+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 11:45:40 on 02-May-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SRC221 in P2(1)/n CELL 0.71073 10.5363 15.0361 17.3668 90.000 99.776 90.000 ZERR 4.00 0.0002 0.0003 0.0003 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N P PD I UNIT 108 180 4 4 4 4 V = 2711.38 F(000) = 1312.0 Mu = 1.90 mm-1 Cell Wt = 2591.64 Rho = 1.587 MERG 2 OMIT -3.00 55.00 OMIT 2 0 2 OMIT 2 0 8 OMIT 2 2 8 EXTI 0.00095 FMAP 2 PLAN 10 SIZE 0.05 0.08 0.10 ACTA BOND $H WGHT 0.05640 4.12450 L.S. 4 TEMP -153.00 FVAR 0.09804 C1 1 0.053005 0.977703 0.210869 11.00000 0.03451 0.03054 = 0.03356 -0.00377 0.00229 0.00947 AFIX 137 H1A 2 0.005906 1.033381 0.214233 11.00000 -1.50000 H1B 2 0.102094 0.962926 0.262393 11.00000 -1.50000 H1C 2 -0.008187 0.929784 0.193408 11.00000 -1.50000 AFIX 0 C2 1 0.247144 1.058432 0.165418 11.00000 0.03522 0.01577 = 0.03286 -0.00630 -0.01632 0.00006 AFIX 137 H2A 2 0.300527 1.065465 0.124781 11.00000 -1.50000 H2B 2 0.302105 1.043626 0.215127 11.00000 -1.50000 H2C 2 0.201269 1.114112 0.171086 11.00000 -1.50000 AFIX 0 C3 1 0.102148 1.019478 0.075604 11.00000 0.02532 0.02100 = 0.02615 0.00027 -0.01519 0.00636 AFIX 23 H3A 2 0.075275 1.081983 0.080769 11.00000 -1.20000 H3B 2 0.023708 0.983841 0.057616 11.00000 -1.20000 AFIX 0 C4 1 0.203442 1.013718 0.005130 11.00000 0.02069 0.01766 = 0.02163 -0.00141 -0.01383 -0.00071 C5 1 0.221281 1.079571 -0.051799 11.00000 0.02998 0.02063 = 0.03090 0.00124 -0.01927 0.00132 AFIX 43 H5 2 0.168475 1.131063 -0.054408 11.00000 -1.20000 AFIX 0 C6 1 0.323896 1.074640 -0.112791 11.00000 0.04216 0.01958 = 0.02328 0.00639 -0.01757 -0.00356 AFIX 43 H6 2 0.325215 1.122700 -0.148156 11.00000 -1.20000 AFIX 0 C7 1 0.408648 1.005156 -0.116160 11.00000 0.03413 0.02606 = 0.01452 0.00255 -0.00535 -0.00865 AFIX 43 H7 2 0.469622 1.002064 -0.150575 11.00000 -1.20000 AFIX 0 C8 1 0.390777 0.938181 -0.059769 11.00000 0.02403 0.01476 = 0.01889 -0.00213 -0.00975 -0.00069 AFIX 43 H8 2 0.444564 0.887211 -0.057500 11.00000 -1.20000 AFIX 0 C9 1 0.286961 0.940476 0.001285 11.00000 0.02130 0.01161 = 0.01711 -0.00058 -0.01387 -0.00158 C10 1 0.259612 0.736019 -0.063353 11.00000 0.01896 0.01467 = 0.01447 -0.00093 -0.01021 0.00110 AFIX 13 H10 2 0.310075 0.787612 -0.078401 11.00000 -1.20000 AFIX 0 C11 1 0.123407 0.768122 -0.069942 11.00000 0.02801 0.02146 = 0.01703 -0.00754 -0.01320 0.00915 AFIX 23 H11A 2 0.114118 0.819724 -0.035931 11.00000 -1.20000 H11B 2 0.061868 0.720497 -0.062291 11.00000 -1.20000 AFIX 0 C12 1 0.118921 0.793060 -0.154832 11.00000 0.03562 0.02390 = 0.01957 -0.00644 -0.01903 0.01205 AFIX 23 H12A 2 0.177267 0.844236 -0.157160 11.00000 -1.20000 H12B 2 0.030491 0.813034 -0.176401 11.00000 -1.20000 AFIX 0 C13 1 0.158125 0.715541 -0.209976 11.00000 0.02970 0.02501 = 0.02022 -0.00392 -0.01757 0.00631 AFIX 23 H13A 2 0.097222 0.665951 -0.207292 11.00000 -1.20000 H13B 2 0.139737 0.738559 -0.264135 11.00000 -1.20000 AFIX 0 C14 1 0.287492 0.675913 -0.199767 11.00000 0.02574 0.02180 = 0.01609 -0.00534 -0.00844 0.00242 AFIX 23 H14A 2 0.354373 0.719103 -0.208762 11.00000 -1.20000 H14B 2 0.291098 0.622413 -0.232552 11.00000 -1.20000 AFIX 0 C15 1 0.293988 0.653713 -0.114443 11.00000 0.02360 0.01664 = 0.01806 -0.00318 -0.01142 0.00295 AFIX 23 H15A 2 0.381922 0.632677 -0.092980 11.00000 -1.20000 H15B 2 0.233471 0.604423 -0.109755 11.00000 -1.20000 AFIX 0 C16 1 0.174507 0.654433 0.096860 11.00000 0.01840 0.01613 = 0.01583 -0.00039 -0.00848 0.00019 AFIX 13 H16 2 0.230120 0.646071 0.149039 11.00000 -1.20000 AFIX 0 C17 1 0.168510 0.560405 0.062681 11.00000 0.02271 0.01397 = 0.02392 -0.00203 -0.01165 -0.00175 AFIX 23 H17A 2 0.256182 0.537464 0.061347 11.00000 -1.20000 H17B 2 0.118698 0.559854 0.008945 11.00000 -1.20000 AFIX 0 C18 1 0.094291 0.498350 0.123185 11.00000 0.02677 0.01655 = 0.02563 0.00121 -0.01241 -0.00066 AFIX 23 H18A 