+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 18:03:35 on 04-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL SHELXL INS file, from DIRDIF output for S92 CELL 0.71073 11.04250 15.40280 16.02740 90.0000 90.0000 90.0000 ZERR 4 0.0002 0.0003 0.0004 0.0000 0.0000 0.0000 LATT -1 SYMM 1/2+X , 1/2-Y , -Z SYMM -X , 1/2+Y , 1/2-Z SYMM 1/2-X , -Y , 1/2+Z SFAC C H N O F PD UNIT 96 96 8 16 24 8 V = 2726.03 F(000) = 1440.0 Mu = 1.39 mm-1 Cell Wt = 2925.01 Rho = 1.782 TEMP -123 SIZE .2 .15 .1 HTAB BOND $H OMIT 0 51 OMIT 9 1 11 OMIT 5 0 6 OMIT -8 8 8 OMIT 0 5 4 OMIT 3 2 18 OMIT 2 0 6 OMIT 4 0 0 OMIT 3 12 8 DFIX 1.33 .008 C2' f1' C2' f2' C2' f3' C2' f1" C2' f2" C2' f3" CONF O2 Pd1 Pd2 O1 CONF O2' Pd2 Pd1 O1' ISOR .008 F1' F2' ISOR .004 F3' L.S. 1 BOND FMAP 2 MPLA 4 O1' o2 C10 N1' Pd1 MPLA 4 O1 o2' C20 N1 Pd2 PLAN 10 WGHT 0.035200 EXTI 0.000932 FVAR 0.19412 PART 0 PD1 6 0.190898 0.052598 0.204123 11.00000 0.02613 0.02853 = 0.02357 0.00263 -0.00091 0.00223 PD2 6 0.071467 0.153013 0.075097 11.00000 0.02714 0.02493 = 0.02197 0.00409 0.00164 0.00050 N1' 3 0.324822 0.138180 0.228614 11.00000 0.03075 0.03076 = 0.02942 0.00053 -0.00234 0.00233 N1 3 0.193272 0.153982 -0.017411 11.00000 0.03071 0.02572 = 0.02256 0.00385 0.00032 0.00153 O1 4 -0.059795 0.166337 0.165631 11.00000 0.03071 0.03443 = 0.02852 0.00608 0.00230 0.00423 O2 4 0.045726 0.115680 0.276216 11.00000 0.03171 0.03524 = 0.03023 0.00619 0.00104 0.00514 O1' 4 0.066433 -0.042105 0.172929 11.00000 0.03457 0.02899 = 0.03217 0.00529 -0.00400 0.00146 O2' 4 0.004939 0.021612 0.052967 11.00000 0.03352 0.03084 = 0.03101 0.00202 -0.00495 -0.00150 F1 5 -0.247320 0.120360 0.275018 11.00000 0.03271 0.07429 = 0.07665 -0.00660 0.01773 -0.00851 F2 5 -0.188089 0.251895 0.285041 11.00000 0.07246 0.03866 = 0.06209 0.01003 0.02581 0.02255 F3 5 -0.135161 0.159069 0.375680 11.00000 0.06212 0.08406 = 0.02988 0.01304 0.01896 0.01980 PART 1 F1' 5 -0.069954 -0.137414 0.006909 10.63000 0.11751 0.07626 = 0.04845 -0.02203 0.02515 -0.05434 F2' 5 -0.187723 -0.093661 0.105190 10.63000 0.02404 0.05144 = 0.15456 0.00216 -0.00856 -0.01418 F3' 5 -0.053751 -0.183518 0.132510 10.63000 0.06953 0.02897 = 0.06611 0.02451 -0.02896 -0.02218 PART 2 F1" 5 -0.001278 -0.182929 0.070572 10.37000 0.10473 F2" 5 -0.149387 -0.133580 0.145991 10.37000 0.13202 F3" 5 -0.131369 -0.114527 0.016697 10.37000 0.06198 PART 0 C1 1 -0.043785 0.147326 0.241129 11.00000 0.03152 0.01969 = 0.02607 0.00547 0.00005 -0.00412 C2 1 -0.154155 0.170069 0.295563 11.00000 0.03522 0.03531 = 0.03144 0.00786 0.00891 0.00270 C1' 1 0.007822 -0.037113 0.105718 11.00000 0.03212 0.02473 = 0.03034 0.00609 0.00447 0.00125 C2' 1 -0.072841 -0.114517 0.086750 11.00000 0.04496 0.04038 = 0.03548 0.00073 -0.00085 -0.00842 C10 1 0.321116 -0.002364 0.139537 11.00000 0.03636 0.03496 = 0.02531 0.00454 -0.00468 0.00752 C11 1 0.429122 0.047040 0.138161 11.00000 0.03068 0.04198 = 0.03515 0.00032 0.00405 0.00351 C12 1 0.529016 0.020103 0.092354 11.00000 0.03792 0.06528 = 0.04446 -0.00719 0.00634 0.00239 AFIX 43 H12 2 0.600690 0.054211 0.091788 11.00000 0.06470 AFIX 0 C13 1 0.523839 -0.056317 0.047690 11.00000 0.04482 0.06126 = 0.03573 -0.00603 0.01217 0.01687 AFIX 43 H13 2 0.592019 -0.075167 0.016407 11.00000 0.05002 AFIX 0 C14 1 0.419006 -0.105403 0.048619 11.00000 0.05878 0.04097 = 0.03488 -0.00422 -0.00623 0.02025 AFIX 43 H14 2 0.415233 -0.157760 0.017397 11.00000 0.03072 AFIX 0 C15 1 0.318003 -0.078585 0.095298 11.00000 0.03647 0.03799 = 0.04569 -0.00125 -0.00536 0.00538 AFIX 43 H15 2 0.247071 -0.113473 0.096232 11.00000 0.09056 AFIX 0 C16 1 0.423484 0.124613 0.189137 11.00000 0.03231 0.03732 = 0.03222 0.00101 0.00172 -0.00382 AFIX 43 H16 2 0.489997 0.163524 0.193012 11.00000 0.02498 AFIX 0 C17 1 0.309303 0.212383 0.286379 11.00000 0.03356 0.03548 = 0.03834 -0.00549 0.00030 0.00135 AFIX 13 H17 2 0.226196 0.236116 0.276678 11.00000 0.02632 AFIX 0 C18 1 0.312315 0.179055 0.374580 11.00000 0.05734 0.04586 = 0.04093 -0.00878 