+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0018pna21 started at 12:47:52 on 06-May-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0018pna21 in Pna2(1) CELL 0.71073 11.5504 22.2264 6.6309 90.000 90.000 90.000 ZERR 4.00 0.0007 0.0010 0.0004 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H N O UNIT 60 124 4 16 V = 1702.31 F(000) = 640.0 Mu = 0.08 mm-1 Cell Wt = 1157.63 Rho = 1.129 MERG 4 OMIT -3.00 55.00 OMIT 2 0 0 SHEL 7 0.77 HTAB N25 O7A EQIV_$1 x-1/2, -y+1/2, z-1 HTAB O1B O7B_$1 EQIV_$2 -x+1, -y+1, z-1/2 HTAB N25 O7B_$2 EQIV_$3 x, y, z-1 HTAB N25 O7B_$3 FMAP 2 PLAN 10 SIZE 0.04 0.10 0.18 ACTA CONF BOND $H WGHT 0.00000 2.42320 L.S. 4 TEMP -153.00 FVAR 0.81301 MOLE 1 C1 1 0.162984 0.159356 -0.150943 11.00000 0.03009 0.02218 = 0.03172 0.00234 0.00286 0.00320 C2 1 0.262585 0.190957 -0.049265 11.00000 0.02739 0.02689 = 0.02900 -0.00577 0.00040 -0.00028 AFIX 23 H2A 2 0.270375 0.231886 -0.106583 11.00000 -1.20000 H2B 2 0.335021 0.168788 -0.078393 11.00000 -1.20000 AFIX 0 C3 1 0.247536 0.195757 0.176160 11.00000 0.06614 0.03805 = 0.03389 0.00019 0.00011 -0.02658 AFIX 23 H3A 2 0.236556 0.154828 0.231868 11.00000 -1.20000 H3B 2 0.176198 0.218977 0.204296 11.00000 -1.20000 AFIX 0 C4 1 0.349271 0.225837 0.286721 11.00000 0.06449 0.03043 = 0.02800 -0.00027 -0.01002 -0.01063 AFIX 23 H4A 2 0.339240 0.220205 0.433790 11.00000 -1.20000 H4B 2 0.422148 0.205635 0.246847 11.00000 -1.20000 AFIX 0 C5 1 0.359546 0.293007 0.241729 11.00000 0.03042 0.02576 = 0.02719 -0.00219 0.00002 -0.00160 AFIX 23 H5A 2 0.387513 0.298663 0.101879 11.00000 -1.20000 H5B 2 0.282286 0.312008 0.252804 11.00000 -1.20000 AFIX 0 C6 1 0.442701 0.323425 0.387426 11.00000 0.02435 0.02054 = 0.02518 0.00347 -0.00157 0.00324 AFIX 23 H6A 2 0.520091 0.304923 0.370941 11.00000 -1.20000 H6B 2 0.416525 0.314964 0.526737 11.00000 -1.20000 AFIX 0 C7 1 0.454984 0.391270 0.363071 11.00000 0.02540 0.02329 = 0.02170 0.00158 0.00520 0.00461 O1A 4 0.074652 0.144628 -0.066792 11.00000 0.03299 0.05540 = 0.03790 -0.01059 0.00761 -0.01344 O1B 4 0.184244 0.147153 -0.342532 11.00000 0.03011 0.04019 = 0.03112 -0.00386 0.00019 -0.00588 AFIX 147 H1 2 0.127867 0.128394 -0.392033 11.00000 0.07294 AFIX 0 O7A 4 0.395850 0.418660 0.237388 11.00000 0.03290 0.02751 = 0.02302 0.00358 -0.00008 0.00367 O7B 4 0.525221 0.417364 0.485069 11.00000 0.02932 0.02264 = 0.02534 0.00110 -0.00280 -0.00092 MOLE 2 C21 1 0.099560 0.324148 -0.292536 11.00000 0.03462 0.02550 = 0.05515 0.00701 -0.00752 -0.00292 AFIX 137 H21A 2 0.105571 0.313800 -0.149253 11.00000 -1.50000 H21B 2 0.161143 0.303741 -0.367748 11.00000 -1.50000 H21C 2 0.024018 0.311278 -0.344178 11.00000 -1.50000 AFIX 0 C22 1 0.112095 0.392946 -0.318448 11.00000 0.02615 0.02528 = 0.03618 0.00386 -0.00136 -0.00054 C23 1 0.234230 0.408321 -0.233169 11.00000 0.02517 0.02325 = 0.02326 