+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 11:26:21 on 29-May-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SRC946 in P2(1)/n CELL 0.71073 15.3839 8.0685 24.1935 90.000 105.877 90.000 ZERR 4.00 0.0004 0.0002 0.0009 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O F P UNIT 96 120 12 28 24 12 V = 2888.46 F(000) = 1400.0 Mu = 0.29 mm-1 Cell Wt = 2717.68 Rho = 1.562 MERG 2 FMAP 2 PLAN 10 SIZE 0.03 0.10 0.18 ACTA EXTI OMIT -3 55 OMIT 14 3 4 OMIT 0 1 9 BOND $H CONF WGHT 0.04630 L.S. 4 TEMP -153.00 FVAR 0.13463 C1 1 0.306325 0.433796 0.061712 11.00000 0.02734 0.02915 = 0.02202 -0.00088 0.00544 -0.01035 AFIX 23 H1A 2 0.254136 0.467941 0.075566 11.00000 -1.20000 H1B 2 0.325382 0.321442 0.076629 11.00000 -1.20000 AFIX 0 C2 1 0.281176 0.434005 -0.002115 11.00000 0.02680 0.02717 = 0.02473 -0.00620 0.00403 -0.00542 C3 1 0.172238 0.962232 0.117863 11.00000 0.01812 0.02573 = 0.02359 0.00109 0.00245 0.00051 AFIX 23 H3A 2 0.137509 1.057808 0.126219 11.00000 -1.20000 H3B 2 0.163118 0.867274 0.141584 11.00000 -1.20000 AFIX 0 C4 1 0.140118 0.918694 0.055909 11.00000 0.02413 0.02628 = 0.02743 -0.00151 0.00231 0.00256 C5 1 0.420235 0.402772 0.234129 11.00000 0.02847 0.02126 = 0.02240 0.00260 0.00663 0.00074 AFIX 23 H5A 2 0.409781 0.283882 0.240150 11.00000 -1.20000 H5B 2 0.371700 0.467181 0.243904 11.00000 -1.20000 AFIX 0 C6 1 0.510192 0.453880 0.272854 11.00000 0.03302 0.02230 = 0.02085 0.00269 0.00608 0.00118 AFIX 23 H6A 2 0.560014 0.402074 0.260369 11.00000 -1.20000 H6B 2 0.517234 0.575807 0.272513 11.00000 -1.20000 AFIX 0 C7 1 0.590265 0.444042 0.371967 11.00000 0.02847 0.03408 = 0.02248 0.00121 -0.00106 0.00772 AFIX 23 H7A 2 0.643669 0.404755 0.360377 11.00000 -1.20000 H7B 2 0.590026 0.386063 0.407988 11.00000 -1.20000 AFIX 0 C8 1 0.600492 0.626119 0.383998 11.00000 0.02197 0.03508 = 0.02241 0.00107 0.00389 0.00484 AFIX 23 H8A 2 0.656309 0.647392 0.415125 11.00000 -1.20000 H8B 2 0.605023 0.685954 0.349168 11.00000 -1.20000 AFIX 0 C9 1 0.528354 0.856032 0.411378 11.00000 0.02709 0.02414 = 0.03269 0.00108 0.00296 -0.00159 AFIX 23 H9A 2 0.532590 0.916394 0.376584 11.00000 -1.20000 H9B 2 0.582703 0.882389 0.443020 11.00000 -1.20000 AFIX 0 C10 1 0.445503 0.908649 0.427321 11.00000 0.03030 0.02825 = 0.02113 -0.00460 -0.00095 0.00083 AFIX 23 H10A 2 0.444018 0.851848 0.463323 11.00000 -1.20000 H10B 2 0.448921 1.029354 0.434961 11.00000 -1.20000 AFIX 0 C11 1 0.349713 0.963252 0.331993 11.00000 0.02672 0.02864 = 0.02216 0.00126 0.00544 0.00722 AFIX 23 H11A 2 0.402688 1.034431 0.333385 11.00000 -1.20000 H11B 2 0.295700 1.034939 0.326001 11.00000 -1.20000 AFIX 0 C12 1 0.336738 0.840961 0.284098 11.00000 0.03612 0.02843 = 0.01733 0.00430 0.00491 0.00816 AFIX 23 H12A 2 0.395451 0.791252 0.283818 11.00000 -1.20000 H12B 2 0.295739 0.751037 0.289061 11.00000 -1.20000 AFIX 0 C13 1 0.548967 0.997667 0.118932 11.00000 0.02113 0.01970 = 0.02229 -0.00283 0.00137 -0.00317 C14 1 0.602504 0.921201 0.088385 11.00000 0.03750 0.02554 = 0.02905 -0.00223 0.01753 -0.00061 AFIX 43 H14 2 0.623393 0.811189 0.097725 11.00000 -1.20000 AFIX 0 C15 1 0.625237 1.004464 0.044725 11.00000 0.04286 0.03842 = 0.03527 -0.00864 0.02060 -0.00949 AFIX 43 H15 2 0.661855 0.951787 0.024045 11.00000 -1.20000 AFIX 0 C16 1 0.595011 1.164547 0.030805 11.00000 0.03755 0.03974 = 0.02491 0.00279 0.00265 -0.01652 AFIX 43 H16 2 0.609947 1.220954 0.000169 11.00000 -1.20000 AFIX 0 C17 1 0.543306 1.242017 0.061355 11.00000 0.03233 0.02697 = 0.03285 0.00571 0.00040 -0.00330 AFIX 43 H17 2 0.523197 1.352457 0.052022 11.00000 -1.20000 AFIX 0 C18 1 0.520491 1.160300 0.105449 11.00000 0.02210 0.02753 = 0.02700 0.00143 0.00161 0.00043 AFIX 43 H18 2 0.485318 1.214924 0.126666 11.00000 -1.20000 AFIX 0 C19 1 0.609547 0.898876 0.237709 11.00000 0.01839 0.02112 = 0.01976 0.00227 0.00510 -0.00017 C20 1 0.612580 1.019154 0.279344 11.00000 0.02460 0.01884 = 0.02694 0.00196 0.00567 0.00045 AFIX 43 H20 2 0.564008 1.095287 0.274725 11.00000 -1.20000 AFIX 0 C21 1 0.685690 1.028673 0.327339 11.00000 0.03088 0.02439 = 0.02268 -0.00421 0.00576 -0.00551 AFIX 43 H21 2 0.686904 1.110565 0.355754 11.00000 -1.20000 AFIX 0 C22 1 0.757025 0.919801 0.334243 11.00000 0.02294 0.03366 = 0.02385 0.00238 -0.00010 -0.00374 AFIX 43 H22 2 0.807702 0.928050 0.367010 11.00000 -1.20000 AFIX 0 C23 1 0.754709 0.799173 0.293601 11.00000 0.02365 0.04189 = 0.03248 