0.00117 0.00413 AFIX 33 H18A 2 0.253293 0.131983 0.380799 11.00000 0.04955 H18B 2 0.292041 0.226295 0.413084 11.00000 0.05661 H18C 2 0.393575 0.157175 0.387317 11.00000 0.05292 AFIX 0 C19 1 0.399035 0.287077 0.270209 11.00000 0.04344 0.03952 = 0.07228 -0.00684 0.00181 -0.00324 AFIX 33 H19A 2 0.391005 0.306871 0.212362 11.00000 0.04277 H19B 2 0.481882 0.266570 0.279814 11.00000 0.03209 H19C 2 0.381307 0.335314 0.308165 11.00000 0.04246 AFIX 0 C20 1 0.132153 0.271577 0.089906 11.00000 0.02915 0.02436 = 0.02842 0.00673 -0.00149 0.00215 C21 1 0.224109 0.293897 0.032086 11.00000 0.03079 0.02721 = 0.03261 0.00491 0.00585 0.00359 C22 1 0.278044 0.374348 0.033537 11.00000 0.03686 0.03236 = 0.04819 0.00744 0.00514 -0.00260 AFIX 43 H22 2 0.337988 0.388597 -0.006714 11.00000 0.03285 AFIX 0 C23 1 0.245280 0.434594 0.093430 11.00000 0.04324 0.02824 = 0.04751 0.00065 0.00395 -0.00175 AFIX 43 H23 2 0.282145 0.490315 0.094228 11.00000 0.07677 AFIX 0 C24 1 0.157953 0.413035 0.152509 11.00000 0.03444 0.03102 = 0.04618 -0.00685 0.00209 0.00587 AFIX 43 H24 2 0.136085 0.453710 0.194442 11.00000 0.01717 AFIX 0 C25 1 0.101790 0.330587 0.150109 11.00000 0.02795 0.03688 = 0.03470 0.00155 0.00270 0.00069 AFIX 43 H25 2 0.042434 0.316059 0.190680 11.00000 0.01965 AFIX 0 C26 1 0.253935 0.224503 -0.024986 11.00000 0.03351 0.03378 = 0.03241 0.00258 0.00720 0.00755 AFIX 43 H26 2 0.315371 0.230817 -0.066033 11.00000 0.02993 AFIX 0 C27 1 0.210204 0.077438 -0.072186 11.00000 0.03479 0.03171 = 0.02608 -0.00408 0.00557 0.00592 AFIX 13 H27 2 0.200480 0.024155 -0.037174 11.00000 0.02636 AFIX 0 C28 1 0.334352 0.074047 -0.112303 11.00000 0.04030 0.03850 = 0.03643 -0.01120 0.00300 0.00298 AFIX 33 H28A 2 0.396677 0.074003 -0.068773 11.00000 0.04494 H28B 2 0.345250 0.124887 -0.148292 11.00000 0.08992 H28C 2 0.341431 0.021057 -0.145794 11.00000 0.04962 AFIX 0 C29 1 0.109073 0.077601 -0.137564 11.00000 0.03918 0.05068 = 0.03074 -0.00996 -0.00065 0.00900 AFIX 33 H29A 2 0.030293 0.079928 -0.109499 11.00000 0.01642 H29B 2 0.114123 0.024578 -0.171181 11.00000 0.12529 H29C 2 0.118085 0.128401 -0.173852 11.00000 0.05191 HKLF 4 Covalent radii and connectivity table for SHELXL INS file, from DIRDIF output for S92 C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 PD 1.380 Pd1 - C10 N1' O1' O2 Pd2 Pd2 - C20 N1 O1 O2' Pd1 N1' - C16 C17 Pd1 N1 - C26 C27 Pd2 O1 - C1 Pd2 O2 - C1 Pd1 O1' - C1' Pd1 O2' - C1' Pd2 F1 - C2 F2 - C2 F3 - C2 F1'_a - C2' F2'_a - C2' F3'_a - C2' F1"_b - C2' F2"_b - C2' F3"_b - C2' C1 - O2 O1 C2 C2 - F3 F1 F2 C1 C1' - O2' O1' C2' C2' - F3"_b F2"_b F3'_a F1'_a F2'_a F1"_b C1' C10 - C15 C11 Pd1 C11 - C12 C10 C16 C12 - C13 C11 C13 - C12 C14 C14 - C13 C15 C15 - C10 C14 C16 - N1' C11 C17 - N1' C18 C19 C18 - C17 C19 - C17 C20 - C25 C21 Pd2 C21 - C22 C20 C26 C22 - C21 C23 C23 - C22 C24 C24 - C23 C25 C25 - C20 C24 C26 - N1 C21 C27 - N1 C28 C29 C28 - C27 C29 - C27 h k l Fo^2 Sigma Why rejected 3 0 0 0.63 0.13 observed but should be systematically absent 17658 Reflections read, of which 1847 rejected -13 =< h =< 13, -16 =< k =< 18, -19 =< l =< 19, Max. 2-theta = 51.00 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 0 1 265.33 3.35 7 19.91 0 0 4 75.37 2.59 2 15.51 2 Inconsistent equivalents 5039 Unique reflections, of which 0 suppressed R(int) = 0.0557 R(sigma) = 0.0476 Friedel opposites not merged Maximum memory for data reduction = 3434 / 50155 Default effective X-H distances for T = -123.0 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 = 4408 / 486549 wR2 = 0.0688 before cycle 1 for 5039 data and 380 / 380 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 1.3047 1.3300 -0.0253 0.0080 DFIX C2' F2"_b 1.2955 1.3300 -0.0345 0.0080 DFIX C2' F3"_b -0.0368 0.0080 ISOR U11 F1'_a 0.0323 0.0080 ISOR U33 F1'_a -0.0251 0.0080 ISOR U13 F1'_a 0.0543 0.0080 ISOR U12 F1'_a 0.0526 0.0080 ISOR U11 F2'_a 0.0252 0.0080 ISOR U22 F2'_a -0.0779 0.0080 ISOR U33 F2'_a -0.0147 0.0040 ISOR U11 F3'_a 0.0259 0.0040 ISOR U22 