 0.383594 0.906672 11.00000 0.02561 0.06490 = 0.01463 -0.00063 0.00216 0.00129 AFIX 23 H23A 2 -0.245687 0.392648 0.955251 11.00000 -1.20000 H23B 2 -0.102003 0.364573 0.927873 11.00000 -1.20000 AFIX 0 C24 1 -0.153984 0.441077 0.862991 11.00000 0.02602 0.04644 = 0.02328 -0.01324 -0.00368 0.00666 AFIX 23 H24A 2 -0.240628 0.461365 0.844674 11.00000 -1.20000 H24B 2 -0.103619 0.467826 0.902683 11.00000 -1.20000 AFIX 0 C25 1 0.150094 0.408359 0.451090 11.00000 0.01757 0.03754 = 0.01498 -0.00163 -0.00078 -0.00695 C26 1 0.233856 0.367006 0.413713 11.00000 0.02612 0.03936 = 0.02432 0.00040 0.00278 0.00254 AFIX 43 H26 2 0.264481 0.332312 0.443061 11.00000 -1.20000 AFIX 0 C27 1 0.272474 0.377357 0.331843 11.00000 0.02611 0.06246 = 0.02892 -0.00753 0.00885 -0.00444 AFIX 43 H27 2 0.329780 0.349502 0.304588 11.00000 -1.20000 AFIX 0 C28 1 0.227178 0.428240 0.290440 11.00000 0.02632 0.07061 = 0.02225 0.00349 0.00397 -0.00947 AFIX 43 H28 2 0.254675 0.435602 0.234958 11.00000 -1.20000 AFIX 0 C29 1 0.142237 0.468406 0.329248 11.00000 0.03122 0.05175 = 0.02771 0.01117 -0.00407 -0.01141 AFIX 43 H29 2 0.110767 0.502999 0.299983 11.00000 -1.20000 AFIX 0 C30 1 0.102486 0.458813 0.410264 11.00000 0.02257 0.03458 = 0.02883 -0.00059 0.00245 -0.00450 AFIX 43 H30 2 0.043804 0.486331 0.437105 11.00000 -1.20000 AFIX 0 C31 1 -0.728692 0.325283 0.841829 11.00000 0.05781 0.02057 = 0.03163 -0.00041 -0.00489 -0.00397 AFIX 137 H31A 2 -0.769259 0.298719 0.799010 11.00000 -1.50000 H31B 2 -0.782890 0.323026 0.892376 11.00000 -1.50000 H31C 2 -0.633355 0.312944 0.855013 11.00000 -1.50000 AFIX 0 C32 1 -0.662832 0.391913 0.729077 11.00000 0.02818 0.03161 = 0.02008 -0.00458 -0.00130 0.00510 AFIX 23 H32A 2 -0.703881 0.361901 0.690226 11.00000 -1.20000 H32B 2 -0.563202 0.382755 0.736760 11.00000 -1.20000 AFIX 0 C33 1 -0.679557 0.453819 0.690803 11.00000 0.03356 0.03008 = 0.01846 -0.00002 0.00078 0.00137 AFIX 23 H33A 2 -0.629479 0.455462 0.637916 11.00000 -1.20000 H33B 2 -0.778628 0.461266 0.677516 11.00000 -1.20000 AFIX 0 C34 1 -0.624702 0.502293 0.749254 11.00000 0.03353 0.02509 = 0.02387 0.00168 0.00107 -0.00295 AFIX 23 H34A 2 -0.525290 0.495617 0.762396 11.00000 -1.20000 H34B 2 -0.635387 0.541915 0.722312 11.00000 -1.20000 AFIX 0 C35 1 -0.368384 0.445442 1.149507 11.00000 0.01749 0.02444 = 0.02075 0.00285 -0.00041 -0.00939 C36 1 -0.437760 0.474117 1.211714 11.00000 0.02016 0.03973 = 0.02680 -0.00822 0.00195 -0.00391 AFIX 43 H36 2 -0.518314 0.497153 1.199504 11.00000 -1.20000 AFIX 0 C37 1 -0.384953 0.467962 1.293352 11.00000 0.03442 0.05283 = 0.02446 -0.01090 0.00618 -0.01802 AFIX 43 H37 2 -0.431771 0.486486 1.337706 11.00000 -1.20000 AFIX 0 C38 1 -0.267255 0.435857 1.311070 11.00000 0.04168 0.04733 = 0.01863 0.00581 -0.00562 -0.02240 AFIX 43 H38 2 -0.232623 0.432666 1.367079 11.00000 -1.20000 AFIX 0 C39 1 -0.198554 0.407942 1.246905 11.00000 0.02927 0.03587 = 0.03355 0.00708 -0.01110 -0.00853 AFIX 43 H39 2 -0.116707 0.385783 1.259176 11.00000 -1.20000 AFIX 0 C40 1 -0.248992 0.412289 1.164936 11.00000 0.01936 0.03352 = 0.02717 -0.00101 -0.00021 -0.00292 AFIX 43 H40 2 -0.203156 0.393140 1.120703 11.00000 -1.20000 AFIX 0 N1 3 1.136387 0.118380 0.141635 11.00000 0.01968 0.02744 = 0.01853 -0.00197 0.00011 0.00010 N2 3 0.977197 0.129169 -0.000584 11.00000 0.02047 0.03070 = 0.01649 -0.00028 0.00246 -0.00361 N3 3 0.860087 0.130583 0.151174 11.00000 0.01687 0.03338 = 0.01781 0.00347 0.00022 -0.00186 N4 3 1.038039 0.178020 0.268847 11.00000 0.02887 0.01947 = 0.02031 -0.00174 0.00082 -0.00118 N5 3 1.008376 0.064567 0.263069 11.00000 0.03837 0.01595 = 0.01900 -0.00278 0.00181 -0.00155 N6 3 0.580962 0.149590 0.407656 11.00000 0.02255 0.02697 = 0.01569 0.00141 0.00330 0.00409 N7 3 0.454411 0.140669 0.556414 11.00000 0.01964 0.02582 = 0.01578 0.00405 0.00078 -0.00103 N8 3 0.334528 0.204388 0.428846 11.00000 0.01958 0.02474 = 0.01691 0.00314 0.00131 0.00304 N9 3 0.513875 0.248768 0.323281 11.00000 0.02560 0.02082 = 0.01601 0.00181 0.00195 -0.00437 N10 3 0.385530 0.148383 0.287902 11.00000 0.02111 0.02364 = 0.01718 -0.00005 -0.00035 -0.00287 N11 3 -0.269757 0.415574 0.675762 11.00000 0.02176 0.03274 = 0.01847 -0.00109 0.00046 0.00731 N12 3 -0.143921 0.422451 0.527836 11.00000 0.02313 0.04750 = 0.01679 0.01152 0.00113 0.00375 N13 3 -0.019345 0.363096 0.658272 11.00000 0.01980 0.02518 = 0.01505 0.00167 0.00048 0.00519 N14 3 -0.188595 0.325609 0.773790 11.00000 0.02344 0.02503 = 0.02121 0.00137 0.00127 -0.00341 N15 3 -0.067898 0.430353 0.789260 11.00000 0.02079 0.02339 = 0.01995 -0.00311 0.00030 0.00254 N16 3 -0.833980 0.439615 0.940624 11.00000 0.01611 0.03218 = 0.02252 0.00183 -0.00075 -0.00078 N17 3 -0.675110 0.429457 1.083172 11.00000 0.01726 0.03455 = 0.01599 -0.00210 0.00019 -0.00134 N18 3 -0.556337 0.429493 0.932057 11.00000 0.01640 0.02888 = 0.01633 0.00116 0.00306 0.00150 N19 3 -0.729556 0.387388 0.810279 11.00000 0.03024 0.01821 = 0.02047 -0.00025 -0.00373 -0.00096 N20 3 -0.702901 0.500425 0.826171 11.00000 0.03332 0.01652 = 0.02064 -0.00137 -0.00036 0.00223 O1 4 0.714516 0.113260 0.018506 11.00000 0.02385 0.04227 = 0.02206 0.01095 -0.00625 -0.01245 O2 4 0.193844 0.170000 0.549273 11.00000 0.01818 0.02956 = 0.01387 0.00171 0.00214 -0.00271 O3 4 0.117477 0.398527 0.535490 11.00000 0.02010 0.03204 = 0.01496 -0.00150 0.00070 -0.00384 O4 4 -0.414602 0.451810 1.064682 11.00000 0.01782 0.03151 = 0.01593 0.00342 -0.00116 -0.00448 P1 5 1.007263 0.122492 0.202246 11.00000 0.01964 0.01994 = 0.01473 -0.00065 -0.00031 -0.00174 P2 5 1.124009 0.127473 0.044795 11.00000 0.01773 0.02271 = 0.01740 -0.00082 0.00240 -0.00018 P3 5 0.849336 0.144618 0.055084 11.00000 0.01584 0.02740 = 0.01741 0.00450 0.00022 -0.00271 P4 5 0.453329 0.187072 0.365436 11.00000 0.01910 0.01840 = 0.01340 0.00122 0.00017 -0.00139 P5 5 0.585994 0.130467 0.501382 11.00000 0.01745 0.01953 = 0.01592 -0.00023 -0.00103 -0.00059 P6 5 0.343941 0.188360 0.523762 11.00000 0.01782 0.02003 = 0.01402 0.00045 0.00126 -0.00112 P7 5 -0.136119 0.383735 0.719962 11.00000 0.01773 0.01955 = 0.01359 -0.00073 0.00028 0.00214 P8 5 -0.271711 0.436532 0.583355 11.00000 0.01842 0.02050 = 0.02054 0.00193 -0.00361 0.00070 P9 5 -0.029042 0.377225 0.562176 11.00000 0.01828 0.02451 = 0.01377 -0.00115 0.00028 -0.00166 P10 5 -0.702242 0.439534 0.881565 11.00000 0.01936 0.01902 = 0.01709 0.00063 -0.00180 0.00072 P11 5 -0.821594 0.427446 1.036772 11.00000 0.01598 0.02436 = 0.02056 -0.00109 0.00065 0.00002 P12 5 -0.544548 0.417248 1.027614 11.00000 0.01606 