0.00091 0.00325 0.01066 AFIX 43 H23 2 0.803455 0.723269 0.298580 11.00000 -1.20000 AFIX 0 C24 1 0.681175 0.788435 0.245357 11.00000 0.02779 0.03102 = 0.02648 -0.00477 0.00586 0.00420 AFIX 43 H24 2 0.679812 0.705075 0.217402 11.00000 -1.20000 AFIX 0 N1 3 0.330164 0.706526 0.162491 11.00000 0.01902 0.01880 = 0.02203 -0.00021 0.00651 -0.00085 N2 3 0.432167 0.982259 0.187317 11.00000 0.02124 0.01443 = 0.02725 -0.00331 0.00683 -0.00008 N3 3 0.501932 0.696039 0.155983 11.00000 0.01808 0.01653 = 0.02462 -0.00318 0.00401 0.00104 O1 4 0.379274 0.548610 0.080879 11.00000 0.02644 0.02089 = 0.01828 -0.00373 0.00542 -0.00583 O2 4 0.266396 1.003342 0.131417 11.00000 0.01752 0.02264 = 0.02239 0.00247 0.00179 0.00000 O3 4 0.416867 0.430377 0.174693 11.00000 0.03116 0.01591 = 0.01765 -0.00040 0.00657 0.00079 O4 4 0.510653 0.398057 0.328384 11.00000 0.03546 0.02830 = 0.01742 0.00450 0.00296 0.00241 O5 4 0.524084 0.682975 0.400683 11.00000 0.02426 0.02471 = 0.03313 -0.00184 0.00914 -0.00060 O6 4 0.363549 0.873512 0.384175 11.00000 0.02494 0.03594 = 0.01939 0.00098 0.00313 0.00024 O7 4 0.298037 0.928295 0.230755 11.00000 0.02554 0.02298 = 0.01944 0.00154 0.00655 0.00501 F1 5 0.350027 0.395114 -0.023192 11.00000 0.04036 0.04464 = 0.02767 -0.00994 0.00995 0.00944 F2 5 0.215470 0.323815 -0.022957 11.00000 0.05511 0.04557 = 0.03061 -0.00787 -0.00065 -0.02829 F3 5 0.250990 0.580323 -0.025164 11.00000 0.03529 0.03264 = 0.02895 0.00357 0.00158 0.00609 F4 5 0.186239 0.792411 0.041564 11.00000 0.04582 0.05419 = 0.04256 -0.02307 -0.00125 0.02120 F5 5 0.145903 1.043407 0.021671 11.00000 0.04996 0.05390 = 0.02601 0.01080 0.00089 -0.00520 F6 5 0.053370 0.871444 0.042252 11.00000 0.02944 0.04067 = 0.03824 -0.00696 -0.00588 -0.00310 P1 6 0.408514 0.607105 0.145979 11.00000 0.02083 0.01715 = 0.01798 -0.00062 0.00394 0.00038 P2 6 0.337443 0.897441 0.177734 11.00000 0.01833 0.01924 = 0.01821 -0.00039 0.00331 0.00174 P3 6 0.516002 0.887273 0.174123 11.00000 0.01737 0.01990 = 0.02103 -0.00256 0.00370 0.00078 HKLF 4 Covalent radii and connectivity table for 01SRC946 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 P 1.100 C1 - O1 C2 C2 - F1 F3 F2 C1 C3 - O2 C4 C4 - F5 F6 F4 C3 C5 - O3 C6 C6 - O4 C5 C7 - O4 C8 C8 - O5 C7 C9 - O5 C10 C10 - O6 C9 C11 - O6 C12 C12 - O7 C11 C13 - C14 C18 P3 C14 - C15 C13 C15 - C14 C16 C16 - C17 C15 C17 - C16 C18 C18 - C17 C13 C19 - C24 C20 P3 C20 - C21 C19 C21 - C22 C20 C22 - C23 C21 C23 - C22 C24 C24 - C23 C19 N1 - P2 P1 N2 - P2 P3 N3 - P1 P3 O1 - C1 P1 O2 - C3 P2 O3 - C5 P1 O4 - C6 C7 O5 - C9 C8 O6 - C11 C10 O7 - C12 P2 F1 - C2 F2 - C2 F3 - C2 F4 - C4 F5 - C4 F6 - C4 P1 - N3 O3 O1 N1 P2 - N2 N1 O7 O2 P3 - N3 N2 C13 C19 23544 Reflections read, of which 747 rejected -19 =< h =< 19, -10 =< k =< 8, -31 =< l =< 31, Max. 2-theta = 54.93 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 6 1 1 106.24 1.41 6 9.89 10 2 2 24.75 0.87 3 7.76 6 1 3 76.00 3.33 2 36.52 10 2 3 79.72 2.21 4 13.69 12 3 4 33.04 0.99 3 14.68 7 0 5 115.31 2.53 3 32.12 9 2 6 34.77 0.88 4 8.05 8 1 7 18.64 0.68 4 3.39 10 2 7 13.97 0.87 3 7.36 10 2 8 16.73 0.81 4 4.13 11 2 8 79.32 2.82 3 29.17 -1 1 9 136.23 1.03 5 36.24 10 1 9 55.21 0.99 5 12.80 10 0 10 10.78 0.73 3 4.22 14 Inconsistent equivalents 6488 Unique reflections, of which 0 suppressed R(int) = 0.0825 R(sigma) = 0.1092 Friedel opposites merged Maximum memory for data reduction = 4128 / 65259 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 = 5207 / 499230 wR2 = 0.1147 before cycle 1 for 6488 data and 389 / 389 parameters GooF = S = 0.979; Restrained GooF = 0.979 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0463 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13484 0.00021 0.994 OSF 2 0.00075 0.00023 3.324 EXTI Mean shift/esd = 0.114 Maximum = 3.324 for EXTI Max. shift = 0.001 A for C14 Max. dU = 0.000 for C11 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5207 / 499230 wR2 = 0.1144 before cycle 2 for 6488 data and 389 / 389 parameters GooF = S = 0.977; Restrained GooF = 0.977 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0463 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13496 0.00022 0.536 OSF 2 0.00121 0.00027 1.658 EXTI Mean shift/esd = 0.041 Maximum = 1.658 for EXTI Max. shift = 0.000 A for C14 Max. dU = 0.000 for C11 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5207 / 499230 wR2 = 0.1144 before cycle 