0.00472 -0.00034 0.00185 AFIX 23 H23A 2 0.239814 0.388590 -0.099670 11.00000 -1.20000 H23B 2 0.291161 0.388045 -0.321698 11.00000 -1.20000 AFIX 0 C24 1 0.277163 0.473588 -0.204842 11.00000 0.01925 0.02415 = 0.02436 0.00253 -0.00135 -0.00088 C26 1 0.012814 0.423012 -0.205076 11.00000 0.02737 0.03658 = 0.04510 0.00012 0.00265 -0.00547 AFIX 137 H26A 2 0.013725 0.466370 -0.231886 11.00000 -1.50000 H26B 2 0.021916 0.415997 -0.060030 11.00000 -1.50000 H26C 2 -0.060983 0.405986 -0.250474 11.00000 -1.50000 AFIX 0 C27 1 0.101943 0.407137 -0.544458 11.00000 0.03349 0.03604 = 0.02962 -0.00356 -0.00758 0.00027 AFIX 137 H27A 2 0.030988 0.389008 -0.598067 11.00000 -1.50000 H27B 2 0.169133 0.390628 -0.615752 11.00000 -1.50000 H27C 2 0.099231 0.450828 -0.563758 11.00000 -1.50000 AFIX 0 C28 1 0.220264 0.505644 -0.028061 11.00000 0.02925 0.02935 = 0.02973 -0.00066 0.00218 0.00014 AFIX 137 H28A 2 0.223108 0.479736 0.091425 11.00000 -1.50000 H28B 2 0.139413 0.514599 -0.061340 11.00000 -1.50000 H28C 2 0.261610 0.543249 -0.000371 11.00000 -1.50000 AFIX 0 C29 1 0.275113 0.512640 -0.392721 11.00000 0.03077 0.02340 = 0.03130 0.00231 0.00014 -0.00042 AFIX 137 H29A 2 0.321852 0.548801 -0.369868 11.00000 -1.50000 H29B 2 0.195148 0.524325 -0.422834 11.00000 -1.50000 H29C 2 0.307015 0.489995 -0.506709 11.00000 -1.50000 AFIX 0 N25 3 0.404111 0.466556 -0.147567 11.00000 0.02640 0.02190 = 0.02309 -0.00135 0.00008 -0.00303 AFIX 137 H25A 2 0.409968 0.442745 -0.036393 11.00000 0.03489 H25B 2 0.434891 0.503361 -0.120387 11.00000 0.04659 H25C 2 0.443338 0.449358 -0.251691 11.00000 0.02732 AFIX 0 HKLF 4 Covalent radii and connectivity table for 07skc0018pna21 in Pna2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C1 C3 C3 - C2 C4 C4 - C5 C3 C5 - C6 C4 C6 - C5 C7 C7 - O7A O7B C6 O1A - C1 O1B - C1 O7A - C7 O7B - C7 C21 - C22 C22 - C26 C27 C21 C23 C23 - C24 C22 C24 - C29 C28 N25 C23 C26 - C22 C27 - C22 C28 - C24 C29 - C24 N25 - C24 Operators for generating equivalent atoms: $1 x-1/2, -y+1/2, z-1 $2 -x+1, -y+1, z-1/2 $3 x, y, z-1 Floating origin restraints generated 10325 Reflections read, of which 448 rejected -14 =< h =< 13, -28 =< k =< 28, -5 =< l =< 8, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2112 Unique reflections, of which 0 suppressed R(int) = 0.0658 R(sigma) = 0.0590 Friedel opposites merged Maximum memory for data reduction = 2742 / 20528 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 = 3357 / 238131 wR2 = 0.1390 before cycle 1 for 2112 data and 192 / 192 parameters GooF = S = 1.115; Restrained GooF = 1.114 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.81301 0.00210 -0.002 OSF Mean shift/esd = 0.001 Maximum = 0.002 for y O7B Max. shift = 0.000 A for H28B Max. dU = 0.000 for H1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3357 / 238131 wR2 = 0.1390 before