0.02265 = 0.01560 0.00167 -0.00055 -0.00079 CL1 6 1.223735 0.203548 0.013909 11.00000 0.02251 0.02503 = 0.03164 0.00096 0.00426 -0.00341 CL2 6 1.239508 0.066116 -0.010376 11.00000 0.03254 0.02618 = 0.02789 -0.00258 0.00777 0.00698 CL3 6 0.805691 0.232562 0.035317 11.00000 0.02918 0.02996 = 0.03299 0.00658 -0.00031 0.00492 CL4 6 0.640956 0.044578 0.513523 11.00000 0.03080 0.02162 = 0.03148 0.00221 -0.00339 0.00519 CL5 6 0.751292 0.169063 0.560659 11.00000 0.02354 0.04106 = 0.02697 -0.00863 -0.00267 -0.00920 CL6 6 0.377634 0.263837 0.591906 11.00000 0.03620 0.02387 = 0.02590 -0.00705 0.00425 -0.00480 CL7 6 -0.306827 0.524453 0.576230 11.00000 0.03757 0.01932 = 0.07758 0.00543 -0.02318 -0.00076 CL8 6 -0.443443 0.405229 0.524006 11.00000 0.02228 0.02958 = 0.02488 -0.00587 -0.00461 -0.00321 CL9 6 -0.053055 0.300121 0.497763 11.00000 0.04435 0.03639 = 0.02589 -0.01286 0.00721 -0.01510 CL10 6 -0.910460 0.347954 1.063914 11.00000 0.02755 0.02513 = 0.03489 0.00469 -0.00123 -0.00481 CL11 6 -0.949736 0.482187 1.094511 11.00000 0.02567 0.02937 = 0.03386 -0.00139 0.00847 0.00462 CL12 6 -0.489007 0.330573 1.046873 11.00000 0.03090 0.02382 = 0.02925 0.00508 -0.00402 0.00179 H20N 2 -0.728578 0.529192 0.851187 11.00000 0.03537 H5N 2 1.012838 0.032340 0.244632 11.00000 0.02216 H15N 2 0.009856 0.417716 0.799953 11.00000 0.02513 H10N 2 0.303782 0.154509 0.280908 11.00000 0.02730 HKLF 4 Covalent radii and connectivity table for 2007src0927 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - N4 C2 - N4 C3 C3 - C4 C2 C4 - N5 C3 C5 - C6 C10 O1 C6 - C5 C7 C7 - C8 C6 C8 - C7 C9 C9 - C8 C10 C10 - C5 C9 C11 - N9 C12 - N9 C13 C13 - C14 C12 C14 - N10 C13 C15 - C16 C20 O2 C16 - C15 C17 C17 - C18 C16 C18 - C17 C19 C19 - C18 C20 C20 - C15 C19 C21 - N14 C22 - N14 C23 C23 - C24 C22 C24 - N15 C23 C25 - C30 C26 O3 C26 - C25 C27 C27 - C28 C26 C28 - C29 C27 C29 - C28 C30 C30 - C25 C29 C31 - N19 C32 - N19 C33 C33 - C34 C32 C34 - N20 C33 C35 - C36 C40 O4 C36 - C35 C37 C37 - C38 C36 C38 - C37 C39 C39 - C40 C38 C40 - C39 C35 N1 - P2 P1 N2 - P2 P3 N3 - P3 P1 N4 - C1 C2 P1 N5 - C4 P1 N6 - P5 P4 N7 - P6 P5 N8 - P6 P4 N9 - C11 C12 P4 N10 - C14 P4 N11 - P8 P7 N12 - P8 P9 N13 - P9 P7 N14 - C21 C22 P7 N15 - C24 P7 N16 - P11 P10 N17 - P11 P12 N18 - P12 P10 N19 - C32 C31 P10 N20 - C34 P10 O1 - C5 P3 O2 - C15 P6 O3 - C25 P9 O4 - C35 P12 P1 - N1 N5 N3 N4 P2 - N1 N2 Cl2 Cl1 P3 P3 - N3 O1 N2 Cl3 P2 P4 - N8 N6 N10 N9 P5 - N6 N7 Cl4 Cl5 P6 - N8 O2 N7 Cl6 P7 - N13 N11 N15 N14 P8 - N11 N12 Cl7 Cl8 P9 - O3 N13 N12 Cl9 P10 - N16 N18 N20 N19 P11 - N16 N17 Cl11 Cl10 P12 - N18 O4 N17 Cl12 Cl1 - P2 Cl2 - P2 Cl3 - P3 Cl4 - P5 Cl5 - P5 Cl6 - P6 Cl7 - P8 Cl8 - P8 Cl9 - P9 Cl10 - P11 Cl11 - P11 Cl12 - P12 Floating origin restraints generated 35250 Reflections read, of which 38 rejected -12 =< h =< 12, -29 =< k =< 28, -20 =< l =< 20, Max. 2-theta = 54.99 0 Systematic absence violations 0 Inconsistent equivalents 15188 Unique reflections, of which 0 suppressed R(int) = 0.0323 R(sigma) = 0.0436 Friedel opposites not merged Maximum memory for data reduction = 6502 / 151418 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 = 8726 / 1190280 wR2 = 0.0714 before cycle 1 for 15188 data and 814 / 814 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38089 0.00022 0.045 OSF 2 0.43599 0.03403 0.000 BASF 1 Mean shift/esd = 0.005 Maximum = 0.045 for OSF Max. shift = 0.001 A for H10N Max. dU = 0.000 for H10N Least-squares cycle 2 Maximum vector length = 511 Memory required = 8726 / 1190280 wR2 = 0.0714 before cycle 2 for 15188 data and 814 / 814 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38089 0.00022 0.004 OSF 2 0.43599 0.03400 0.000 BASF 1 Mean shift/esd = 0.002 Maximum = 0.009 for x N10 Max. shift = 0.000 A for H10N Max. dU = 0.000 for H10N Least-squares cycle 3 Maximum vector length = 511 Memory required = 8726 / 1190280 wR2 = 0.0713 before cycle 3 for 15188 data and 814 / 814 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38089 0.00022 0.000 OSF 2 0.43599 0.03399 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.002 for y H5N Max. shift = 0.000 A for H5N Max. dU = 0.000 for H5N Least-squares cycle 4 Maximum vector length = 511 Memory required = 8726 / 1190280 wR2 = 0.0714 before cycle 4 for 15188 data and 814 / 814 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38089 0.00022 -0.001 OSF 2 0.43600 0.03400 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for z P12 Max. shift = 0.000 A for H5N Max. dU = 0.000 for H15N No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.9446 0.2528 0.2252 137 0.980 0.000 C1 N4 H1A H1B 1.0827 0.2364 0.1778 137 0.980 0.000 C1 N4 H1A H1C 1.0925 0.2650 0.2694 137 0.980 0.000 C1 N4 H1A H2A 0.8753 0.1821 0.3455 23 0.990 0.000 C2 N4 C3 H2B 1.0146 0.2089 0.3868 23 0.990 0.000 C2 N4 C3 H3A 1.1046 0.1124 0.4050 23 0.990 0.000 C3 C4 C2 H3B 0.9608 0.1182 0.4510 23 0.990 0.000 C3 C4 C2 H4A 0.9694 0.0278 0.3759 23 0.990 0.000 C4 N5 C3 H4B 0.8457 0.0690 0.3398 23 0.990 0.000 C4 N5 C3 H6 0.8152 0.0877 -0.1264 43 0.950 0.000 C6 C5 C7 H7 0.7100 0.1031 -0.2597 43 0.950 0.000 C7 C8 C6 H8 0.4933 0.1463 -0.2723 43 0.950 0.000 C8 C7 C9 H9 0.3821 0.1775 -0.1539 43 0.950 0.000 C9 C8 C10 H10 0.4856 0.1638 -0.0202 43 0.950 0.000 C10 C5 C9 H11A 0.6854 0.2711 0.3919 137 0.980 0.000 C11 N9 H11A H11B 0.5449 0.2902 0.4347 137 0.980 0.000 C11 N9 H11A H11C 0.6001 0.3278 0.3576 137 0.980 0.000 C11 N9 H11A H12A 0.6704 0.2252 0.2482 23 0.990 0.000 C12 N9 C13 H12B 0.5939 0.2854 0.2191 23 0.990 0.000 C12 N9 C13 H13A 0.4017 0.2304 0.1683 23 0.990 0.000 C13 C14 C12 H13B 0.5384 0.2070 0.1249 23 0.990 0.000 C13 C14 C12 H14A 0.4098 0.1244 0.1670 23 0.990 0.000 C14 N10 C13 H14B 0.5522 0.1261 0.2207 23 0.990 0.000 C14 N10 C13 H16 0.2268 0.0710 0.6306 43 0.950 0.000 C16 C15 C17 H17 0.1606 0.0488 0.7667 43 0.950 0.000 C17 C18 C16 H18 0.0503 0.1208 0.8448 43 0.950 0.000 C18 C17 C19 H19 0.0062 0.2153 0.7895 43 0.950 0.000 C19 C18 C20 H20 0.0769 0.2393 0.6545 43 0.950 0.000 C20 C15 C19 H21A -0.2682 0.2429 0.7575 137 0.980 0.000 C21 N14 H21A H21B -0.2025 0.2696 0.6751 137 0.980 0.000 C21 N14 H21A H21C -0.3493 0.2931 0.7044 137 0.980 0.000 C21 N14 H21A H22A -0.2839 0.3029 0.8805 23 0.990 0.000 C22 N14 C23 H22B -0.3563 0.3578 0.8323 23 0.990 0.000 C22 N14 C23 H23A -0.2457 0.3926 0.9552 23 0.990 0.000 C23 C24 C22 H23B -0.1020 0.3646 0.9279 23 0.990 0.000 C23 C24 C22 H24A -0.2406 0.4614 0.8447 23 0.990 0.000 C24 N15 C23 H24B -0.1036 0.4678 0.9027 23 0.990 0.000 C24 N15 C23 H26 0.2645 