F3'_a -0.0245 0.0040 ISOR U23 F3'_a 0.0290 0.0040 ISOR U13 F3'_a 0.0222 0.0040 ISOR U12 F3'_a Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.000 rms deviation 0.000 0.021 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.033 0.000 GooF = S = 1.053; Restrained GooF = 1.099 for 24 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0352 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19412 0.00029 0.010 OSF 2 0.00093 0.00026 0.000 EXTI Mean shift/esd = 0.002 Maximum = -0.021 for U11 Pd2 Max. shift = 0.000 A for F1"_b Max. dU = 0.000 for F2"_b Largest correlation matrix elements 0.631 EXTI / OSF 0.561 z F2"_b / x F2"_b 0.508 U11 Pd2 / OSF Idealized hydrogen atom generation before cycle 2 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H12 0.6007 0.0542 0.0918 43 0.950 0.000 C12 C13 C11 H13 0.5920 -0.0752 0.0164 43 0.950 0.000 C13 C12 C14 H14 0.4152 -0.1578 0.0174 43 0.950 0.000 C14 C13 C15 H15 0.2471 -0.1135 0.0962 43 0.950 0.000 C15 C10 C14 H16 0.4900 0.1635 0.1930 43 0.950 0.000 C16 N1' C11 H17 0.2262 0.2361 0.2767 13 1.000 0.000 C17 N1' C18 C19 H18A 0.2533 0.1320 0.3808 33 0.980 0.000 C18 C17 H18A H18B 0.2920 0.2263 0.4131 33 0.980 0.000 C18 C17 H18A H18C 0.3936 0.1572 0.3873 33 0.980 0.000 C18 C17 H18A H19A 0.3910 0.3069 0.2124 33 0.980 0.000 C19 C17 H19A H19B 0.4819 0.2666 0.2798 33 0.980 0.000 C19 C17 H19A H19C 0.3813 0.3353 0.3082 33 0.980 0.000 C19 C17 H19A H22 0.3380 0.3886 -0.0067 43 0.950 0.000 C22 C21 C23 H23 0.2821 0.4903 0.0942 43 0.950 0.000 C23 C22 C24 H24 0.1361 0.4537 0.1944 43 0.950 0.000 C24 C23 C25 H25 0.0424 0.3161 0.1907 43 0.950 0.000 C25 C20 C24 H26 0.3154 0.2308 -0.0660 43 0.950 0.000 C26 N1 C21 H27 0.2005 0.0242 -0.0372 13 1.000 0.000 C27 N1 C28 C29 H28A 0.3967 0.0740 -0.0688 33 0.980 0.000 C28 C27 H28A H28B 0.3452 0.1249 -0.1483 33 0.980 0.000 C28 C27 H28A H28C 0.3414 0.0211 -0.1458 33 0.980 0.000 C28 C27 H28A H29A 0.0303 0.0799 -0.1095 33 0.980 0.000 C29 C27 H29A H29B 0.1141 0.0246 -0.1712 33 0.980 0.000 C29 C27 H29A H29C 0.1181 0.1284 -0.1739 33 0.980 0.000 C29 C27 H29A SHELXL INS file, from DIRDIF output for S92 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Pd1 0.19090 0.05260 0.20412 1.00000 0.02613 0.02853 0.02357 0.00263 -0.00091 0.00223 0.02608 0.00057 0.00003 0.00002 0.00002 0.00000 0.00017 0.00019 0.00018 0.00015 0.00013 0.00014 0.00011 Pd2 0.07147 0.15301 0.07510 1.00000 0.02714 0.02493 0.02197 0.00409 0.00164 0.00050 0.02468 0.00055 0.00003 0.00002 0.00002 0.00000 0.00017 0.00018 0.00018 0.00014 0.00013 0.00013 0.00010 N1' 0.32482 0.13818 0.22861 1.00000 0.03075 0.03076 0.02942 0.00053 -0.00234 0.00233 0.03031 0.00606 0.00029 0.00024 0.00022 0.00000 0.00188 0.00211 0.00205 0.00166 0.00156 0.00160 0.00082 N1 0.19327 0.15398 -0.01741 1.00000 0.03071 0.02572 0.02256 0.00385 0.00032 0.00153 0.02633 0.00600 0.00029 0.00024 0.00020 0.00000 0.00166 0.00185 0.00184 0.00160 0.00149 0.00176 0.00073 O1 -0.05979 0.16634 0.16563 1.00000 0.03071 0.03443 0.02852 0.00608 0.00230 0.00423 0.03122 0.00518 0.00025 0.00019 0.00018 0.00000 0.00151 0.00190 0.00173 0.00139 0.00126 0.00136 0.00069 O2 0.04573 0.11568 0.27622 1.00000 0.03171 0.03524 0.03023 0.00619 0.00104 0.00514 0.03239 0.00531 0.00025 0.00020 0.00019 0.00000 0.00168 0.00180 0.00182 0.00141 0.00132 0.00129 0.00074 O1' 0.06643 -0.04210 0.17293 1.00000 0.03457 0.02899 0.03217 0.00529 -0.00400 0.00146 0.03191 0.00513 0.00026 0.00019 0.00018 0.00000 0.00156 0.00168 0.00174 0.00135 0.00140 0.00146 0.00068 O2' 0.00494 0.02161 0.05297 1.00000 0.03352 0.03084 0.03101 0.00202 -0.00495 -0.00150 0.03179 0.00516 0.00025 0.00020 0.00020 0.00000 0.00160 0.00187 0.00188 0.00146 0.00133 0.00122 0.00074 F1 -0.24732 0.12036 0.27502 1.00000 0.03271 0.07429 0.07665 -0.00660 0.01773 -0.00851 0.06122 0.00561 0.00024 0.00022 0.00021 0.00000 0.00152 0.00241 0.00241 0.00187 0.00151 0.00146 0.00093 F2 -0.18809 0.25189 0.28504 1.00000 0.07246 0.03866 0.06209 0.01003 0.02581 0.02255 0.05774 0.00598 