+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0232 started at 16:38:33 on 27-Mar-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0232 in P2(1) CELL 0.71073 6.3073 17.6438 9.5481 90.000 96.552 90.000 ZERR 2.00 0.0001 0.0004 0.0002 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O P UNIT 36 48 10 8 6 V = 1055.62 F(000) = 488.0 Mu = 0.32 mm-1 Cell Wt = 934.66 Rho = 1.470 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 10 SIZE 0.04 0.18 0.22 MOVE 1 1 1 -1 ACTA BOND WGHT 0.01680 0.62000 L.S. 4 TEMP -153.00 FVAR 1.18146 C1 1 0.059782 0.086012 0.674626 11.00000 0.01936 0.01433 = 0.01503 0.00083 0.00173 0.00033 C2 1 0.221453 0.044986 0.622557 11.00000 0.01630 0.02241 = 0.03399 -0.00787 0.00207 -0.00082 AFIX 43 H2 2 0.364017 0.063306 0.633374 11.00000 -1.20000 AFIX 0 C3 1 0.171209 -0.023348 0.554331 11.00000 0.02021 0.02099 = 0.03429 -0.00972 0.00306 0.00221 AFIX 43 H3 2 0.281085 -0.052208 0.519534 11.00000 -1.20000 AFIX 0 C4 1 -0.036114 -0.049936 0.536355 11.00000 0.02364 0.01706 = 0.01857 -0.00053 -0.00076 -0.00435 AFIX 43 H4 2 -0.068838 -0.096779 0.489780 11.00000 -1.20000 AFIX 0 C5 1 -0.195430 -0.007614 0.586899 11.00000 0.01781 0.02344 = 0.02010 0.00183 0.00043 -0.00521 AFIX 43 H5 2 -0.338406 -0.025494 0.574221 11.00000 -1.20000 AFIX 0 C6 1 -0.149197 0.060749 0.656019 11.00000 0.01557 0.02195 = 0.01728 0.00098 0.00357 0.00040 AFIX 43 H6 2 -0.259532 0.089723 0.690009 11.00000 -1.20000 AFIX 0 C7 1 0.571601 0.118238 1.013825 11.00000 0.02324 0.01733 = 0.01743 -0.00238 0.00078 0.00481 C8 1 0.761362 0.155178 0.999553 11.00000 0.02515 0.02025 = 0.01691 -0.00119 0.00416 0.00225 AFIX 43 H8 2 0.776638 0.185000 0.918472 11.00000 -1.20000 AFIX 0 C9 1 0.929268 0.147737 1.106390 11.00000 0.02433 0.02971 = 0.02358 -0.00802 0.00002 0.00164 AFIX 43 H9 2 1.060517 0.172919 1.098534 11.00000 -1.20000 AFIX 0 C10 1 0.906755 0.103698 1.224812 11.00000 0.03461 0.03004 = 0.02213 -0.00300 -0.00508 0.00927 AFIX 43 H10 2 1.022584 0.098480 1.297012 11.00000 -1.20000 AFIX 0 C11 1 0.714424 0.067465 1.236923 11.00000 0.04834 0.02755 = 0.01813 0.00318 0.00318 0.00746 AFIX 43 H11 2 0.697908 0.037985 1.318227 11.00000 -1.20000 AFIX 0 C12 1 0.545837 0.074200 1.130368 11.00000 0.03129 0.02147 = 0.02341 0.00326 0.00573 0.00108 AFIX 43 H12 2 0.414636 0.048857 1.137584 11.00000 -1.20000 AFIX 0 C13 1 0.787718 0.257104 0.462432 11.00000 0.01894 0.02183 = 0.02096 -0.00367 0.00643 0.00148 AFIX 23 H13A 2 0.800387 0.202944 0.489175 11.00000 -1.20000 H13B 2 0.928149 0.274582 0.438173 11.00000 -1.20000 AFIX 0 C14 1 0.620112 0.266503 0.335609 11.00000 0.02644 0.02595 = 0.01596 0.00004 0.00386 0.00334 AFIX 23 H14A 2 0.614566 0.320197 0.305316 11.00000 -1.20000 H14B 2 0.659757 0.235394 0.256321 11.00000 -1.20000 AFIX 0 C15 1 0.403107 0.242332 0.372222 11.00000 0.02386 0.02429 = 0.01802 -0.00408 -0.00239 -0.00043 AFIX 23 H15A 2 0.296741 0.246888 0.288000 11.00000 -1.20000 H15B 2 0.408320 0.188638 0.402520 11.00000 -1.20000 AFIX 0 C16 1 -0.073108 0.390859 0.937819 11.00000 0.01859 0.02546 = 0.02631 -0.00438 0.00633 0.00177 