cycle 2 for 2112 data and 192 / 192 parameters GooF = S = 1.115; Restrained GooF = 1.114 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.81300 0.00210 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y O7A Max. shift = 0.000 A for H27A Max. dU = 0.000 for H1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3357 / 238131 wR2 = 0.1390 before cycle 3 for 2112 data and 192 / 192 parameters GooF = S = 1.115; Restrained GooF = 1.114 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.81300 0.00210 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H26C Max. dU = 0.000 for H1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3357 / 238131 wR2 = 0.1390 before cycle 4 for 2112 data and 192 / 192 parameters GooF = S = 1.115; Restrained GooF = 1.114 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.81300 0.00210 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C29 Max. shift = 0.000 A for H26C Max. dU = 0.000 for H1 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 H2A 0.2704 0.2319 -0.1066 23 0.990 0.000 C2 C1 C3 H2B 0.3350 0.1688 -0.0784 23 0.990 0.000 C2 C1 C3 H3A 0.2366 0.1548 0.2319 23 0.990 0.000 C3 C2 C4 H3B 0.1762 0.2190 0.2043 23 0.990 0.000 C3 C2 C4 H4A 0.3392 0.2202 0.4338 23 0.990 0.000 C4 C5 C3 H4B 0.4221 0.2056 0.2468 23 0.990 0.000 C4 C5 C3 H5A 0.3875 0.2987 0.1019 23 0.990 0.000 C5 C6 C4 H5B 0.2823 0.3120 0.2528 23 0.990 0.000 C5 C6 C4 H6A 0.5201 0.3049 0.3709 23 0.990 0.000 C6 C5 C7 H6B 0.4165 0.3150 0.5267 23 0.990 0.000 C6 C5 C7 H1 0.1279 0.1284 -0.3920 147 0.840 0.000 O1B C1 H1 H21A 0.1056 0.3138 -0.1493 137 0.980 0.000 C21 C22 H21A H21B 0.1611 0.3037 -0.3677 137 0.980 0.000 C21 C22 H21A H21C 0.0240 0.3113 -0.3442 137 0.980 0.000 C21 C22 H21A H23A 0.2398 0.3886 -0.0997 23 0.990 0.000 C23 C24 C22 H23B 0.2912 0.3880 -0.3217 23 0.990 0.000 C23 C24 C22 H26A 0.0137 0.4664 -0.2319 137 0.980 0.000 C26 C22 H26A H26B 0.0219 0.4160 -0.0600 137 0.980 0.000 C26 C22 H26A H26C -0.0610 0.4060 -0.2505 137 0.980 0.000 C26 C22 H26A H27A 0.0310 0.3890 -0.5981 137 0.980 0.000 C27 C22 H27A H27B 0.1691 0.3906 -0.6158 137 0.980 0.000 C27 C22 H27A H27C 0.0992 0.4508 -0.5638 137 0.980 0.000 C27 C22 H27A H28A 0.2231 0.4797 0.0914 137 0.980 0.000 C28 C24 H28A H28B 0.1394 0.5146 -0.0613 137 0.980 0.000 C28 C24 H28A H28C 0.2616 0.5432 -0.0004 137 0.980 0.000 C28 C24 H28A H29A 0.3219 0.5488 -0.3699 137 0.980 0.000 C29 C24 H29A H29B 0.1951 0.5243 -0.4228 137 0.980 0.000 C29 C24 H29A H29C 0.3070 0.4900 -0.5067 137 0.980 0.000 C29 C24 H29A H25A 0.4100 0.4427 -0.0364 137 0.910 0.000 N25 C24 H25A H25B 0.4349 0.5034 -0.1204 137 0.910 0.000 N25 C24 H25A H25C 0.4433 0.4494 -0.2517 137 0.910 0.000 N25 C24 H25A 07skc0018pna21 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.16298 0.15936 -0.15094 1.00000 0.03009 0.02217 0.03172 0.00234 0.00286 0.00320 