0.3323 0.4431 43 0.950 0.000 C26 C25 C27 H27 0.3298 0.3495 0.3046 43 0.950 0.000 C27 C28 C26 H28 0.2547 0.4356 0.2350 43 0.950 0.000 C28 C29 C27 H29 0.1108 0.5030 0.3000 43 0.950 0.000 C29 C28 C30 H30 0.0438 0.4863 0.4371 43 0.950 0.000 C30 C25 C29 H31A -0.7692 0.2987 0.7990 137 0.980 0.000 C31 N19 H31A H31B -0.7829 0.3230 0.8924 137 0.980 0.000 C31 N19 H31A H31C -0.6333 0.3129 0.8550 137 0.980 0.000 C31 N19 H31A H32A -0.7039 0.3619 0.6902 23 0.990 0.000 C32 N19 C33 H32B -0.5632 0.3828 0.7368 23 0.990 0.000 C32 N19 C33 H33A -0.6295 0.4555 0.6379 23 0.990 0.000 C33 C34 C32 H33B -0.7786 0.4613 0.6775 23 0.990 0.000 C33 C34 C32 H34A -0.5253 0.4956 0.7624 23 0.990 0.000 C34 N20 C33 H34B -0.6354 0.5419 0.7223 23 0.990 0.000 C34 N20 C33 H36 -0.5183 0.4971 1.1995 43 0.950 0.000 C36 C35 C37 H37 -0.4318 0.4865 1.3377 43 0.950 0.000 C37 C38 C36 H38 -0.2326 0.4327 1.3671 43 0.950 0.000 C38 C37 C39 H39 -0.1167 0.3858 1.2592 43 0.950 0.000 C39 C40 C38 H40 -0.2032 0.3931 1.1207 43 0.950 0.000 C40 C39 C35 2007src0927 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 1.03960 0.23800 0.23228 1.00000 0.04463 0.01917 0.03781 0.00078 0.00094 -0.00166 0.03388 0.00570 0.00036 0.00013 0.00022 0.00000 0.00186 0.00149 0.00192 0.00132 0.00148 0.00131 0.00073 H1A 0.94465 0.25275 0.22517 1.00000 0.05082 0.00000 0.00000 H1B 1.08268 0.23643 0.17778 1.00000 0.05082 0.00000 0.00000 H1C 1.09251 0.26496 0.26943 1.00000 0.05082 0.00000 0.00000 C2 0.97631 0.17593 0.35196 1.00000 0.02777 0.03438 0.02096 -0.00727 0.00104 0.00326 0.02770 0.00522 0.00031 0.00014 0.00018 0.00000 0.00145 0.00169 0.00150 0.00126 0.00117 0.00123 0.00065 H2A 0.87527 0.18205 0.34549 1.00000 0.03324 0.00000 0.00000 H2B 1.01464 0.20892 0.38678 1.00000 0.03324 0.00000 0.00000 C3 1.00377 0.11752 0.39571 1.00000 0.02894 0.03783 0.01430 -0.00116 0.00194 0.00314 0.02700 0.00505 0.00030 0.00014 0.00017 0.00000 0.00144 0.00171 0.00135 0.00123 0.00109 0.00126 0.00063 H3A 1.10465 0.11240 0.40503 1.00000 0.03239 0.00000 0.00000 H3B 0.96081 0.11822 0.45098 1.00000 0.03239 0.00000 0.00000 C4 0.94746 0.06555 0.34605 1.00000 0.03193 0.03110 0.01960 0.00241 0.00317 -0.00604 0.02750 0.00509 0.00032 0.00014 0.00018 0.00000 0.00155 0.00161 0.00149 0.00125 0.00119 0.00125 0.00064 H4A 0.96940 0.02781 0.37587 1.00000 0.03299 0.00000 0.00000 H4B 0.84571 0.06897 0.33982 1.00000 0.03299 0.00000 0.00000 C5 0.65858 0.12440 -0.06340 1.00000 0.01865 0.03589 0.01754 0.00547 -0.00351 -0.01022 0.02411 0.00465 0.00027 0.00014 0.00017 0.00000 0.00123 0.00162 0.00135 0.00120 0.00103 0.00115 0.00060 C6 0.72695 0.10612 -0.13198 1.00000 0.02746 0.03091 0.03108 -0.00284 -0.00347 0.00484 0.02991 0.00519 0.00031 0.00014 0.00020 0.00000 0.00146 0.00162 0.00168 0.00129 0.00125 0.00121 0.00067 H6 0.81520 0.08774 -0.12639 1.00000 0.03589 0.00000 0.00000 C7 0.66371 0.11514 -0.21104 1.00000 0.03756 0.04153 0.02271 -0.00506 0.00153 0.00075 0.03392 0.00550 0.00033 0.00015 0.00020 0.00000 0.00170 0.00188 0.00156 0.00137 0.00128 0.00141 0.00071 H7 0.71001 0.10315 -0.25970 1.00000 0.04070 0.00000 0.00000 C8 0.53623 0.14098 -0.21865 1.00000 0.03099 0.04119 0.01914 0.00298 -0.00657 -0.00364 0.03060 0.00513 0.00031 0.00015 0.00019 0.00000 0.00151 0.00181 0.00147 0.00130 0.00119 0.00130 0.00068 H8 0.49328 0.14635 -0.27231 1.00000 0.03672 0.00000 0.00000 C9 0.47039 0.15919 -0.14836 1.00000 0.02407 0.08200 0.03275 -0.00542 -0.00748 0.01265 0.04645 0.00639 0.00034 0.00020 0.00022 0.00000 0.00155 0.00283 0.00191 0.00183 0.00137 0.00169 0.00096 H9 0.38210 0.17754 -0.15392 1.00000 0.05574 0.00000 0.00000 C10 0.53104 0.15118 -0.06884 1.00000 0.02448 0.09505 0.02250 -0.00344 0.00067 0.00454 0.04734 0.00650 0.00033 0.00020 0.00022 0.00000 0.00155 0.00316 0.00168 0.00183 0.00128 0.00175 0.00100 H10 0.48562 0.16382 -0.02019 1.00000 0.05681 0.00000 0.00000 C11 0.59265 0.28774 0.38174 1.00000 0.03968 0.02832 0.02808 -0.00169 0.00154 -0.01584 0.03202 0.00492 0.00034 0.00014 0.00020 0.00000 0.00174 0.00163 0.00165 0.00129 0.00133 0.00132 0.00071 H11A 0.68535 0.27114 0.39186 1.00000 0.04803 0.00000 0.00000 H11B 0.54490 0.29019 0.43467 1.00000 0.04803 0.00000 0.00000 H11C 0.60010 0.32779 0.35755 1.00000 0.04803 0.00000 0.00000 C12 0.57902 0.24467 0.24109 1.00000 0.02335 0.03157 0.01940 0.00422 0.00538 -0.00393 0.02467 0.00492 0.00029 0.00014 0.00017 0.00000 0.00136 0.00158 0.00144 0.00118 0.00110 0.00113 0.00061 H12A 0.67040 0.22516 0.24821 1.00000 0.02961 0.00000 0.00000 H12B 0.59387 0.28545 0.21913 1.00000 0.02961 0.00000 0.00000 C13 0.49068 0.20945 0.17855 1.00000 0.02289 0.03756 0.01115 0.00475 0.00135 -0.00129 0.02385 0.00479 0.00028 0.00013 0.00017 0.00000 0.00131 0.00165 0.00125 0.00114 0.00102 0.00114 0.00059 H13A 0.40175 0.23043 0.16826 1.00000 0.02862 0.00000 0.00000 H13B 0.53841 0.20702 0.12490 1.00000 0.02862 0.00000 0.00000 C14 0.46320 0.14700 0.21025 1.00000 0.02752 0.03091 0.01433 -0.00575 0.00096 0.00188 0.02424 0.00479 0.00030 0.00013 0.00017 0.00000 0.00137 0.00158 0.00130 0.00114 0.00106 0.00113 0.00059 H14A 0.40982 0.12436 0.16701 1.00000 0.02909 0.00000 0.00000 H14B 0.55220 0.12611 0.22074 1.00000 0.02909 0.00000 0.00000 C15 0.15775 0.15689 0.63225 1.00000 0.01434 0.03037 0.01402 0.00114 0.00085 -0.00317 0.01957 0.00445 0.00025 0.00013 0.00016 0.00000 0.00114 0.00149 0.00127 0.00110 0.00096 0.00102 0.00055 C16 0.18297 0.10037 0.66344 1.00000 0.02944 0.02738 0.02283 0.00172 0.00624 -0.00022 0.02643 0.00514 0.00031 0.00013 0.00019 0.00000 0.00150 0.00155 0.00151 0.00120 0.00118 0.00117 0.00062 H16 0.22682 0.07102 0.63059 1.00000 0.03172 0.00000 0.00000 C17 0.14301 0.08728 0.74366 1.00000 0.03252 0.03787 0.03188 0.01049 0.00866 -0.00050 0.03392 0.00602 0.00033 0.00016 0.00021 0.00000 0.00168 0.00181 0.00179 0.00145 0.00135 0.00134 0.00073 H17 0.16061 0.04882 0.76673 1.00000 0.04071 0.00000 0.00000 C18 0.07785 0.13001 0.78991 1.00000 0.02813 0.04929 0.01934 0.00473 0.00493 -0.00373 0.03216 0.00561 0.00031 0.00016 0.00020 0.00000 0.00151 0.00199 0.00149 0.00141 0.00117 0.00142 0.00070 H18 0.05025 0.12081 0.84484 1.00000 0.03859 0.00000 0.00000 C19 0.05214 0.18627 0.75713 1.00000 0.02596 0.04610 0.02443 -0.00853 0.00717 0.00210 0.03203 0.00551 0.00031 0.00016 0.00019 0.00000 0.00148 0.00192 0.00157 0.00142 0.00121 0.00134 0.00070 H19 0.00618 0.21527 0.78950 1.00000 0.03843 0.00000 0.00000 C20 0.09298 0.20065 0.67734 1.00000 0.02035 0.03090 0.02912 -0.00009 0.00323 0.00380 0.02674 0.00515 0.00028 0.00014 0.00019 0.00000 0.00130 0.00160 0.00157 