3 for 6488 data and 389 / 389 parameters GooF = S = 0.977; Restrained GooF = 0.977 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0463 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13497 0.00022 0.066 OSF 2 0.00126 0.00030 0.154 EXTI Mean shift/esd = 0.004 Maximum = 0.154 for EXTI Max. shift = 0.000 A for C21 Max. dU = 0.000 for C16 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5207 / 499230 wR2 = 0.1144 before cycle 4 for 6488 data and 389 / 389 parameters GooF = S = 0.977; Restrained GooF = 0.977 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0463 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13497 0.00022 0.003 OSF 2 0.00126 0.00031 0.006 EXTI Mean shift/esd = 0.001 Maximum = 0.006 for EXTI Max. shift = 0.000 A for C14 Max. dU = 0.000 for C4 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.2541 0.4680 0.0756 23 0.990 0.000 C1 O1 C2 H1B 0.3253 0.3214 0.0767 23 0.990 0.000 C1 O1 C2 H3A 0.1375 1.0577 0.1262 23 0.990 0.000 C3 O2 C4 H3B 0.1631 0.8671 0.1416 23 0.990 0.000 C3 O2 C4 H5A 0.4098 0.2839 0.2401 23 0.990 0.000 C5 O3 C6 H5B 0.3717 0.4672 0.2439 23 0.990 0.000 C5 O3 C6 H6A 0.5600 0.4020 0.2604 23 0.990 0.000 C6 O4 C5 H6B 0.5173 0.5758 0.2725 23 0.990 0.000 C6 O4 C5 H7A 0.6436 0.4048 0.3603 23 0.990 0.000 C7 O4 C8 H7B 0.5901 0.3860 0.4080 23 0.990 0.000 C7 O4 C8 H8A 0.6563 0.6474 0.4151 23 0.990 0.000 C8 O5 C7 H8B 0.6050 0.6860 0.3491 23 0.990 0.000 C8 O5 C7 H9A 0.5325 0.9164 0.3765 23 0.990 0.000 C9 O5 C10 H9B 0.5827 0.8825 0.4430 23 0.990 0.000 C9 O5 C10 H10A 0.4440 0.8518 0.4633 23 0.990 0.000 C10 O6 C9 H10B 0.4489 1.0293 0.4349 23 0.990 0.000 C10 O6 C9 H11A 0.4027 1.0345 0.3334 23 0.990 0.000 C11 O6 C12 H11B 0.2957 1.0350 0.3260 23 0.990 0.000 C11 O6 C12 H12A 0.3954 0.7913 0.2838 23 0.990 0.000 C12 O7 C11 H12B 0.2957 0.7512 0.2891 23 0.990 0.000 C12 O7 C11 H14 0.6233 0.8111 0.0976 43 0.950 0.000 C14 C15 C13 H15 0.6619 0.9518 0.0241 43 0.950 0.000 C15 C14 C16 H16 0.6100 1.2209 0.0002 43 0.950 0.000 C16 C17 C15 H17 0.5231 1.3524 0.0520 43 0.950 0.000 C17 C16 C18 H18 0.4853 1.2150 0.1266 43 0.950 0.000 C18 C17 C13 H20 0.5640 1.0952 0.2747 43 0.950 0.000 C20 C21 C19 H21 0.6869 1.1105 0.3558 43 0.950 0.000 C21 C22 C20 H22 0.8077 0.9280 0.3670 43 0.950 0.000 C22 C23 C21 H23 0.8035 0.7233 0.2986 43 0.950 0.000 C23 C22 C24 H24 0.6798 0.7051 0.2174 43 0.950 0.000 C24 C23 C19 01SRC946 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.30632 0.43381 0.06173 1.00000 0.02749 0.02917 0.02245 -0.00074 0.00545 -0.01020 0.02664 0.00503 0.00019 0.00036 0.00011 0.00000 0.00160 0.00187 0.00154 0.00133 0.00117 0.00130 0.00069 H1A 0.25411 0.46801 0.07556 1.00000 0.03197 0.00000 0.00000 H1B 0.32534 0.32145 0.07665 1.00000 0.03197 0.00000 0.00000 C2 0.28124 0.43403 -0.00210 1.00000 0.02736 0.02730 0.02438 -0.00616 0.00418 -0.00564 0.02691 0.00521 0.00019 0.00038 0.00012 0.00000 0.00166 0.00191 0.00160 0.00135 0.00124 0.00130 0.00069 C3 0.17222 0.96214 0.11787 1.00000 0.01780 0.02582 0.02419 0.00114 0.00238 0.00071 0.02327 0.00500 0.00017 0.00036 0.00011 0.00000 0.00146 0.00173 0.00154 0.00129 0.00111 0.00115 0.00064 H3A 0.13747 1.05765 0.12624 1.00000 0.02792 0.00000 0.00000 H3B 0.16313 0.86713 0.14158 1.00000 0.02792 0.00000 0.00000 C4 0.14009 0.91867 0.05592 1.00000 0.02515 0.02611 0.02682 -0.00133 0.00262 0.00279 0.02691 0.00545 0.00019 0.00038 0.00012 0.00000 0.00169 0.00188 0.00164 0.00141 0.00124 0.00127 0.00070 C5 0.42024 0.40278 0.23410 1.00000 0.02929 0.02136 0.02200 0.00254 0.00694 0.00087 0.02423 0.00518 0.00018 0.00036 0.00011 0.00000 0.00158 0.00170 0.00153 0.00128 0.00117 0.00123 0.00064 H5A 0.40977 0.28389 0.24012 1.00000 0.02908 0.00000 0.00000 H5B 0.37171 0.46720 0.24388 1.00000 0.02908 0.00000 0.00000 C6 0.51021 0.45384 0.27284 1.00000 0.03273 0.02235 0.02167 0.00269 0.00603 0.00105 0.02586 0.00534 0.00019 0.00037 0.00011 0.00000 0.00168 0.00175 0.00156 0.00129 0.00120 0.00125 0.00067 H6A 0.56003 0.40197 0.26037 1.00000 0.03103 0.00000 0.00000 H6B 0.51728 0.57576 0.27249 1.00000 0.03103 0.00000 0.00000 C7 0.59025 0.44406 0.37193 1.00000 0.02911 0.03401 0.02274 0.00110 -0.00074 0.00772 0.03016 0.00537 0.00019 0.00037 0.00012 0.00000 0.00168 0.00200 0.00156 0.00139 0.00120 0.00132 0.00072 H7A 0.64364 0.40484 0.36030 1.00000 0.03619 0.00000 0.00000 H7B 0.59007 0.38603 0.40795 1.00000 0.03619 0.00000 0.00000 C8 0.60045 