0.02800 0.00810 0.00039 0.00019 0.00077 0.00000 0.00234 0.00207 0.00267 0.00200 0.00215 0.00178 0.00102 C2 0.26259 0.19096 -0.04927 1.00000 0.02739 0.02689 0.02900 -0.00577 0.00040 -0.00028 0.02776 0.00773 0.00037 0.00020 0.00078 0.00000 0.00213 0.00214 0.00249 0.00211 0.00213 0.00174 0.00097 H2A 0.27038 0.23189 -0.10658 1.00000 0.03331 0.00000 0.00000 H2B 0.33502 0.16879 -0.07839 1.00000 0.03331 0.00000 0.00000 C3 0.24754 0.19576 0.17616 1.00000 0.06614 0.03805 0.03389 0.00019 0.00011 -0.02658 0.04603 0.00875 0.00052 0.00023 0.00084 0.00000 0.00367 0.00266 0.00303 0.00249 0.00285 0.00264 0.00141 H3A 0.23656 0.15483 0.23187 1.00000 0.05523 0.00000 0.00000 H3B 0.17620 0.21898 0.20430 1.00000 0.05523 0.00000 0.00000 C4 0.34927 0.22584 0.28672 1.00000 0.06449 0.03043 0.02800 -0.00027 -0.01002 -0.01063 0.04097 0.00822 0.00047 0.00019 0.00083 0.00000 0.00340 0.00236 0.00279 0.00224 0.00274 0.00236 0.00128 H4A 0.33924 0.22020 0.43379 1.00000 0.04917 0.00000 0.00000 H4B 0.42215 0.20563 0.24685 1.00000 0.04917 0.00000 0.00000 C5 0.35955 0.29301 0.24173 1.00000 0.03042 0.02575 0.02719 -0.00219 0.00002 -0.00160 0.02779 0.00730 0.00037 0.00017 0.00074 0.00000 0.00222 0.00199 0.00249 0.00196 0.00210 0.00176 0.00098 H5A 0.38751 0.29866 0.10188 1.00000 0.03334 0.00000 0.00000 H5B 0.28229 0.31201 0.25280 1.00000 0.03334 0.00000 0.00000 C6 0.44270 0.32343 0.38743 1.00000 0.02435 0.02054 0.02518 0.00347 -0.00157 0.00324 0.02336 0.00727 0.00035 0.00016 0.00070 0.00000 0.00203 0.00189 0.00241 0.00178 0.00182 0.00157 0.00093 H6A 0.52009 0.30492 0.37094 1.00000 0.02803 0.00000 0.00000 H6B 0.41653 0.31496 0.52674 1.00000 0.02803 0.00000 0.00000 C7 0.45498 0.39127 0.36307 1.00000 0.02540 0.02329 0.02170 0.00158 0.00520 0.00461 0.02346 0.00779 0.00036 0.00017 0.00073 0.00000 0.00199 0.00194 0.00210 0.00193 0.00191 0.00174 0.00087 O1A 0.07465 0.14463 -0.06679 1.00000 0.03299 0.05540 0.03790 -0.01059 0.00761 -0.01344 0.04210 0.00583 0.00028 0.00016 0.00059 0.00000 0.00170 0.00212 0.00218 0.00182 0.00172 0.00157 0.00091 O1B 0.18424 0.14715 -0.34253 1.00000 0.03011 0.04019 0.03112 -0.00386 0.00019 -0.00588 0.03381 0.00579 0.00029 0.00015 0.00051 0.00000 0.00172 0.00188 0.00197 0.00160 0.00157 0.00148 0.00080 H1 0.12787 0.12839 -0.39203 1.00000 0.07291 0.00000 0.02313 O7A 0.39585 0.41866 0.23739 1.00000 0.03290 0.02751 0.02302 0.00358 -0.00008 0.00367 0.02781 0.00518 0.00025 0.00012 0.00048 0.00000 0.00157 0.00144 0.00173 0.00138 0.00150 0.00131 0.00071 O7B 0.52522 0.41736 0.48507 1.00000 0.02932 0.02264 0.02534 0.00110 -0.00280 -0.00092 0.02577 0.00496 0.00024 0.00012 0.00048 0.00000 0.00151 0.00133 0.00172 0.00137 0.00144 0.00123 0.00068 C21 0.09956 0.32415 -0.29254 1.00000 0.03462 0.02549 0.05515 0.00701 -0.00752 -0.00292 0.03842 0.00869 0.00042 0.00018 0.00092 0.00000 0.00242 0.00213 0.00378 