0.00129 0.00114 0.00115 0.00062 H20 0.07689 0.23932 0.65454 1.00000 0.03209 0.00000 0.00000 C21 -0.25790 0.27893 0.72351 1.00000 0.03268 0.03165 0.04866 -0.00358 -0.00010 -0.00847 0.03769 0.00544 0.00035 0.00015 0.00023 0.00000 0.00170 0.00175 0.00215 0.00155 0.00150 0.00132 0.00079 H21A -0.26819 0.24290 0.75754 1.00000 0.05654 0.00000 0.00000 H21B -0.20247 0.26962 0.67505 1.00000 0.05654 0.00000 0.00000 H21C -0.34930 0.29312 0.70437 1.00000 0.05654 0.00000 0.00000 C22 -0.26591 0.34019 0.84943 1.00000 0.02557 0.04703 0.02101 0.00941 0.00228 -0.00519 0.03117 0.00544 0.00031 0.00015 0.00019 0.00000 0.00145 0.00193 0.00148 0.00137 0.00116 0.00130 0.00069 H22A -0.28388 0.30290 0.88053 1.00000 0.03741 0.00000 0.00000 H22B -0.35627 0.35780 0.83234 1.00000 0.03741 0.00000 0.00000 C23 -0.18854 0.38359 0.90667 1.00000 0.02561 0.06493 0.01463 -0.00064 0.00216 0.00130 0.03502 0.00557 0.00031 0.00017 0.00019 0.00000 0.00146 0.00228 0.00142 0.00146 0.00112 0.00146 0.00075 H23A -0.24570 0.39265 0.95525 1.00000 0.04202 0.00000 0.00000 H23B -0.10201 0.36457 0.92788 1.00000 0.04202 0.00000 0.00000 C24 -0.15399 0.44108 0.86299 1.00000 0.02602 0.04647 0.02328 -0.01325 -0.00368 0.00667 0.03202 0.00533 0.00031 0.00015 0.00019 0.00000 0.00145 0.00193 0.00158 0.00141 0.00119 0.00135 0.00072 H24A -0.24063 0.46136 0.84467 1.00000 0.03842 0.00000 0.00000 H24B -0.10362 0.46782 0.90268 1.00000 0.03842 0.00000 0.00000 C25 0.15010 0.40836 0.45109 1.00000 0.01757 0.03754 0.01498 -0.00163 -0.00079 -0.00694 0.02339 0.00460 0.00027 0.00014 0.00017 0.00000 0.00125 0.00163 0.00137 0.00119 0.00102 0.00111 0.00059 C26 0.23386 0.36701 0.41371 1.00000 0.02611 0.03934 0.02432 0.00041 0.00277 0.00254 0.02988 0.00539 0.00030 0.00015 0.00020 0.00000 0.00144 0.00180 0.00159 0.00132 0.00121 0.00128 0.00067 H26 0.26448 0.33231 0.44306 1.00000 0.03586 0.00000 0.00000 C27 0.27247 0.37736 0.33185 1.00000 0.02611 0.06243 0.02893 -0.00752 0.00884 -0.00443 0.03898 0.00597 0.00033 0.00018 0.00021 0.00000 0.00155 0.00239 0.00179 0.00165 0.00132 0.00152 0.00082 H27 0.32978 0.34950 0.30459 1.00000 0.04678 0.00000 0.00000 C28 0.22718 0.42824 0.29044 1.00000 0.02632 0.07062 0.02224 0.00349 0.00399 -0.00948 0.03966 0.00591 0.00032 0.00018 0.00021 0.00000 0.00153 0.00252 0.00162 0.00165 0.00123 0.00162 0.00083 H28 0.25467 0.43560 0.23496 1.00000 0.04759 0.00000 0.00000 C29 0.14224 0.46840 0.32925 1.00000 0.03120 0.05172 0.02772 0.01118 -0.00406 -0.01138 0.03699 0.00563 0.00033 0.00017 0.00021 0.00000 0.00164 0.00212 0.00169 0.00152 0.00133 0.00145 0.00079 H29 0.11077 0.50300 0.29998 1.00000 0.04439 0.00000 0.00000 C30 0.10249 0.45881 0.41026 1.00000 0.02257 0.03457 0.02882 -0.00060 0.00245 -0.00449 0.02862 0.00514 0.00030 0.00014 0.00020 0.00000 0.00139 0.00168 0.00164 0.00132 0.00119 0.00119 0.00066 H30 0.04381 0.48633 0.43711 1.00000 0.03434 0.00000 0.00000 C31 -0.72869 0.32528 0.84183 1.00000 0.05780 0.02058 0.03162 -0.00040 -0.00488 -0.00397 0.03680 0.00575 0.00040 0.00014 0.00022 0.00000 0.00216 0.00155 0.00179 0.00131 0.00156 0.00142 0.00078 H31A -0.76924 0.29872 0.79901 1.00000 0.05521 0.00000 0.00000 H31B -0.78290 0.32302 0.89237 1.00000 0.05521 0.00000 0.00000 H31C -0.63335 0.31295 0.85502 1.00000 0.05521 0.00000 0.00000 C32 -0.66283 0.39191 0.72908 1.00000 0.02817 0.03162 0.02009 -0.00459 -0.00130 0.00511 0.02667 0.00518 0.00031 0.00014 0.00018 0.00000 0.00147 0.00161 0.00148 0.00123 0.00116 0.00122 0.00063 H32A -0.70389 0.36190 0.69023 1.00000 0.03201 0.00000 0.00000 H32B -0.56321 0.38275 0.73676 1.00000 0.03201 0.00000 0.00000 C33 -0.67956 0.45382 0.69081 1.00000 0.03356 0.03008 0.01846 0.00000 0.00078 0.00137 0.02737 0.00514 0.00032 0.00013 0.00018 0.00000 0.00156 0.00158 0.00146 0.00120 0.00119 0.00123 0.00064 H33A -0.62948 0.45546 0.63792 1.00000 0.03285 0.00000 0.00000 H33B -0.77863 0.46127 0.67752 1.00000 0.03285 0.00000 0.00000 C34 -0.62470 0.50229 0.74925 1.00000 0.03355 0.02509 0.02386 0.00168 0.00107 -0.00294 0.02749 0.00517 0.00032 0.00014 0.00019 0.00000 0.00155 0.00146 0.00154 0.00119 0.00121 0.00119 0.00062 H34A -0.52529 0.49562 0.76239 1.00000 0.03299 0.00000 0.00000 H34B -0.63538 0.54192 0.72231 1.00000 0.03299 0.00000 0.00000 C35 -0.36839 0.44544 1.14951 1.00000 0.01748 0.02444 0.02075 0.00285 -0.00041 -0.00939 0.02092 0.00451 0.00027 0.00012 0.00018 0.00000 0.00122 0.00141 0.00142 0.00112 0.00103 0.00104 0.00057 C36 -0.43776 0.47412 1.21171 1.00000 0.02015 0.03972 0.02680 -0.00822 0.00195 -0.00390 0.02887 0.00503 0.00030 0.00015 0.00019 0.00000 0.00135 0.00177 0.00160 0.00136 0.00116 0.00121 0.00066 H36 -0.51832 0.49715 1.19951 1.00000 0.03464 0.00000 0.00000 C37 -0.38495 0.46796 1.29335 1.00000 0.03442 0.05283 0.02447 -0.01091 0.00618 -0.01803 0.03713 0.00522 0.00034 0.00016 0.00020 0.00000 0.00170 0.00212 0.00163 0.00151 0.00132 0.00150 0.00079 H37 -0.43177 0.48649 1.33771 1.00000 0.04455 0.00000 0.00000 C38 -0.26726 0.43586 1.31107 1.00000 0.04169 0.04733 0.01862 0.00581 -0.00562 -0.02241 0.03602 0.00523 0.00035 0.00016 0.00020 0.00000 0.00179 0.00199 0.00150 0.00139 0.00131 0.00156 0.00078 H38 -0.23263 0.43266 1.36708 1.00000 0.04323 0.00000 0.00000 C39 -0.19856 0.40794 1.24690 1.00000 0.02925 0.03586 0.03357 0.00707 -0.01110 -0.00854 0.03315 0.00519 0.00033 0.00015 0.00021 0.00000 0.00153 0.00174 0.00180 0.00140 0.00132 0.00129 0.00073 H39 -0.11671 0.38579 1.25917 1.00000 0.03979 0.00000 0.00000 C40 -0.24899 0.41229 1.16494 1.00000 0.01935 0.03350 0.02716 -0.00102 -0.00021 -0.00292 0.02669 0.00491 0.00028 0.00014 0.00019 0.00000 0.00129 0.00161 0.00157 0.00127 0.00111 0.00114 0.00063 H40 -0.20316 0.39314 1.12071 1.00000 0.03203 0.00000 0.00000 N1 1.13638 0.11838 0.14163 1.00000 0.01968 0.02744 0.01853 -0.00197 0.00011 0.00010 0.02189 0.00385 0.00022 0.00011 0.00014 0.00000 0.00108 0.00125 0.00115 0.00098 0.00088 0.00092 0.00048 N2 0.97720 0.12917 -0.00058 1.00000 0.02047 0.03069 0.01650 -0.00029 0.00246 -0.00361 0.02251 0.00389 0.00022 0.00011 0.00014 0.00000 0.00110 0.00130 0.00113 0.00098 0.00088 0.00097 0.00049 N3 0.86009 0.13058 0.15117 1.00000 0.01688 0.03337 0.01781 0.00346 0.00022 -0.00186 0.02269 0.00399 0.00022 0.00011 0.00014 0.00000 0.00103 0.00133 0.00116 0.00101 0.00086 0.00097 0.00049 N4 1.03803 0.17802 0.26885 1.00000 0.02887 0.01945 0.02031 -0.00174 0.00082 -0.00118 0.02288 0.00401 0.00025 0.00010 0.00015 0.00000 0.00122 0.00117 0.00120 0.00094 0.00096 0.00093 0.00049 N5 1.00837 0.06457 0.26307 1.00000 0.03837 0.01594 0.01901 -0.00279 