+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0701 started at 16:52:28 on 14-Jun-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0701 in P-1 CELL 0.71073 8.3400 10.7116 11.0362 107.886 96.645 99.433 ZERR 2.00 0.0002 0.0002 0.0003 0.001 0.001 0.002 LATT 1 SFAC C H N O P UNIT 36 44 2 8 2 V = 910.98 F(000) = 368.0 Mu = 0.17 mm-1 Cell Wt = 694.67 Rho = 1.266 MERG 2 OMIT -3.00 55.00 OMIT -1 0 2 OMIT 2 0 0 OMIT 1 -3 2 OMIT 1 -2 1 OMIT 0 -2 1 OMIT -1 2 0 FMAP 2 PLAN 20 SIZE 0.30 0.42 0.58 ACTA BOND WGHT 0.03980 0.39150 L.S. 4 TEMP -153.00 FVAR 1.21198 C1 1 -0.020990 0.304536 0.229414 11.00000 0.01567 0.01898 = 0.01702 0.00993 0.00350 0.00476 C2 1 -0.072774 0.185579 0.124553 11.00000 0.02043 0.02267 = 0.02185 0.00636 0.00600 0.00331 AFIX 43 H2 2 0.002913 0.152567 0.071117 11.00000 -1.20000 AFIX 0 C3 1 -0.236132 0.115379 0.098554 11.00000 0.02451 0.02869 = 0.02558 0.00778 0.00112 -0.00290 AFIX 43 H3 2 -0.271906 0.034318 0.027320 11.00000 -1.20000 AFIX 0 C4 1 -0.346560 0.163986 0.176826 11.00000 0.01620 0.04056 = 0.03121 0.02007 0.00127 -0.00090 AFIX 43 H4 2 -0.457675 0.115824 0.159083 11.00000 -1.20000 AFIX 0 C5 1 -0.295408 0.282317 0.280591 11.00000 0.01970 0.04406 = 0.02592 0.01870 0.00992 0.01180 AFIX 43 H5 2 -0.371767 0.315413 0.333285 11.00000 -1.20000 AFIX 0 C6 1 -0.132505 0.352897 0.307913 11.00000 0.02115 0.02798 = 0.01764 0.00996 0.00535 0.00975 AFIX 43 H6 2 -0.097274 0.433596 0.379614 11.00000 -1.20000 AFIX 0 C7 1 0.242546 0.408895 0.112536 11.00000 0.01418 0.01820 = 0.01811 0.00720 0.00226 0.00012 C8 1 0.309326 0.308325 0.034221 11.00000 0.01885 0.02324 = 0.02316 0.00634 0.00557 0.00423 AFIX 43 H8 2 0.327561 0.234490 0.060467 11.00000 -1.20000 AFIX 0 C9 1 0.348880 0.316975 -0.082239 11.00000 0.02185 0.03696 = 0.02128 0.00251 0.00639 0.00099 AFIX 43 H9 2 0.394642 0.248944 -0.135536 11.00000 -1.20000 AFIX 0 C10 1 0.321941 0.424326 -0.121099 11.00000 0.02357 0.04465 = 0.01584 0.01124 0.00078 -0.00842 AFIX 43 H10 2 0.350627 0.430032 -0.200354 11.00000 -1.20000 AFIX 0 C11 1 0.253609 0.523053 -0.045201 11.00000 0.02596 0.03238 = 0.02301 0.01736 -0.00329 -0.00369 AFIX 43 H11 2 0.234087 0.595825 -0.072769 11.00000 -1.20000 AFIX 0 C12 1 0.213445 0.515728 0.071634 11.00000 0.01948 0.02244 = 0.02217 0.00993 0.00016 0.00126 AFIX 43 H12 2 0.166148 0.583439 0.123749 11.00000 -1.20000 AFIX 0 C13 1 0.342217 0.318540 0.516093 11.00000 0.03832 0.01892 = 0.01855 0.00602 -0.00174 0.00407 AFIX 137 H13A 2 0.303258 0.270491 0.573249 11.00000 -1.50000 H13B 2 0.320954 0.409458 0.544852 11.00000 -1.50000 H13C 2 0.461058 0.323592 0.518954 11.00000 -1.50000 AFIX 0 C14 1 0.244681 0.109491 0.324762 11.00000 0.01568 0.01858 = 0.01853 0.00711 0.00313 0.00531 C15 1 0.203265 -0.100328 0.373853 11.00000 0.02446 0.01224 = 0.02432 0.00535 0.00171 0.00121 C16 1 0.044938 -0.164884 0.276135 