0.62609 0.38397 1.00000 0.02179 0.03534 0.02275 0.00126 0.00384 0.00505 0.02707 0.00542 0.00018 0.00037 0.00012 0.00000 0.00156 0.00200 0.00153 0.00137 0.00116 0.00127 0.00069 H8A 0.65629 0.64736 0.41508 1.00000 0.03248 0.00000 0.00000 H8B 0.60496 0.68595 0.34914 1.00000 0.03248 0.00000 0.00000 C9 0.52831 0.85606 0.41135 1.00000 0.02731 0.02427 0.03245 0.00092 0.00296 -0.00195 0.02904 0.00547 0.00018 0.00036 0.00013 0.00000 0.00167 0.00188 0.00174 0.00137 0.00126 0.00125 0.00071 H9A 0.53254 0.91638 0.37654 1.00000 0.03484 0.00000 0.00000 H9B 0.58265 0.88249 0.44299 1.00000 0.03484 0.00000 0.00000 C10 0.44546 0.90863 0.42728 1.00000 0.03006 0.02838 0.02159 -0.00487 -0.00094 0.00072 0.02826 0.00521 0.00018 0.00038 0.00012 0.00000 0.00166 0.00187 0.00152 0.00134 0.00118 0.00130 0.00069 H10A 0.44397 0.85181 0.46328 1.00000 0.03391 0.00000 0.00000 H10B 0.44887 1.02933 0.43492 1.00000 0.03391 0.00000 0.00000 C11 0.34972 0.96331 0.33199 1.00000 0.02719 0.02866 0.02274 0.00135 0.00574 0.00724 0.02641 0.00555 0.00019 0.00037 0.00011 0.00000 0.00162 0.00183 0.00157 0.00133 0.00117 0.00126 0.00068 H11A 0.40270 1.03447 0.33337 1.00000 0.03170 0.00000 0.00000 H11B 0.29572 1.03502 0.32601 1.00000 0.03170 0.00000 0.00000 C12 0.33671 0.84108 0.28409 1.00000 0.03628 0.02854 0.01715 0.00407 0.00473 0.00800 0.02783 0.00552 0.00020 0.00037 0.00011 0.00000 0.00174 0.00184 0.00147 0.00131 0.00119 0.00133 0.00069 H12A 0.39541 0.79133 0.28381 1.00000 0.03340 0.00000 0.00000 H12B 0.29570 0.75117 0.28906 1.00000 0.03340 0.00000 0.00000 C13 0.54897 0.99768 0.11897 1.00000 0.02112 0.01974 0.02284 -0.00284 0.00154 -0.00297 0.02211 0.00490 0.00017 0.00035 0.00011 0.00000 0.00151 0.00170 0.00153 0.00127 0.00113 0.00118 0.00064 C14 0.60246 0.92123 0.08832 1.00000 0.03695 0.02576 0.02933 -0.00237 0.01722 -0.00078 0.02907 0.00556 0.00019 0.00038 0.00012 0.00000 0.00178 0.00189 0.00169 0.00140 0.00135 0.00134 0.00071 H14 0.62325 0.81112 0.09759 1.00000 0.03489 0.00000 0.00000 C15 0.62525 1.00447 0.04477 1.00000 0.04310 0.03870 0.03463 -0.00833 0.02051 -0.00912 0.03686 0.00590 0.00021 0.00043 0.00013 0.00000 0.00194 0.00225 0.00192 0.00160 0.00148 0.00159 0.00081 H15 0.66193 0.95185 0.02412 1.00000 0.04424 0.00000 0.00000 C16 0.59504 1.16448 0.03084 1.00000 0.03750 0.03996 0.02490 0.00275 0.00277 -0.01617 0.03526 0.00554 0.00020 0.00043 0.00013 0.00000 0.00181 0.00219 0.00167 0.00154 0.00135 0.00154 0.00079 H16 0.61003 1.22089 0.00022 1.00000 0.04231 0.00000 0.00000 C17 0.54328 1.24196 0.06134 1.00000 0.03177 0.02714 0.03301 0.00591 0.00019 -0.00335 0.03235 0.00552 0.00019 0.00040 0.00013 0.00000 0.00175 0.00194 0.00179 0.00147 0.00135 0.00134 0.00075 H17 0.52314 1.35237 0.05198 1.00000 0.03882 0.00000 0.00000 C18 0.52048 1.16033 0.10542 1.00000 0.02218 0.02777 0.02721 0.00160 0.00178 0.00047 0.02670 0.00521 0.00018 0.00037 0.00012 0.00000 0.00151 0.00185 0.00164 0.00136 0.00118 0.00123 0.00068 H18 0.48528 1.21499 0.12661 1.00000 0.03204 0.00000 0.00000 C19 0.60959 0.89886 0.23775 1.00000 0.01840 0.02115 0.02003 0.00235 0.00521 -0.00007 0.01987 0.00502 0.00017 0.00034 0.00011 0.00000 0.00141 0.00167 0.00142 0.00125 0.00106 0.00116 0.00061 C20 0.61259 1.01905 0.27932 1.00000 0.02493 0.01884 0.02655 0.00183 0.00570 0.00040 0.02370 0.00518 0.00018 0.00035 0.00012 0.00000 0.00157 0.00168 0.00155 0.00131 0.00116 0.00119 0.00064 H20 0.56402 1.09519 0.27468 1.00000 0.02844 0.00000 0.00000 C21 0.68568 1.02860 0.32734 1.00000 0.03111 0.02436 0.02315 -0.00420 0.00595 -0.00539 0.02650 0.00527 0.00018 0.00037 0.00012 0.00000 0.00168 0.00179 0.00158 0.00131 0.00122 0.00131 0.00068 H21 0.68687 1.11047 0.35576 1.00000 0.03180 0.00000 0.00000 C22 0.75699 0.91978 0.33423 1.00000 0.02264 0.03365 0.02445 0.00244 -0.00011 -0.00375 0.02820 0.00543 0.00018 0.00037 0.00012 0.00000 0.00161 0.00200 0.00159 0.00142 0.00116 0.00131 0.00071 H22 0.80766 0.92802 0.36700 1.00000 0.03384 0.00000 0.00000 C23 0.75470 0.79921 0.29360 1.00000 0.02406 0.04196 0.03241 0.00062 0.00341 0.01062 0.03366 0.00576 0.00019 0.00041 0.00012 0.00000 0.00164 0.00219 0.00177 0.00158 0.00127 0.00141 0.00077 H23 0.80346 0.72335 0.29856 1.00000 0.04039 0.00000 0.00000 C24 0.68116 0.78847 0.24537 1.00000 0.02801 0.03115 0.02643 -0.00451 0.00578 0.00441 0.02885 0.00560 0.00018 0.00038 0.00012 0.00000 0.00162 0.00194 0.00162 0.00138 0.00123 0.00133 0.00071 