0.00028 0.00019 0.00019 0.00000 0.00196 0.00174 0.00211 0.00161 0.00172 0.00158 0.00084 F3 -0.13516 0.15907 0.37568 1.00000 0.06212 0.08406 0.02988 0.01304 0.01896 0.01980 0.05869 0.00618 0.00025 0.00023 0.00018 0.00000 0.00184 0.00251 0.00171 0.00177 0.00134 0.00189 0.00089 F1'_a -0.06996 -0.13741 0.00691 0.63000 0.11750 0.07625 0.04844 -0.02202 0.02513 -0.05433 0.08073 0.00913 0.00072 0.00046 0.00032 0.00000 0.00477 0.00403 0.00328 0.00296 0.00338 0.00420 0.00200 F2'_a -0.18772 -0.09366 0.10519 0.63000 0.02404 0.05144 0.15456 0.00215 -0.00855 -0.01418 0.07668 0.00973 0.00038 0.00036 0.00049 0.00000 0.00233 0.00313 0.00535 0.00344 0.00295 0.00216 0.00183 F3'_a -0.05375 -0.18352 0.13251 0.63000 0.06952 0.02896 0.06612 0.02451 -0.02897 -0.02218 0.05487 0.00791 0.00050 0.00028 0.00035 0.00000 0.00259 0.00213 0.00274 0.00211 0.00238 0.00202 0.00128 F1"_b -0.00127 -0.18292 0.07055 0.37000 0.10474 0.02367 0.00104 0.00070 0.00104 0.00000 0.00396 F2"_b -0.14937 -0.13359 0.14600 0.37000 0.13205 0.02904 0.00135 0.00114 0.00084 0.00000 0.00575 F3"_b -0.13138 -0.11452 0.01670 0.37000 0.06199 0.01608 0.00091 0.00075 0.00056 0.00000 0.00312 C1 -0.04379 0.14733 0.24113 1.00000 0.03152 0.01969 0.02607 0.00547 0.00005 -0.00412 0.02576 0.00709 0.00033 0.00028 0.00026 0.00000 0.00216 0.00214 0.00238 0.00197 0.00177 0.00187 0.00090 C2 -0.15416 0.17007 0.29556 1.00000 0.03522 0.03531 0.03144 0.00786 0.00891 0.00270 0.03399 0.00850 0.00038 0.00030 0.00030 0.00000 0.00243 0.00288 0.00268 0.00225 0.00197 0.00190 0.00108 C1' 0.00782 -0.03711 0.10572 1.00000 0.03212 0.02473 0.03034 0.00609 0.00447 0.00125 0.02906 0.00783 0.00037 0.00030 0.00028 0.00000 0.00225 0.00262 0.00260 0.00208 0.00186 0.00174 0.00101 C2' -0.07284 -0.11452 0.08675 1.00000 0.04497 0.04039 0.03548 0.00073 -0.00085 -0.00842 0.04028 0.00769 0.00040 0.00029 0.00027 0.00000 0.00281 0.00287 0.00298 0.00230 0.00248 0.00226 0.00114 C10 0.32112 -0.00236 0.13954 1.00000 0.03636 0.03496 0.02531 0.00454 -0.00468 0.00752 0.03221 0.00809 0.00041 0.00030 0.00029 0.00000 0.00244 0.00272 0.00247 0.00200 0.00200 0.00206 0.00102 C11 0.42912 0.04704 0.13816 1.00000 0.03068 0.04198 0.03515 0.00032 0.00405 0.00351 0.03594 0.00819 0.00040 0.00032 0.00029 0.00000 0.00226 0.00271 0.00257 0.00226 0.00196 0.00233 0.00102 C12 0.52902 0.02010 0.09235 1.00000 0.03792 0.06528 0.04446 -0.00719 0.00634 0.00239 0.04922 0.00976 0.00044 0.00039 0.00036 0.00000 0.00279 0.00409 0.00350 0.00292 0.00232 0.00234 0.00145 H12 0.60069 0.05421 0.09179 1.00000 0.06471 0.00000 0.01723 C13 0.52384 -0.05632 0.04769 1.00000 0.04482 0.06126 0.03573 -0.00603 0.01217 0.01687 0.04727 0.01014 0.00044 0.00041 0.00032 0.00000 0.00283 0.00369 0.00287 0.00292 0.00217 0.00271 0.00133 H13 0.59202 -0.07517 0.01641 1.00000 0.05003 0.00000 0.01492 C14 0.41901 -0.10540 0.04862 1.00000 0.05878 0.04097 0.03488 -0.00422 -0.00623 0.02025 0.04488 0.00946 0.00047 0.00034 0.00032 0.00000 0.00332 0.00307 0.00285 0.00239 0.00247 0.00262 0.00128 H14 0.41523 -0.15776 0.01740 1.00000 0.03072 0.00000 0.01201 C15 0.31800 -0.07859 0.09530 1.00000 0.03647 0.03799 0.04569 -0.00125 -0.00536 0.00538 0.04005 0.00861 0.00044 0.00032 0.00031 0.00000 0.00256 0.00290 0.00322 0.00230 0.00226 0.00210 0.00119 H15 0.24707 -0.11347 0.09623 1.00000 0.09056 0.00000 0.02400 C16 0.42348 0.12461 0.18914 1.00000 0.03231 0.03732 0.03222 0.00101 0.00172 -0.00382 0.03395 0.00784 0.00040 0.00029 0.00028 0.00000 0.00240 0.00268 0.00263 0.00207 0.00205 0.00193 0.00105 H16 0.49000 0.16352 0.19301 1.00000 0.02497 0.00000 0.01095 C17 0.30930 0.21238 0.28638 1.00000 0.03356 0.03548 0.03834 -0.00549 0.00030 0.00135 0.03579 0.00798 0.00043 0.00030 0.00030 0.00000 0.00238 0.00266 0.00286 0.00219 0.00220 0.00195 0.00107 H17 0.22620 0.23612 0.27668 1.00000 0.02633 0.00000 0.01156 C18 0.31232 0.17905 0.37458 1.00000 0.05734 0.04586 0.04093 -0.00878 0.00117 0.00413 0.04804 0.00971 0.00054 0.00034 0.00033 0.00000 0.00327 0.00333 0.00311 0.00263 