+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + ssf1328 started at 12:57:03 on 06-May-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL ssf1328 in P2(1)/c CELL 0.69050 6.6154 30.4775 15.2817 90.000 90.924 90.000 ZERR 8.00 0.0015 0.0068 0.0034 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 104 200 8 32 V = 3080.71 F(000) = 1136.0 Mu = 0.08 mm-1 Cell Wt = 2074.72 Rho = 1.118 MERG 2 EXTI 0.02763 SHEL 7 0.77 HTAB N45 O31A HTAB N25 O1A EQIV_$1 x, -y+1/2, z+1/2 HTAB N45 O1A_$1 EQIV_$2 x-1, y, z HTAB N45 O31B_$2 HTAB N25 O1B_$2 EQIV_$3 x-1, -y+1/2, z-1/2 HTAB N25 O31A_$3 FMAP 2 PLAN 10 SIZE 0.01 0.03 0.08 ACTA CONF BOND $H WGHT 0.06430 L.S. 4 TEMP -153.00 FVAR 0.20207 MOLE 1 C1 1 0.727142 0.206119 0.982480 11.00000 0.03753 0.03401 = 0.02939 -0.00517 -0.00145 -0.00050 C2 1 0.613478 0.182875 1.051988 11.00000 0.03094 0.04954 = 0.03519 0.00050 -0.00064 0.00523 AFIX 43 H2 2 0.548472 0.201171 1.093265 11.00000 -1.20000 AFIX 0 C3 1 0.590827 0.139803 1.063982 11.00000 0.03420 0.04783 = 0.03512 0.00808 0.00156 0.00423 AFIX 43 H3 2 0.514144 0.130358 1.112520 11.00000 -1.20000 AFIX 0 C4 1 0.675789 0.106471 1.007658 11.00000 0.03137 0.04302 = 0.04159 0.00740 -0.00613 -0.00231 C5 1 0.739214 0.030300 0.995599 11.00000 0.06016 0.04216 = 0.07900 0.00358 0.00155 0.00577 AFIX 137 H5A 2 0.665089 0.026002 0.940221 11.00000 -1.50000 H5B 2 0.731656 0.003491 1.030802 11.00000 -1.50000 H5C 2 0.881002 0.036979 0.983603 11.00000 -1.50000 AFIX 0 O1A 4 0.620421 0.224592 0.923037 11.00000 0.03691 0.04299 = 0.03544 0.00649 -0.00635 0.00060 O1B 4 0.914451 0.208917 0.991164 11.00000 0.02998 0.04798 = 0.03669 0.00394 -0.00205 -0.00147 O4A 4 0.651039 0.066138 1.042794 11.00000 0.04392 0.03853 = 0.05463 0.00895 0.00098 -0.00015 O4B 4 0.760874 0.112337 0.938752 11.00000 0.04744 0.04847 = 0.04137 0.00188 0.00177 0.00304 MOLE 2 C21 1 0.102859 0.100764 0.708665 11.00000 0.06546 0.04257 = 0.04930 -0.00651 -0.01607 0.00363 AFIX 137 H21A 2 0.121966 0.123190 0.663590 11.00000 -1.50000 H21B 2 -0.033174 0.103444 0.732555 11.00000 -1.50000 H21C 2 0.119121 0.071578 0.682802 11.00000 -1.50000 AFIX 0 C22 1 0.259828 0.107127 0.782027 11.00000 0.04137 0.03774 = 0.03235 -0.00111 -0.00528 0.00392 C23 1 0.227394 0.149391 0.835933 11.00000 0.03226 0.03902 = 0.03010 -0.00048 -0.00364 0.00064 AFIX 23 H23A 2 0.110266 0.143838 0.873897 11.00000 -1.20000 H23B 2 0.346909 0.152480 0.875275 11.00000 -1.20000 AFIX 0 C24 1 0.192292 0.194331 0.793443 11.00000 0.03572 0.03611 = 0.02756 -0.00487 -0.00289 0.00298 C26 1 0.472354 0.104639 0.743867 11.00000 0.05828 0.05036 = 0.04847 0.00131 0.00570 0.01413 AFIX 137 H26A 2 0.490717 0.076115 0.715481 11.00000 -1.50000 H26B 2 0.573289 0.108113 0.791003 11.00000 -1.50000 H26C 2 0.488950 0.128099 0.700718 11.00000 -1.50000 AFIX 0 C27 1 0.239354 0.068804 0.847164 11.00000 0.05436 0.04111 = 0.04698 0.00043 -0.00620 0.00298 AFIX 137 H27A 2 0.103902 0.069185 0.872191 11.00000 -1.50000 H27B 2 0.340920 0.071915 0.894148 11.00000 -1.50000 H27C 2 0.260227 