11.00000 0.02207 0.02252 = 0.03869 0.00258 -0.00132 0.00112 AFIX 137 H16A 2 -0.045003 -0.123322 0.308227 11.00000 -1.50000 H16B 2 0.017684 -0.261115 0.263320 11.00000 -1.50000 H16C 2 0.059776 -0.151952 0.193682 11.00000 -1.50000 AFIX 0 C17 1 0.186324 -0.125393 0.500256 11.00000 0.05182 0.02005 = 0.03158 0.01294 0.00905 0.00348 AFIX 137 H17A 2 0.285538 -0.076175 0.564847 11.00000 -1.50000 H17B 2 0.173072 -0.221632 0.486450 11.00000 -1.50000 H17C 2 0.089419 -0.094565 0.531129 11.00000 -1.50000 AFIX 0 C18 1 0.354250 -0.144649 0.324104 11.00000 0.02375 0.01941 = 0.03655 0.00727 0.00208 0.00521 AFIX 137 H18A 2 0.361617 -0.128685 0.241919 11.00000 -1.50000 H18B 2 0.344772 -0.240520 0.310780 11.00000 -1.50000 H18C 2 0.453752 -0.093331 0.387523 11.00000 -1.50000 AFIX 0 N1 3 0.254635 0.246942 0.383453 11.00000 0.02100 0.01595 = 0.01580 0.00910 0.00384 0.00354 O1 4 0.202095 0.536988 0.361837 11.00000 0.03002 0.01686 = 0.02098 0.00371 0.00531 0.00328 O2 4 0.310482 0.315217 0.298120 11.00000 0.01694 0.02210 = 0.02335 0.01509 0.00558 0.00500 O3 4 0.242280 0.057078 0.210830 11.00000 0.03275 0.02496 = 0.01794 0.00594 0.00748 0.00953 O4 4 0.230050 0.049183 0.413720 11.00000 0.02768 0.01331 = 0.01746 0.00590 0.00344 0.00331 P1 5 0.184145 0.404526 0.262538 11.00000 0.01577 0.01388 = 0.01630 0.00612 0.00312 0.00311 HKLF 4 Covalent radii and connectivity table for 2007src0701 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 C1 - C2 C6 P1 C2 - C3 C1 C3 - C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - C8 C12 P1 C8 - C9 C7 C9 - C10 C8 C10 - C11 C9 C11 - C10 C12 C12 - C11 C7 C13 - N1 C14 - O3 O4 N1 C15 - O4 C16 C17 C18 C16 - C15 C17 - C15 C18 - C15 N1 - C14 O2 C13 O1 - P1 O2 - N1 P1 O3 - C14 O4 - C14 C15 P1 - O1 O2 C7 C1 20954 Reflections read, of which 12 rejected -10 =< h =< 10, -13 =< k =< 13, -14 =< l =< 14, Max. 2-theta = 55.00 0 Systematic absence violations 0 Inconsistent equivalents 4157 Unique reflections, of which 0 suppressed R(int) = 0.0358 R(sigma) = 0.0292 Friedel opposites merged Maximum memory for data reduction = 2179 / 41435 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 = 2802 / 274852 wR2 = 0.0902 before cycle 1 for 4157 data and 221 / 221 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0398 * P )^2 + 0.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21338 0.00183 0.765 OSF Mean shift/esd = 0.219 Maximum = -0.779 for U22 C12 Max. shift = 0.007 A for H17A Max. dU = 0.000 for C12 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2802 / 274852 wR2 = 0.0900 before cycle 2 for 4157 data and 221 / 221 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0398 * P )^2 + 0.