2 0.074904 0.439914 0.097619 11.00000 -1.20000 H18B 2 0.158138 0.487432 0.171030 11.00000 -1.20000 AFIX 0 C19 1 -0.041463 0.533584 0.152139 11.00000 0.02680 0.01792 = 0.02275 0.00516 -0.01084 -0.00395 AFIX 23 H19A 2 -0.113355 0.527774 0.107629 11.00000 -1.20000 H19B 2 -0.060197 0.493684 0.194149 11.00000 -1.20000 AFIX 0 C20 1 -0.038668 0.629473 0.182007 11.00000 0.02395 0.01969 = 0.02375 -0.00052 -0.00533 -0.00104 AFIX 23 H20A 2 0.008860 0.632940 0.236230 11.00000 -1.20000 H20B 2 -0.127327 0.651716 0.181176 11.00000 -1.20000 AFIX 0 C21 1 0.037100 0.690692 0.120905 11.00000 0.01974 0.01434 = 0.02562 -0.00044 -0.00702 0.00028 AFIX 23 H21A 2 -0.024665 0.699167 0.071740 11.00000 -1.20000 H21B 2 0.054097 0.750214 0.144807 11.00000 -1.20000 AFIX 0 C22 1 0.447144 0.678089 0.030994 11.00000 0.02052 0.01230 = 0.01921 -0.00043 -0.01302 0.00469 AFIX 13 H22 2 0.424992 0.621285 0.001853 11.00000 -1.20000 AFIX 0 C23 1 0.483975 0.654362 0.109922 11.00000 0.02310 0.02819 = 0.01694 0.00530 -0.00984 0.00080 AFIX 23 H23A 2 0.421095 0.614373 0.128694 11.00000 -1.20000 H23B 2 0.501218 0.706664 0.144755 11.00000 -1.20000 AFIX 0 C24 1 0.612680 0.603952 0.097713 11.00000 0.02447 0.02585 = 0.02954 0.00506 -0.01727 0.00592 AFIX 23 H24A 2 0.587222 0.548085 0.069047 11.00000 -1.20000 H24B 2 0.659900 0.587120 0.149908 11.00000 -1.20000 AFIX 0 C25 1 0.717714 0.658767 0.049484 11.00000 0.01811 0.03245 = 0.02782 0.00386 -0.01359 0.00724 AFIX 23 H25A 2 0.744686 0.713412 0.079671 11.00000 -1.20000 H25B 2 0.795274 0.620879 0.052659 11.00000 -1.20000 AFIX 0 C26 1 0.682272 0.684292 -0.029000 11.00000 0.01855 0.02880 = 0.02562 0.00645 -0.00830 0.00321 AFIX 23 H26A 2 0.666484 0.632716 -0.064781 11.00000 -1.20000 H26B 2 0.745549 0.725056 -0.046413 11.00000 -1.20000 AFIX 0 C27 1 0.552539 0.733659 -0.017962 11.00000 0.01704 0.02205 = 0.02063 0.00056 -0.01232 0.00106 AFIX 23 H27A 2 0.505448 0.749329 -0.070488 11.00000 -1.20000 H27B 2 0.576540 0.790147 0.010041 11.00000 -1.20000 AFIX 0 N1 3 0.158125 0.990165 0.144412 11.00000 0.02437 0.01442 = 0.02233 -0.00223 -0.01083 -0.00042 P1 4 0.288190 0.733465 0.038947 11.00000 0.01688 0.01145 = 0.01528 -0.00082 -0.00898 0.00087 PD1 5 0.256339 0.867122 0.099637 11.00000 0.01932 0.01066 = 0.01389 -0.00079 -0.00789 -0.00004 I1 6 0.262681 0.805371 0.245092 11.00000 0.04499 0.01879 = 0.01674 -0.00004 -0.01321 0.00194 HKLF 4 Covalent radii and connectivity table for 02SRC221 in P2(1)/n C 0.770 H 0.320 N 0.700 P 1.100 PD 1.380 I 1.330 C1 - N1 C2 - N1 C3 - N1 C4 C4 - C9 C5 C3 C5 - C4 C6 C6 - C7 C5 C7 - C6 C8 C8 - C7 C9 C9 - C4 C8 Pd1 C10 - C11 C15 P1 C11 - C10 C12 C12 - C11 C13 C13 - C14 C12 C14 - C13 C15 C15 - C14 C10 C16 - C17 C21 P1 C17 - C16 C18 C18 - C19 C17 C19 - C20 C18 C20 - C19 C21 C21 - C16 C20 C22 - C23 C27 P1 C23 - C22 C24 C24 - C23 C25 C25 - C26 C24 C26 - C25 C27 C27 - C26 C22 N1 - C3 C2 C1 Pd1 P1 - C10 C22 C16 Pd1 Pd1 - C9 N1 P1 I1 I1 - Pd1 39037 Reflections read, of which 3422 rejected -13 =< h =< 13, -19 =< k =< 19, -21 =< l =< 22, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -2 2 1 344.38 3.75 12 29.27 0 2 1 149.41 2.67 6 42.29 -4 5 2 198.35 1.92 9 17.04 -3 12 10 48.95 1.04 5 23.85 4 Inconsistent equivalents 5499 Unique reflections, of which 0 suppressed R(int) = 0.0924 R(sigma) = 0.0513 Friedel opposites merged Maximum memory for data reduction = 3669 / 55940 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 = 4585 / 355017 wR2 = 0.1027 before cycle 1 for 5499 data and 283 / 283 parameters GooF = S = 1.007; Restrained GooF = 1.007 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0564 * P )^2 + 4.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09810 0.00018 0.344 OSF 2 0.00102 0.00021 0.323 EXTI Mean shift/esd = 0.110 Maximum = -0.609 for z C11 Max. shift = 0.007 A for H1A Max. dU = 0.000 for C17 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4585 / 355017 wR2 = 0.1026 before cycle 2 for 5499 data and 283 / 283 parameters GooF = S = 1.008; Restrained GooF = 1.008 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0564 * P )^2 + 4.