AFIX 23 H16A 2 -0.102374 0.341444 0.980820 11.00000 -1.20000 H16B 2 -0.211752 0.415300 0.906580 11.00000 -1.20000 AFIX 0 C17 1 0.052746 0.440509 1.047203 11.00000 0.02710 0.02405 = 0.02125 -0.00614 0.00681 0.00230 AFIX 23 H17A 2 0.072138 0.491268 1.006349 11.00000 -1.20000 H17B 2 -0.028974 0.446829 1.129010 11.00000 -1.20000 AFIX 0 C18 1 0.269241 0.406909 1.096750 11.00000 0.02523 0.02932 = 0.01714 -0.00653 0.00184 0.00127 AFIX 23 H18A 2 0.348711 0.442252 1.164102 11.00000 -1.20000 H18B 2 0.249449 0.358827 1.147102 11.00000 -1.20000 AFIX 0 N1 3 0.470023 0.203633 0.697815 11.00000 0.01705 0.01430 = 0.01818 -0.00078 0.00283 0.00063 N2 3 0.424023 0.355569 0.724712 11.00000 0.02175 0.01415 = 0.02174 -0.00109 0.00615 0.00066 N3 3 0.262033 0.257737 0.908829 11.00000 0.02233 0.01659 = 0.01925 -0.00263 0.00604 -0.00168 N4 3 0.725065 0.302024 0.582079 11.00000 0.01451 0.02030 = 0.01720 -0.00164 0.00066 -0.00166 N5 3 0.045218 0.378020 0.813214 11.00000 0.01640 0.02110 = 0.01966 -0.00192 0.00225 0.00273 O1 4 0.092219 0.154234 0.747134 11.00000 0.01533 0.01554 = 0.02433 -0.00411 0.00391 -0.00032 O2 4 0.397833 0.118337 0.908331 11.00000 0.02121 0.01557 = 0.01985 0.00189 0.00054 -0.00103 O3 4 0.339446 0.289997 0.485604 11.00000 0.01517 0.02239 = 0.02029 0.00014 -0.00069 0.00285 O4 4 0.394721 0.392288 0.980196 11.00000 0.01719 0.02278 = 0.02003 -0.00695 0.00099 -0.00015 P1 5 0.315574 0.188856 0.813481 11.00000 0.01641 0.01310 = 0.01718 -0.00090 0.00282 -0.00046 P2 5 0.488939 0.286926 0.631509 11.00000 0.01346 0.01401 = 0.01604 0.00004 0.00170 -0.00009 P3 5 0.288539 0.342372 0.853311 11.00000 0.01557 0.01369 = 0.01716 -0.00260 0.00172 0.00023 H4N 2 0.824185 0.310991 0.651031 11.00000 0.04115 H5N 2 0.057520 0.419527 0.768166 11.00000 0.02805 HKLF 4 Covalent radii and connectivity table for 2008src0232 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 C1 - C6 C2 O1 C2 - C1 C3 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 C6 - C1 C5 C7 - C12 C8 O2 C8 - C7 C9 C9 - C8 C10 C10 - C11 C9 C11 - C10 C12 C12 - C7 C11 C13 - N4 C14 C14 - C15 C13 C15 - O3 C14 C16 - N5 C17 C17 - C18 C16 C18 - O4 C17 N1 - P1 P2 N2 - P2 P3 N3 - P1 P3 N4 - C13 P2 N5 - C16 P3 O1 - C1 P1 O2 - C7 P1 O3 - C15 P2 O4 - C18 P3 P1 - N1 N3 O2 O1 P2 - N2 O3 N1 N4 P3 - O4 N2 N3 N5 Floating origin restraints generated 12418 Reflections read, of which 27 rejected -8 =< h =< 8, -22 =< k =< 22, -10 =< l =< 12, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 4543 Unique reflections, of which 0 suppressed R(int) = 0.0295 R(sigma) = 0.0376 Friedel opposites not merged Maximum memory for data reduction = 2543 / 45992 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 = 3326 / 348773 wR2 = 0.0654 before cycle 1 for 4543 data and 279 / 279 parameters GooF = S = 1.010; Restrained GooF = 1.009 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0168 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18172 0.00120 0.215 OSF Mean shift/esd = 0.066 Maximum = -0.445 for y P2 Max. shift = 0.001 A for H4N Max. dU = 0.000 for H5N Least-squares