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21298 0.00182 -0.215 OSF Mean shift/esd = 0.075 Maximum = -0.272 for U22 C12 Max. shift = 0.003 A for H17A Max. dU = 0.000 for C12 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2802 / 274852 wR2 = 0.0899 before cycle 3 for 4157 data and 221 / 221 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0398 * P )^2 + 0.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21297 0.00182 -0.007 OSF Mean shift/esd = 0.003 Maximum = 0.031 for tors H16A Max. shift = 0.000 A for H16C Max. dU = 0.000 for C13 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2802 / 274852 wR2 = 0.0900 before cycle 4 for 4157 data and 221 / 221 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0398 * P )^2 + 0.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21297 0.00182 -0.001 OSF Mean shift/esd = 0.001 Maximum = -0.006 for U23 C17 Max. shift = 0.000 A for H16C Max. dU = 0.000 for C12 Largest correlation matrix elements 0.512 U23 C11 / U22 C11 0.506 U23 C4 / U22 C4 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0028 0.1526 0.0711 43 0.950 0.000 C2 C3 C1 H3 -0.2717 0.0342 0.0273 43 0.950 0.000 C3 C4 C2 H4 -0.4577 0.1158 0.1591 43 0.950 0.000 C4 C5 C3 H5 -0.3717 0.3153 0.3332 43 0.950 0.000 C5 C4 C6 H6 -0.0975 0.4336 0.3795 43 0.950 0.000 C6 C5 C1 H8 0.3275 0.2345 0.0605 43 0.950 0.000 C8 C9 C7 H9 0.3944 0.2488 -0.1356 43 0.950 0.000 C9 C10 C8 H10 0.3505 0.4299 -0.2004 43 0.950 0.000 C10 C11 C9 H11 0.2344 0.5959 -0.0727 43 0.950 0.000 C11 C10 C12 H12 0.1659 0.5834 0.1236 43 0.950 0.000 C12 C11 C7 H13A 0.3033 0.2707 0.5733 137 0.980 0.000 C13 N1 H13A H13B 0.3213 0.4095 0.5447 137 0.980 0.000 C13 N1 H13A H13C 0.4611 0.3234 0.5188 137 0.980 0.000 C13 N1 H13A H16A -0.0448 -0.1228 0.3078 137 0.980 0.000 C16 C15 H16A H16B 0.0171 -0.2610 0.2638 137 0.980 0.000 C16 C15 H16A H16C 0.0601 -0.1526 0.1934 137 0.980 0.000 C16 C15 H16A H17A 0.2859 -0.0770 0.5645 137 0.980 0.000 C17 C15 H17A H17B 0.1719 -0.2218 0.4861 137 0.980 0.000 C17 C15 H17A H17C 0.0900 -0.0939 0.5314 137 0.980 0.000 C17 C15 H17A H18A 0.3616 -0.1285 0.2419 137 0.980 0.000 C18 C15 H18A H18B 0.3447 -0.2406 0.3105 137 0.980 0.000 C18 C15 H18A H18C 0.4538 -0.0935 0.3874 137 0.980 0.000 C18 C15 H18A 2007src0701 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.02095 0.30452 0.22948 1.00000 0.01557 0.01899 0.01704 0.01012 0.00342 0.00482 0.01604 0.00276 0.00015 0.00012 0.00012 0.00000 0.00057 0.00060 0.00059 0.00048 0.00046 0.00046 0.00025 C2 -0.07288 0.18556 0.12457 1.00000 0.02041 0.02267 0.02170 0.00639 0.00604 0.00344 0.02176 0.00297 0.00016 0.00013 0.00013 0.00000 0.00063 0.00066 0.00066 0.00053 0.00051 0.00051 0.00027 H2 0.00279 0.15260 0.07109 1.00000 0.02611 0.00000 0.00000 C3 -0.23601 0.11533 0.09853 1.00000 0.02462 0.02805 0.02563 0.00757 0.00097 -0.00272 0.02772 0.00316 0.00018 0.00015 0.00014 0.00000 0.00071 0.00074 0.00073 0.00058 0.00056 0.00057 0.00031 H3 -0.27171 0.03425 0.02731 1.00000 0.03326 0.00000 0.00000 C4 -0.34653 0.16396 0.17682 1.00000 0.01605 0.04056 0.03098 0.01998 0.00128 -0.00083 0.02836 0.00335 0.00017 0.00016 0.00015 0.00000 0.00063 0.00084 0.00077 0.00066 0.00055 0.00057 0.00032 H4 -0.45765 0.11581 0.15906 1.00000 0.03404 0.00000 0.00000 C5 -0.29539 0.28225 0.28053 1.00000 0.01940 0.04357 0.02582 0.01862 0.00965 0.01150 0.02687 0.00342 0.00017 0.00016 0.00014 0.00000 0.00066 0.00086 0.00072 0.00065 0.00055 0.00060 0.00031 H5 -0.37175 0.31533 0.33324 1.00000 0.03224 0.00000 0.00000 C6 -0.13260 0.35282 0.30783 1.00000 0.02099 0.02782 0.01758 0.01011 0.00536 0.00960 0.02083 0.00309 0.00016 0.00014 0.00013 0.00000 0.00063 0.00069 0.00063 0.00053 0.00050 0.00053 0.00027 H6 -0.09747 0.43357 0.37949 1.00000 0.02499 0.00000 0.00000 C7 0.24266 0.40891 0.11261 1.00000 0.01378 0.01823 0.01775 0.00725 0.00202 0.00002 0.01676 0.00269 0.00015 0.00012 0.00012 0.00000 0.00056 0.00060 0.00060 0.00048 0.00046 0.00045 0.00025 C8 0.30930 0.30831 0.03424 1.00000 0.01878 0.02301 0.02337 0.00668 0.00536 0.00401 0.02187 0.00294 0.00016 0.00014 0.00013 0.00000 0.00062 0.00066 0.00068 0.00054 0.00051 0.00050 0.00028 H8 0.32752 0.23447 0.06047 1.00000 0.02625 0.00000 0.00000 C9 0.34876 0.31691 -0.08225 1.00000 0.02155 0.03645 0.02130 0.00228 0.00619 0.00094 0.02858 0.00312 0.00017 0.00016 0.00014 0.00000 0.00068 0.00081 0.00070 0.00060 0.00055 0.00059 0.00032 H9 0.39441 0.24883 -0.13559 1.00000 0.03429 0.00000 0.00000 C10 0.32189 0.42425 -0.12108 1.00000 0.02339 0.04471 0.01585 0.01121 0.00068 -0.00834 0.02984 0.00312 0.00018 0.00016 0.00014 0.00000 0.00069 0.00089 0.00064 0.00061 0.00053 0.00061 0.00034 H10 0.35053 0.42993 -0.20036 1.00000 0.03580 0.00000 0.00000 C11 0.25372 0.52305 -0.04515 1.00000 0.02551 0.03239 0.02314 0.01718 -0.00352 -0.00388 0.02702 0.00309 0.00017 0.00015 0.00014 0.00000 0.00070 0.00077 0.00070 0.00060 0.00055 0.00057 0.00031 H11 0.23441 0.59589 -0.07268 1.00000 0.03242 0.00000 0.00000 C12 0.21340 0.51576 0.07157 1.00000 0.01916 0.02174 0.02230 0.00987 -0.00004 0.00125 0.02116 0.00289 0.00016 0.00013 0.00013 0.00000 0.00062 0.00065 0.00066 0.00053 0.00050 0.00050 0.00027 H12 0.16591 0.58340 0.12358 1.00000 0.02539 0.00000 0.00000 C13 0.34230 0.31853 0.51604 1.00000 0.03780 0.01888 0.01828 0.00583 -0.00174 0.00401 0.02587 0.00300 0.00019 0.00014 0.00013 0.00000 0.00080 0.00066 0.00065 0.00052 0.00057 0.00057 0.00030 H13A 0.30326 0.27066 0.57331 1.00000 0.03881 0.00000 0.00000 H13B 0.32130 0.40953 0.54472 1.00000 0.03881 0.00000 0.00000 H13C 0.46110 0.32336 0.51883 1.00000 0.03881 0.00000 0.00000 C14 0.24473 0.10946 0.32477 1.00000 0.01555 0.01848 0.01842 0.00704 0.00313 0.00517 0.01707 0.00278 0.00015 0.00013 0.00012 0.00000 0.00057 0.00060 0.00062 0.00049 0.00046 0.00046 0.00025 C15 0.20332 -0.10029 0.37391 1.00000 0.02454 0.01211 0.02430 0.00523 0.00193 