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09808 0.00018 -0.119 OSF 2 0.00104 0.00021 0.095 EXTI Mean shift/esd = 0.037 Maximum = -0.193 for z C11 Max. shift = 0.002 A for H2A Max. dU = 0.000 for C17 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4585 / 355017 wR2 = 0.1026 before cycle 3 for 5499 data and 283 / 283 parameters GooF = S = 1.008; Restrained GooF = 1.008 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0564 * P )^2 + 4.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09808 0.00018 -0.004 OSF 2 0.00104 0.00021 -0.003 EXTI Mean shift/esd = 0.002 Maximum = -0.009 for U11 C16 Max. shift = 0.000 A for H2B Max. dU = 0.000 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4585 / 355017 wR2 = 0.1026 before cycle 4 for 5499 data and 283 / 283 parameters GooF = S = 1.008; Restrained GooF = 1.008 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0564 * P )^2 + 4.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09808 0.00018 0.000 OSF 2 0.00104 0.00021 -0.003 EXTI Mean shift/esd = 0.000 Maximum = 0.003 for U33 C15 Max. shift = 0.000 A for H2B Max. dU = 0.000 for C15 Largest correlation matrix elements 0.579 U33 I1 / OSF 0.554 EXTI / OSF 0.522 U22 I1 / OSF 0.572 U11 Pd1 / OSF 0.539 U11 I1 / OSF 0.562 U33 Pd1 / OSF 0.532 U22 Pd1 / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.0065 1.0335 0.2147 137 0.980 0.000 C1 N1 H1A H1B 0.1020 0.9624 0.2624 137 0.980 0.000 C1 N1 H1A H1C -0.0087 0.9301 0.1933 137 0.980 0.000 C1 N1 H1A H2A 0.3011 1.0652 0.1250 137 0.980 0.000 C2 N1 H2A H2B 0.3017 1.0438 0.2154 137 0.980 0.000 C2 N1 H2A H2C 0.2013 1.1142 0.1707 137 0.980 0.000 C2 N1 H2A H3A 0.0751 1.0820 0.0808 23 0.990 0.000 C3 N1 C4 H3B 0.0236 0.9838 0.0576 23 0.990 0.000 C3 N1 C4 H5 0.1683 1.1311 -0.0544 43 0.950 0.000 C5 C4 C6 H6 0.3250 1.1227 -0.1482 43 0.950 0.000 C6 C7 C5 H7 0.4698 1.0020 -0.1505 43 0.950 0.000 C7 C6 C8 H8 0.4446 0.8873 -0.0574 43 0.950 0.000 C8 C7 C9 H10 0.3101 0.7876 -0.0784 13 1.000 0.000 C10 C11 C15 P1 H11A 0.1140 0.8198 -0.0361 23 0.990 0.000 C11 C10 C12 H11B 0.0617 0.7206 -0.0625 23 0.990 0.000 C11 C10 C12 H12A 0.1773 0.8443 -0.1571 23 0.990 0.000 C12 C11 C13 H12B 0.0305 0.8131 -0.1764 23 0.990 0.000 C12 C11 C13 H13A 0.0972 0.6660 -0.2075 23 0.990 0.000 C13 C14 C12 H13B 0.1399 0.7386 -0.2642 23 0.990 0.000 C13 C14 C12 H14A 0.3543 0.7191 -0.2088 23 0.990 0.000 C14 C13 C15 H14B 0.2910 0.6224 -0.2326 23 0.990 0.000 C14 C13 C15 H15A 0.3818 0.6327 -0.0931 23 0.990 0.000 C15 C14 C10 H15B 0.2333 0.6045 -0.1099 23 0.990 0.000 C15 C14 C10 H16 0.2302 0.6460 0.1491 13 1.000 0.000 C16 C17 C21 P1 H17A 0.2561 0.5374 0.0613 23 0.990 0.000 C17 C16 C18 H17B 0.1187 0.5599 0.0089 23 0.990 0.000 C17 C16 C18 H18A 0.0747 0.4399 0.0976 23 0.990 0.000 C18 C19 C17 H18B 0.1580 0.4874 0.1710 23 0.990 0.000 C18 C19 C17 H19A -0.1135 0.5277 0.1077 23 0.990 0.000 C19 C20 C18 H19B -0.0602 0.4937 0.1942 23 0.990 0.000 C19 C20 C18 H20A 0.0087 0.6329 0.2363 23 0.990 0.000 C20 C19 C21 H20B -0.1274 0.6517 0.1812 23 0.990 0.000 C20 C19 C21 H21A -0.0246 0.6991 0.0718 23 0.990 0.000 C21 C16 C20 H21B 0.0541 0.7502 0.1448 23 0.990 0.000 C21 C16 C20 H22 0.4250 0.6213 0.0020 13 1.000 0.000 C22 C23 C27 P1 H23A 0.4210 0.6143 0.1286 23 0.990 0.000 C23 C22 C24 H23B 0.5011 0.7066 0.1447 23 0.990 0.000 C23 C22 C24 H24A 0.5872 0.5480 0.0691 23 0.990 0.000 C24 C23 C25 H24B 0.6598 0.5871 0.1499 23 0.990 0.000 C24 C23 C25 H25A 0.7449 0.7134 0.0796 23 0.990 0.000 C25 C26 C24 H25B 0.7953 0.6208 0.0525 23 0.990 0.000 C25 C26 C24 H26A 0.6663 0.6327 -0.0647 23 0.990 0.000 C26 C25 C27 H26B 0.7454 0.7250 -0.0464 23 0.990 0.000 C26 C25 C27 H27A 0.5054 0.7491 -0.0706 23 0.990 0.000 C27 C26 C22 H27B 