0.00236 0.00267 0.00202 0.00130 H21A 0.10557 0.31380 -0.14925 1.00000 0.05763 0.00000 0.00000 H21B 0.16114 0.30374 -0.36775 1.00000 0.05763 0.00000 0.00000 H21C 0.02402 0.31128 -0.34418 1.00000 0.05763 0.00000 0.00000 C22 0.11210 0.39295 -0.31845 1.00000 0.02615 0.02528 0.03618 0.00386 -0.00136 -0.00054 0.02920 0.00801 0.00038 0.00018 0.00079 0.00000 0.00218 0.00208 0.00282 0.00207 0.00214 0.00180 0.00105 C23 0.23423 0.40832 -0.23317 1.00000 0.02517 0.02325 0.02326 0.00472 -0.00034 0.00185 0.02389 0.00712 0.00034 0.00017 0.00069 0.00000 0.00203 0.00200 0.00230 0.00192 0.00192 0.00163 0.00091 H23A 0.23981 0.38859 -0.09967 1.00000 0.02867 0.00000 0.00000 H23B 0.29116 0.38805 -0.32170 1.00000 0.02867 0.00000 0.00000 C24 0.27716 0.47359 -0.20484 1.00000 0.01925 0.02414 0.02436 0.00253 -0.00135 -0.00088 0.02259 0.00711 0.00033 0.00018 0.00070 0.00000 0.00192 0.00199 0.00231 0.00178 0.00182 0.00162 0.00090 C26 0.01281 0.42301 -0.20508 1.00000 0.02737 0.03658 0.04510 0.00012 0.00265 -0.00547 0.03635 0.00855 0.00037 0.00021 0.00086 0.00000 0.00227 0.00246 0.00324 0.00243 0.00233 0.00192 0.00120 H26A 0.01372 0.46637 -0.23189 1.00000 0.05453 0.00000 0.00000 H26B 0.02192 0.41600 -0.06003 1.00000 0.05453 0.00000 0.00000 H26C -0.06098 0.40599 -0.25047 1.00000 0.05453 0.00000 0.00000 C27 0.10194 0.40714 -0.54446 1.00000 0.03349 0.03604 0.02962 -0.00356 -0.00758 0.00027 0.03305 0.00796 0.00040 0.00020 0.00079 0.00000 0.00238 0.00244 0.00270 0.00232 0.00234 0.00198 0.00107 H27A 0.03099 0.38901 -0.59807 1.00000 0.04957 0.00000 0.00000 H27B 0.16913 0.39063 -0.61575 1.00000 0.04957 0.00000 0.00000 H27C 0.09923 0.45083 -0.56376 1.00000 0.04957 0.00000 0.00000 C28 0.22026 0.50564 -0.02806 1.00000 0.02925 0.02935 0.02973 -0.00066 0.00218 0.00014 0.02944 0.00798 0.00037 0.00019 0.00075 0.00000 0.00218 0.00221 0.00263 0.00211 0.00227 0.00183 0.00101 H28A 0.22311 0.47974 0.09142 1.00000 0.04416 0.00000 0.00000 H28B 0.13941 0.51460 -0.06134 1.00000 0.04416 0.00000 0.00000 H28C 0.26161 0.54325 -0.00037 1.00000 0.04416 0.00000 0.00000 C29 0.27511 0.51264 -0.39272 1.00000 0.03077 0.02340 0.03130 0.00231 0.00014 -0.00042 0.02849 0.00795 0.00039 0.00018 0.00074 0.00000 0.00226 0.00203 0.00264 0.00197 0.00212 0.00188 0.00101 H29A 0.32185 0.54880 -0.36987 1.00000 0.04274 0.00000 0.00000 H29B 0.19515 0.52432 -0.42283 1.00000 0.04274 0.00000 0.00000 H29C 0.30701 0.49000 -0.50671 1.00000 0.04274 0.00000 0.00000 N25 0.40411 0.46656 -0.14757 1.00000 0.02640 0.02190 0.02309 -0.00135 0.00008 -0.00303 0.02379 0.00602 0.00028 0.00015 0.00059 0.00000 0.00177 0.00164 0.00198 0.00165 0.00168 0.00146 0.00077 H25A 0.40997 0.44274 -0.03639 1.00000 0.03489 0.00000 0.01373 H25B 0.43489 0.50336 -0.12039 1.00000 0.04659 0.00000 0.01554 H25C 0.44334 0.44936 -0.25169 1.00000 0.02732 0.00000 0.01258 Final Structure