0.00277 0.00274 0.00133 H18A 0.25329 0.13198 0.38080 1.00000 0.04954 0.00000 0.01614 H18B 0.29204 0.22629 0.41308 1.00000 0.05661 0.00000 0.01596 H18C 0.39357 0.15718 0.38732 1.00000 0.05293 0.00000 0.01543 C19 0.39904 0.28708 0.27021 1.00000 0.04344 0.03952 0.07228 -0.00684 0.00181 -0.00324 0.05175 0.00939 0.00044 0.00035 0.00042 0.00000 0.00317 0.00311 0.00455 0.00298 0.00268 0.00225 0.00152 H19A 0.39100 0.30687 0.21236 1.00000 0.04278 0.00000 0.01491 H19B 0.48188 0.26657 0.27981 1.00000 0.03209 0.00000 0.01245 H19C 0.38131 0.33531 0.30817 1.00000 0.04247 0.00000 0.01358 C20 0.13215 0.27158 0.08991 1.00000 0.02915 0.02436 0.02842 0.00673 -0.00149 0.00215 0.02731 0.00736 0.00036 0.00027 0.00028 0.00000 0.00206 0.00234 0.00258 0.00195 0.00182 0.00169 0.00096 C21 0.22411 0.29390 0.03209 1.00000 0.03079 0.02721 0.03261 0.00491 0.00585 0.00359 0.03020 0.00813 0.00038 0.00029 0.00029 0.00000 0.00230 0.00251 0.00264 0.00206 0.00187 0.00172 0.00103 C22 0.27804 0.37435 0.03354 1.00000 0.03686 0.03236 0.04819 0.00744 0.00514 -0.00260 0.03913 0.00846 0.00040 0.00031 0.00033 0.00000 0.00264 0.00287 0.00311 0.00237 0.00220 0.00191 0.00121 H22 0.33799 0.38860 -0.00671 1.00000 0.03285 0.00000 0.01239 C23 0.24528 0.43459 0.09343 1.00000 0.04324 0.02824 0.04750 0.00065 0.00395 -0.00175 0.03966 0.00862 0.00041 0.00033 0.00032 0.00000 0.00262 0.00284 0.00329 0.00240 0.00225 0.00213 0.00118 H23 0.28214 0.49032 0.09423 1.00000 0.07678 0.00000 0.01988 C24 0.15795 0.41304 0.15251 1.00000 0.03444 0.03102 0.04618 -0.00685 0.00209 0.00587 0.03722 0.00849 0.00039 0.00031 0.00033 0.00000 0.00258 0.00266 0.00325 0.00233 0.00213 0.00192 0.00116 H24 0.13609 0.45371 0.19444 1.00000 0.01717 0.00000 0.00968 C25 0.10179 0.33059 0.15011 1.00000 0.02795 0.03688 0.03470 0.00155 0.00270 0.00069 0.03318 0.00767 0.00037 0.00029 0.00030 0.00000 0.00231 0.00300 0.00277 0.00225 0.00186 0.00183 0.00111 H25 0.04243 0.31606 0.19068 1.00000 0.01965 0.00000 0.01059 C26 0.25393 0.22450 -0.02499 1.00000 0.03351 0.03378 0.03241 0.00258 0.00720 0.00755 0.03323 0.00828 0.00040 0.00030 0.00029 0.00000 0.00237 0.00278 0.00276 0.00213 0.00204 0.00198 0.00108 H26 0.31537 0.23082 -0.06603 1.00000 0.02992 0.00000 0.01129 C27 0.21020 0.07744 -0.07219 1.00000 0.03479 0.03171 0.02608 -0.00408 0.00557 0.00592 0.03086 0.00767 0.00036 0.00029 0.00029 0.00000 0.00226 0.00257 0.00238 0.00208 0.00198 0.00175 0.00100 H27 0.20048 0.02415 -0.03717 1.00000 0.02637 0.00000 0.01124 C28 0.33435 0.07405 -0.11230 1.00000 0.04030 0.03850 0.03643 -0.01120 0.00300 0.00299 0.03841 0.00830 0.00040 0.00032 0.00031 0.00000 0.00280 0.00314 0.00281 0.00233 0.00212 0.00207 0.00121 H28A 0.39668 0.07400 -0.06877 1.00000 0.04493 0.00000 0.01416 H28B 0.34525 0.12489 -0.14829 1.00000 0.08992 0.00000 0.02364 H28C 0.34143 0.02106 -0.14579 1.00000 0.04962 0.00000 0.01508 C29 0.10907 0.07760 -0.13756 1.00000 0.03918 0.05068 0.03074 -0.00996 -0.00065 0.00900 0.04020 0.00839 0.00040 0.00035 0.00032 0.00000 0.00276 0.00349 0.00274 0.00254 0.00203 0.00216 0.00125 H29A 0.03029 0.07993 -0.10950 1.00000 0.01642 0.00000 0.01045 H29B 0.11412 0.02458 -0.17118 1.00000 0.12528 0.00000 0.03104 H29C 0.11809 0.12840 -0.17385 1.00000 0.05190 0.00000 0.01620 Final Structure Factor Calculation for SHELXL INS file, from DIRDIF output for S92 Total number of l.s. parameters = 380 Maximum vector length = 511 Memory required = 4030 / 27090 wR2 = 0.0688 before cycle 2 for 5039 data and 2 / 380 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 1.3047 1.3300 -0.0253 0.0080 DFIX C2' F2"_b 1.2955 1.3300 -0.0345 0.0080 DFIX C2' F3"_b -0.0368 0.0080 ISOR U11 F1'_a 0.0323 0.0080 ISOR U33 F1'_a -0.0251 0.0080 ISOR U13 F1'_a 0.0543 0.0080 ISOR U12 F1'_a 0.0526 0.0080 ISOR U11 F2'_a 0.0252 0.0080 ISOR U22 F2'_a -0.0779 0.0080 ISOR U33 F2'_a -0.0147 0.0040 ISOR U11 F3'_a 0.0259 0.0040 ISOR U22 F3'_a -0.0245 0.0040 ISOR U23 F3'_a 0.0290 0.0040 ISOR U13 F3'_a 0.0222 0.0040 ISOR U12 F3'_a Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.000 rms deviation 0.000 0.021 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.033 0.000 GooF = S = 1.053; Restrained GooF = 1.099 for 24 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0352 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0296 for 4674 Fo > 4sig(Fo) and 0.0343 for all 5039 data wR2 = 0.0688, GooF = S = 1.053, Restrained GooF = 1.099 for all data Flack x parameter = -0.0071 with esd 0.0263 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 = 38.