cycle 2 Maximum vector length = 511 Memory required = 3326 / 348773 wR2 = 0.0654 before cycle 2 for 4543 data and 279 / 279 parameters GooF = S = 1.009; Restrained GooF = 1.009 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0168 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18172 0.00120 0.005 OSF Mean shift/esd = 0.022 Maximum = -0.143 for y P2 Max. shift = 0.001 A for H4N Max. dU = 0.000 for H5N Least-squares cycle 3 Maximum vector length = 511 Memory required = 3326 / 348773 wR2 = 0.0654 before cycle 3 for 4543 data and 279 / 279 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0168 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18172 0.00120 0.002 OSF Mean shift/esd = 0.001 Maximum = -0.005 for U11 H4N Max. shift = 0.000 A for H5N Max. dU = 0.000 for H4N Least-squares cycle 4 Maximum vector length = 511 Memory required = 3326 / 348773 wR2 = 0.0654 before cycle 4 for 4543 data and 279 / 279 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0168 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18172 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for U22 N1 Max. shift = 0.000 A for H5N Max. dU = 0.000 for H4N 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 H2 0.6360 0.9367 0.3667 43 0.950 0.000 C2 C1 C3 H3 0.7189 1.0522 0.4805 43 0.950 0.000 C3 C4 C2 H4 1.0688 1.0968 0.5102 43 0.950 0.000 C4 C3 C5 H5 1.3384 1.0255 0.4258 43 0.950 0.000 C5 C4 C6 H6 1.2596 0.9103 0.3101 43 0.950 0.000 C6 C1 C5 H8 0.2234 0.8150 0.0815 43 0.950 0.000 C8 C7 C9 H9 -0.0605 0.8271 -0.0985 43 0.950 0.000 C9 C8 C10 H10 -0.0226 0.9015 -0.2970 43 0.950 0.000 C10 C11 C9 H11 0.3021 0.9620 -0.3182 43 0.950 0.000 C11 C10 C12 H12 0.5854 0.9512 -0.1376 43 0.950 0.000 C12 C7 C11 H13A 0.0718 0.7254 0.5618 23 0.990 0.000 C13 N4 C14 H13B 0.1996 0.7971 0.5108 23 0.990 0.000 C13 N4 C14 H14A 0.3402 0.7646 0.7437 23 0.990 0.000 C14 C15 C13 H14B 0.3854 0.6798 0.6947 23 0.990 0.000 C14 C15 C13 H15A 0.5916 0.8114 0.5975 23 0.990 0.000 C15 O3 C14 H15B 0.7032 0.7531 0.7120 23 0.990 0.000 C15 O3 C14 H16A 1.2117 0.5847 0.0934 23 0.990 0.000 C16 N5 C17 H16B 1.1024 0.6586 0.0192 23 0.990 0.000 C16 N5 C17 H17A 1.0290 0.5532 -0.1290 23 0.990 0.000 C17 C18 C16 H17B 0.9279 0.5088 -0.0063 23 0.990 0.000 C17 C18 C16 H18A 0.7506 0.6412 -0.1471 23 0.990 0.000 C18 O4 C17 H18B 0.6513 0.5578 -0.1641 23 0.990 0.000 C18 O4 C17 2008src0232 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.94023 0.91402 0.32540 1.00000 0.01940 0.01441 0.01493 0.00068 0.00171 0.00024 0.01626 0.00345 0.00030 0.00011 0.00020 0.00000 0.00091 0.00086 0.00091 0.00074 0.00074 0.00072 0.00038 C2 0.77859 0.95502 0.37747 1.00000 0.01630 0.02238 0.03415 -0.00768 0.00219 -0.00081 0.02433 0.00383 0.00033 0.00012 0.00024 0.00000 0.00095 0.00104 0.00123 0.00091 0.00087 0.00081 0.00046 H2 0.63605 0.93668 0.36668 1.00000 0.02919 0.00000 0.00000 C3 0.82883 1.02336 0.44566 1.00000 0.02021 0.02097 0.03432 -0.00968 0.00310 0.00230 0.02517 0.00387 0.00034 0.00012 0.00025 0.00000 0.00096 0.00101 0.00120 0.00092 0.00087 0.00082 0.00045 H3 0.71895 1.05222 