H24 0.67978 0.70512 0.21741 1.00000 0.03463 0.00000 0.00000 N1 0.33017 0.70655 0.16249 1.00000 0.01893 0.01873 0.02225 -0.00028 0.00657 -0.00084 0.01979 0.00404 0.00013 0.00027 0.00009 0.00000 0.00120 0.00136 0.00121 0.00102 0.00091 0.00094 0.00051 N2 0.43216 0.98222 0.18728 1.00000 0.02121 0.01457 0.02708 -0.00331 0.00677 0.00003 0.02092 0.00408 0.00014 0.00027 0.00009 0.00000 0.00124 0.00133 0.00130 0.00101 0.00095 0.00093 0.00052 N3 0.50191 0.69604 0.15597 1.00000 0.01825 0.01640 0.02481 -0.00310 0.00412 0.00096 0.02017 0.00399 0.00013 0.00027 0.00009 0.00000 0.00118 0.00134 0.00124 0.00102 0.00091 0.00093 0.00051 O1 0.37931 0.54861 0.08091 1.00000 0.02632 0.02091 0.01839 -0.00372 0.00540 -0.00573 0.02201 0.00326 0.00011 0.00023 0.00007 0.00000 0.00106 0.00114 0.00100 0.00081 0.00077 0.00080 0.00044 O2 0.26641 1.00338 0.13145 1.00000 0.01748 0.02273 0.02266 0.00252 0.00183 -0.00005 0.02168 0.00332 0.00011 0.00023 0.00007 0.00000 0.00100 0.00115 0.00102 0.00084 0.00075 0.00078 0.00044 O3 0.41684 0.43035 0.17469 1.00000 0.03122 0.01588 0.01808 -0.00030 0.00668 0.00086 0.02174 0.00334 0.00012 0.00022 0.00007 0.00000 0.00109 0.00111 0.00099 0.00080 0.00078 0.00079 0.00043 O4 0.51064 0.39808 0.32838 1.00000 0.03551 0.02850 0.01721 0.00453 0.00282 0.00229 0.02794 0.00359 0.00013 0.00024 0.00007 0.00000 0.00116 0.00125 0.00101 0.00089 0.00081 0.00089 0.00047 O5 0.52409 0.68299 0.40069 1.00000 0.02420 0.02485 0.03341 -0.00186 0.00927 -0.00046 0.02722 0.00357 0.00012 0.00024 0.00008 0.00000 0.00106 0.00125 0.00116 0.00094 0.00084 0.00084 0.00047 O6 0.36358 0.87357 0.38419 1.00000 0.02499 0.03607 0.01925 0.00111 0.00309 0.00036 0.02735 0.00353 0.00012 0.00024 0.00008 0.00000 0.00105 0.00131 0.00101 0.00092 0.00077 0.00087 0.00047 O7 0.29802 0.92827 0.23075 1.00000 0.02564 0.02303 0.01978 0.00162 0.00670 0.00505 0.02272 0.00350 0.00012 0.00023 0.00007 0.00000 0.00105 0.00117 0.00099 0.00083 0.00076 0.00080 0.00044 F1 0.35004 0.39511 -0.02316 1.00000 0.04088 0.04466 0.02768 -0.00971 0.01024 0.00947 0.03757 0.00318 0.00011 0.00022 0.00007 0.00000 0.00107 0.00122 0.00096 0.00084 0.00077 0.00083 0.00045 F2 0.21548 0.32380 -0.02294 1.00000 0.05528 0.04555 0.03068 -0.00763 -0.00071 -0.02812 0.04629 0.00300 0.00012 0.00023 0.00007 0.00000 0.00118 0.00126 0.00101 0.00088 0.00082 0.00095 0.00051 F3 0.25101 0.58029 -0.02512 1.00000 0.03551 0.03271 0.02900 0.00345 0.00167 0.00604 0.03382 0.00307 0.00011 0.00021 0.00007 0.00000 0.00100 0.00113 0.00094 0.00081 0.00072 0.00078 0.00043 F4 0.18624 0.79248 0.04156 1.00000 0.04621 0.05424 0.04258 -0.02293 -0.00118 0.02111 0.05030 0.00338 0.00012 0.00024 0.00008 0.00000 0.00118 0.00138 0.00113 0.00098 0.00086 0.00096 0.00055 F5 0.14593 1.04340 0.02171 1.00000 0.04981 0.05413 0.02619 0.01075 0.00080 -0.00515 0.04527 0.00336 0.00012 0.00025 0.00007 0.00000 0.00120 0.00136 0.00100 0.00093 0.00081 0.00092 0.00050 F6 0.05335 0.87147 0.04226 1.00000 0.02922 0.04096 0.03818 -0.00693 -0.00602 -0.00321 0.03912 0.00297 0.00011 0.00022 0.00007 0.00000 0.00104 0.00118 0.00104 0.00086 0.00074 0.00079 0.00046 P1 0.40851 0.60711 0.14597 1.00000 0.02110 0.01721 0.01812 -0.00059 0.00404 0.00036 0.01907 0.00131 0.00004 0.00009 0.00003 0.00000 0.00038 0.00042 0.00037 0.00031 0.00028 0.00029 0.00018 P2 0.33745 0.89744 0.17773 1.00000 0.01848 0.01937 0.01826 -0.00039 0.00334 0.00176 0.01903 0.00131 0.00004 0.00009 0.00003 0.00000 0.00037 0.00043 0.00037 0.00031 0.00027 0.00029 0.00018 P3 0.51600 0.88728 0.17412 1.00000 0.01747 0.02002 0.02112 -0.00256 0.00370 0.00073 0.01985 0.00131 0.00004 0.00009 0.00003 0.00000 0.00037 0.00043 0.00038 0.00032 0.00028 0.00029 0.00018 Final Structure Factor Calculation for 01SRC946 in P2(1)/n Total number of l.s. parameters = 389 Maximum vector length = 511 Memory required = 4818 / 25039 wR2 = 0.1144 before cycle 5 for 6488 data and 0 / 389 parameters GooF = S = 0.977; Restrained GooF = 0.977 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0463 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0496 for 3777 Fo > 4sig(Fo) and 0.1175 for all 6488 data wR2 = 0.1144, GooF = S = 0.977, Restrained GooF = 0.977 for all data Occupancy sum of asymmetric unit = 43.00 for non-hydrogen and 30.00 for hydrogen atoms Principal mean square atomic displacements U 0.0391 0.0227 0.0181 C1 0.0332 0.0299 0.0176 C2 0.0273 0.0255 0.0170 C3 0.0337 