0.00149 0.02100 0.00286 0.00017 0.00012 0.00013 0.00000 0.00066 0.00059 0.00067 0.00050 0.00053 0.00049 0.00027 C16 0.04492 -0.16490 0.27606 1.00000 0.02205 0.02268 0.03840 0.00290 -0.00122 0.00122 0.03040 0.00314 0.00018 0.00015 0.00016 0.00000 0.00069 0.00071 0.00086 0.00062 0.00061 0.00055 0.00033 H16A -0.04483 -0.12280 0.30776 1.00000 0.04559 0.00000 0.00000 H16B 0.01714 -0.26098 0.26380 1.00000 0.04559 0.00000 0.00000 H16C 0.06014 -0.15264 0.19340 1.00000 0.04559 0.00000 0.00000 C17 0.18628 -0.12548 0.50014 1.00000 0.05190 0.01991 0.03177 0.01303 0.00886 0.00331 0.03388 0.00364 0.00022 0.00015 0.00015 0.00000 0.00099 0.00070 0.00081 0.00061 0.00071 0.00065 0.00036 H17A 0.28592 -0.07701 0.56453 1.00000 0.05082 0.00000 0.00000 H17B 0.17194 -0.22184 0.48606 1.00000 0.05082 0.00000 0.00000 H17C 0.08998 -0.09389 0.53142 1.00000 0.05082 0.00000 0.00000 C18 0.35424 -0.14465 0.32401 1.00000 0.02366 0.01906 0.03677 0.00717 0.00187 0.00516 0.02721 0.00324 0.00017 0.00014 0.00015 0.00000 0.00068 0.00066 0.00081 0.00058 0.00059 0.00053 0.00031 H18A 0.36160 -0.12853 0.24189 1.00000 0.04081 0.00000 0.00000 H18B 0.34466 -0.24056 0.31052 1.00000 0.04081 0.00000 0.00000 H18C 0.45379 -0.09347 0.38743 1.00000 0.04081 0.00000 0.00000 N1 0.25457 0.24690 0.38351 1.00000 0.02079 0.01615 0.01588 0.00925 0.00390 0.00340 0.01669 0.00235 0.00013 0.00010 0.00010 0.00000 0.00053 0.00051 0.00051 0.00041 0.00041 0.00040 0.00022 O1 0.20208 0.53700 0.36183 1.00000 0.03006 0.01655 0.02116 0.00355 0.00535 0.00335 0.02335 0.00207 0.00012 0.00009 0.00009 0.00000 0.00051 0.00046 0.00048 0.00037 0.00039 0.00037 0.00021 O2 0.31045 0.31519 0.29804 1.00000 0.01675 0.02210 0.02323 0.01514 0.00553 0.00498 0.01863 0.00204 0.00011 0.00009 0.00009 0.00000 0.00043 0.00046 0.00047 0.00038 0.00035 0.00035 0.00020 O3 0.24234 0.05713 0.21078 1.00000 0.03281 0.02450 0.01778 0.00600 0.00735 0.00948 0.02461 0.00217 0.00012 0.00010 0.00009 0.00000 0.00054 0.00050 0.00048 0.00038 0.00040 0.00041 0.00022 O4 0.22999 0.04916 0.41368 1.00000 0.02746 0.01304 0.01755 0.00584 0.00338 0.00315 0.01936 0.00196 0.00011 0.00009 0.00009 0.00000 0.00049 0.00042 0.00045 0.00034 0.00036 0.00035 0.00020 P1 0.18414 0.40454 0.26253 1.00000 0.01575 0.01385 0.01626 0.00615 0.00315 0.00315 0.01499 0.00069 0.00004 0.00003 0.00003 0.00000 0.00016 0.00016 0.00017 0.00012 0.00012 0.00011 0.00010 Final Structure Factor Calculation for 2007src0701 in P-1 Total number of l.s. parameters = 221 Maximum vector length = 511 Memory required = 2581 / 24017 wR2 = 0.0899 before cycle 5 for 4157 data and 0 / 221 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0398 * P )^2 + 0.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0350 for 3622 Fo > 4sig(Fo) and 0.0426 for all 4157 data wR2 = 0.0899, GooF = S = 1.040, Restrained GooF = 1.040 for all data Occupancy sum of asymmetric unit = 24.