0.48046 1.00000 0.03020 0.00000 0.00000 C4 1.03611 1.04996 0.46362 1.00000 0.02366 0.01714 0.01848 -0.00055 -0.00084 -0.00430 0.02001 0.00360 0.00031 0.00011 0.00021 0.00000 0.00097 0.00094 0.00098 0.00079 0.00079 0.00082 0.00041 H4 1.06881 1.09682 0.51016 1.00000 0.02401 0.00000 0.00000 C5 1.19541 1.00765 0.41313 1.00000 0.01777 0.02335 0.01996 0.00178 0.00026 -0.00527 0.02051 0.00362 0.00032 0.00012 0.00021 0.00000 0.00091 0.00101 0.00102 0.00084 0.00079 0.00081 0.00041 H5 1.33838 1.02553 0.42581 1.00000 0.02461 0.00000 0.00000 C6 1.14922 0.93927 0.34403 1.00000 0.01550 0.02177 0.01729 0.00097 0.00352 0.00036 0.01806 0.00358 0.00030 0.00011 0.00021 0.00000 0.00089 0.00097 0.00095 0.00079 0.00074 0.00078 0.00039 H6 1.25957 0.91029 0.31008 1.00000 0.02167 0.00000 0.00000 C7 0.42839 0.88178 -0.01381 1.00000 0.02319 0.01730 0.01737 -0.00239 0.00075 0.00478 0.01941 0.00362 0.00031 0.00011 0.00021 0.00000 0.00094 0.00090 0.00095 0.00077 0.00077 0.00080 0.00040 C8 0.23864 0.84485 0.00045 1.00000 0.02513 0.02017 0.01685 -0.00127 0.00399 0.00222 0.02059 0.00365 0.00032 0.00011 0.00021 0.00000 0.00098 0.00102 0.00097 0.00079 0.00078 0.00083 0.00041 H8 0.22336 0.81503 0.08153 1.00000 0.02471 0.00000 0.00000 C9 0.07071 0.85229 -0.10638 1.00000 0.02433 0.02959 0.02362 -0.00805 -0.00003 0.00173 0.02606 0.00384 0.00034 0.00013 0.00023 0.00000 0.00101 0.00116 0.00108 0.00092 0.00084 0.00091 0.00046 H9 -0.06055 0.82712 -0.09851 1.00000 0.03127 0.00000 0.00000 C10 0.09326 0.89632 -0.22481 1.00000 0.03461 0.02992 0.02217 -0.00305 -0.00517 0.00933 0.02955 0.00416 0.00038 0.00013 0.00024 0.00000 0.00119 0.00118 0.00109 0.00092 0.00092 0.00100 0.00049 H10 -0.02256 0.90152 -0.29702 1.00000 0.03546 0.00000 0.00000 C11 0.28558 0.93256 -0.23693 1.00000 0.04850 0.02749 0.01808 0.00332 0.00332 0.00767 0.03139 0.00454 0.00041 0.00013 0.00024 0.00000 0.00143 0.00118 0.00106 0.00088 0.00100 0.00106 0.00052 H11 0.30209 0.96204 -0.31824 1.00000 0.03767 0.00000 0.00000 C12 0.45415 0.92583 -0.13038 1.00000 0.03132 0.02148 0.02346 0.00328 0.00582 0.00100 0.02521 0.00408 0.00037 0.00012 0.00023 0.00000 0.00114 0.00104 0.00110 0.00086 0.00090 0.00090 0.00046 H12 0.58535 0.95117 -0.13759 1.00000 0.03025 0.00000 0.00000 C13 0.21227 0.74290 0.53755 1.00000 0.01896 0.02184 0.02095 -0.00364 0.00644 0.00139 0.02026 0.00356 0.00030 0.00012 0.00022 0.00000 0.00088 0.00098 0.00105 0.00080 0.00078 0.00079 0.00041 H13A 0.07184 0.72542 0.56180 1.00000 0.02432 0.00000 0.00000 H13B 0.19958 0.79706 0.51081 1.00000 0.02432 0.00000 0.00000 C14 0.37988 0.73351 0.66442 1.00000 0.02646 0.02592 0.01587 -0.00011 0.00377 0.00322 0.02265 0.00369 0.00031 0.00012 0.00021 0.00000 0.00097 0.00103 0.00102 0.00081 0.00080 0.00086 0.00043 H14A 0.34023 0.76463 0.74369 1.00000 0.02718 0.00000 0.00000 H14B 0.38543 0.67982 0.69473 1.00000 0.02718 0.00000 0.00000 C15 0.59684 0.75768 0.62777 1.00000 0.02393 0.02429 0.01807 -0.00411 -0.00246 -0.00051 0.02247 0.00358 0.00032 0.00012 0.00022 0.00000 0.00099 0.00106 0.00100 0.00084 0.00082 0.00086 0.00043 H15A 0.59159 