0.040955 0.816550 11.00000 -1.50000 AFIX 0 C28 1 0.349853 0.207740 0.726614 11.00000 0.04413 0.04326 = 0.03748 0.00188 0.00103 0.00090 AFIX 137 H28A 2 0.485536 0.204311 0.752394 11.00000 -1.50000 H28B 2 0.328585 0.238459 0.709904 11.00000 -1.50000 H28C 2 0.336578 0.189056 0.674646 11.00000 -1.50000 AFIX 0 C29 1 -0.021228 0.200705 0.755953 11.00000 0.04178 0.04409 = 0.04045 -0.00162 -0.01202 0.00582 AFIX 137 H29A 2 -0.040860 0.231573 0.739992 11.00000 -1.50000 H29B 2 -0.120199 0.192337 0.799971 11.00000 -1.50000 H29C 2 -0.039561 0.182293 0.703853 11.00000 -1.50000 AFIX 0 N25 3 0.211575 0.226568 0.868383 11.00000 0.03189 0.03603 = 0.03332 0.00254 -0.00254 0.00024 AFIX 137 H25A 2 0.337468 0.224536 0.892931 11.00000 0.06462 H25B 2 0.117544 0.220265 0.909338 11.00000 0.05113 H25C 2 0.191313 0.254295 0.847961 11.00000 0.04095 AFIX 0 MOLE 3 C31 1 1.208518 0.174350 1.241456 11.00000 0.03317 0.03855 = 0.03278 0.00196 -0.00752 0.00030 C32 1 1.101463 0.151758 1.167634 11.00000 0.03258 0.04750 = 0.03548 -0.00297 -0.00541 0.00527 AFIX 43 H32 2 1.036149 0.170030 1.125495 11.00000 -1.20000 AFIX 0 C33 1 1.087806 0.108728 1.154584 11.00000 0.03920 0.04997 = 0.04468 -0.00760 -0.01397 0.00285 AFIX 43 H33 2 1.017344 0.098710 1.103741 11.00000 -1.20000 AFIX 0 C34 1 1.174464 0.076108 1.213620 11.00000 0.03022 0.04430 = 0.04774 -0.01098 -0.00825 0.00036 C35 1 1.230227 0.000442 1.236221 11.00000 0.06702 0.03796 = 0.07377 -0.00134 -0.02229 0.00753 AFIX 137 H35A 2 1.378038 0.001701 1.233657 11.00000 -1.50000 H35B 2 1.183065 -0.028042 1.214240 11.00000 -1.50000 H35C 2 1.187973 0.004176 1.296939 11.00000 -1.50000 AFIX 0 O31A 4 1.101180 0.190265 1.301389 11.00000 0.03643 0.04085 = 0.03710 -0.00635 0.00322 -0.00118 O31B 4 1.395231 0.178925 1.235790 11.00000 0.03210 0.04959 = 0.03045 -0.00156 -0.00233 -0.00381 O34A 4 1.264140 0.083581 1.281464 11.00000 0.04964 0.04505 = 0.04864 -0.00323 -0.01552 -0.00229 O34B 4 1.144231 0.035033 1.182953 11.00000 0.05154 0.04202 = 0.06078 -0.00838 -0.01623 0.00150 MOLE 4 C41 1 0.735442 0.033871 1.367574 11.00000 0.05499 0.03937 = 0.05607 0.00117 -0.01236 0.00322 AFIX 137 H41A 2 0.773529 0.005805 1.394442 11.00000 -1.50000 H41B 2 0.821089 0.039440 1.317036 11.00000 -1.50000 H41C 2 0.593491 0.032734 1.348355 11.00000 -1.50000 AFIX 0 C42 1 0.764008 0.070933 1.434831 11.00000 0.04404 0.03507 = 0.03458 0.00054 -0.00494 -0.00272 C43 1 0.722799 0.114018 1.384619 11.00000 0.03365 0.03921 = 0.03165 -0.00032 -0.00665 -0.00188 AFIX 23 H43A 2 0.836857 0.118035 1.344239 11.00000 -1.20000 H43B 2 0.600995 0.108855 1.347557 11.00000 -1.20000 AFIX 0 C44 1 0.691307 0.158384 1.430386 11.00000 0.03363 0.03601 = 0.02683 0.00537 -0.00385 0.00352 C46 1 0.620642 0.062653 1.509631 11.00000 0.07440 0.04513 = 0.05800 0.01246 0.00799 -0.00163 AFIX 137 H46A 2 0.642149 0.032951 1.532513 11.00000 -1.50000 H46B 2 0.480741 0.065582 1.488369 11.00000 -1.50000 H46C 2 0.646491 0.084082 1.556296 11.00000 -1.50000 AFIX 0 C47 1 0.984007 0.068332 1.469398 11.00000 