0.0251 0.0219 C4 0.0295 0.0241 0.0191 C5 0.0336 0.0247 0.0193 C6 0.0426 0.0301 0.0178 C7 0.0371 0.0249 0.0192 C8 0.0380 0.0259 0.0233 C9 0.0394 0.0282 0.0172 C10 0.0354 0.0234 0.0204 C11 0.0419 0.0260 0.0156 C12 0.0282 0.0228 0.0154 C13 0.0406 0.0261 0.0205 C14 0.0548 0.0316 0.0242 C15 0.0588 0.0247 0.0223 C16 0.0473 0.0263 0.0234 C17 0.0325 0.0276 0.0200 C18 0.0231 0.0185 0.0180 C19 0.0281 0.0246 0.0184 C20 0.0342 0.0266 0.0187 C21 0.0383 0.0281 0.0182 C22 0.0479 0.0342 0.0189 C23 0.0378 0.0260 0.0227 C24 0.0224 0.0193 0.0177 N1 0.0280 0.0211 0.0137 N2 0.0272 0.0182 0.0151 N3 0.0300 0.0210 0.0151 O1 0.0273 0.0215 0.0162 O2 0.0316 0.0179 0.0157 O3 0.0383 0.0301 0.0154 O4 0.0338 0.0245 0.0234 O5 0.0361 0.0274 0.0186 O6 0.0295 0.0197 0.0189 O7 0.0565 0.0365 0.0198 F1 0.0827 0.0401 0.0161 F2 0.0440 0.0347 0.0228 F3 0.0953 0.0343 0.0214 F4 0.0669 0.0468 0.0221 F5 0.0564 0.0415 0.0195 F6 0.0222 0.0181 0.0169 P1 0.0220 0.0184 0.0167 P2 0.0243 0.0180 0.0172 P3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.015 0.022 0.030 0.038 0.049 0.062 0.084 0.119 1.000 Number in group 681. 697. 604. 671. 593. 667. 625. 667. 636. 647. GooF 0.848 0.913 0.866 0.978 1.044 1.082 1.030 0.974 0.998 1.019 K 3.793 0.842 0.977 0.934 0.964 0.960 0.994 0.998 1.017 1.017 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.15 1.32 1.66 inf Number in group 679. 626. 643. 662. 653. 628. 658. 645. 646. 648. GooF 0.847 0.873 0.927 0.910 0.935 1.001 1.004 1.003 0.962 1.253 K 1.064 1.056 0.999 1.004 1.008 1.011 1.007 1.027 1.027 0.997 R1 0.329 0.274 0.238 0.197 0.147 0.108 0.070 0.051 0.046 0.035 Recommended weighting scheme: WGHT 0.0447 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) 1 3 0 913.04 724.59 4.00 0.071 2.65 -5 1 6 2440.61 2966.25 3.90 0.144 2.60 -1 7 12 25.17 194.52 3.83 0.037 1.00 -5 2 7 353.33 254.34 3.82 0.042 2.18 12 4 6 325.87 216.23 3.65 0.039 0.96 10 2 16 47.17 184.29 3.63 0.036 0.90 9 3 7 105.71 198.19 3.56 0.037 1.20 8 4 20 -175.39 218.79 3.55 0.039 0.81 7 3 22 -146.30 268.97 3.52 0.043 0.82 9 4 8 58.57 169.93 3.47 0.034 1.09 0 4 3 693.91 560.76 3.46 0.063 1.95 -2 5 17 75.52 193.45 3.45 0.037 1.06 -15 0 21 700.46 128.78 3.43 0.030 0.86 0 3 16 211.02 298.63 3.43 0.046 1.28 -11 8 1 -58.74 323.30 3.42 0.048 0.81 -13 3 14 130.92 25.29 3.41 0.013 1.01 -8 2 6 1742.98 1463.45 3.41 0.101 1.71 -3 1 11 167.77 266.84 3.34 0.043 2.10 -1 9 8 -58.74 311.72 3.32 0.047 0.86 5 0 11 509.15 387.53 3.28 0.052 1.53 -10 0 2 58.74 241.55 3.25 0.041 1.52 -5 2 1 208.99 119.31 3.15 0.029 2.43 8 8 3 335.53 764.96 3.15 0.073 0.87 -3 1 1 349.20 174.70 3.11 0.035 4.32 2 4 1 455.52 354.26 3.10 0.050 1.93 12 1 11 3792.64 3161.70 3.10 0.149 0.95 10 7 10 642.27 129.63 3.08 0.030 0.80 -13 5 1 109.95 211.00 3.07 0.038 0.94 -5 2 14 519.94 639.09 3.06 0.067 1.53 -8 3 7 128.77 208.16 3.04 0.038 1.52 -7 2 3 1644.37 1403.36 3.04 0.099 1.93 -6 1 3 297.65 394.57 3.04 0.053 2.44 2 5 4 437.47 583.67 3.04 0.064 1.50 -5 4 20 46.11 207.16 3.03 0.038 1.03 -4 3 5 116.97 194.87 3.02 0.037 2.10 1 5 20 33.50 145.26 3.00 0.032 0.93 4 6 5 203.43 298.10 2.96 0.046 1.19 -7 1 5 1493.56 1286.26 2.96 0.095 2.09 14 1 10 58.19 290.71 2.95 0.045 0.87 0 4 5 2101.85 1796.45 2.93 0.112 1.85 -1 7 4 16.63 114.35 2.91 0.028 1.13 -16 3 12 79.20 199.30 2.90 0.037 0.89 6 2 1 4782.20 5511.46 2.90 0.196 2.05 8 9 3 -117.20 110.54 2.90 0.028 0.79 5 1 0 2971.15 3431.49 2.90 0.155 2.78 -6 1 9 1189.87 1390.84 2.87 0.099 2.03 3 1 17 299.12 401.80 2.86 0.053 1.22 2 7 5 126.99 26.22 2.86 0.014 1.10 3 2 9 504.74 419.50 2.84 0.054 1.84 9 1 17 29.42 121.48 2.84 0.029 0.93 Bond lengths and angles C1 - Distance Angles O1 1.4315 (0.0031) C2 1.4857 (0.0038) 107.08 (0.21) H1A 0.9900 110.30 110.30 H1B 0.9900 110.30 110.30 108.55 C1 - O1 C2 H1A C2 - Distance Angles F1 1.3318 (0.0031) F3 1.3333 (0.0033) 105.76 (0.23) F2 1.3378 (0.0031) 107.29 (0.23) 106.83 (0.22) C1 1.4857 (0.0038) 112.95 (0.23) 113.39 (0.24) 110.21 (0.23) C2 - F1 F3 F2 C3 - Distance Angles O2 1.4344 (0.0030) C4 1.4861 (0.0038) 108.80 (0.21) H3A 0.9900 109.93 109.93 H3B 0.9900 109.93 109.93 108.32 C3 - O2 C4 H3A C4 - Distance Angles F5 1.3215 (0.0033) F6 1.3393 (0.0032) 107.21 (0.22) F4 1.3403 (0.0032) 106.54 (0.23) 106.42 (0.24) C3 1.4861 (0.0038) 113.02 (0.25) 110.49 (0.23) 112.77 (0.23) C4 - F5 F6 F4 C5 - Distance Angles O3 1.4410 (0.0030) C6 1.5014 (0.0038) 110.85 (0.21) H5A 0.9900 