0.81138 0.59746 1.00000 0.02696 0.00000 0.00000 H15B 0.70322 0.75314 0.71199 1.00000 0.02696 0.00000 0.00000 C16 1.07311 0.60916 0.06220 1.00000 0.01862 0.02542 0.02639 -0.00414 0.00644 0.00181 0.02318 0.00380 0.00031 0.00012 0.00023 0.00000 0.00092 0.00107 0.00110 0.00089 0.00084 0.00084 0.00044 H16A 1.21175 0.58471 0.09344 1.00000 0.02781 0.00000 0.00000 H16B 1.10240 0.65857 0.01919 1.00000 0.02781 0.00000 0.00000 C17 0.94727 0.55952 -0.04716 1.00000 0.02710 0.02393 0.02124 -0.00613 0.00674 0.00235 0.02378 0.00383 0.00033 0.00012 0.00022 0.00000 0.00105 0.00104 0.00105 0.00085 0.00085 0.00088 0.00044 H17A 1.02901 0.55319 -0.12895 1.00000 0.02854 0.00000 0.00000 H17B 0.92786 0.50877 -0.00629 1.00000 0.02854 0.00000 0.00000 C18 0.73077 0.59311 -0.09676 1.00000 0.02529 0.02932 0.01724 -0.00653 0.00197 0.00127 0.02399 0.00389 0.00034 0.00013 0.00022 0.00000 0.00102 0.00111 0.00101 0.00086 0.00084 0.00088 0.00045 H18A 0.75056 0.64119 -0.14713 1.00000 0.02878 0.00000 0.00000 H18B 0.65132 0.55775 -0.16410 1.00000 0.02878 0.00000 0.00000 N1 0.52996 0.79640 0.30218 1.00000 0.01699 0.01445 0.01814 -0.00079 0.00282 0.00061 0.01646 0.00289 0.00025 0.00009 0.00017 0.00000 0.00074 0.00078 0.00081 0.00063 0.00063 0.00061 0.00033 N2 0.57597 0.64445 0.27530 1.00000 0.02166 0.01416 0.02165 -0.00102 0.00613 0.00067 0.01887 0.00310 0.00026 0.00009 0.00018 0.00000 0.00078 0.00083 0.00085 0.00066 0.00067 0.00064 0.00035 N3 0.73797 0.74228 0.09116 1.00000 0.02227 0.01661 0.01915 -0.00259 0.00609 -0.00155 0.01905 0.00293 0.00026 0.00009 0.00018 0.00000 0.00079 0.00079 0.00089 0.00067 0.00069 0.00067 0.00035 N4 0.27497 0.69799 0.41793 1.00000 0.01451 0.02035 0.01720 -0.00175 0.00063 -0.00167 0.01744 0.00302 0.00026 0.00009 0.00018 0.00000 0.00072 0.00086 0.00085 0.00067 0.00065 0.00065 0.00034 N5 0.95480 0.62201 0.18678 1.00000 0.01640 0.02094 0.01968 -0.00206 0.00223 0.00261 0.01899 0.00310 0.00026 0.00010 0.00019 0.00000 0.00076 0.00086 0.00088 0.00073 0.00067 0.00069 0.00035 O1 0.90781 0.84579 0.25289 1.00000 0.01531 0.01558 0.02430 -0.00423 0.00386 -0.00029 0.01828 0.00241 0.00021 0.00007 0.00015 0.00000 0.00063 0.00066 0.00075 0.00056 0.00055 0.00052 0.00029 O2 0.60214 0.88168 0.09166 1.00000 0.02126 0.01550 0.01972 0.00179 0.00054 -0.00111 0.01896 0.00246 0.00021 0.00008 0.00014 0.00000 0.00069 0.00064 0.00071 0.00056 0.00056 0.00055 0.00029 O3 0.66056 0.71003 0.51440 1.00000 0.01510 0.02236 0.02034 0.00022 -0.00066 0.00283 0.01947 0.00243 0.00019 0.00008 0.00014 0.00000 0.00059 0.00067 0.00071 0.00059 0.00051 0.00059 0.00028 O4 0.60529 0.60774 0.01980 1.00000 0.01726 0.02273 0.02009 -0.00696 0.00110 -0.00012 0.02011 0.00240 0.00021 0.00008 0.00015 0.00000 0.00064 0.00073 0.00074 0.00059 0.00056 0.00058 0.00030 P1 0.68442 0.81113 0.18652 1.00000 0.01642 0.01311 0.01717 -0.00089 0.00281 -0.00045 0.01550 0.00086 0.00007 0.00003 0.00005 0.00000 0.00021 0.00022 0.00024 0.00019 0.00018 0.00019 0.00011 P2 0.51106 0.71306 0.36849 1.00000 0.01349 0.01403 0.01603 0.00004 0.00170 -0.00009 0.01452 0.00084 0.00007 