0.05838 0.04473 = 0.04841 -0.00305 -0.01770 0.00924 AFIX 137 H47A 2 1.004559 0.090040 1.516007 11.00000 -1.50000 H47B 2 1.076754 0.074426 1.421535 11.00000 -1.50000 H47C 2 1.010500 0.038879 1.492615 11.00000 -1.50000 AFIX 0 C48 1 0.855683 0.170701 1.497593 11.00000 0.05177 0.04332 = 0.03339 -0.00215 -0.00971 0.00183 AFIX 137 H48A 2 0.988908 0.167481 1.471211 11.00000 -1.50000 H48B 2 0.846626 0.151312 1.548538 11.00000 -1.50000 H48C 2 0.836770 0.201198 1.516067 11.00000 -1.50000 AFIX 0 C49 1 0.480314 0.163704 1.468813 11.00000 0.04294 0.04794 = 0.03731 0.00592 0.00303 0.00688 AFIX 137 H49A 2 0.460295 0.194314 1.486300 11.00000 -1.50000 H49B 2 0.467713 0.144625 1.520056 11.00000 -1.50000 H49C 2 0.377930 0.155578 1.424670 11.00000 -1.50000 AFIX 0 N45 3 0.703300 0.191733 1.357829 11.00000 0.02964 0.03816 = 0.03378 -0.00388 -0.00120 0.00016 AFIX 137 H45A 2 0.824542 0.189264 1.330967 11.00000 0.03270 H45B 2 0.690943 0.219185 1.380541 11.00000 0.04445 H45C 2 0.601657 0.186885 1.318172 11.00000 0.04998 AFIX 0 HKLF 4 Covalent radii and connectivity table for ssf1328 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C3 C1 C3 - C2 C4 C4 - O4B O4A C3 C5 - O4A O1A - C1 O1B - C1 O4A - C4 C5 O4B - C4 C21 - C22 C22 - C21 C26 C27 C23 C23 - C24 C22 C24 - N25 C28 C29 C23 C26 - C22 C27 - C22 C28 - C24 C29 - C24 N25 - C24 C31 - O31B O31A C32 C32 - C33 C31 C33 - C32 C34 C34 - O34A O34B C33 C35 - O34B O31A - C31 O31B - C31 O34A - C34 O34B - C34 C35 C41 - C42 C42 - C46 C41 C47 C43 C43 - C44 C42 C44 - N45 C48 C49 C43 C46 - C42 C47 - C42 C48 - C44 C49 - C44 N45 - C44 Operators for generating equivalent atoms: $1 x, -y+1/2, z+1/2 $2 x-1, y, z $3 x-1, -y+1/2, z-1/2 19356 Reflections read, of which 268 rejected -7 =< h =< 7, -33 =< k =< 33, -16 =< l =< 16, Max. 2-theta = 45.08 0 Systematic absence violations 0 Inconsistent equivalents 4405 Unique reflections, of which 0 suppressed R(int) = 0.1059 R(sigma) = 0.0846 Friedel opposites merged Maximum memory for data reduction = 4339 / 43573 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 = 5417 / 437330 wR2 = 0.1321 before cycle 1 for 4405 data and 346 / 346 parameters GooF = S = 0.972; Restrained GooF = 0.972 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0643 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20206 0.00054 -0.011 OSF 2 0.02760 0.00211 -0.013 EXTI Mean shift/esd = 0.002 Maximum = -0.013 for EXTI Max. shift = 0.000 A for H27B Max. dU = 0.000 for H25B Least-squares cycle 2 Maximum vector length = 511 Memory required = 5417 / 437330 wR2 = 0.1321 before cycle 2 for 4405 data and 346 / 346 parameters GooF = S = 0.972; Restrained GooF = 0.972 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0643 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20206 0.00054 -0.010 OSF 2 0.02758 0.00211 -0.008 EXTI Mean shift/esd = 0.001 Maximum = -0.010 for OSF Max. shift = 0.000 A for H5A Max. dU = 0.000 for H25B Least-squares cycle 3 Maximum vector length = 511 Memory required = 5417 / 437330 wR2 = 