109.47 109.47 H5B 0.9900 109.47 109.47 108.05 C5 - O3 C6 H5A C6 - Distance Angles O4 1.4154 (0.0031) C5 1.5014 (0.0038) 105.64 (0.21) H6A 0.9900 110.61 110.61 H6B 0.9900 110.61 110.61 108.75 C6 - O4 C5 H6A C7 - Distance Angles O4 1.4289 (0.0032) C8 1.4972 (0.0040) 114.91 (0.22) H7A 0.9900 108.54 108.54 H7B 0.9900 108.54 108.54 107.53 C7 - O4 C8 H7A C8 - Distance Angles O5 1.4193 (0.0031) C7 1.4972 (0.0040) 108.78 (0.23) H8A 0.9900 109.93 109.93 H8B 0.9900 109.93 109.93 108.33 C8 - O5 C7 H8A C9 - Distance Angles O5 1.4183 (0.0034) C10 1.4906 (0.0038) 109.10 (0.23) H9A 0.9900 109.86 109.86 H9B 0.9900 109.86 109.86 108.28 C9 - O5 C10 H9A C10 - Distance Angles O6 1.4264 (0.0031) C9 1.4906 (0.0038) 113.66 (0.23) H10A 0.9900 108.83 108.83 H10B 0.9900 108.83 108.83 107.69 C10 - O6 C9 H10A C11 - Distance Angles O6 1.4204 (0.0032) C12 1.4929 (0.0039) 108.00 (0.24) H11A 0.9900 110.10 110.10 H11B 0.9900 110.10 110.10 108.43 C11 - O6 C12 H11A C12 - Distance Angles O7 1.4472 (0.0031) C11 1.4929 (0.0039) 107.83 (0.23) H12A 0.9900 110.14 110.14 H12B 0.9900 110.14 110.14 108.45 C12 - O7 C11 H12A C13 - Distance Angles C14 1.3932 (0.0038) C18 1.3939 (0.0039) 119.03 (0.26) P3 1.7893 (0.0028) 120.37 (0.22) 120.59 (0.21) C13 - C14 C18 C14 - Distance Angles C15 1.3735 (0.0040) C13 1.3932 (0.0038) 120.24 (0.29) H14 0.9500 119.88 119.88 C14 - C15 C13 C15 - Distance Angles C14 1.3735 (0.0040) C16 1.3822 (0.0046) 120.29 (0.29) H15 0.9500 119.85 119.85 C15 - C14 C16 C16 - Distance Angles C17 1.3751 (0.0043) C15 1.3822 (0.0046) 119.95 (0.29) H16 0.9500 120.03 120.03 C16 - C17 C15 C17 - Distance Angles C16 1.3751 (0.0043) C18 1.3779 (0.0039) 120.36 (0.30) H17 0.9500 119.82 119.82 C17 - C16 C18 C18 - Distance Angles C17 1.3779 (0.0039) C13 1.3939 (0.0039) 120.11 (0.28) H18 0.9500 119.94 119.94 C18 - C17 C13 C19 - Distance Angles C24 1.3888 (0.0037) C20 1.3887 (0.0037) 118.93 (0.24) P3 1.7998 (0.0026) 119.99 (0.21) 121.07 (0.20) C19 - C24 C20 C20 - Distance Angles C21 1.3802 (0.0037) C19 1.3887 (0.0037) 120.43 (0.25) H20 0.9500 119.78 119.78 C20 - C21 C19 C21 - Distance Angles C22 1.3792 (0.0039) C20 1.3802 (0.0037) 120.27 (0.27) H21 0.9500 119.86 119.86 C21 - C22 C20 C22 - Distance Angles C23 1.3767 (0.0040) C21 1.3792 (0.0039) 119.96 (0.25) H22 0.9500 120.02 120.02 C22 - C23 C21 C23 - Distance Angles C22 1.3767 (0.0040) C24 1.3879 (0.0038) 120.01 (0.27) H23 0.9500 119.99 119.99 C23 - C22 C24 C24 - Distance Angles C23 1.3879 (0.0038) C19 1.3888 (0.0037) 120.38 (0.27) H24 0.9500 119.81 119.81 C24 - C23 C19 N1 - Distance Angles P2 1.5805 (0.0023) P1 1.5874 (0.0022) 122.76 (0.13) N1 - P2 N2 - Distance Angles P2 1.5685 (0.0022) P3 1.6050 (0.0022) 121.81 (0.14) N2 - P2 N3 - Distance Angles P1 1.5645 (0.0022) P3 1.6027 (0.0023) 122.24 (0.13) N3 - P1 O1 - Distance Angles C1 1.4315 (0.0031) P1 1.5861 (0.0018) 119.89 (0.16) O1 - C1 O2 - Distance Angles C3 1.4344 (0.0030) P2 1.5840 (0.0018) 119.68 (0.17) O2 - C3 O3 - Distance Angles C5 1.4410 (0.0030) P1 1.5763 (0.0019) 123.76 (0.17) O3 - C5 O4 - Distance Angles C6 1.4154 (0.0031) C7 1.4289 (0.0032) 113.45 (0.21) O4 - C6 O5 - Distance Angles C9 1.4183 (0.0034) C8 1.4193 (0.0031) 111.71 (0.21) O5 - C9 O6 - Distance Angles C11 1.4204 (0.0032) C10 1.4264 (0.0032) 115.88 (0.21) O6 - C11 O7 - Distance Angles C12 1.4472 (0.0031) P2 1.5814 (0.0018) 119.43 (0.17) O7 - C12 F1 - Distance Angles C2 1.3318 (0.0031) F1 - F2 - Distance Angles C2 1.3378 (0.0031) F2 - F3 - Distance Angles C2 1.3333 (0.0033) F3 - F4 - Distance Angles C4 1.3403 (0.0032) F4 - F5 - Distance Angles C4 1.3215 (0.0033) F5 - F6 - Distance Angles C4 1.3393 (0.0032) F6 - P1 - Distance Angles N3 1.5645 (0.0022) O3 1.5763 (0.0019) 112.73 (0.11) O1 1.5861 (0.0018) 106.78 (0.11) 97.76 (0.10) N1 1.5874 (0.0022) 117.24 (0.12) 108.79 (0.11) 111.83 (0.11) P1 - N3 O3 O1 P2 - Distance Angles N2 1.5685 (0.0022) N1 1.5805 (0.0023) 117.58 (0.12) O7 1.5814 (0.0018) 111.04 (0.11) 108.91 (0.11) O2 1.5840 (0.0018) 107.59 (0.11) 111.70 (0.11) 98.33 (0.10) P2 - N2 N1 O7 P3 - Distance Angles N3 1.6027 (0.0023) N2 1.6050 (0.0022) 117.27 (0.11) C13 1.7893 (0.0028) 108.64 (0.12) 108.51 (0.13) C19 1.7998 (0.0026) 107.51 (0.12) 107.68 (0.12) 106.76 (0.12) P3 - N3 N2 C13 Selected torsion angles 57.50 ( 0.31) O1 - C1 - C2 - F1 -62.81 ( 0.30) O1 - C1 - C2 - F3 177.49 ( 0.22) O1 - C1 - C2 - F2 -62.92 ( 0.29) O2 - C3 - C4 - F5 