0.5765 0.7902 0.0099 23 0.990 0.000 C27 C26 C22 02SRC221 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.05301 0.97766 0.21096 1.00000 0.03434 0.03041 0.03342 -0.00350 0.00242 0.00929 0.03311 0.00875 0.00046 0.00032 0.00028 0.00000 0.00236 0.00247 0.00252 0.00199 0.00209 0.00195 0.00109 H1A 0.00646 1.03350 0.21468 1.00000 0.04967 0.00000 0.00000 H1B 0.10204 0.96236 0.26237 1.00000 0.04967 0.00000 0.00000 H1C -0.00867 0.93009 0.19326 1.00000 0.04967 0.00000 0.00000 C2 0.24722 1.05843 0.16547 1.00000 0.03496 0.01598 0.03286 -0.00651 -0.01651 -0.00009 0.03053 0.00693 0.00044 0.00026 0.00028 0.00000 0.00231 0.00205 0.00247 0.00173 0.00202 0.00169 0.00111 H2A 0.30108 1.06516 0.12504 1.00000 0.04580 0.00000 0.00000 H2B 0.30171 1.04383 0.21539 1.00000 0.04580 0.00000 0.00000 H2C 0.20132 1.11420 0.17073 1.00000 0.04580 0.00000 0.00000 C3 0.10201 1.01949 0.07561 1.00000 0.02557 0.02124 0.02561 0.00028 -0.01533 0.00627 0.02643 0.00705 0.00039 0.00028 0.00025 0.00000 0.00205 0.00208 0.00217 0.00169 0.00182 0.00162 0.00101 H3A 0.07511 1.08199 0.08079 1.00000 0.03172 0.00000 0.00000 H3B 0.02359 0.98382 0.05764 1.00000 0.03172 0.00000 0.00000 C4 0.20345 1.01374 0.00511 1.00000 0.02081 0.01785 0.02128 -0.00159 -0.01343 -0.00071 0.02196 0.00635 0.00037 0.00026 0.00024 0.00000 0.00187 0.00190 0.00195 0.00157 0.00164 0.00150 0.00092 C5 0.22119 1.07958 -0.05181 1.00000 0.03017 0.02036 0.03081 0.00139 -0.01914 0.00144 0.02995 0.00704 0.00041 0.00029 0.00026 0.00000 0.00218 0.00202 0.00233 0.00180 0.00197 0.00172 0.00109 H5 0.16834 1.13105 -0.05442 1.00000 0.03594 0.00000 0.00000 C6 0.32379 1.07469 -0.11282 1.00000 0.04183 0.01973 0.02312 0.00638 -0.01726 -0.00368 0.03088 0.00724 0.00044 0.00029 0.00025 0.00000 0.00248 0.00197 0.00216 0.00175 0.00200 0.00186 0.00110 H6 0.32504 1.12273 -0.14822 1.00000 0.03706 0.00000 0.00000 C7 0.40879 1.00511 -0.11613 1.00000 0.03411 0.02577 0.01434 0.00258 -0.00529 -0.00841 0.02584 0.00693 0.00043 0.00028 0.00024 0.00000 0.00227 0.00216 0.00189 0.00167 0.00176 0.00181 0.00097 H7 0.46983 1.00200 -0.15050 1.00000 0.03101 0.00000 0.00000 C8 0.39080 0.93822 -0.05970 1.00000 0.02384 0.01480 0.01893 -0.00219 -0.01003 -0.00056 0.02078 0.00633 0.00038 0.00025 0.00023 0.00000 0.00193 0.00187 0.00197 0.00151 0.00165 0.00149 0.00091 H8 0.44462 0.88726 -0.05737 1.00000 0.02494 0.00000 0.00000 C9 0.28699 0.94046 0.00129 1.00000 0.02153 0.01154 0.01693 -0.00048 -0.01406 -0.00166 0.01869 0.00601 0.00036 0.00023 0.00023 0.00000 0.00182 0.00175 0.00188 0.00141 0.00159 0.00141 0.00089 C10 0.25955 0.73602 -0.06338 1.00000 0.01855 0.01438 0.01521 -0.00102 -0.00980 0.00120 0.01752 0.00617 0.00035 0.00025 0.00022 0.00000 0.00176 0.00175 0.00180 0.00147 0.00153 0.00143 0.00084 H10 0.31006 0.78760 -0.07840 1.00000 0.02103 0.00000 0.00000 C11 0.12333 0.76819 -0.07012 1.00000 0.02794 0.02152 0.01677 -0.00755 -0.01350 0.00932 0.02409 0.00678 0.00039 0.00028 0.00023 0.00000 0.00206 0.00199 0.00194 0.00162 0.00169 0.00166 0.00097 H11A 0.11399 0.81978 -0.03611 1.00000 0.02891 0.00000 0.00000 H11B 0.06173 0.72058 -0.06253 1.00000 0.02891 0.00000 0.00000 C12 0.11890 0.79313 -0.15481 1.00000 0.03534 0.02350 0.02037 -0.00649 -0.01885 0.01208 0.02915 0.00723 0.00043 0.00028 0.00024 0.00000 0.00231 0.00211 0.00212 0.00169 0.00188 0.00177 0.00108 H12A 0.17726 0.84431 -0.15710 1.00000 0.03498 0.00000 0.00000 H12B 0.03048 0.81311 -0.17639 1.00000 0.03498 0.00000 0.00000 C13 0.15818 0.71555 -0.21006 1.00000 0.03017 0.02496 0.01931 -0.00436 -0.01802 0.00672 0.02740 0.00699 0.00041 0.00029 0.00024 0.00000 0.00214 0.00210 0.00205 0.00167 0.00180 0.00176 0.00103 H13A 0.09722 0.66598 -0.20745 1.00000 0.03289 0.00000 0.00000 H13B 0.13990 0.73863 -0.26420 1.00000 0.03289 0.00000 0.00000 C14 0.28739 0.67591 -0.19982 1.00000 0.02528 0.02158 0.01671 -0.00536 -0.00824 0.00244 0.02257 0.00680 0.00039 