0.1321 before cycle 3 for 4405 data and 346 / 346 parameters GooF = S = 0.972; Restrained GooF = 0.972 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0643 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20206 0.00054 -0.001 OSF 2 0.02758 0.00211 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for EXTI Max. shift = 0.000 A for H47B Max. dU = 0.000 for H25B Least-squares cycle 4 Maximum vector length = 511 Memory required = 5417 / 437330 wR2 = 0.1321 before cycle 4 for 4405 data and 346 / 346 parameters GooF = S = 0.972; Restrained GooF = 0.972 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0643 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20206 0.00054 0.000 OSF 2 0.02758 0.00211 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C4 Max. dU = 0.000 for H25B Largest correlation matrix elements 0.636 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.5485 0.2012 1.0933 43 0.950 0.000 C2 C3 C1 H3 0.5141 0.1304 1.1125 43 0.950 0.000 C3 C2 C4 H5A 0.6651 0.0260 0.9402 137 0.980 0.000 C5 O4A H5A H5B 0.7317 0.0035 1.0308 137 0.980 0.000 C5 O4A H5A H5C 0.8810 0.0370 0.9836 137 0.980 0.000 C5 O4A H5A H21A 0.1220 0.1232 0.6636 137 0.980 0.000 C21 C22 H21A H21B -0.0332 0.1034 0.7326 137 0.980 0.000 C21 C22 H21A H21C 0.1191 0.0716 0.6828 137 0.980 0.000 C21 C22 H21A H23A 0.1103 0.1438 0.8739 23 0.990 0.000 C23 C24 C22 H23B 0.3469 0.1525 0.8753 23 0.990 0.000 C23 C24 C22 H26A 0.4907 0.0761 0.7155 137 0.980 0.000 C26 C22 H26A H26B 0.5733 0.1081 0.7910 137 0.980 0.000 C26 C22 H26A H26C 0.4890 0.1281 0.7007 137 0.980 0.000 C26 C22 H26A H27A 0.1039 0.0692 0.8722 137 0.980 0.000 C27 C22 H27A H27B 0.3409 0.0719 0.8941 137 0.980 0.000 C27 C22 H27A H27C 0.2602 0.0410 0.8165 137 0.980 0.000 C27 C22 H27A H28A 0.4855 0.2043 0.7524 137 0.980 0.000 C28 C24 H28A H28B 0.3286 0.2385 0.7099 137 0.980 0.000 C28 C24 H28A H28C 0.3366 0.1891 0.6746 137 0.980 0.000 C28 C24 H28A H29A -0.0409 0.2316 0.7400 137 0.980 0.000 C29 C24 H29A H29B -0.1202 0.1923 0.8000 137 0.980 0.000 C29 C24 H29A H29C -0.0396 0.1823 0.7039 137 0.980 0.000 C29 C24 H29A H25A 0.3375 0.2245 0.8929 137 0.910 0.000 N25 C24 H25A H25B 0.1175 0.2203 0.9093 137 0.910 0.000 N25 C24 H25A H25C 0.1913 0.2543 0.8480 137 0.910 0.000 N25 C24 H25A H32 1.0361 0.1700 1.1255 43 0.950 0.000 C32 C33 C31 H33 1.0173 0.0987 1.1037 43 0.950 0.000 C33 C32 C34 H35A 1.3780 0.0017 1.2337 137 0.980 0.000 C35 O34B H35A H35B 1.1831 -0.0280 1.2142 137 0.980 0.000 C35 O34B H35A H35C 1.1880 0.0042 1.2969 137 0.980 0.000 C35 O34B H35A H41A 0.7735 0.0058 1.3944 137 0.980 0.000 C41 C42 H41A H41B 0.8211 0.0394 1.3170 137 0.980 0.000 C41 C42 H41A H41C 0.5935 0.0327 1.3484 137 0.980 0.000 C41 C42 H41A H43A 0.8369 0.1180 1.3442 23 0.990 0.000 C43 C44 C42 H43B 0.6010 0.1089 1.3476 23 0.990 0.000 C43 C44 C42 H46A 0.6422 0.0330 1.5325 137 0.980 0.000 C46 C42 H46A H46B 0.4807 0.0656 1.4884 137 0.980 0.000 C46 C42 H46A H46C 0.6465 0.0841 1.5563 137 0.980 0.000 C46 C42 H46A H47A 1.0046 0.0900 1.5160 137 0.980 