Factor Calculation for 07skc0018pna21 in Pna2(1) Total number of l.s. parameters = 192 Maximum vector length = 511 Memory required = 3167 / 25046 wR2 = 0.1390 before cycle 5 for 2112 data and 2 / 192 parameters GooF = S = 1.115; Restrained GooF = 1.114 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0692 for 1685 Fo > 4sig(Fo) and 0.0944 for all 2112 data wR2 = 0.1390, GooF = S = 1.115, Restrained GooF = 1.114 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 31.00 for hydrogen atoms Principal mean square atomic displacements U 0.0350 0.0281 0.0209 C1 0.0338 0.0274 0.0221 C2 0.0822 0.0339 0.0220 C3 0.0697 0.0296 0.0235 C4 0.0311 0.0284 0.0239 C5 0.0271 0.0261 0.0169 C6 0.0317 0.0211 0.0175 C7 0.0673 0.0331 0.0259 O1A 0.0439 0.0307 0.0268 O1B 0.0350 0.0277 0.0207 O7A 0.0310 0.0241 0.0222 O7B 0.0593 0.0322 0.0238 C21 0.0376 0.0260 0.0240 C22 0.0284 0.0251 0.0182 C23 0.0271 0.0217 0.0189 C24 0.0456 0.0390 0.0245 C26 0.0407 0.0353 0.0232 C27 0.0318 0.0294 0.0272 C28 0.0319 0.0308 0.0228 C29 0.0280 0.0234 0.0199 N25 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.020 0.031 0.041 0.051 0.061 0.074 0.093 0.121 0.173 1.000 Number in group 221. 206. 223. 216. 198. 213. 202. 212. 208. 213. GooF 1.166 1.205 1.238 1.127 1.187 1.161 1.063 1.043 0.912 0.994 K 1.842 1.363 1.098 1.026 1.039 1.030 1.002 0.987 1.005 1.003 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.17 1.34 1.69 inf Number in group 212. 212. 215. 213. 203. 214. 216. 204. 210. 213. GooF 1.242 1.220 1.265 1.123 1.139 1.104 1.063 0.934 0.893 1.093 K 1.155 1.086 1.067 1.050 1.032 1.011 0.986 0.991 1.018 0.999 R1 0.257 0.205 0.215 0.160 0.144 0.098 0.075 0.049 0.040 0.027 Recommended weighting scheme: WGHT 0.0000 2.4227 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) 3 3 0 17.71 0.68 3.44 0.007 3.42 12 11 2 2.67 41.71 3.28 0.053 0.84 5 5 7 8.24 58.64 3.27 0.062 0.86 3 14 4 3.64 29.79 3.24 0.044 1.10 0 0 6 377.68 215.42 3.23 0.119 1.11 9 7 6 110.88 48.97 3.22 0.057 0.81 2 15 6 110.49 46.61 3.16 0.056 0.88 8 3 5 61.61 22.48 2.97 0.039 0.97 3 2 0 6604.80 7233.37 2.92 0.692 3.64 2 2 1 5172.18 5650.11 2.87 0.611 4.05 1 1 1 1552.98 1780.76 2.80 0.343 5.57 13 10 0 28.34 0.00 2.80 0.000 0.83 2 17 5 9.85 47.30 2.78 0.056 0.92 9 9 5 48.59 13.28 2.77 0.030 0.86 12 7 4 108.15 30.84 2.77 0.045 0.81 3 22 3 37.17 9.50 2.77 0.025 0.89 7 4 2 200.16 136.31 2.76 0.095 1.43 11 10 5 89.31 32.22 2.67 0.046 0.77 6 12 0 16.27 1.94 2.67 0.011 1.33 3 27 1 24.10 65.75 2.64 0.066 0.80 11 18 1 185.82 118.08 2.63 0.088 0.79 1 13 7 67.44 14.34 2.61 0.031 0.83 6 4 3 183.26 257.20 2.60 0.130 1.40 9 16 3 14.75 48.85 2.59 0.057 0.87 6 10 5 72.90 22.80 2.56 0.039 0.98 9 12 5 -9.82 22.95 2.55 0.039 0.83 9 12 3 280.91 198.55 2.54 0.115 0.95 1 9 5 24.50 59.26 2.52 0.063 1.16 11 18 2 107.46 47.65 2.52 0.056 0.78 4 1 8 112.68 