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0304 0.0261 0.0217 Pd1 0.0289 0.0262 0.0190 Pd2 0.0336 0.0306 0.0267 N1' 0.0314 0.0276 0.0199 N1 0.0406 0.0284 0.0247 O1 0.0418 0.0302 0.0252 O2 0.0382 0.0337 0.0238 O1' 0.0382 0.0302 0.0270 O2' 0.0888 0.0691 0.0257 F1 0.1026 0.0436 0.0271 F2 0.1019 0.0533 0.0209 F3 0.1645 0.0425 0.0351 F1'_a 0.1552 0.0572 0.0177 F2'_a 0.1102 0.0390 0.0153 F3'_a 0.0333 0.0283 0.0157 C1 0.0470 0.0326 0.0224 C2 0.0378 0.0288 0.0206 C1' 0.0515 0.0354 0.0339 C2' 0.0432 0.0334 0.0200 C10 0.0433 0.0368 0.0277 C11 0.0675 0.0472 0.0330 C12 0.0719 0.0485 0.0214 C13 0.0735 0.0334 0.0278 C14 0.0493 0.0399 0.0310 C15 0.0394 0.0335 0.0290 C16 0.0426 0.0341 0.0307 C17 0.0589 0.0515 0.0338 C18 0.0738 0.0445 0.0369 C19 0.0334 0.0298 0.0187 C20 0.0404 0.0259 0.0243 C21 0.0521 0.0379 0.0273 C22 0.0499 0.0411 0.0280 C23 0.0488 0.0383 0.0245 C24 0.0381 0.0345 0.0270 C25 0.0451 0.0305 0.0241 C26 0.0397 0.0330 0.0199 C27 0.0487 0.0415 0.0250 C28 0.0586 0.0361 0.0259 C29 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.047 0.072 0.093 0.115 0.138 0.163 0.190 0.233 0.305 1.000 Number in group 510. 513. 493. 506. 499. 504. 513. 491. 505. 505. GooF 0.884 1.026 1.086 1.063 1.109 1.010 0.987 1.083 1.167 1.089 K 1.008 0.960 0.969 0.976 0.986 0.997 1.006 1.020 1.016 1.002 Resolution(A) 0.83 0.86 0.89 0.93 0.98 1.04 1.12 1.23 1.41 1.77 inf Number in group 522. 507. 484. 507. 508. 504. 498. 509. 492. 508. GooF 0.868 0.878 0.951 1.014 1.082 1.100 1.124 1.100 1.175 1.181 K 0.995 1.010 1.016 1.007 1.011 1.020 1.013 1.013 1.011 0.989 R1 0.075 0.058 0.047 0.047 0.043 0.033 0.028 0.023 0.023 0.020 Recommended weighting scheme: WGHT 0.0374 0.0000 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) 0 6 6 1097.84 1361.08 4.36 0.134 1.85 9 2 8 1321.94 1671.04 3.89 0.149 1.04 3 0 13 3582.99 2912.36 3.79 0.196 1.17 2 9 0 576.74 731.63 3.66 0.098 1.63 3 0 3 8720.02 10357.75 3.62 0.370 3.03 0 4 10 746.47 580.44 3.58 0.088 1.48 0 6 8 258.78 363.49 3.51 0.069 1.58 7 7 0 1334.18 1598.10 3.48 0.145 1.28 10 0 7 6478.43 5253.87 3.36 0.264 0.99 2 5 12 7737.32 9572.52 3.35 0.356 1.20 -3 2 2 5923.40 6824.60 3.27 0.300 3.07 -4 12 3 1154.19 1437.78 3.26 0.138 1.14 -8 6 9 632.15 786.52 3.23 0.102 1.00 8 7 11 419.74 649.49 3.20 0.093 0.91 3 8 9 2341.00 1983.06 3.20 0.162 1.23 -4 11 5 234.44 396.77 3.18 0.072 1.16 -2 4 1 5337.12 6533.23 3.18 0.294 3.10 6 8 4 1299.86 1092.79 3.16 0.120 1.26 -1 7 9 7076.20 6190.20 3.16 0.286 1.37 5 0 9 485.77 597.06 3.16 0.089 1.39 -7 2 9 389.96 484.00 3.15 0.080 1.17 5 8 14 343.77 527.13 3.14 0.083 0.90 -2 5 8 441.56 551.99 3.10 0.085 1.61 2 4 1 6177.18 7001.44 3.00 0.304 3.10 0 11 13 4490.53 3597.85 2.96 0.218 0.93 -8 2 11 132.97 233.61 2.95 0.056 0.99 0 3 11 112.79 196.63 2.93 0.051 1.40 -7 9 5 627.69 799.30 2.92 0.103 1.09 4 0 11 1857.50 2158.43 2.91 0.169 1.29 -6 11 7 2218.53 2617.71 2.91 0.186 1.00 -4 12 7 3138.79 3933.17 2.88 0.228 1.04 3 3 0 4111.59 4696.89 2.87 0.249 2.99 6 10 0 484.24 388.34 2.85 0.072 1.18 -3 7 12 1092.63 892.56 2.85 0.109 1.09 8 0 2 3744.08 3289.96 2.84 0.209 1.36 1 6 17 1999.01 2520.23 2.83 0.183 0.88 -3 1 15 5693.59 4794.72 2.83 0.252 1.02 0 3 2 780.47 685.07 2.83 0.095 4.32 -8 9 7 906.11 1118.05 2.82 0.122 0.97 0 14 0 832.19 1163.85 2.82 0.124 1.10 5 0 5 207.58 257.30 2.81 0.058 1.82 3 5 0 6920.16 6152.05 2.81 0.285 2.36 2 6 0 40660.28 36269.88 2.81 0.692 2.33 0 10 6 2259.16 2572.27 2.80 0.184 1.33 -8 7 1 2851.01 