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0212 0.0153 0.0116 C1 0.0255 0.0217 0.0181 C2 0.0370 0.0270 0.0191 C3 0.0473 0.0225 0.0153 C4 0.0446 0.0211 0.0149 C5 0.0293 0.0176 0.0156 C6 0.0213 0.0167 0.0123 C7 0.0253 0.0224 0.0179 C8 0.0458 0.0215 0.0185 C9 0.0572 0.0179 0.0144 C10 0.0465 0.0201 0.0144 C11 0.0279 0.0183 0.0173 C12 0.0415 0.0190 0.0171 C13 0.0192 0.0177 0.0143 C14 0.0273 0.0238 0.0119 C15 0.0461 0.0268 0.0182 C16 0.0538 0.0319 0.0159 C17 0.0397 0.0233 0.0187 C18 0.0210 0.0190 0.0101 N1 0.0310 0.0231 0.0159 O1 0.0284 0.0163 0.0112 O2 0.0335 0.0240 0.0164 O3 0.0281 0.0175 0.0125 O4 0.0165 0.0157 0.0128 P1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.035 0.051 0.071 0.090 0.112 0.137 0.175 0.240 1.000 Number in group 427. 427. 412. 407. 406. 417. 419. 413. 411. 418. GooF 0.977 1.025 1.030 1.207 1.092 0.998 0.955 1.124 0.950 1.016 K 1.506 1.005 0.989 0.984 0.988 0.983 0.999 1.007 1.011 0.997 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.63 inf Number in group 424. 421. 407. 411. 428. 405. 415. 413. 414. 419. GooF 0.950 0.889 0.987 0.858 0.893 0.838 0.958 0.940 1.206 1.624 K 0.994 1.021 1.017 1.006 1.005 1.004 1.006 1.007 1.011 0.983 R1 0.080 0.070 0.064 0.048 0.046 0.034 0.031 0.025 0.032 0.036 Recommended weighting scheme: WGHT 0.0355 0.4108 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 -12 6 75.34 156.70 8.01 0.149 0.84 1 0 1 2297.62 5430.23 7.02 0.879 5.89 -1 1 1 8.76 27.92 5.65 0.063 5.62 0 2 0 11.44 32.02 5.17 0.068 4.98 0 4 3 262.98 199.81 4.68 0.169 1.76 -2 4 3 11.83 26.20 4.61 0.061 1.78 1 3 2 33.45 54.24 4.30 0.088 2.20 1 1 5 65.12 42.82 4.24 0.078 1.77 -4 2 4 45.79 29.71 3.72 0.065 1.63 0 5 3 210.04 167.57 3.64 0.154 1.52 -1 3 3 219.14 176.51 3.54 0.159 2.13 3 3 2 16.53 8.28 3.54 0.034 1.63 -4 3 2 217.38 175.62 3.51 0.158 1.78 -3 1 3 66.23 48.14 3.44 0.083 2.25 -4 1 3 235.95 288.62 3.44 0.203 1.87 0 -5 4 375.58 314.15 3.35 0.211 1.92 2 -2 3 19.86 10.96 3.35 0.039 2.57 -1 -4 1 3.54 0.51 3.34 0.009 2.38 -2 -4 6 13.01 6.28 3.31 0.030 1.59 -1 5 2 16.22 27.00 3.30 0.062 1.73 0 -6 3 261.06 215.50 3.28 0.175 1.74 1 2 4 198.79 243.35 3.24 0.186 1.88 0 -6 2 5.12 1.43 3.23 0.014 1.76 -3 -4 10 68.78 92.22 3.22 0.115 1.05 -1 0 6 65.91 48.70 3.19 0.083 1.75 2 -4 5 40.97 57.22 3.13 0.090 1.75 0 -4 2 18.48 10.81 3.12 0.039 2.61 1 -8 10 25.02 39.29 3.07 0.075 0.96 -4 0 4 5.01 1.58 3.05 0.015 1.75 -1 1 3 35.14 24.06 3.04 0.059 3.00 3 -8 5 8.31 3.26 3.03 0.022 1.20 -6 2 2 41.86 28.45 3.03 0.064 1.36 -2 -4 8 32.08 21.19 3.01 0.055 1.30 1 5 1 35.35 24.36 3.00 0.059 1.72 -2 3 4 22.18 13.85 2.99 0.044 1.79 -1 -1 1 146.99 182.33 2.98 0.161 5.85 -3 0 4 187.93 155.45 2.98 0.149 2.06 -2 -1 10 55.00 36.32 2.97 0.072 1.07 1 5 0 114.95 92.03 2.96 0.114 1.85 -3 0 2 216.12 257.95 2.96 0.192 2.59 -1 -11 9 10.82 20.98 2.96 0.055 0.85 -2 -2 7 40.48 28.40 2.93 0.064 1.52 0 0 4 6.41 2.44 2.91 0.019 2.58 2 1 5 482.68 416.01 2.88 0.243 1.60 -6 12 0 -19.53 18.74 2.86 0.052 0.78 0 -3 3 157.13 189.95 2.85 0.164 2.93 -3 -5 9 27.58 17.70 2.84 0.050 1.10 -5 -4 1 2.50 0.03 2.75 0.002 1.28 -3 -4 7 2.37 7.11 2.75 0.032 1.35 4 1 4 43.75 31.71 2.74 0.067 1.39 Bond lengths and angles C1 - Distance Angles C2 1.3959 (0.0018) C6 1.3972 (0.0018) 119.96 (0.12) P1 1.7948 (0.0012) 121.90 (0.09) 118.04 (0.10) C1 - C2 C6 C2 - Distance Angles C3 1.3931 (0.0019) C1 1.3959 (0.0018) 119.80 (0.12) C2 - C3 C3 - Distance Angles C4 1.3902 (0.0021) C2 1.3931 (0.0019) 119.97 (0.13) C3 - C4 C4 - Distance Angles C5 1.3844 (0.0022) C3 1.3902 (0.0021) 120.30 (0.13) C4 - C5 C5 - Distance Angles C4 1.3844 (0.0022) C6 1.3909 (0.0019) 120.22 (0.13) C5 - C4 C6 - Distance Angles C5 1.3909 (0.0019) C1 1.3972 (0.0018) 119.75 (0.13) C6 - C5 C7 - Distance Angles C8 1.3975 (0.0018) C12 1.3996 (0.0018) 119.58 (0.12) P1 1.7902 (0.0013) 122.76 (0.10) 117.61 (0.10) C7 - C8 C12 C8 - Distance Angles C9 1.3894 (0.0020) C7 1.3975 (0.0018) 119.63 (0.13) C8 - C9 C9 - Distance Angles C10 1.3859 (0.0023) C8 1.3894 (0.0020) 120.37 (0.14) C9 - C10 C10 - Distance Angles C11 1.3813 (0.0022) C9 1.3859 (0.0023) 120.37 (0.13) C10 - C11 C11 - Distance Angles C10 1.3813 (0.0022) C12 1.3900 (0.0019) 119.93 (0.13) C11 - C10 C12 - Distance Angles C11 1.3900 (0.0019) C7 1.3996 (0.0018) 120.10 (0.13) C12 - C11 C13 - Distance Angles N1 1.4637 (0.0017) C13 - C14 - Distance Angles O3 1.2060 (0.0015) O4 1.3365 (0.0015) 127.43 (0.12) N1 1.3987 (0.0016) 123.71 (0.12) 108.77 (0.10) C14 - O3 O4 C15 - Distance Angles O4 1.4947 (0.0015) C16 1.5171 (0.0019) 110.24 (0.11) C17 1.5158 (0.0020) 102.29 (0.10) 110.43 (0.12) C18 1.5195 (0.0019) 109.29 (0.10) 113.00 (0.12) 111.06 (0.12) C15 - O4 C16 C17 C16 - Distance Angles C15 1.5171 (0.0019) C16 - C17 - Distance Angles C15 1.5158 (0.0020) C17 - C18 - Distance Angles C15 1.5195 (0.0019) C18 - N1 - Distance Angles C14 1.3987 (0.0016) O2 1.4338 (0.0013) 108.49 (0.09) C13 1.4637 (0.0017) 121.45 (0.10) 110.33 (0.10) N1 - C14 O2 O1 - Distance Angles P1 1.4745 (0.0009) O1 - O2 - Distance Angles N1 1.4338 (0.0013) P1 1.6262 (0.0009) 112.80 (0.07) O2 - N1 O3 - Distance Angles C14 1.2060 (0.0015) O3 - O4 - Distance Angles C14 1.3365 (0.0015) C15 1.4947 (0.0015) 119.69 (0.10) O4 - C14 P1 - Distance Angles O1 1.4745 (0.0009) O2 1.6262 (0.0009) 114.16 (0.05) C7 1.7902 (0.0013) 115.02 (0.06) 98.36 (0.05) C1 1.7948 (0.0012) 112.41 (0.06) 107.11 (0.05) 108.67 (0.06) P1 - O1 O2 C7 FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.0424 for 4157 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.2191 0.4033 0.1801 [ 0.81 A from C7 ] Deepest hole -0.40 at 0.1774 0.3443 0.2217 [ 0.65 