63.33 2.48 0.065 0.80 3 19 5 67.24 7.92 2.44 0.023 0.86 9 10 0 81.58 138.34 2.43 0.096 1.11 4 12 5 152.21 95.95 2.42 0.080 1.01 7 24 1 29.22 73.15 2.41 0.070 0.80 1 15 6 119.69 69.59 2.40 0.068 0.88 5 4 6 123.41 67.94 2.39 0.067 0.98 2 6 5 62.05 31.15 2.38 0.045 1.22 1 22 4 63.25 27.94 2.38 0.043 0.86 1 28 1 47.28 17.91 2.37 0.034 0.79 5 6 3 63.22 31.62 2.37 0.046 1.47 3 4 8 128.04 56.69 2.36 0.061 0.80 7 15 4 26.33 6.10 2.34 0.020 0.92 14 5 0 -8.16 17.81 2.34 0.034 0.81 10 15 3 27.09 0.96 2.33 0.008 0.84 4 20 4 42.96 14.09 2.33 0.031 0.88 0 3 5 89.53 138.23 2.32 0.096 1.31 0 21 1 26.05 56.32 2.32 0.061 1.05 3 14 5 33.05 67.81 2.29 0.067 0.98 6 2 3 38.79 17.93 2.29 0.034 1.44 4 19 2 343.70 268.31 2.28 0.133 1.03 Bond lengths and angles C1 - Distance Angles O1A 1.2081 (0.0055) O1B 1.3220 (0.0059) 123.03 (0.45) C2 1.5071 (0.0061) 124.35 (0.47) 112.56 (0.41) C1 - O1A O1B C2 - Distance Angles C1 1.5071 (0.0061) C3 1.5086 (0.0071) 112.85 (0.42) H2A 0.9900 109.02 109.02 H2B 0.9900 109.02 109.02 107.80 C2 - C1 C3 H2A C3 - Distance Angles C2 1.5086 (0.0071) C4 1.5379 (0.0068) 114.52 (0.46) H3A 0.9900 108.63 108.63 H3B 0.9900 108.63 108.63 107.58 C3 - C2 C4 H3A C4 - Distance Angles C5 1.5271 (0.0056) C3 1.5379 (0.0068) 113.03 (0.42) H4A 0.9900 108.98 108.98 H4B 0.9900 108.98 108.98 107.77 C4 - C5 C3 H4A C5 - Distance Angles C6 1.5208 (0.0058) C4 1.5271 (0.0056) 111.08 (0.37) H5A 0.9900 109.42 109.42 H5B 0.9900 109.42 109.42 108.03 C5 - C6 C4 H5A C6 - Distance Angles C5 1.5208 (0.0058) C7 1.5232 (0.0051) 115.57 (0.35) H6A 0.9900 108.39 108.39 H6B 0.9900 108.39 108.39 107.45 C6 - C5 C7 H6A C7 - Distance Angles O7A 1.2376 (0.0051) O7B 1.2841 (0.0052) 123.42 (0.36) C6 1.5232 (0.0051) 120.46 (0.40) 116.05 (0.38) C7 - O7A O7B O1A - Distance Angles C1 1.2081 (0.0055) O1A - O1B - Distance Angles C1 1.3220 (0.0059) H1 0.8400 109.47 O1B - C1 O7A - Distance Angles C7 1.2376 (0.0051) O7A - O7B - Distance Angles C7 1.2841 (0.0052) O7B - C21 - Distance Angles C22 1.5456 (0.0056) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - C22 H21A H21B C22 - Distance Angles C26 1.5254 (0.0063) C27 1.5360 (0.0071) 109.48 (0.40) C21 1.5456 (0.0056) 107.95 (0.39) 107.73 (0.41) C23 1.5578 (0.0058) 113.94 (0.40) 112.23 (0.39) 105.16 (0.35) C22 - C26 C27 C21 C23 - Distance Angles C24 1.5445 (0.0052) C22 1.5578 (0.0058) 122.75 (0.33) H23A 0.9900 106.64 106.64 H23B 0.9900 106.64 106.64 106.58 C23 - C24 C22 H23A C24 - Distance Angles C29 1.5185 (0.0060) C28 1.5211 (0.0062) 110.96 (0.34) N25 1.5227 (0.0051) 106.16 (0.35) 105.78 (0.35) C23 1.5445 (0.0052) 115.60 (0.37) 113.26 (0.34) 104.07 (0.30) C24 - C29 C28 N25 C26 - Distance Angles C22 1.5254 (0.0063) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C22 H26A H26B C27 - Distance Angles C22 1.5360 (0.0071) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C22 