2517.47 2.78 0.182 1.17 3 7 5 4224.74 3768.07 2.78 0.223 1.63 10 4 0 1546.22 1776.17 2.78 0.153 1.06 -2 12 8 3427.57 2926.62 2.76 0.197 1.06 2 8 2 6910.94 7756.50 2.75 0.320 1.77 4 10 7 466.69 645.23 2.74 0.092 1.16 Bond lengths and angles Pd1 - Distance Angles C10 1.9636 (0.0046) N1' 2.0196 (0.0035) 81.24 (0.17) O1' 2.0656 (0.0030) 93.16 (0.16) 174.38 (0.13) O2 2.2020 (0.0029) 179.35 (0.17) 98.23 (0.13) 87.38 (0.12) Pd2 2.8996 (0.0004) 100.78 (0.13) 97.09 (0.10) 84.34 (0.08) 78.92 (0.08) Pd1 - C10 N1' O1' O2 Pd2 - Distance Angles C20 1.9597 (0.0042) N1 2.0019 (0.0032) 81.55 (0.17) O1 2.0612 (0.0029) 93.58 (0.15) 173.27 (0.13) O2' 2.1822 (0.0031) 177.59 (0.16) 96.47 (0.13) 88.28 (0.12) Pd1 2.8996 (0.0004) 104.78 (0.12) 103.10 (0.10) 82.58 (0.08) 76.96 (0.08) Pd2 - C20 N1 O1 O2' N1' - Distance Angles C16 1.2771 (0.0054) C17 1.4808 (0.0058) 122.33 (0.38) Pd1 2.0196 (0.0035) 114.93 (0.30) 122.72 (0.27) N1' - C16 C17 N1 - Distance Angles C26 1.2819 (0.0058) C27 1.4818 (0.0056) 123.51 (0.35) Pd2 2.0019 (0.0032) 115.31 (0.30) 121.17 (0.27) N1 - C26 C27 O1 - Distance Angles C1 1.2574 (0.0048) Pd2 2.0612 (0.0029) 123.74 (0.25) O1 - C1 O2 - Distance Angles C1 1.2373 (0.0047) Pd1 2.2020 (0.0029) 121.13 (0.27) O2 - C1 O1' - Distance Angles C1' 1.2591 (0.0052) Pd1 2.0656 (0.0030) 120.40 (0.28) O1' - C1' O2' - Distance Angles C1' 1.2386 (0.0052) Pd2 2.1822 (0.0031) 123.90 (0.29) O2' - C1' F1 - Distance Angles C2 1.3240 (0.0054) F1 - F2 - Distance Angles C2 1.3256 (0.0050) F2 - F3 - Distance Angles C2 1.3121 (0.0054) F3 - F1'_a - Distance Angles C2' 1.3277 (0.0055) F1'_a - F2'_a - Distance Angles C2' 1.3416 (0.0056) F2'_a - F3'_a - Distance Angles C2' 1.3084 (0.0051) F3'_a - F1"_b - Distance Angles C2' 1.3424 (0.0075) F1"_b - F2"_b - Distance Angles C2' 1.3047 (0.0077) F2"_b - F3"_b - Distance Angles C2' 1.2955 (0.0071) F3"_b - C1 - Distance Angles O2 1.2373 (0.0047) O1 1.2574 (0.0048) 129.90 (0.37) C2 1.5392 (0.0057) 117.68 (0.37) 112.40 (0.35) C1 - O2 O1 C2 - Distance Angles F3 1.3121 (0.0054) F1 1.3240 (0.0054) 107.03 (0.38) F2 1.3256 (0.0050) 107.00 (0.41) 107.37 (0.37) C1 1.5392 (0.0057) 113.50 (0.35) 110.04 (0.38) 111.60 (0.36) C2 - F3 F1 F2 C1' - Distance Angles O2' 1.2386 (0.0052) O1' 1.2591 (0.0053) 129.93 (0.42) C2' 1.5189 (0.0062) 114.93 (0.39) 115.13 (0.38) C1' - O2' O1' C2' - Distance Angles F3"_b 1.2955 (0.0071) F2"_b 1.3047 (0.0077) 107.91 (0.93) F3'_a 1.3084 (0.0051) 124.48 (0.67) 60.89 (0.82) F1'_a 1.3277 (0.0055) 34.58 (0.47) 131.08 (0.88) 108.70 (0.51) F2'_a 1.3416 (0.0056) 73.69 (0.62) 44.03 (0.74) 102.91 (0.49) 107.37 (0.58) F1"_b 1.3424 (0.0075) 97.24 (0.83) 110.20 (1.05) 51.39 (0.68) 65.86 (0.74) 141.92 (0.71) C1' 1.5189 (0.0062) 117.78 (0.64) 114.26 (0.82) 115.53 (0.39) 112.79 (0.41) 108.81 (0.40) 108.03 (0.63) C2' - F3"_b F2"_b F3'_a F1'_a F2'_a F1"_b C10 - Distance Angles C15 1.3719 (0.0068) C11 1.4149 (0.0066) 118.25 (0.44) Pd1 1.9636 (0.0046) 128.54 (0.37) 113.18 (0.34) C10 - C15 C11 C11 - Distance Angles C12 1.3885 (0.0067) C10 1.4149 (0.0066) 121.14 (0.46) C16 1.4488 (0.0064) 125.36 (0.45) 113.49 (0.39) C11 - C12 C10 C12 - Distance Angles C13 1.3788 (0.0081) C11 1.3885 (0.0067) 119.78 (0.49) H12 0.9500 120.11 120.11 C12 - C13 C11 C13 - Distance Angles C12 1.3788 (0.0081) C14 1.3827 (0.0077) 119.73 (0.44) H13 0.9500 120.14 120.14 C13 - C12 C14 C14 - Distance Angles C13 1.3827 (0.0077) C15 1.4051 (0.0070) 120.63 (0.49) H14 0.9500 119.68 119.68 C14 - C13 C15 C15 - Distance Angles C10 1.3719 (0.0068) C14 1.4051 (0.0070) 120.45 (0.48) H15 0.9500 119.77 119.77 C15 - C10 C14 C16 - Distance Angles N1' 1.2771 (0.0054) C11 1.4488 (0.0064) 116.81 (0.40) H16 0.9500 121.60 121.60 C16 - N1' C11 C17 - Distance Angles N1' 1.4808 (0.0058) C18 1.5043 (0.0069) 108.76 (0.38) C19 1.5403 (0.0067) 113.38 (0.39) 113.50 (0.45) H17 1.0000 106.93 106.93 106.93 C17 - N1' C18 C19 C18 - Distance Angles C17 1.5043 (0.0070) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C17 H18A H18B