0.00003 0.00005 0.00000 0.00020 0.00022 0.00024 0.00018 0.00017 0.00018 0.00010 P3 0.71145 0.65762 0.14669 1.00000 0.01556 0.01371 0.01718 -0.00258 0.00173 0.00025 0.01549 0.00086 0.00007 0.00003 0.00005 0.00000 0.00022 0.00021 0.00024 0.00019 0.00018 0.00019 0.00011 H4N 0.17600 0.68912 0.34898 1.00000 0.04076 0.05306 0.00438 0.00162 0.00313 0.00000 0.00788 H5N 0.94254 0.58051 0.23197 1.00000 0.02736 0.04624 0.00408 0.00151 0.00279 0.00000 0.00672 Final Structure Factor Calculation for 2008src0232 in P2(1) Total number of l.s. parameters = 279 Maximum vector length = 511 Memory required = 3049 / 26068 wR2 = 0.0654 before cycle 5 for 4543 data and 2 / 279 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0168 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0282 for 4430 Fo > 4sig(Fo) and 0.0294 for all 4543 data wR2 = 0.0654, GooF = S = 1.010, Restrained GooF = 1.010 for all data Flack x parameter = 0.0156 with esd 0.0582 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 30.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0195 0.0154 0.0139 C1 0.0381 0.0188 0.0161 C2 0.0397 0.0212 0.0146 C3 0.0271 0.0186 0.0143 C4 0.0277 0.0192 0.0146 C5 0.0220 0.0179 0.0143 C6 0.0269 0.0175 0.0138 C7 0.0260 0.0202 0.0156 C8 0.0364 0.0238 0.0179 C9 0.0463 0.0238 0.0186 C10 0.0511 0.0261 0.0170 C11 0.0322 0.0246 0.0189 C12 0.0254 0.0218 0.0135 C13 0.0294 0.0231 0.0155 C14 0.0284 0.0246 0.0144 C15 0.0302 0.0242 0.0152 C16 0.0290 0.0283 0.0140 C17 0.0327 0.0250 0.0143 C18 0.0185 0.0168 0.0140 N1 0.0249 0.0179 0.0137 N2 0.0252 0.0173 0.0147 N3 0.0212 0.0176 0.0135 N4 0.0233 0.0189 0.0148 N5 0.0261 0.0151 0.0136 O1 0.0232 0.0189 0.0148 O2 0.0237 0.0213 0.0135 O3 0.0286 0.0174 0.0143 O4 0.0179 0.0157 0.0129 P1 0.0160 0.0140 0.0135 P2 0.0186 0.0156 0.0123 P3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.054 0.080 0.102 0.125 0.147 0.174 0.209 0.254 0.328 1.000 Number in group 480. 428. 459. 477. 432. 452. 455. 448. 456. 456. GooF 1.128 1.025 1.000 1.026 1.009 0.939 0.951 0.963 0.933 1.090 K 1.027 0.973 0.979 0.998 1.002 1.014 1.012 1.008 1.004 1.002 Resolution(A) 0.77 0.80 0.84 0.88 0.93 0.99 1.06 1.17 1.33 1.68 inf Number in group 463. 448. 464. 451. 458. 447. 447. 453. 456. 456. GooF 1.074 0.937 0.911 1.002 0.908 0.906 0.949 0.784 0.940 1.505 K 1.040 1.026 1.020 1.033 1.007 0.989 0.987 0.992 1.004 1.006 R1 0.059 0.050 0.041 0.043 0.033 0.028 0.022 0.015 0.019 0.023 Recommended weighting scheme: WGHT 0.0140 0.5550 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 7 9 26.90 84.56 6.01 0.106 0.79 -1 -1 5 29.59 10.24 5.15 0.037 1.87 -2 0 2 84.86 128.68 5.04 0.130 2.76 -1 1 5 31.75 13.75 4.65 0.043 1.87 -2 -7 1 262.93 330.41 4.04 0.209 1.95 -2 7 1 277.93 339.76 4.00 0.212 1.95 2 -3 4 507.12 426.62 3.95 0.237 1.72 2 -4 0 1087.77 951.25 3.94 0.354 2.55 -2 0 4 1428.54 1233.51 3.82 0.404 2.00 3 0 7 39.81 63.91 3.73 0.092 1.08 -4 -3 6 27.10 48.04 3.63 0.080 1.16 -4 -19 4 20.79 41.97 3.55 0.074 0.77 5 10 2 30.30 56.35 3.49 0.086 0.98 0 0 5 16.65 30.82 3.44 0.064 1.90 3 2 0 545.26 474.25 3.43 0.250 