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2587 / 22227 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2191 0.4033 0.1801 1.00000 0.05 0.28 0.81 C7 0.98 P1 1.93 C8 1.94 C12 Q2 1 -0.1599 0.1563 0.1072 1.00000 0.05 0.28 0.69 C3 0.72 C2 1.43 H3 1.46 H2 Q3 1 0.2506 0.5161 0.0194 1.00000 0.05 0.27 0.69 C12 0.74 C11 1.48 H12 1.52 H11 Q4 1 0.0694 0.3529 0.2418 1.00000 0.05 0.26 0.81 C1 0.99 P1 1.91 C6 1.95 C2 Q5 1 -0.2096 0.3006 0.3027 1.00000 0.05 0.25 0.70 C5 0.76 C6 1.45 H5 1.50 H6 Q6 1 0.2718 0.3650 0.0734 1.00000 0.05 0.25 0.64 C7 0.77 C8 1.52 H8 1.77 C12 Q7 1 -0.3035 0.2194 0.2394 1.00000 0.05 0.25 0.67 C5 0.76 C4 1.46 H5 1.53 H4 Q8 1 -0.0573 0.2545 0.1797 1.00000 0.05 0.23 0.64 C1 0.78 C2 1.55 H2 1.74 C6 Q9 1 0.2440 0.4632 0.0992 1.00000 0.05 0.22 0.64 C7 0.78 C12 1.50 H12 1.79 C8 Q10 1 -0.0696 0.3141 0.2700 1.00000 0.05 0.22 0.64 C1 0.80 C6 1.54 H6 1.76 C2 Q11 1 0.3122 0.4745 -0.0646 1.00000 0.05 0.22 0.71 C10 0.77 C11 1.52 H10 1.57 H11 Q12 1 -0.2762 0.1358 0.1604 1.00000 0.05 0.20 0.72 C4 0.78 C3 1.49 H4 1.54 H3 Q13 1 0.2024 -0.1059 0.4408 1.00000 0.05 0.20 0.76 C15 0.77 C17 1.38 H17A 1.44 H17C Q14 1 -0.0089 0.1683 0.0161 1.00000 0.05 0.19 0.68 H2 1.34 C2 2.25 H16C 2.26 C3 Q15 1 0.2774 -0.1248 0.3531 1.00000 0.05 0.18 0.74 C15 0.78 C18 1.42 H18B 1.43 H18C Q16 1 0.1276 -0.1358 0.3230 1.00000 0.05 0.18 0.75 C15 0.77 C16 1.41 H16B 1.42 H16C Q17 1 0.3234 0.3201 -0.0204 1.00000 0.05 0.17 0.67 C8 0.73 C9 1.47 H8 1.51 H9 Q18 1 0.3512 -0.1003 0.5433 1.00000 0.05 0.17 0.67 H17A 1.36 C17 1.72 H17B 2.02 H18C Q19 1 -0.3532 0.3440 0.3835 1.00000 0.05 0.16 0.53 H5 1.32 C5 2.11 C6 2.20 H6 Q20 1 0.2982 -0.0032 0.6350 1.00000 0.05 0.16 0.90 H17A 1.70 C17 1.89 H17C 2.23 H18C Shortest distances between peaks (including symmetry equivalents) 8 10 1.03 5 7 1.06 6 9 1.07 7 12 1.12 3 11 1.12 6 17 1.16 3 9 1.19 13 15 1.20 2 12 1.21 2 8 1.23 15 16 1.23 5 10 1.26 1 9 1.27 4 10 1.27 1 6 1.28 13 16 1.29 4 8 1.31 18 20 1.38 13 18 1.56 1 4 1.58 5 19 1.62 2 14 1.71 7 19 1.87 11 17 1.88 8 14 1.88 5 12 1.91 3 6 1.91 9 17 1.95 5 8 1.97 7 10 1.98 9 11 1.99 8 12 1.99 2 10 2.01 2 7 2.02 15 18 2.04 13 20 2.08 3 17 2.21 6 11 2.21 7 8 2.24 10 12 2.26 2 5 2.36 1 17 2.44 1 3 2.45 4 5 2.52 2 4 2.53 1 8 2.58 4 14 2.59 4 9 2.66 4 6 2.67 6 14 2.75 16 18 2.77 10 19 2.82 1 14 2.84 1 10 2.84 10 14 2.91 12 14 2.92 15 20 2.95 18 19 2.96 12 19 2.99 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.01: 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. 3.14: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.16: Structure factors and derivatives 2.10: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.41: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.02: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0701 finished at 16:53:21 Total CPU time: 7.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++