C19 - Distance Angles C17 1.5403 (0.0067) H19A 0.9800 109.47 H19B 0.9800 109.47 109.47 H19C 0.9800 109.47 109.47 109.47 C19 - C17 H19A H19B C20 - Distance Angles C25 1.3673 (0.0063) C21 1.4171 (0.0060) 118.42 (0.39) Pd2 1.9597 (0.0042) 128.40 (0.33) 113.07 (0.32) C20 - C25 C21 C21 - Distance Angles C22 1.3751 (0.0066) C20 1.4171 (0.0060) 121.19 (0.43) C26 1.4449 (0.0064) 125.35 (0.41) 113.44 (0.39) C21 - C22 C20 C22 - Distance Angles C21 1.3751 (0.0066) C23 1.3833 (0.0069) 120.20 (0.45) H22 0.9500 119.90 119.90 C22 - C21 C23 C23 - Distance Angles C22 1.3833 (0.0069) C24 1.3917 (0.0066) 119.56 (0.45) H23 0.9500 120.22 120.22 C23 - C22 C24 C24 - Distance Angles C23 1.3917 (0.0066) C25 1.4138 (0.0062) 119.99 (0.45) H24 0.9500 120.01 120.01 C24 - C23 C25 C25 - Distance Angles C20 1.3673 (0.0063) C24 1.4138 (0.0062) 120.58 (0.42) H25 0.9500 119.71 119.71 C25 - C20 C24 C26 - Distance Angles N1 1.2819 (0.0058) C21 1.4449 (0.0064) 116.60 (0.39) H26 0.9500 121.70 121.70 C26 - N1 C21 C27 - Distance Angles N1 1.4818 (0.0056) C28 1.5151 (0.0060) 113.14 (0.36) C29 1.5314 (0.0063) 108.18 (0.33) 111.69 (0.39) H27 1.0000 107.88 107.88 107.88 C27 - N1 C28 C29 C28 - Distance Angles C27 1.5151 (0.0060) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C27 H28A H28B C29 - Distance Angles C27 1.5314 (0.0063) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - C27 H29A H29B Selected torsion angles -12.50 ( 0.12) O2 - Pd1 - Pd2 - O1 -14.02 ( 0.12) O2' - Pd2 - Pd1 - O1' Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 2.9098 (0.0118) x - 8.1597 (0.0155) y + 12.9209 (0.0117) z = 2.7644 (0.0036) * 0.0069 (0.0017) O1' * -0.0063 (0.0016) O2 * -0.0078 (0.0019) C10 * 0.0072 (0.0018) N1' -0.0006 (0.0019) Pd1 Rms deviation of fitted atoms = 0.0070 7.3801 (0.0088) x - 5.2962 (0.0171) y + 10.5719 (0.0131) z = 0.4562 (0.0033) Angle to previous plane (with approximate esd) = 27.12 ( 0.13 ) * -0.0274 (0.0016) O1 * 0.0257 (0.0015) O2' * 0.0312 (0.0018) C20 * -0.0295 (0.0017) N1 0.0547 (0.0017) Pd2 Rms deviation of fitted atoms = 0.0285 FMAP and GRID set by program FMAP 2 3 19 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.0298 for 2847 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.67 at 0.0042 0.8331 0.0282 [ 0.72 A from F1" ] Deepest hole -0.53 at 0.0218 0.1530 0.1102 [ 0.79 A from PD2 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 3944 / 23518 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0042 -0.1669 0.0282 1.00000 0.05 0.67 0.72 F1" 1.00 F1' 1.50 C2' 1.71 F3" Q2 1 -0.1773 -0.0963 0.0463 1.00000 0.05 0.64 0.75 F3" 0.95 F2' 1.35 C2' 1.49 F1' Q3 1 -0.0953 -0.1584 0.1547 1.00000 0.05 0.60 0.70 F3' 0.72 F2" 1.31 C2' 1.63 F2' Q4 1 -0.0254 -0.1964 0.0994 1.00000 0.05 0.44 0.57 F1" 0.65 F3' 1.38 C2' 1.81 F1' Q5 1 -0.1840 -0.1122 0.1301 1.00000 0.05 0.38 0.49 F2' 0.57 F2" 1.41 C2' 1.81 F3' Q6 1 0.3206 -0.0537 0.1565 1.00000 0.05 0.32 0.84 C10 1.05 C15 1.56 H15 1.98 C11 Q7 1 -0.0866 0.0625 0.1237 1.00000 0.05 0.32 1.64 O2' 1.76 O1 1.88 C1' 2.19 H22 Q8 1 0.3162 0.1758 0.2416 1.00000 0.05 0.31 0.62 N1' 0.92 C17 1.47 H17 1.65 C16 Q9 1 -0.1745 -0.0615 0.1315 1.00000 0.05 0.30 0.67 F2' 1.17 F2" 1.56 C2' 2.07 F3" Q10 1 0.0747 0.2855 -0.0661 1.00000 0.05 0.29 2.28 C21 2.29 C26 2.37 H16 2.52 H12 Shortest distances between peaks (including symmetry equivalents) 5 9 0.79 1 4 1.27 3 5 1.27 3 4 1.31 2 5 1.37 2 9 1.47 3 9 1.77 7 9 2.14 2 3 2.18 4 5 2.23 1 2 2.30 1 3 2.31 2 4 2.43 4 9 2.70 1 5 2.77 5 7 2.90 2 7 2.92 Time profile in seconds ----------------------- 0.22: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 2.45: 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 1.56: Structure factors and derivatives 1.30: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.22: Solve l.s. equations 0.02: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.05: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 18:03:42 Total CPU time: 6.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++