2.03 6 10 5 5.25 24.53 3.41 0.057 0.78 2 4 3 1400.29 1254.49 3.38 0.407 1.90 -3 0 1 75.70 102.61 3.36 0.116 2.09 0 5 2 1515.58 1682.64 3.30 0.471 2.83 2 4 0 1060.32 945.64 3.26 0.353 2.55 -2 -3 4 339.82 284.80 3.24 0.194 1.90 -1 15 7 280.84 219.77 3.23 0.170 0.89 -1 0 4 1788.19 1991.43 3.22 0.513 2.31 -4 -13 2 13.90 30.29 3.19 0.063 1.02 3 4 3 14.41 6.21 3.19 0.029 1.55 0 -6 4 38.41 21.61 3.17 0.053 1.85 2 0 5 9.28 19.89 3.16 0.051 1.55 0 6 4 42.71 24.30 3.15 0.057 1.85 8 1 0 121.38 82.88 3.12 0.105 0.78 5 -17 2 -2.29 8.63 3.11 0.034 0.78 2 3 8 6.36 17.19 3.10 0.048 1.05 3 -1 0 335.03 288.25 3.08 0.195 2.07 -2 3 4 346.20 286.88 3.07 0.195 1.90 2 -1 3 2042.89 1857.03 3.05 0.495 2.09 5 12 4 73.70 101.33 3.04 0.116 0.86 3 0 1 3695.41 3426.01 3.03 0.673 1.99 3 0 2 118.98 148.59 3.03 0.140 1.84 3 -2 0 541.29 479.16 3.02 0.252 2.03 5 -17 0 31.01 57.69 3.02 0.087 0.80 5 -14 2 34.64 56.66 3.00 0.087 0.86 -3 4 1 861.54 777.73 2.92 0.320 1.89 -3 2 4 431.21 373.72 2.91 0.222 1.64 0 -5 2 1538.15 1686.72 2.90 0.472 2.83 -2 1 5 201.17 166.28 2.89 0.148 1.70 1 5 4 451.99 395.82 2.89 0.229 1.83 -1 -18 4 300.47 245.52 2.87 0.180 0.90 0 7 3 732.00 652.42 2.87 0.294 1.97 -4 -10 1 210.04 256.59 2.84 0.184 1.17 0 1 4 27.36 16.63 2.80 0.047 2.35 1 -5 2 1052.35 948.31 2.79 0.354 2.52 Bond lengths and angles C1 - Distance Angles C6 1.3835 (0.0026) C2 1.3876 (0.0027) 120.95 (0.18) O1 1.3922 (0.0023) 115.22 (0.16) 123.83 (0.17) C1 - C6 C2 C2 - Distance Angles C1 1.3876 (0.0027) C3 1.3897 (0.0029) 118.86 (0.19) C2 - C1 C3 - Distance Angles C4 1.3812 (0.0029) C2 1.3897 (0.0029) 120.99 (0.19) C3 - C4 C4 - Distance Angles C3 1.3812 (0.0029) C5 1.3819 (0.0028) 119.25 (0.19) C4 - C3 C5 - Distance Angles C4 1.3819 (0.0028) C6 1.3899 (0.0029) 120.88 (0.18) C5 - C4 C6 - Distance Angles C1 1.3835 (0.0026) C5 1.3899 (0.0029) 119.04 (0.18) C6 - C1 C7 - Distance Angles C12 1.3822 (0.0029) C8 1.3830 (0.0028) 121.78 (0.19) O2 1.4011 (0.0024) 115.17 (0.18) 122.91 (0.18) C7 - C12 C8 C8 - Distance Angles C7 1.3830 (0.0028) C9 1.3903 (0.0030) 118.60 (0.19) C8 - C7 C9 - Distance Angles C8 1.3903 (0.0030) C10 1.3924 (0.0032) 120.57 (0.20) C9 - C8 C10 - Distance Angles C11 1.3878 (0.0035) C9 1.3924 (0.0032) 119.74 (0.21) C10 - C11 C11 - Distance Angles C10 1.3878 (0.0035) C12 1.3902 (0.0032) 120.15 (0.21) C11 - C10 C12 - Distance Angles C7 1.3822 (0.0029) C11 1.3902 (0.0032) 119.15 (0.21) C12 - C7 C13 - Distance Angles N4 1.4805 (0.0025) C14 1.5232 (0.0028) 109.46 (0.16) C13 - N4 C14 - Distance Angles C15 1.5121 (0.0028) C13 1.5232 (0.0028) 110.46 (0.17) C14 - C15 C15 - Distance Angles O3 1.4626 (0.0024) C14 1.5121 (0.0028) 109.97 (0.16) C15 - O3 C16 - Distance Angles N5 1.4920 (0.0026) C17 1.5160 (0.0029) 111.51 (0.16) C16 - N5 C17 - Distance Angles C18 1.5141 (0.0030) C16 1.5160 (0.0029) 111.84 (0.17) C17 - C18 C18 - Distance Angles O4 1.4603 (0.0024) C17 1.5141 (0.0030) 112.25 (0.17) C18 - O4 N1 - Distance Angles P1 1.5754 (0.0016) P2 1.6107 (0.0016) 120.37 (0.10) N1 - P1 N2 - Distance Angles P2 1.5836 (0.0016) P3 1.5911 (0.0017) 121.20 (0.10) N2 - P2 N3 - Distance Angles P1 1.5777 (0.0017) P3 1.6002 (0.0017) 119.36 (0.11) N3 - P1 N4 - Distance Angles C13 1.4805 (0.0025) P2 1.6344 (0.0016) 117.91 (0.13) N4 - C13 N5 - Distance Angles C16 1.4920 (0.0026) P3 1.6622 (0.0017) 113.99 (0.14) N5 - C16 O1 - Distance Angles C1 1.3922 (0.0023) P1 1.5991 (0.0014) 126.91 (0.12) O1 - C1 O2 - Distance Angles C7 1.4011 (0.0024) P1 1.5911 (0.0014) 126.00 (0.12) O2 - C7 O3 - Distance Angles C15 1.4626 (0.0024) P2 1.5916 (0.0014) 116.31 (0.12) O3 - C15 O4 - Distance Angles C18 1.4603 (0.0024) P3 1.5829 (0.0014) 117.57 (0.12) O4 - C18 P1 - Distance Angles N1 1.5754 (0.0016) N3 1.5777 (0.0017) 117.89 (0.09) O2 1.5911 (0.0014) 109.91 (0.08) 110.56 (0.09) O1 1.5991 (0.0014) 111.89 (0.08) 106.63 (0.08) 98.16 (0.07) P1 - N1 N3 O2 P2 - Distance Angles N2 1.5836 (0.0016) O3 1.5916 (0.0014) 107.51 (0.09) N1 1.6107 (0.0016) 116.20 (0.09) 108.16 (0.08) N4 1.6344 (0.0016) 109.90 (0.09) 102.12 (0.08) 111.88 (0.08) P2 - N2 O3 N1 P3 - Distance Angles O4 1.5829 (0.0014) N2 1.5911 (0.0017) 106.98 (0.08) N3 1.6002 (0.0017) 108.45 (0.08) 118.53 (0.09) N5 1.6622 (0.0017) 105.36 (0.08) 109.28 (0.09) 107.48 (0.09) P3 - O4 N2 N3 FMAP and GRID set by program FMAP 2 1 30 GRID -3.704 -1 -2 3.704 1 2 R1 = 0.0279 for 2486 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.26 at 0.2487 0.1995 0.8996 [ 0.76 A from N3 ] Deepest hole -0.28 at 0.3343 0.1298 0.8440 [ 0.58 A from P3 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3140 / 35289 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7513 0.6995 0.1004 1.00000 0.05 0.26 0.76 N3 0.91 P3 1.97 O4 1.99 N5 Q2 1 0.5468 0.7935 0.2206 1.00000 0.05 0.23 0.80 N1 1.01 P1 2.03 P2 2.03 N3 Q3 1 0.3721 0.7226 0.3936 1.00000 0.05 0.23 0.81 N4 0.95 P2 1.39 H4N 1.83 C13 Q4 1 0.6989 0.7684 0.1412 1.00000 0.05 0.21 0.73 N3 0.88 P1 1.96 P3 2.03 N1 Q5 1 0.5778 0.6868 0.3046 1.00000 0.05 0.21 0.80 N2 0.91 P2 1.88 P3 1.96 N1 Q6 1 0.5369 0.8109 0.0174 1.00000 0.05 0.20 1.44 C7 1.47 O2 1.77 P1 1.84 N3 Q7 1 0.7790 0.7669 0.0242 1.00000 0.05 0.19 0.84 N3 1.89 P1 1.95 H9 2.32 P3 Q8 1 0.0511 0.9122 -0.1212 1.00000 0.05 0.19 1.07 C9 1.09 C10 1.68 H9 1.70 H10 Q9 1 0.6401 0.6656 0.2160 1.00000 0.05 0.18 0.82 N2 0.85 P3 1.94 P2 1.95 N3 Q10 1 0.4530 0.8811 -0.0873 1.00000 0.05 0.18 0.74 C7 0.89 C12 1.60 H12 1.79 C8 Shortest distances between peaks (including symmetry equivalents) 5 9 1.04 4 7 1.28 1 4 1.33 2 4 1.36 1 7 1.41 1 9 1.50 6 10 1.64 4 6 1.65 6 7 1.71 3 5 1.75 2 6 1.96 4 9 2.00 2 5 2.05 4 5 2.31 2 9 2.33 1 5 2.35 2 3 2.43 1 2 2.46 1 6 2.47 2 7 2.55 8 10 2.58 3 9 2.72 7 9 2.77 7 10 2.99 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: 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 0.02: Analyse other restraints etc. 2.44: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.20: Structure factors and derivatives 1.97: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.47: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0232 finished at 16:38:40 Total CPU time: 6.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++