0.00028 0.00023 0.00000 0.00201 0.00201 0.00198 0.00159 0.00170 0.00163 0.00093 H14A 0.35431 0.71907 -0.20881 1.00000 0.02708 0.00000 0.00000 H14B 0.29097 0.62240 -0.23260 1.00000 0.02708 0.00000 0.00000 C15 0.29386 0.65374 -0.11457 1.00000 0.02375 0.01642 0.01789 -0.00346 -0.01201 0.00304 0.02117 0.00651 0.00038 0.00026 0.00023 0.00000 0.00193 0.00185 0.00193 0.00156 0.00164 0.00157 0.00091 H15A 0.38179 0.63267 -0.09313 1.00000 0.02540 0.00000 0.00000 H15B 0.23332 0.60446 -0.10990 1.00000 0.02540 0.00000 0.00000 C16 0.17461 0.65438 0.09694 1.00000 0.01832 0.01598 0.01620 -0.00012 -0.00837 0.00035 0.01815 0.00635 0.00036 0.00025 0.00022 0.00000 0.00178 0.00181 0.00184 0.00149 0.00154 0.00146 0.00085 H16 0.23024 0.64599 0.14911 1.00000 0.02178 0.00000 0.00000 C17 0.16849 0.56036 0.06265 1.00000 0.02271 0.01407 0.02339 -0.00211 -0.01126 -0.00169 0.02183 0.00647 0.00038 0.00024 0.00024 0.00000 0.00188 0.00188 0.00207 0.00153 0.00168 0.00149 0.00092 H17A 0.25613 0.53736 0.06130 1.00000 0.02619 0.00000 0.00000 H17B 0.11867 0.55989 0.00892 1.00000 0.02619 0.00000 0.00000 C18 0.09416 0.49834 0.12315 1.00000 0.02696 0.01634 0.02517 0.00149 -0.01264 -0.00050 0.02482 0.00687 0.00039 0.00027 0.00024 0.00000 0.00204 0.00189 0.00210 0.00167 0.00175 0.00161 0.00096 H18A 0.07471 0.43992 0.09756 1.00000 0.02978 0.00000 0.00000 H18B 0.15801 0.48737 0.17098 1.00000 0.02978 0.00000 0.00000 C19 -0.04153 0.53356 0.15216 1.00000 0.02685 0.01770 0.02254 0.00526 -0.01114 -0.00392 0.02415 0.00687 0.00039 0.00027 0.00024 0.00000 0.00201 0.00189 0.00208 0.00164 0.00175 0.00163 0.00095 H19A -0.11346 0.52775 0.10767 1.00000 0.02898 0.00000 0.00000 H19B -0.06020 0.49365 0.19418 1.00000 0.02898 0.00000 0.00000 C20 -0.03876 0.62948 0.18205 1.00000 0.02384 0.01990 0.02309 -0.00054 -0.00569 -0.00097 0.02340 0.00689 0.00039 0.00026 0.00025 0.00000 0.00198 0.00199 0.00213 0.00163 0.00177 0.00159 0.00094 H20A 0.00871 0.63295 0.23628 1.00000 0.02808 0.00000 0.00000 H20B -0.12743 0.65174 0.18118 1.00000 0.02808 0.00000 0.00000 C21 0.03712 0.69065 0.12095 1.00000 0.01972 0.01388 0.02666 -0.00045 -0.00655 0.00049 0.02131 0.00682 0.00037 0.00025 0.00025 0.00000 0.00188 0.00183 0.00217 0.00156 0.00172 0.00146 0.00092 H21A -0.02461 0.69910 0.07177 1.00000 0.02557 0.00000 0.00000 H21B 0.05409 0.75018 0.14483 1.00000 0.02557 0.00000 0.00000 C22 0.44718 0.67807 0.03110 1.00000 0.02030 0.01227 0.01949 -0.00035 -0.01292 0.00466 0.01926 0.00641 0.00036 0.00024 0.00023 0.00000 0.00185 0.00172 0.00193 0.00148 0.00161 0.00145 0.00088 H22 0.42499 0.62127 0.00197 1.00000 0.02311 0.00000 0.00000 C23 0.48386 0.65433 0.10985 1.00000 0.02286 0.02775 0.01770 0.00510 -0.01005 0.00066 0.02434 0.00718 0.00038 0.00029 0.00023 0.00000 0.00200 0.00216 0.00201 0.00169 0.00168 0.00169 0.00095 H23A 0.42095 0.61432 0.12857 1.00000 0.02921 0.00000 0.00000 H23B 0.50106 0.70661 0.14472 1.00000 0.02921 0.00000 0.00000 C24 0.61263 0.60393 0.09769 1.00000 0.02456 0.02555 0.02948 0.00511 -0.01690 0.00606 0.02904 0.00758 0.00039 0.00030 0.00026 0.00000 0.00203 0.00213 0.00228 0.00182 0.00184 0.00172 0.00105 H24A 0.58721 0.54803 0.06906 1.00000 0.03484 0.00000 0.00000 H24B 0.65984 0.58714 0.14990 1.00000 0.03484 0.00000 0.00000 C25 0.71780 0.65877 0.04938 1.00000 0.01766 0.03287 0.02779 0.00385 -0.01340 0.00702 0.02812 0.00760 0.00038 0.00031 0.00025 0.00000 0.00189 0.00231 0.00227 0.00191 0.00177 0.00174 0.00102 H25A 0.74490 0.71339 0.07957 1.00000 0.03374 0.00000 0.00000 H25B 0.79529 0.62084 0.05246 1.00000 0.03374 0.00000 0.00000 C26 0.68214 0.68427 -0.02894 1.00000 0.01843 0.02827 0.02631 0.00628 -0.00814 0.00345 0.02573 0.00752 0.00039 0.00029 0.00026 0.00000 0.00190 0.00223 0.00223 0.00178 0.00176 0.00166 0.00098 H26A 0.66634 0.63268 -0.06471 1.00000 0.03088 0.00000 0.00000 H26B 0.74537 0.72503 -0.04641 1.00000 0.03088 0.00000 0.00000 C27 0.55253 0.73360 -0.01802 1.00000 0.01676 0.02177 0.02166 0.00047 -0.01209 0.00124 0.02185 0.00661 0.00035 0.00027 0.00023 0.00000 0.00176 0.00196 0.00199 0.00164 0.00160 0.00153 0.00091 H27A 0.50540 0.74912 -0.07057 1.00000 0.02622 0.00000 0.00000 H27B 0.57648 0.79017 0.00987 1.00000 0.02622 0.00000 0.00000 N1 0.15819 0.99014 0.14442 1.00000 0.02453 0.01436 0.02217 -0.00223 -0.01057 -0.00039 0.02205 0.00546 0.00032 0.00021 0.00020 0.00000 0.00167 0.00157 0.00173 0.00134 0.00144 0.00132 0.00078 P1 0.28818 0.73346 0.03893 1.00000 0.01674 0.01137 0.01529 -0.00082 -0.00899 0.00088 0.01583 0.00154 0.00009 0.00006 0.00006 0.00000 0.00044 0.00044 0.00048 0.00036 0.00039 0.00035 0.00023 Pd1 0.25634 0.86712 0.09964 1.00000 0.01924 0.01061 0.01383 -0.00081 -0.00795 -0.00007 0.01582 0.00046 0.00003 0.00002 0.00002 0.00000 0.00017 0.00016 0.00017 0.00010 0.00012 0.00010 0.00012 I1 0.26268 0.80537 0.24509 1.00000 0.04492 0.01873 0.01665 -0.00003 -0.01330 0.00192 0.02893 0.00045 0.00003 0.00002 0.00001 0.00000 0.00020 0.00016 0.00017 0.00010 0.00013 0.00011 0.00012 Final Structure Factor Calculation for 02SRC221 in P2(1)/n Total number of l.s. parameters = 283 Maximum vector length = 511 Memory required = 4302 / 25039 wR2 = 0.1026 before cycle 5 for 5499 data and 0 / 283 parameters GooF = S = 1.008; Restrained GooF = 1.008 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0564 * P )^2 + 4.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0385 for 4549 Fo > 4sig(Fo) and 0.0513 for all 5499 data wR2 = 0.1026, GooF = S = 1.008, Restrained GooF = 1.008 for all data Occupancy sum of asymmetric unit = 31.00 for non-hydrogen and 45.00 for hydrogen atoms Principal mean square atomic displacements U 0.0452 0.0316 0.0226 C1 0.0613 0.0196 0.0107 C2 0.0500 0.0219 0.0074 C3 0.0416 0.0180 0.0063 C4 0.0598 0.0207 0.0094 C5 0.0630 0.0197 0.0100 C6 0.0445 0.0211 0.0119 C7 0.0381 0.0154 0.0089 C8 0.0403 0.0117 0.0040 C9 0.0324 0.0142 0.0059 C10 0.0501 0.0156 0.0066 C11 0.0630 0.0181 0.0064 C12 0.0547 0.0224 0.0051 C13 0.0379 0.0204 0.0094 C14 0.0408 0.0155 0.0072 C15 0.0309 0.0160 0.0075 C16 0.0413 0.0153 0.0089 C17 0.0467 0.0164 0.0114 C18 0.0451 0.0162 0.0111 C19 0.0351 0.0201 0.0150 C20 0.0364 0.0139 0.0136 C21 0.0401 0.0128 0.0049 C22 0.0378 0.0276 0.0077 C23 0.0531 0.0283 0.0058 C24 0.0444 0.0346 0.0053 C25 0.0385 0.0291 0.0096 C26 0.0379 0.0218 0.0058 C27 0.0410 0.0150 0.0101 N1 0.0302 0.0113 0.0060 P1 0.0298 0.0107 0.0069 Pd1 0.0580 0.0187 0.0101 I1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.031 0.046 0.063 0.082 0.104 0.130 0.165 0.224 1.000 Number in group 553. 568. 544. 562. 543. 541. 542. 544. 550. 552. GooF 0.890 0.968 1.091 1.059 1.102 0.935 1.057 1.006 0.915 1.030 K 1.479 0.931 0.964 0.965 0.978 0.977 1.001 1.018 1.035 1.015 Resolution(A) 0.77 0.82 0.86 0.90 0.95 1.01 1.08 1.19 1.36 1.69 inf Number in group 560. 562. 534. 562. 534. 549. 551. 543. 553. 551. GooF 0.916 0.871 0.909 0.939 0.923 0.925 0.914 0.900 1.186 1.443 K 0.964 1.020 1.030 1.035 1.043 1.042 1.051 1.042 1.021 0.979 R1 0.082 0.073 0.077 0.068 0.061 0.047 0.040 0.034 0.035 0.037 Recommended weighting scheme: WGHT 0.0512 3.7701 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 0 2 3409.11 5213.95 5.72 0.159 2.37 2 1 7 5124.02 3666.65 5.06 0.134 2.06 4 2 2 1998.68 2896.64 5.01 0.119 2.26 3 1 9 6645.17 4851.85 4.95 0.154 1.55 6 2 2 574.31 973.59 4.92 0.069 1.61 5 2 3 731.11 1176.43 4.83 0.076 1.80 4 3 2 467.38 868.38 4.82 0.065 2.15 3 5 7 1585.03 1068.27 4.76 0.072 1.58 -5 1 5 220.64 539.08 4.67 0.051 1.91 4 2 9 251.57 43.61 4.67 0.015 1.40 4 3 4 3477.52 2546.63 4.37 0.111 1.91 3 1 11 3940.27 3008.21 3.99 0.121 1.33 2 3 1 1028.60 698.57 3.98 0.058 3.45 4 1 3 1021.33 702.83 3.98 0.059 2.20 -3 5 1 531.75 863.08 3.94 0.065 2.28 -5 1 6 400.53 669.48 3.80 0.057 1.82 2 2 4 3514.67 4578.22 3.80 0.149 2.83 3 1 10 4371.64 3410.48 3.79 