176.95 ( 0.22) O2 - C3 - C4 - F6 57.99 ( 0.32) O2 - C3 - C4 - F4 -171.26 ( 0.21) O3 - C5 - C6 - O4 58.32 ( 0.31) O4 - C7 - C8 - O5 -58.92 ( 0.32) O5 - C9 - C10 - O6 164.20 ( 0.21) O6 - C11 - C12 - O7 -1.14 ( 0.41) C18 - C13 - C14 - C15 177.90 ( 0.22) P3 - C13 - C14 - C15 -0.24 ( 0.44) C13 - C14 - C15 - C16 1.16 ( 0.45) C14 - C15 - C16 - C17 -0.68 ( 0.44) C15 - C16 - C17 - C18 -0.71 ( 0.41) C16 - C17 - C18 - C13 1.61 ( 0.39) C14 - C13 - C18 - C17 -177.42 ( 0.20) P3 - C13 - C18 - C17 0.12 ( 0.40) C24 - C19 - C20 - C21 -178.65 ( 0.21) P3 - C19 - C20 - C21 0.67 ( 0.42) C19 - C20 - C21 - C22 -1.12 ( 0.43) C20 - C21 - C22 - C23 0.79 ( 0.44) C21 - C22 - C23 - C24 0.01 ( 0.45) C22 - C23 - C24 - C19 -0.46 ( 0.42) C20 - C19 - C24 - C23 178.33 ( 0.23) P3 - C19 - C24 - C23 166.95 ( 0.18) C2 - C1 - O1 - P1 -119.16 ( 0.21) C4 - C3 - O2 - P2 -73.47 ( 0.26) C6 - C5 - O3 - P1 -176.88 ( 0.22) C5 - C6 - O4 - C7 67.26 ( 0.31) C8 - C7 - O4 - C6 178.64 ( 0.22) C10 - C9 - O5 - C8 -178.48 ( 0.22) C7 - C8 - O5 - C9 123.11 ( 0.25) C12 - C11 - O6 - C10 -66.47 ( 0.32) C9 - C10 - O6 - C11 134.71 ( 0.20) C11 - C12 - O7 - P2 -135.42 ( 0.14) P3 - N3 - P1 - O3 118.37 ( 0.15) P3 - N3 - P1 - O1 -7.94 ( 0.21) P3 - N3 - P1 - N1 84.06 ( 0.20) C5 - O3 - P1 - N3 -164.04 ( 0.18) C5 - O3 - P1 - O1 -47.75 ( 0.21) C5 - O3 - P1 - N1 167.00 ( 0.20) C1 - O1 - P1 - N3 50.36 ( 0.21) C1 - O1 - P1 - O3 -63.51 ( 0.22) C1 - O1 - P1 - N1 10.94 ( 0.21) P2 - N1 - P1 - N3 140.30 ( 0.14) P2 - N1 - P1 - O3 -112.85 ( 0.15) P2 - N1 - P1 - O1 7.96 ( 0.21) P3 - N2 - P2 - N1 134.31 ( 0.15) P3 - N2 - P2 - O7 -119.14 ( 0.16) P3 - N2 - P2 - O2 -10.97 ( 0.21) P1 - N1 - P2 - N2 -138.35 ( 0.14) P1 - N1 - P2 - O7 114.12 ( 0.15) P1 - N1 - P2 - O2 -73.23 ( 0.22) C12 - O7 - P2 - N2 57.78 ( 0.22) C12 - O7 - P2 - N1 174.21 ( 0.19) C12 - O7 - P2 - O2 -174.73 ( 0.18) C3 - O2 - P2 - N2 54.81 ( 0.21) C3 - O2 - P2 - N1 -59.45 ( 0.19) C3 - O2 - P2 - O7 5.26 ( 0.21) P1 - N3 - P3 - N2 -118.16 ( 0.16) P1 - N3 - P3 - C13 126.65 ( 0.16) P1 - N3 - P3 - C19 -5.23 ( 0.21) P2 - N2 - P3 - N3 118.26 ( 0.16) P2 - N2 - P3 - C13 -126.53 ( 0.16) P2 - N2 - P3 - C19 -33.91 ( 0.26) C14 - C13 - P3 - N3 145.11 ( 0.21) C18 - C13 - P3 - N3 -162.43 ( 0.22) C14 - C13 - P3 - N2 16.59 ( 0.25) C18 - C13 - P3 - N2 81.76 ( 0.25) C14 - C13 - P3 - C19 -99.22 ( 0.22) C18 - C13 - P3 - C19 33.51 ( 0.25) C24 - C19 - P3 - N3 -147.73 ( 0.21) C20 - C19 - P3 - N3 160.72 ( 0.22) C24 - C19 - P3 - N2 -20.51 ( 0.25) C20 - C19 - P3 - N2 -82.92 ( 0.25) C24 - C19 - P3 - C13 95.85 ( 0.23) C20 - C19 - P3 - C13 FMAP and GRID set by program FMAP 2 3 31 GRID -0.893 -2 -2 0.893 2 2 R1 = 0.1171 for 6488 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.38 at 0.5618 0.8737 0.2173 [ 0.79 A from C19 ] Deepest hole -0.38 at 0.3416 0.9119 0.1425 [ 0.88 A from P2 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4566 / 28982 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5618 0.8737 0.2173 1.00000 0.05 0.38 0.79 C19 1.09 P3 1.90 C20 1.90 C24 Q2 1 0.4410 0.6031 0.2073 1.00000 0.05 0.34 1.43 P1 1.59 O3 1.70 H6B 1.80 C5 Q3 1 0.3395 0.3272 0.1803 1.00000 0.05 0.33 1.49 O3 1.59 H5A 1.65 C5 1.86 H5B Q4 1 0.5794 0.5997 0.1412 1.00000 0.05 0.31 1.55 N3 2.21 H14 2.23 H24 2.27 H22 Q5 1 0.4796 0.6193 0.1679 1.00000 0.05 0.31 0.80 N3 1.08 P1 1.84 O3 2.23 P3 Q6 1 0.7750 0.8500 0.3927 1.00000 0.05 0.31 1.10 H22 1.48 C22 2.19 F3 2.30 C21 Q7 1 0.2495 0.8772 0.0068 1.00000 0.05 0.29 1.60 F4 2.19 F5 2.21 H15 2.30 H8A Q8 1 0.5405 0.3981 0.4133 1.00000 0.05 0.29 0.81 H7B 1.46 C7 1.98 O4 2.03 F6 Q9 1 0.3412 0.4808 0.0705 1.00000 0.05 0.28 0.64 C1 0.79 O1 1.33 H1B 1.38 H1A Q10 1 0.7343 0.7835 0.1712 1.00000 0.05 0.28 1.69 H24 2.07 H21 2.12 H14 2.17 C24 Shortest distances between peaks (including symmetry equivalents) 2 5 1.26 4 5 1.83 1 5 2.53 2 3 2.69 4 10 2.73 1 2 2.83 5 9 2.93 1 4 2.94 3 9 2.94 2 4 2.99 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. 0.55: 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 3.36: Structure factors and derivatives 9.69: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.44: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.16: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.17: Fourier summations 0.00: Peaksearch 0.05: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 11:26:36 Total elapsed time: 14.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++