H27A H27B C28 - Distance Angles C24 1.5211 (0.0062) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C24 H28A H28B C29 - Distance Angles C24 1.5185 (0.0060) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - C24 H29A H29B N25 - Distance Angles C24 1.5227 (0.0051) H25A 0.9100 109.47 H25B 0.9100 109.47 109.47 H25C 0.9100 109.47 109.47 109.47 N25 - C24 H25A H25B Selected torsion angles 7.14 ( 0.67) O1A - C1 - C2 - C3 -170.38 ( 0.42) O1B - C1 - C2 - C3 178.03 ( 0.37) C1 - C2 - C3 - C4 69.31 ( 0.63) C2 - C3 - C4 - C5 167.36 ( 0.42) C3 - C4 - C5 - C6 -177.05 ( 0.40) C4 - C5 - C6 - C7 3.10 ( 0.59) C5 - C6 - C7 - O7A -179.83 ( 0.37) C5 - C6 - C7 - O7B -54.21 ( 0.58) C26 - C22 - C23 - C24 70.93 ( 0.53) C27 - C22 - C23 - C24 -172.23 ( 0.42) C21 - C22 - C23 - C24 -56.35 ( 0.56) C22 - C23 - C24 - C29 73.27 ( 0.54) C22 - C23 - C24 - C28 -172.34 ( 0.41) C22 - C23 - C24 - N25 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.90 2.767(5) 158.7 N25-H25A...O7A 0.84 1.76 2.596(4) 171.5 O1B-H1...O7B_$1 0.91 1.95 2.845(4) 167.2 N25-H25B...O7B_$2 0.91 2.11 3.014(5) 173.2 N25-H25C...O7B_$3 FMAP and GRID set by program FMAP 2 3 17 GRID -3.571 -2 24 3.571 2 1 R1 = 0.0944 for 2112 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.26 at 0.3326 0.5177 0.1582 [ 1.45 A from H28C ] Deepest hole -0.23 at 0.6028 0.4919 0.2147 [ 1.18 A from H25B ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3600 / 31292 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3326 0.5177 0.1582 1.00000 0.05 0.26 1.45 H28C 1.58 H28A 1.81 C28 2.22 H25B Q2 1 0.2247 0.2786 0.1092 1.00000 0.05 0.24 1.38 H5B 1.57 H3B 1.82 C5 1.84 H2A Q3 1 0.1627 0.3065 0.1177 1.00000 0.05 0.24 1.65 H5B 1.90 H21A 2.04 H3B 2.44 C5 Q4 1 0.0016 0.4067 -0.5370 1.00000 0.05 0.24 0.66 H27A 1.16 C27 1.50 H27C 1.95 C22 Q5 1 0.3818 0.2628 0.6770 1.00000 0.05 0.24 1.58 H6B 1.93 H4A 2.05 H2A 2.33 H21C Q6 1 0.3979 0.4801 0.2867 1.00000 0.05 0.24 1.40 O7A 1.74 H29C 2.06 H25B 2.14 C7 Q7 1 0.5423 0.3396 0.3611 1.00000 0.05 0.23 0.81 H6A 1.22 C6 1.53 C7 1.90 H6B Q8 1 -0.0192 0.3345 -0.5783 1.00000 0.05 0.23 1.35 H27A 1.61 H4B 1.71 H21C 2.04 H4A Q9 1 -0.1399 0.3633 -0.4266 1.00000 0.05 0.23 1.76 H26C 2.09 H4A 2.12 O1B 2.28 H21C Q10 1 0.3990 0.1207 -0.0328 1.00000 0.05 0.22 1.33 H2B 1.63 H26C 1.65 H26B 1.99 C26 Shortest distances between peaks (including symmetry equivalents) 2 3 0.95 1 6 1.41 4 8 1.65 8 9 1.83 4 9 2.03 9 10 2.67 5 9 2.90 5 8 2.98 3 8 2.98 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.50: 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 0.92: Structure factors and derivatives 0.53: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.11: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0018pna21 finished at 12:47:54 Total CPU time: 2.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++