0.129 1.43 4 4 5 2311.58 3066.04 3.78 0.122 1.71 6 4 5 1197.17 1641.35 3.75 0.089 1.35 3 0 5 14043.20 17898.63 3.71 0.295 2.25 -3 5 2 3814.44 2908.67 3.71 0.119 2.26 3 1 7 3206.38 2482.78 3.62 0.110 1.84 -3 2 4 1435.60 1951.62 3.60 0.098 2.74 3 5 6 365.74 180.79 3.58 0.030 1.69 3 0 3 1372.11 1002.39 3.56 0.070 2.76 6 3 0 220.54 423.70 3.56 0.045 1.64 -4 4 8 283.31 514.35 3.54 0.050 1.63 -2 6 6 3485.74 4447.07 3.42 0.147 1.84 -10 8 6 -111.24 272.39 3.40 0.036 0.91 -5 0 9 342.09 600.90 3.39 0.054 1.54 2 8 6 164.25 23.73 3.37 0.011 1.46 1 3 10 1808.22 1375.11 3.31 0.082 1.56 5 5 14 63.56 226.55 3.27 0.033 0.93 8 7 13 184.72 537.85 3.25 0.051 0.79 2 1 0 847.10 559.03 3.20 0.052 4.91 2 1 2 2998.94 3761.71 3.20 0.135 3.99 1 10 14 550.13 844.41 3.14 0.064 0.93 5 1 3 297.03 130.61 3.12 0.025 1.84 2 3 4 10945.79 9019.03 3.10 0.210 2.61 -5 4 5 997.74 1345.04 3.06 0.081 1.71 1 1 4 5255.73 4304.03 3.05 0.145 3.63 4 5 4 437.81 270.15 3.02 0.036 1.70 4 16 3 600.27 250.44 3.01 0.035 0.87 -3 0 19 10207.84 6928.50 3.00 0.184 0.91 5 6 11 757.45 1042.18 3.00 0.071 1.05 9 5 2 6255.91 5109.02 2.98 0.158 1.05 0 8 5 3427.30 2756.07 2.97 0.116 1.65 2 1 3 3137.63 2544.26 2.97 0.111 3.46 -3 2 5 15532.53 18990.05 2.97 0.304 2.52 Bond lengths and angles C1 - Distance Angles N1 1.7418 (0.0066) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - N1 H1A H1B C2 - Distance Angles N1 1.3969 (0.0050) H2A 0.9800 109.47 H2B 0.9800 109.47 109.47 H2C 0.9800 109.47 109.47 109.47 C2 - N1 H2A H2B C3 - Distance Angles N1 1.3165 (0.0049) C4 1.7588 (0.0069) 112.50 (0.33) H3A 0.9900 109.10 109.10 H3B 0.9900 109.10 109.10 107.84 C3 - N1 C4 H3A C4 - Distance Angles C9 1.4188 (0.0055) C5 1.4336 (0.0063) 110.46 (0.40) C3 1.7588 (0.0069) 121.73 (0.34) 127.72 (0.35) C4 - C9 C5 C5 - Distance Angles C4 1.4336 (0.0063) C6 1.6388 (0.0076) 126.33 (0.37) H5 0.9500 116.84 116.84 C5 - C4 C6 C6 - Distance Angles C7 1.3847 (0.0066) C5 1.6388 (0.0076) 124.26 (0.38) H6 0.9500 117.87 117.87 C6 - C7 C5 C7 - Distance Angles C6 1.3847 (0.0066) C8 1.4391 (0.0059) 109.81 (0.42) H7 0.9500 125.09 125.09 C7 - C6 C8 C8 - Distance Angles C7 1.4391 (0.0059) C9 1.6471 (0.0067) 127.03 (0.35) H8 0.9500 116.48 116.48 C8 - C7 C9 C9 - Distance Angles C4 1.4188 (0.0055) C8 1.6471 (0.0067) 122.07 (0.34) Pd1 2.1036 (0.0041) 100.78 (0.30) 136.20 (0.24) C9 - C4 C8 C10 - Distance Angles C11 1.5002 (0.0053) C15 1.6003 (0.0055) 120.61 (0.29) P1 1.7514 (0.0038) 94.82 (0.27) 122.03 (0.25) H10 1.0000 105.91 105.91 105.91 C10 - C11 C15 P1 C11 - Distance Angles C10 1.5002 (0.0053) C12 1.5108 (0.0061) 91.55 (0.34) H11A 0.9900 113.37 113.37 H11B 0.9900 113.37 113.37 110.69 C11 - C10 C12 H11A C12 - Distance Angles C11 1.5108 (0.0061) C13 1.6085 (0.0060) 115.60 (0.33) H12A 0.9900 108.38 108.38 H12B 0.9900 108.38 108.38 107.45 C12 - C11 C13 H12A C13 - Distance Angles C14 1.4690 (0.0056) C12 1.6085 (0.0060) 123.30 (0.31) H13A 0.9900 106.50 106.50 H13B 0.9900 106.50 106.50 106.51 C13 - C14 C12 H13A C14 - Distance Angles C13 1.4690 (0.0056) C15 1.5077 (0.0058) 95.46 (0.35) H14A 0.9900 112.65 112.65 H14B 0.9900 112.65 112.65 110.14 C14 - C13 C15 H14A C15 - Distance Angles C14 1.5077 (0.0058) C10 1.6003 (0.0055) 113.44 (0.32) H15A 0.9900 108.88 108.88 H15B 0.9900 108.88 108.88 107.72 C15 - C14 C10 H15A C16 - Distance Angles C17 1.5311 (0.0052) C21 1.6658 (0.0058) 114.75 (0.31) P1 2.0664 (0.0043) 109.34 (0.29) 122.27 (0.25) H16 1.0000 102.44 102.44 102.44 C16 - C17 C21 P1 C17 - Distance Angles C16 1.5311 (0.0052) C18 1.6930 (0.0063) 105.10 (0.34) H17A 0.9900 110.72 110.73 H17B 0.9900 110.73 110.73 108.82 C17 - C16 C18 H17A C18 - Distance Angles C19 1.6802 (0.0063) C17 1.6930 (0.0063) 121.29 (0.30) H18A 0.9900 107.01 107.01 H18B 0.9900 107.01 107.01 106.75 C18 - C19 C17 H18A C19 - Distance Angles C20 1.5314 (0.0057) C18 1.6802 (0.0063) 115.49 (0.33) H19A 0.9900 108.40 108.40 