0.00182 -0.00155 0.02442 0.00441 0.00027 0.00012 0.00016 0.00000 0.00142 0.00123 0.00127 0.00102 0.00103 0.00101 0.00053 N6 0.58096 0.14959 0.40766 1.00000 0.02254 0.02698 0.01569 0.00141 0.00330 0.00408 0.02168 0.00407 0.00024 0.00011 0.00014 0.00000 0.00113 0.00128 0.00117 0.00097 0.00091 0.00093 0.00049 N7 0.45441 0.14067 0.55641 1.00000 0.01964 0.02581 0.01578 0.00405 0.00078 -0.00104 0.02041 0.00385 0.00022 0.00010 0.00014 0.00000 0.00106 0.00124 0.00113 0.00094 0.00086 0.00090 0.00048 N8 0.33453 0.20439 0.42885 1.00000 0.01957 0.02473 0.01691 0.00313 0.00132 0.00304 0.02039 0.00392 0.00022 0.00010 0.00014 0.00000 0.00108 0.00123 0.00114 0.00094 0.00087 0.00090 0.00047 N9 0.51387 0.24877 0.32328 1.00000 0.02559 0.02082 0.01601 0.00180 0.00195 -0.00437 0.02078 0.00388 0.00023 0.00010 0.00014 0.00000 0.00115 0.00116 0.00115 0.00090 0.00090 0.00090 0.00048 N10 0.38554 0.14838 0.28790 1.00000 0.02110 0.02365 0.01718 -0.00005 -0.00036 -0.00288 0.02067 0.00398 0.00025 0.00010 0.00015 0.00000 0.00114 0.00122 0.00116 0.00093 0.00091 0.00092 0.00048 N11 -0.26976 0.41557 0.67576 1.00000 0.02176 0.03273 0.01846 -0.00109 0.00046 0.00730 0.02432 0.00414 0.00024 0.00011 0.00015 0.00000 0.00114 0.00136 0.00123 0.00103 0.00093 0.00098 0.00052 N12 -0.14392 0.42245 0.52784 1.00000 0.02313 0.04747 0.01679 0.01152 0.00114 0.00374 0.02912 0.00456 0.00024 0.00012 0.00015 0.00000 0.00117 0.00164 0.00123 0.00113 0.00095 0.00111 0.00058 N13 -0.01934 0.36310 0.65827 1.00000 0.01980 0.02518 0.01503 0.00166 0.00048 0.00519 0.02000 0.00395 0.00022 0.00010 0.00014 0.00000 0.00107 0.00122 0.00115 0.00091 0.00088 0.00090 0.00047 N14 -0.18860 0.32561 0.77379 1.00000 0.02344 0.02501 0.02122 0.00136 0.00126 -0.00341 0.02321 0.00398 0.00024 0.00010 0.00015 0.00000 0.00114 0.00124 0.00123 0.00097 0.00093 0.00094 0.00050 N15 -0.06790 0.43035 0.78926 1.00000 0.02079 0.02339 0.01993 -0.00312 0.00030 0.00255 0.02138 0.00401 0.00025 0.00011 0.00015 0.00000 0.00112 0.00121 0.00121 0.00097 0.00091 0.00094 0.00048 N16 -0.83398 0.43962 0.94062 1.00000 0.01611 0.03217 0.02251 0.00182 -0.00075 -0.00079 0.02363 0.00406 0.00023 0.00011 0.00015 0.00000 0.00103 0.00133 0.00125 0.00104 0.00089 0.00095 0.00050 N17 -0.67511 0.42946 1.08317 1.00000 0.01726 0.03452 0.01599 -0.00210 0.00019 -0.00134 0.02260 0.00390 0.00023 0.00011 0.00014 0.00000 0.00102 0.00135 0.00114 0.00100 0.00086 0.00095 0.00049 N18 -0.55634 0.42949 0.93206 1.00000 0.01639 0.02888 0.01634 0.00115 0.00306 0.00150 0.02048 0.00392 0.00022 0.00011 0.00014 0.00000 0.00103 0.00126 0.00114 0.00097 0.00084 0.00092 0.00047 N19 -0.72956 0.38739 0.81028 1.00000 0.03023 0.01820 0.02047 -0.00024 -0.00373 -0.00097 0.02306 0.00393 0.00025 0.00010 0.00015 0.00000 0.00123 0.00114 0.00123 0.00095 0.00098 0.00093 0.00050 N20 -0.70290 0.50043 0.82617 1.00000 0.03332 0.01652 0.02064 -0.00137 -0.00036 0.00223 0.02352 0.00432 0.00026 0.00011 0.00016 0.00000 0.00133 0.00119 0.00127 0.00100 0.00101 0.00099 0.00051 O1 0.71451 0.11326 0.01851 1.00000 0.02385 0.04227 0.02206 0.01094 -0.00625 -0.01245 0.02954 0.00343 0.00020 0.00010 0.00013 0.00000 0.00100 0.00125 0.00109 0.00093 0.00083 0.00089 0.00048 O2 0.19384 0.17000 0.54927 1.00000 0.01818 0.02956 0.01387 0.00171 0.00214 -0.00271 0.02050 0.00319 0.00019 0.00009 0.00011 0.00000 0.00087 0.00105 0.00093 0.00078 0.00071 0.00074 0.00040 O3 0.11748 0.39853 0.53549 1.00000 0.02010 0.03203 0.01496 -0.00150 0.00070 -0.00385 0.02236 0.00323 0.00019 0.00009 0.00012 0.00000 0.00093 0.00113 0.00097 0.00082 0.00073 0.00078 0.00042 O4 -0.41460 0.45181 1.06468 1.00000 0.01782 0.03150 0.01594 0.00342 -0.00116 -0.00448 0.02179 0.00317 0.00018 0.00009 0.00012 0.00000 0.00089 0.00109 0.00097 0.00080 0.00074 0.00077 0.00041 P1 1.00726 0.12249 0.20225 1.00000 0.01964 0.01994 0.01473 -0.00065 -0.00031 -0.00174 0.01812 0.00114 0.00007 0.00003 0.00004 0.00000 0.00031 0.00034 0.00032 0.00027 0.00025 0.00026 0.00014 P2 1.12401 0.12747 0.04479 1.00000 0.01773 0.02271 0.01740 -0.00082 0.00240 -0.00018 0.01924 0.00118 0.00007 0.00003 0.00004 0.00000 0.00030 0.00035 0.00034 0.00028 0.00025 0.00026 0.00014 P3 0.84934 0.14462 0.05508 1.00000 0.01584 0.02740 0.01741 0.00450 0.00022 -0.00271 0.02022 0.00121 0.00007 0.00003 0.00005 0.00000 0.00031 0.00038 0.00035 0.00029 0.00026 0.00026 0.00015 P4 0.45333 0.18707 0.36544 1.00000 0.01910 0.01840 0.01340 0.00122 0.00017 -0.00139 0.01698 0.00114 0.00007 0.00003 0.00004 0.00000 0.00031 0.00033 0.00032 0.00026 0.00025 0.00025 0.00013 P5 0.58599 0.13047 0.50138 1.00000 0.01745 0.01953 0.01592 -0.00023 -0.00103 -0.00059 0.01767 0.00114 0.00007 0.00003 0.00004 0.00000 0.00030 0.00034 0.00033 0.00027 0.00025 0.00026 0.00014 P6 0.34394 0.18836 0.52376 1.00000 0.01783 0.02003 0.01402 0.00045 0.00126 -0.00112 0.01728 0.00115 0.00007 0.00003 0.00004 0.00000 0.00031 0.00033 0.00032 0.00026 0.00024 0.00025 0.00013 P7 -0.13612 0.38373 0.71996 1.00000 0.01773 0.01956 0.01359 -0.00073 0.00028 0.00214 0.01696 0.00115 0.00007 0.00003 0.00004 0.00000 0.00031 0.00033 0.00032 0.00026 0.00025 0.00025 0.00013 P8 -0.27171 0.43653 0.58336 1.00000 0.01842 0.02050 0.02055 0.00193 -0.00361 0.00070 0.01992 0.00118 0.00007 0.00003 0.00005 0.00000 0.00031 0.00035 0.00036 0.00028 0.00027 0.00026 0.00014 P9 -0.02904 0.37723 0.56218 1.00000 0.01828 0.02451 0.01377 -0.00115 0.00028 -0.00166 0.01886 0.00116 0.00007 0.00003 0.00004 0.00000 0.00031 0.00036 0.00033 0.00028 0.00025 0.00026 0.00014 P10 -0.70224 0.43953 0.88157 1.00000 0.01936 0.01902 0.01710 0.00063 -0.00180 0.00072 0.01854 0.00117 0.00007 0.00003 0.00004 0.00000 0.00031 0.00034 0.00035 0.00027 0.00026 0.00025 0.00014 P11 -0.82159 0.42745 1.03677 1.00000 0.01598 0.02436 0.02057 -0.00109 0.00065 0.00003 0.02030 0.00120 0.00007 0.00003 0.00005 0.00000 0.00030 0.00037 0.00036 0.00029 0.00026 0.00026 0.00015 P12 -0.54455 0.41725 1.02761 1.00000 0.01606 0.02265 0.01560 0.00167 -0.00055 -0.00079 0.01813 0.00115 0.00007 0.00003 0.00004 0.00000 0.00030 0.00035 0.00033 0.00027 0.00025 0.00025 0.00014 Cl1 1.22373 0.20355 0.01391 1.00000 0.02251 0.02504 0.03164 0.00096 0.00426 -0.00341 0.02632 0.00120 0.00007 0.00003 0.00005 0.00000 0.00031 0.00035 0.00038 0.00029 0.00028 0.00025 0.00015 Cl2 1.23951 0.06612 -0.01038 1.00000 0.03254 0.02618 0.02789 -0.00258 0.00777 0.00698 0.02872 0.00132 0.00008 0.00003 0.00005 0.00000 0.00036 0.00036 0.00038 0.00029 0.00029 0.00028 0.00015 Cl3 0.80569 0.23256 0.03532 1.00000 0.02919 0.02997 0.03299 0.00658 -0.00031 