H19B 0.9900 108.40 108.41 107.46 C19 - C20 C18 H19A C20 - Distance Angles C19 1.5314 (0.0057) C21 1.7026 (0.0062) 106.34 (0.35) H20A 0.9900 110.46 110.46 H20B 0.9900 110.46 110.46 108.65 C20 - C19 C21 H20A C21 - Distance Angles C16 1.6658 (0.0058) C20 1.7026 (0.0062) 119.97 (0.29) H21A 0.9900 107.33 107.33 H21B 0.9900 107.33 107.33 106.91 C21 - C16 C20 H21A C22 - Distance Angles C23 1.4028 (0.0053) C27 1.7258 (0.0062) 120.74 (0.31) P1 1.8963 (0.0040) 98.19 (0.31) 118.24 (0.24) H22 1.0000 106.13 106.13 106.13 C22 - C23 C27 P1 C23 - Distance Angles C22 1.4028 (0.0053) C24 1.5991 (0.0061) 95.24 (0.35) H23A 0.9900 112.69 112.69 H23B 0.9900 112.69 112.69 110.17 C23 - C22 C24 H23A C24 - Distance Angles C23 1.5991 (0.0061) C25 1.7110 (0.0068) 118.10 (0.33) H24A 0.9900 107.78 107.78 H24B 0.9900 107.78 107.78 107.13 C24 - C23 C25 H24A C25 - Distance Angles C26 1.4017 (0.0059) C24 1.7110 (0.0068) 121.23 (0.33) H25A 0.9900 107.02 107.02 H25B 0.9900 107.02 107.02 106.75 C25 - C26 C24 H25A C26 - Distance Angles C25 1.4017 (0.0059) C27 1.5935 (0.0058) 96.07 (0.36) H26A 0.9900 112.54 112.54 H26B 0.9900 112.54 112.54 110.06 C26 - C25 C27 H26A C27 - Distance Angles C26 1.5935 (0.0058) C22 1.7258 (0.0062) 118.02 (0.31) H27A 0.9900 107.80 107.80 H27B 0.9900 107.80 107.80 107.14 C27 - C26 C22 H27A N1 - Distance Angles C3 1.3165 (0.0049) C2 1.3969 (0.0050) 99.76 (0.34) C1 1.7418 (0.0066) 113.56 (0.33) 112.35 (0.35) Pd1 2.3171 (0.0034) 96.92 (0.27) 110.88 (0.28) 120.48 (0.23) N1 - C3 C2 C1 P1 - Distance Angles C10 1.7514 (0.0038) C22 1.8963 (0.0040) 86.50 (0.18) C16 2.0664 (0.0043) 119.54 (0.17) 111.97 (0.17) Pd1 2.3203 (0.0010) 115.38 (0.13) 127.63 (0.12) 97.84 (0.12) P1 - C10 C22 C16 Pd1 - Distance Angles C9 2.1036 (0.0041) N1 2.3171 (0.0034) 89.59 (0.14) P1 2.3203 (0.0010) 91.78 (0.11) 162.03 (0.08) I1 2.6814 (0.0004) 164.52 (0.09) 84.34 (0.09) 98.38 (0.03) Pd1 - C9 N1 P1 I1 - Distance Angles Pd1 2.6814 (0.0004) I1 - FMAP and GRID set by program FMAP 2 3 22 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.0506 for 5499 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.10 at 0.2573 0.8702 0.1009 [ 0.05 A from PD1 ] Deepest hole -1.26 at 0.1971 0.8633 0.0662 [ 0.78 A from PD1 ] Mean = 0.00, Rms deviation from mean = 0.14 e/A^3, Highest memory used = 4221 / 27003 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2467 0.4419 0.2498 1.00000 0.05 0.91 1.67 H18B 1.67 H1B 1.75 H2B 2.06 I1 Q2 1 0.2560 0.7438 0.1010 1.00000 0.05 0.86 1.19 P1 1.59 C16 1.74 H16 1.85 PD1 Q3 1 0.7308 0.6237 -0.0972 1.00000 0.05 0.82 0.96 H26A 1.64 C26 1.75 H26B 2.26 H18A Q4 1 0.7258 0.6987 0.0549 1.00000 0.05 0.81 0.49 H25A 0.61 C25 1.39 H25B 1.47 C26 Q5 1 0.2482 0.8067 -0.0457 1.00000 0.05 0.77 0.98 H10 1.12 C10 1.43 C11 1.46 H11A Q6 1 0.2626 0.5226 0.1019 1.00000 0.05 0.65 0.73 H17A 1.24 C17 1.84 H18B 1.91 C18 Q7 1 0.3149 0.8776 0.0554 1.00000 0.05 0.62 1.08 PD1 1.33 C9 2.20 P1 2.45 C4 Q8 1 -0.1072 0.4921 0.2062 1.00000 0.05 0.56 0.57 H19B 1.40 C19 1.78 H19A 2.25 C20 Q9 1 0.2655 0.5320 0.0305 1.00000 0.05 0.56 0.57 H17A 1.32 C17 1.58 H17B 2.27 H22 Q10 1 0.1759 0.8969 0.1449 1.00000 0.05 0.53 1.33 PD1 1.41 N1 2.23 C1 2.27 C3 Shortest distances between peaks (including symmetry equivalents) 6 9 1.25 1 10 1.99 5 7 2.07 3 6 2.20 2 7 2.29 7 10 2.33 2 10 2.61 3 9 2.61 2 5 2.70 1 6 2.87 1 3 2.88 3 4 2.88 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: 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. 0.82: 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 2.11: Structure factors and derivatives 3.02: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.23: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.27: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.11: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 11:45:47 Total elapsed time: 6.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++