0.00492 0.03074 0.00134 0.00008 0.00003 0.00005 0.00000 0.00036 0.00038 0.00042 0.00031 0.00030 0.00029 0.00016 Cl4 0.64096 0.04458 0.51352 1.00000 0.03080 0.02161 0.03148 0.00222 -0.00339 0.00519 0.02806 0.00127 0.00007 0.00003 0.00005 0.00000 0.00035 0.00034 0.00039 0.00028 0.00029 0.00027 0.00015 Cl5 0.75129 0.16906 0.56066 1.00000 0.02354 0.04106 0.02697 -0.00863 -0.00267 -0.00920 0.03060 0.00116 0.00007 0.00004 0.00005 0.00000 0.00033 0.00042 0.00038 0.00031 0.00028 0.00029 0.00016 Cl6 0.37763 0.26384 0.59191 1.00000 0.03620 0.02387 0.02590 -0.00705 0.00425 -0.00480 0.02859 0.00120 0.00008 0.00003 0.00005 0.00000 0.00038 0.00035 0.00037 0.00028 0.00029 0.00029 0.00015 Cl7 -0.30683 0.52445 0.57623 1.00000 0.03758 0.01932 0.07758 0.00543 -0.02318 -0.00076 0.04536 0.00145 0.00009 0.00003 0.00007 0.00000 0.00043 0.00036 0.00070 0.00039 0.00043 0.00030 0.00024 Cl8 -0.44344 0.40523 0.52401 1.00000 0.02228 0.02958 0.02488 -0.00587 -0.00461 -0.00321 0.02570 0.00110 0.00007 0.00003 0.00004 0.00000 0.00031 0.00036 0.00036 0.00028 0.00026 0.00026 0.00015 Cl9 -0.05305 0.30012 0.49776 1.00000 0.04436 0.03639 0.02590 -0.01287 0.00721 -0.01511 0.03542 0.00126 0.00008 0.00004 0.00005 0.00000 0.00043 0.00042 0.00039 0.00032 0.00032 0.00034 0.00018 Cl10 -0.91046 0.34795 1.06391 1.00000 0.02755 0.02514 0.03489 0.00469 -0.00123 -0.00481 0.02924 0.00124 0.00007 0.00003 0.00005 0.00000 0.00034 0.00036 0.00041 0.00030 0.00030 0.00027 0.00016 Cl11 -0.94974 0.48219 1.09451 1.00000 0.02567 0.02937 0.03386 -0.00139 0.00846 0.00463 0.02947 0.00132 0.00007 0.00003 0.00005 0.00000 0.00033 0.00037 0.00041 0.00031 0.00029 0.00028 0.00016 Cl12 -0.48901 0.33057 1.04687 1.00000 0.03091 0.02382 0.02926 0.00508 -0.00402 0.00179 0.02810 0.00124 0.00007 0.00003 0.00005 0.00000 0.00036 0.00035 0.00038 0.00029 0.00029 0.00027 0.00015 H20N -0.72853 0.52921 0.85119 1.00000 0.03535 0.06252 0.00363 0.00166 0.00224 0.00000 0.01016 H5N 1.01281 0.03237 0.24466 1.00000 0.02216 0.05658 0.00316 0.00153 0.00198 0.00000 0.00867 H15N 0.00987 0.41773 0.79997 1.00000 0.02509 0.05503 0.00342 0.00144 0.00200 0.00000 0.00852 H10N 0.30388 0.15450 0.28090 1.00000 0.02720 0.05637 0.00355 0.00144 0.00204 0.00000 0.00888 Final Structure Factor Calculation for 2007src0927 in P2(1) Total number of l.s. parameters = 814 Maximum vector length = 511 Memory required = 7914 / 27090 wR2 = 0.0714 before cycle 5 for 15188 data and 2 / 814 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0316 for 14428 Fo > 4sig(Fo) and 0.0345 for all 15188 data wR2 = 0.0714, GooF = S = 1.034, Restrained GooF = 1.034 for all data Occupancy sum of asymmetric unit = 88.00 for non-hydrogen and 60.00 for hydrogen atoms Principal mean square atomic displacements U 0.0448 0.0378 0.0190 C1 0.0385 0.0272 0.0175 C2 0.0389 0.0281 0.0141 C3 0.0376 0.0270 0.0179 C4 0.0426 0.0164 0.0133 C5 0.0381 0.0282 0.0235 C6 0.0429 0.0375 0.0214 C7 0.0437 0.0324 0.0158 C8 0.0857 0.0355 0.0181 C9 0.0955 0.0242 0.0223 C10 0.0509 0.0281 0.0171 C11 0.0336 0.0262 0.0142 C12 0.0385 0.0229 0.0102 C13 0.0333 0.0270 0.0124 C14 0.0310 0.0145 0.0132 C15 0.0324 0.0276 0.0193 C16 0.0470 0.0347 0.0201 C17 0.0505 0.0295 0.0165 C18 0.0491 0.0306 0.0164 C19 0.0322 0.0295 0.0185 C20 0.0494 0.0404 0.0233 C21 0.0510 0.0259 0.0167 C22 0.0650 0.0257 0.0144 C23 0.0549 0.0241 0.0171 C24 0.0398 0.0169 0.0135 C25 0.0398 0.0269 0.0229 C26 0.0649 0.0329 0.0191 C27 0.0728 0.0271 0.0191 C28 0.0615 0.0261 0.0233 C29 0.0362 0.0289 0.0208 C30 0.0598 0.0305 0.0201 C31 0.0369 0.0246 0.0185 C32 0.0340 0.0296 0.0185 C33 0.0345 0.0257 0.0223 C34 0.0319 0.0200 0.0108 C35 0.0443 0.0229 0.0194 C36 0.0669 0.0238 0.0207 C37 0.0689 0.0221 0.0171 C38 0.0519 0.0285 0.0191 C39 0.0342 0.0273 0.0186 C40 0.0279 0.0198 0.0180 N1 0.0319 0.0201 0.0156 N2 0.0343 0.0171 0.0167 N3 0.0290 0.0216 0.0180 N4 0.0385 0.0205 0.0143 N5 0.0298 0.0205 0.0147 N6 0.0274 0.0196 0.0143 N7 0.0271 0.0183 0.0158 N8 0.0282 0.0196 0.0146 N9 0.0256 0.0195 0.0169 N10 0.0365 0.0186 0.0178 N11 0.0517 0.0227 0.0129 N12 0.0284 0.0170 0.0145 N13 0.0278 0.0222 0.0196 N14 0.0263 0.0202 0.0176 N15 0.0326 0.0224 0.0159 N16 0.0348 0.0173 0.0156 N17 0.0292 0.0185 0.0137 N18 0.0322 0.0191 0.0178 N19 0.0338 0.0209 0.0159 N20 0.0541 0.0184 0.0161 O1 0.0303 0.0183 0.0129 O2 0.0333 0.0190 0.0148 O3 0.0337 0.0167 0.0149 O4 0.0215 0.0184 0.0144 P1 0.0229 0.0192 0.0156 P2 0.0297 0.0162 0.0148 P3 0.0204 0.0174 0.0131 P4 0.0197 0.0184 0.0149 P5 0.0205 0.0175 0.0138 P6 0.0211 0.0163 0.0135 P7 0.0243 0.0207 0.0147 P8 0.0250 0.0179 0.0136 P9 0.0210 0.0192 0.0154 P10 0.0247 0.0203 0.0160 P11 0.0232 0.0165 0.0147 P12 0.0327 0.0272 0.0191 Cl1 0.0389 0.0297 0.0177 Cl2 0.0387 0.0317 0.0219 Cl3 0.0360 0.0299 0.0182 Cl4 0.0472 0.0291 0.0156 Cl5 0.0400 0.0281 0.0177 Cl6 0.0908 0.0266 0.0186 Cl7 0.0336 0.0280 0.0155 Cl8 0.0604 0.0291 0.0168 Cl9 0.0384 0.0284 0.0209 Cl10 0.0382 0.0314 0.0188 Cl11 0.0357 0.0292 0.0194 Cl12 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.036 0.053 0.069 0.085 0.103 0.122 0.147 0.182 0.237 1.000 Number in group 1529. 1514. 1533. 1539. 1523. 1472. 1553. 1497. 1496. 1532. GooF 1.089 1.050 1.068 0.992 1.035 1.022 1.013 0.976 1.027 1.068 K 1.140 1.006 0.994 0.997 1.000 1.006 1.006 1.007 1.006 1.004 Resolution(A) 0.77 0.80 0.84 0.88 0.92 0.98 1.06 1.16 1.33 1.68 inf Number in group 1553. 1521. 1513. 1506. 1529. 1495. 1507. 1543. 1499. 1522. GooF 1.041 0.974 0.998 0.981 0.979 0.942 0.961 0.909 0.937 1.495 K 1.016 1.014 1.024 1.018 1.015 1.004 0.993 0.994 0.997 1.008 R1 0.072 0.060 0.050 0.044 0.040 0.035 0.029 0.022 0.019 0.023 Recommended weighting scheme: WGHT 0.0197 2.3153 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) 1 0 6 456.38 223.78 7.21 0.058 2.55 1 0 8 476.87 773.40 6.69 0.108 1.95 4 -2 4 3786.28 2981.66 6.26 0.212 2.01 4 2 4 3715.59 2981.52 5.59 0.212 2.01 0 -2 2 118.01 254.13 5.33 0.062 6.51 3 4 3 4834.31 3992.77 5.31 0.245 2.45 4 -2 2 970.18 1295.83 5.14 0.140 2.25 3 -4 3 4789.18 3997.75 5.11 0.245 2.45 0 0 6 123.38 1.07 4.75 0.004 2.67 -2 -3 7 2955.72 3555.60 4.74 0.231 2.02 -1 11 3 330.26 207.20 4.66 0.056 1.87 4 2 2 1013.60 1299.83 4.63 0.140 2.25 4 0 15 193.62 12.37 4.60 0.014 0.96 -1 -11 3 327.53 206.24 4.60 0.056 1.87 -4 4 3 604.19 845.44 4.60 0.113 2.07 -3 0 9 6732.21 8258.32 4.51 0.352 1.58 4 -21 11 640.41 276.67 4.46 0.065 0.81 -3 1 5 3599.24 4310.36 4.20 0.255 2.30 3 5 3 3307.71 2813.10 4.20 0.206 2.33 1 2 13 1049.92 1377.11 4.12 0.144 1.21 -1 8 4 3297.92 2804.63 4.00 0.205 2.24 -1 0 8 45.77 115.15 3.94 0.042 1.97 -3 -2 2 162.69 85.60 3.93 0.036 2.92 -1 1 8 142.75 73.55 3.93 0.033 1.96 -2 0 2 42.97 4.39 3.90 0.008 4.20 -1 -8 4 3264.00 2802.94 3.88 0.205 2.24 -2 6 6 1403.47 1716.04 3.82 0.161 2.00 6 14 5 451.16 615.77 3.78 0.096 1.06 -10 12 2 93.16 206.74 3.77 0.056 0.86 -8 5 10 313.20 496.08 3.76 0.086 0.96 -7 0 13 84.71 2.84 3.76 0.007 0.93 -4 -4 3 638.66 841.21 3.72 0.113 2.07 -3 -1 5 3542.58 4302.27 3.70 0.254 2.30 -2 -2 6 3269.62 2791.61 3.68 0.205 2.32 0 -6 5 102.81 177.62 3.67 0.052 2.43 8 -4 15 32.18 115.91 3.65 0.042 0.78 -3 2 2 156.85 88.18 3.59 0.036 2.92 -3 6 9 3097.91 3747.53 3.57 0.237 1.45 3 0 0 217.67 141.00 3.54 0.046 3.23 1 -2 13 1084.69 1379.07 3.52 0.144 1.21 -4 0 3 20223.15 17764.73 3.49 0.517 2.23 0 -2 8 6713.88 5938.43 3.49 0.299 1.97 -5 9 1 3626.24 4361.80 3.49 0.256 1.52 0 -1 7 2113.71 2463.61 3.47 0.193 2.27 5 0 3 1313.48 1561.48 3.47 0.153 1.80 4 -1 3 7338.14 6537.17 3.46 0.314 2.17 5 -14 9 73.22 16.80 3.44 0.016 1.00 -1 6 11 354.08 521.63 3.44 0.089 1.35 -2 -4 3 2113.77 1790.83 3.42 0.164 3.05 4 1 3 7305.95 6533.72 3.42 0.314 2.17 Bond lengths and angles C1 - Distance Angles N4 1.4647 (0.0038) C1 - C2 - Distance Angles N4 1.4771 (0.0038) C3 1.5028 (0.0043) 112.14 (0.24) C2 - N4 C3 - Distance Angles C4 1.5013 (0.0041) C2 1.5028 (0.0043) 111.78 (0.23) C3 - C4 C4 - Distance Angles N5 1.4711 (0.0038) C3 1.5013 (0.0041) 109.92 (0.24) C4 - N5 C5 - Distance Angles C6 1.3632 (0.0042) C10 1.3728 (0.0044) 122.61 (0.27) O1 1.4247 (0.0031) 120.60 (0.26) 116.70 (0.27) C5 - C6 C10 C6 - Distance Angles C5 1.3632 (0.0042) C7 1.4029 (0.0042) 118.34 (0.28) C6 - C5 C7 - Distance Angles C8 1.3651 (0.0043) C6 1.4029 (0.0042) 120.57 (0.30) C7 - C8 C8 - Distance Angles C7 1.3651 (0.0044) C9 1.3731 (0.0047) 119.66 (0.28) C8 - C7 C9 - Distance Angles C8 1.3731 (0.0047) C10 1.3964 (0.0045) 121.10 (0.31) C9 - C8 C10 - Distance Angles C5 1.3728 (0.0044) C9 1.3964 (0.0045) 117.71 (0.32) C10 - C5 C11 - Distance Angles N9 1.4740 (0.0035) C11 - C12 - Distance Angles N9 1.4804 (0.0035) C13 1.5167 (0.0038) 111.82 (0.22) C12 - N9 C13 - Distance Angles C14 1.5132 (0.0040) C12 1.5167 (0.0038) 111.10 (0.22) C13 - C14 C14 - Distance Angles N10 1.4740 (0.0036) C13 1.5132 (0.0040) 111.32 (0.23) C14 - N10 C15 - Distance Angles C16 1.3787 (0.0040) C20 1.3795 (0.0040) 122.68 (0.27) O2 1.4155 (0.0031) 118.94 (0.25) 118.31 (0.25) C15 - C16 C20 C16 - Distance Angles C15 1.3787 (0.0040) C17 1.3848 (0.0042) 118.58 (0.29) C16 - C15 C17 - Distance Angles C18 1.3750 (0.0047) C16 1.3848 (0.0042) 119.96 (0.31) C17 - C18 C18 - Distance Angles C17 1.3750 (0.0047) C19 1.3836 (0.0049) 120.56 (0.29) C18 - C17 C19 - Distance Angles C18 1.3836 (0.0049) C20 1.3874 (0.0042) 120.48 (0.30) C19 - C18 C20 - Distance Angles C15 1.3795 (0.0040) C19 1.3874 (0.0042) 117.72 (0.28) C20 - C15 C21 - Distance Angles N14 1.4678 (0.0038) C21 - C22 - Distance Angles N14 1.4807 (0.0038) C23 1.5167 (0.0045) 112.49 (0.24) C22 - N14 C23 - Distance Angles C24 1.5069 (0.0048) C22 1.5167 (0.0045) 112.26 (0.25) C23 - C24 C24 - Distance Angles N15 1.4865 (0.0038) C23 1.5069 (0.0048) 111.68 (0.26) C24 - N15 C25 - Distance Angles C30 1.3767 (0.0043) C26 1.3797 (0.0043) 122.45 (0.28) O3 1.4149 (0.0032) 119.96 (0.27) 117.55 (0.26) C25 - C30 C26 C26 - Distance Angles C25 1.3797 (0.0043) C27 1.3941 (0.0044) 118.41 (0.30) C26 - C25 C27 - Distance Angles C28 1.3819 (0.0053) C26 1.3941 (0.0044) 119.83 (0.32) C27 - C28 C28 - Distance Angles C29 1.3796 (0.0052) C27 1.3819 (0.0053) 120.35 (0.31) C28 - C29 C29 - Distance Angles C28 1.3796 (0.0052) C30 1.3818 (0.0044) 120.65 (0.32) C29 - C28 C30 - Distance Angles C25 1.3767 (0.0043) C29 1.3818 (0.0044) 118.30 (0.31) C30 - C25 C31 - Distance Angles N19 1.4787 (0.0038) C31 - C32 - Distance Angles N19 1.4739 (0.0037) C33 1.5213 (0.0042) 111.96 (0.24) C32 - N19 C33 - Distance Angles C34 1.5175 (0.0041) C32 1.5213 (0.0042) 111.83 (0.24) C33 - C34 C34 - Distance Angles N20 1.4671 (0.0039) C33 1.5175 (0.0041) 108.51 (0.25) C34 - N20 C35 - Distance Angles C36 1.3777 (0.0042) C40 1.3891 (0.0039) 122.85 (0.28) O4 1.4234 (0.0032) 119.85 (0.25) 117.22 (0.26) C35 - C36 C40 C36 - Distance Angles C35 1.3777 (0.0042) C37 1.3950 (0.0043) 117.32 (0.29) C36 - C35 C37 - Distance Angles C38 1.3691 (0.0050) C36 1.3950 (0.0043) 121.56 (0.31) C37 - C38 C38 - Distance Angles C37 1.3691 (0.0050) C39 1.3901 (0.0050) 119.84 (0.29) C38 - C37 C39 - Distance Angles C40 1.3890 (0.0041) C38 1.3901 (0.0050) 120.32 (0.31) C39 - C40 C40 - Distance Angles C39 1.3890 (0.0041) C35 1.3891 (0.0039) 118.08 (0.30) C40 - C39 N1 - Distance Angles P2 1.5647 (0.0024) P1 1.6099 (0.0024) 123.63 (0.14) N1 - P2 N2 - Distance Angles P2 1.5760 (0.0022) P3 1.5868 (0.0024) 117.05 (0.15) N2 - P2 N3 - Distance Angles P3 1.5705 (0.0024) P1 1.6301 (0.0022) 122.89 (0.15) N3 - P3 N4 - Distance Angles C1 1.4647 (0.0038) C2 1.4771 (0.0038) 113.50 (0.24) P1 1.6582 (0.0024) 115.70 (0.20) 119.09 (0.19) N4 - C1 C2 N5 - Distance Angles C4 1.4711 (0.0038) P1 1.6211 (0.0026) 122.38 (0.21) N5 - C4 N6 - Distance Angles P5 1.5598 (0.0024) P4 1.6230 (0.0023) 122.84 (0.15) N6 - P5 N7 - Distance Angles P6 1.5875 (0.0023) P5 1.5888 (0.0024) 117.25 (0.14) N7 - P6 N8 - Distance Angles P6 1.5614 (0.0023) P4 1.6061 (0.0023) 122.64 (0.14) N8 - P6 N9 - Distance Angles C11 1.4740 (0.0035) C12 1.4804 (0.0035) 112.00 (0.22) P4 1.6525 (0.0023) 114.71 (0.19) 118.58 (0.19) N9 - C11 C12 N10 - Distance Angles C14 1.4740 (0.0036) P4 1.6338 (0.0024) 116.66 (0.19) N10 - C14 N11 - Distance Angles P8 1.5517 (0.0025) P7 1.6199 (0.0023) 122.32 (0.15) N11 - P8 N12 - Distance Angles P8 1.5784 (0.0026) P9 1.5889 (0.0025) 119.02 (0.15) N12 - P8 N13 - Distance Angles P9 1.5707 (0.0023) P7 1.5936 (0.0023) 121.85 (0.14) N13 - P9 N14 - Distance Angles C21 1.4678 (0.0038) C22 1.4807 (0.0038) 111.79 (0.24) P7 1.6496 (0.0024) 114.68 (0.21) 115.21 (0.20) N14 - C21 C22 N15 - Distance Angles C24 1.4865 (0.0038) P7 1.6458 (0.0024) 114.50 (0.19) N15 - C24 N16 - Distance Angles P11 1.5643 (0.0025) P10 1.6122 (0.0024) 122.69 (0.14) N16 - P11 N17 - Distance Angles P11 1.5805 (0.0022) P12 1.5927 (0.0024) 116.68 (0.14) N17 - P11 N18 - Distance Angles P12 1.5550 (0.0023) P10 1.6206 (0.0022) 123.40 (0.14) N18 - P12 N19 - Distance Angles C32 1.4739 (0.0038) C31 1.4787 (0.0038) 111.60 (0.25) P10 1.6478 (0.0024) 119.82 (0.20) 115.46 (0.20) N19 - C32 C31 N20 - Distance Angles C34 1.4671 (0.0039) P10 1.6258 (0.0025) 119.27 (0.20) N20 - C34 O1 - Distance Angles C5 1.4247 (0.0031) P3 1.5781 (0.0020) 123.32 (0.17) O1 - C5 O2 - Distance Angles C15 1.4155 (0.0031) P6 1.5768 (0.0019) 123.69 (0.16) O2 - C15 O3 - Distance Angles C25 1.4149 (0.0032) P9 1.5689 (0.0020) 122.62 (0.16) O3 - C25 O4 - Distance Angles C35 1.4234 (0.0032) P12 1.5766 (0.0019) 122.19 (0.16) O4 - C35 P1 - Distance Angles N1 1.6099 (0.0024) N5 1.6211 (0.0026) 109.04 (0.13) N3 1.6301 (0.0022) 112.78 (0.12) 112.27 (0.13) N4 1.6582 (0.0024) 107.67 (0.13) 102.43 (0.13) 112.05 (0.13) P1 - N1 N5 N3 P2 - Distance Angles N1 1.5647 (0.0024) N2 1.5760 (0.0022) 119.95 (0.12) Cl2 1.9950 (0.0010) 108.86 (0.10) 108.82 (0.10) Cl1 2.0263 (0.0010) 109.22 (0.09) 107.28 (0.10) 101.06 (0.04) P3 2.6974 (0.0010) 90.12 (0.09) 31.60 (0.09) 133.85 (0.04) 111.96 (0.04) P2 - N1 N2 Cl2 Cl1 P3 - Distance Angles N3 1.5705 (0.0024) O1 1.5781 (0.0020) 107.62 (0.12) N2 1.5868 (0.0024) 118.59 (0.12) 110.22 (0.12) Cl3 2.0355 (0.0010) 110.64 (0.10) 101.95 (0.09) 106.57 (0.10) P2 2.6974 (0.0010) 89.83 (0.09) 136.02 (0.10) 31.36 (0.08) 109.16 (0.04) P3 - N3 O1 N2 Cl3 P4 - Distance Angles N8 1.6061 (0.0023) N6 1.6230 (0.0023) 114.37 (0.12) N10 1.6338 (0.0024) 109.26 (0.12) 108.94 (0.13) N9 1.6525 (0.0023) 109.11 (0.12) 109.06 (0.12) 105.75 (0.12) P4 - N8 N6 N10 P5 - Distance Angles N6 1.5598 (0.0024) N7 1.5888 (0.0024) 119.57 (0.12) Cl4 2.0021 (0.0010) 110.90 (0.10) 107.43 (0.09) Cl5 2.0275 (0.0009) 109.47 (0.10) 108.31 (0.09) 99.21 (0.04) P5 - N6 N7 Cl4 P6 - Distance Angles N8 1.5614 (0.0023) O2 1.5768 (0.0019) 106.66 (0.11) N7 1.5875 (0.0023) 119.51 (0.12) 110.88 (0.12) Cl6 2.0315 (0.0010) 109.58 (0.09) 102.18 (0.08) 106.69 (0.09) P6 - N8 O2 N7 P7 - Distance Angles N13 1.5936 (0.0023) N11 1.6199 (0.0023) 115.43 (0.12) N15 1.6458 (0.0024) 108.92 (0.12) 108.27 (0.13) N14 1.6496 (0.0024) 109.39 (0.12) 108.66 (0.13) 105.74 (0.12) P7 - N13 N11 N15 P8 - Distance Angles N11 1.5517 (0.0025) N12 1.5784 (0.0026) 119.41 (0.13) Cl7 1.9993 (0.0010) 110.41 (0.10) 107.41 (0.11) Cl8 2.0142 (0.0009) 109.23 (0.10) 108.37 (0.10) 100.31 (0.04) P8 - N11 N12 Cl7 P9 - Distance Angles O3 1.5689 (0.0020) N13 1.5707 (0.0023) 107.57 (0.11) N12 1.5889 (0.0025) 109.96 (0.12) 119.10 (0.13) Cl9 2.0198 (0.0010) 102.16 (0.08) 109.30 (0.10) 107.43 (0.11) P9 - O3 N13 N12 P10 - Distance Angles N16 1.6122 (0.0024) N18 1.6206 (0.0022) 113.64 (0.12) N20 1.6258 (0.0025) 109.26 (0.13) 112.11 (0.13) N19 1.6478 (0.0024) 107.15 (0.13) 111.43 (0.12) 102.58 (0.13) P10 - N16 N18 N20 P11 - Distance Angles N16 1.5643 (0.0025) N17 1.5805 (0.0022) 119.80 (0.13) Cl11 1.9922 (0.0010) 108.70 (0.10) 109.10 (0.10) Cl10 2.0292 (0.0010) 110.11 (0.10) 107.73 (0.10) 99.49 (0.04) P11 - N16 N17 Cl11 P12 - Distance Angles N18 1.5550 (0.0023) O4 1.5766 (0.0019) 108.45 (0.12) N17 1.5927 (0.0024) 119.01 (0.12) 110.11 (0.12) Cl12 2.0336 (0.0010) 109.14 (0.10) 101.94 (0.08) 106.84 (0.10) P12 - N18 O4 N17 Cl1 - Distance Angles P2 2.0263 (0.0010) Cl1 - Cl2 - Distance Angles P2 1.9950 (0.0010) Cl2 - Cl3 - Distance Angles P3 2.0355 (0.0010) Cl3 - Cl4 - Distance Angles P5 2.0021 (0.0010) Cl4 - Cl5 - Distance Angles P5 2.0275 (0.0009) Cl5 - Cl6 - Distance Angles P6 2.0315 (0.0010) Cl6 - Cl7 - Distance Angles P8 1.9993 (0.0010) Cl7 - Cl8 - Distance Angles P8 2.0142 (0.0009) Cl8 - Cl9 - Distance Angles P9 2.0198 (0.0010) Cl9 - Cl10 - Distance Angles P11 2.0292 (0.0010) Cl10 - Cl11 - Distance Angles P11 1.9922 (0.0010) Cl11 - Cl12 - Distance Angles P12 2.0336 (0.0010) Cl12 - FMAP and GRID set by program FMAP 2 3 69 GRID -1.515 -2 -1 1.515 2 1 R1 = 0.0316 for 8143 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.4458 0.3940 0.9536 [ 0.87 A from N18 ] Deepest hole -0.34 at 0.5377 0.4131 0.0133 [ 0.84 A from P12 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 7268 / 88359 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.5542 0.3940 0.9536 1.00000 0.05 0.32 0.87 N18 1.29 P12 2.08 P10 2.14 CL12 Q2 1 -0.4794 0.5007 1.0492 1.00000 0.05 0.32 1.28 O4 2.00 P12 2.27 C35 2.45 H36 Q3 1 -0.2598 0.4235 0.6336 1.00000 0.05 0.30 0.71 N11 0.86 P8 2.01 P7 2.06 N12 Q4 1 -0.8435 0.3922 1.0571 1.00000 0.05 0.29 0.88 P11 1.19 CL10 1.87 N17 2.15 N16 Q5 1 1.0359 0.1263 0.0291 1.00000 0.05 0.29 0.73 N2 0.88 P2 1.91 P3 2.03 N1 Q6 1 0.7451 0.1324 0.5605 1.00000 0.05 0.29 0.82 CL5 1.78 P5 2.32 CL4 2.79 H3B Q7 1 1.0127 0.1723 0.3067 1.00000 0.05 0.28 0.67 N4 0.82 C2 1.50 H2A 1.52 H2B Q8 1 -0.9457 0.3415 1.1280 1.00000 0.05 0.28 1.10 CL10 2.49 H1B 2.72 P11 2.75 H40 Q9 1 1.0361 0.1539 0.2451 1.00000 0.05 0.27 0.66 N4 1.01 P1 1.89 C2 1.89 C1 Q10 1 0.5388 0.1671 0.3893 1.00000 0.05 0.26 0.63 N6 1.01 P4 2.01 P5 2.12 N9 Q11 1 -0.1995 0.4295 0.5493 1.00000 0.05 0.26 0.67 N12 0.91 P8 2.03 P9 2.18 N11 Q12 1 0.5560 0.1453 0.4449 1.00000 0.05 0.25 0.66 N6 1.00 P5 1.84 P4 2.07 N7 Q13 1 -0.1321 0.4108 0.4713 1.00000 0.05 0.25 0.95 N12 1.89 P9 1.97 H38 2.35 P8 Q14 1 -0.1015 0.3925 0.5302 1.00000 0.05 0.25 0.79 N12 0.92 P9 2.12 P8 2.12 O3 Q15 1 0.9235 0.1463 0.0200 1.00000 0.05 0.25 0.73 N2 0.93 P3 2.01 P2 2.15 O1 Q16 1 -0.7359 0.4422 1.0564 1.00000 0.05 0.25 0.77 N17 0.94 P11 2.00 P12 2.06 N16 Q17 1 0.1545 0.1843 0.6569 1.00000 0.05 0.25 0.73 C15 0.78 C20 1.44 H20 1.81 O2 Q18 1 0.4209 0.1537 0.3287 1.00000 0.05 0.25 0.74 N10 1.00 P4 1.35 H10N 1.96 C14 Q19 1 -0.8955 0.5109 1.1066 1.00000 0.05 0.24 0.85 CL11 1.91 H6 2.30 P11 2.71 C6 Q20 1 0.9779 0.0926 0.3712 1.00000 0.05 0.24 0.72 C3 0.78 C4 1.40 H3A 1.41 H3B Shortest distances between peaks (including symmetry equivalents) 10 12 1.02 13 14 1.06 7 9 1.10 5 15 1.18 11 14 1.30 11 13 1.49 3 11 1.49 10 18 1.50 4 16 1.53 4 8 1.91 7 20 2.10 12 18 2.25 16 19 2.34 3 14 2.40 9 20 2.52 6 12 2.58 1 16 2.67 2 16 2.81 4 19 2.82 1 2 2.91 3 13 2.93 Time profile in seconds ----------------------- 0.12: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.02: 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 0.01: Analyse other restraints etc. 5.35: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.01: Generate idealized H-atoms 43.05: Structure factors and derivatives 91.45: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.30: Apply other restraints 5.73: Solve l.s. equations 0.00: Generate HTAB table 0.07: Other dependent quantities, CIF, tables 0.52: Analysis of variance 0.17: Merge reflections for Fourier and .fcf 0.41: Fourier summations 0.16: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0927 finished at 14:33:48 Total CPU time: 147.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++