0.000 C47 C42 H47A H47B 1.0768 0.0744 1.4215 137 0.980 0.000 C47 C42 H47A H47C 1.0105 0.0389 1.4926 137 0.980 0.000 C47 C42 H47A H48A 0.9889 0.1675 1.4712 137 0.980 0.000 C48 C44 H48A H48B 0.8466 0.1513 1.5485 137 0.980 0.000 C48 C44 H48A H48C 0.8368 0.2012 1.5161 137 0.980 0.000 C48 C44 H48A H49A 0.4603 0.1943 1.4863 137 0.980 0.000 C49 C44 H49A H49B 0.4677 0.1446 1.5201 137 0.980 0.000 C49 C44 H49A H49C 0.3779 0.1556 1.4247 137 0.980 0.000 C49 C44 H49A H45A 0.8245 0.1893 1.3310 137 0.910 0.000 N45 C44 H45A H45B 0.6909 0.2192 1.3805 137 0.910 0.000 N45 C44 H45A H45C 0.6017 0.1869 1.3182 137 0.910 0.000 N45 C44 H45A ssf1328 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.72714 0.20612 0.98248 1.00000 0.03753 0.03400 0.02938 -0.00517 -0.00145 -0.00050 0.03366 0.00509 0.00048 0.00010 0.00019 0.00000 0.00212 0.00200 0.00180 0.00150 0.00150 0.00157 0.00077 C2 0.61348 0.18288 1.05199 1.00000 0.03094 0.04953 0.03518 0.00051 -0.00064 0.00523 0.03856 0.00538 0.00044 0.00011 0.00019 0.00000 0.00185 0.00242 0.00189 0.00168 0.00144 0.00164 0.00082 H2 0.54847 0.20117 1.09327 1.00000 0.04627 0.00000 0.00000 C3 0.59083 0.13980 1.06398 1.00000 0.03420 0.04783 0.03511 0.00808 0.00157 0.00423 0.03904 0.00548 0.00045 0.00011 0.00020 0.00000 0.00186 0.00242 0.00187 0.00170 0.00143 0.00168 0.00082 H3 0.51415 0.13036 1.11252 1.00000 0.04684 0.00000 0.00000 C4 0.67579 0.10647 1.00766 1.00000 0.03137 0.04301 0.04159 0.00740 -0.00614 -0.00232 0.03873 0.00539 0.00047 0.00011 0.00022 0.00000 0.00186 0.00232 0.00207 0.00181 0.00159 0.00163 0.00082 C5 0.73921 0.03030 0.99560 1.00000 0.06015 0.04216 0.07900 0.00358 0.00155 0.00577 0.06043 0.00641 0.00055 0.00012 0.00024 0.00000 0.00252 0.00246 0.00288 0.00210 0.00210 0.00196 0.00108 H5A 0.66508 0.02600 0.94022 1.00000 0.09065 0.00000 0.00000 H5B 0.73166 0.00349 1.03080 1.00000 0.09065 0.00000 0.00000 H5C 0.88100 0.03698 0.98360 1.00000 0.09065 0.00000 0.00000 O1A 0.62042 0.22459 0.92304 1.00000 0.03690 0.04298 0.03543 0.00649 -0.00636 0.00060 0.03851 0.00334 0.00029 0.00007 0.00012 0.00000 0.00128 0.00143 0.00122 0.00103 0.00099 0.00105 0.00056 O1B 0.91445 0.20892 0.99116 1.00000 0.02997 0.04798 0.03668 0.00394 -0.00205 -0.00147 0.03824 0.00344 0.00030 0.00007 0.00012 0.00000 0.00132 0.00147 0.00125 0.00104 0.00093 0.00105 0.00057 O4A 0.65104 0.06614 1.04279 1.00000 0.04392 0.03852 0.05462 0.00895 0.00098 -0.00014 0.04568 0.00371 0.00031 0.00007 0.00014 0.00000 0.00138 0.00150 0.00144 0.00119 0.00109 0.00113 0.00060 O4B 0.76087 0.11234 0.93875 1.00000 0.04744 0.04846 0.04137 0.00188 0.00177 0.00304 0.04574 0.00368 0.00033 0.00007 0.00014 0.00000 0.00141 0.00154 0.00142 0.00116 0.00113 0.00114 0.00060 C21 0.10286 0.10076 0.70867 1.00000 0.06547 0.04256 0.04930 -0.00651 -0.01608 0.00362 0.05262 0.00542 0.00054 0.00011 0.00021 0.00000 0.00247 0.00226 0.00216 0.00176 0.00182 0.00190 0.00097 H21A 0.12196 0.12319 0.66359 1.00000 0.07894 0.00000 0.00000 H21B -0.03317 0.10344 0.73256 1.00000 0.07894 0.00000 0.00000 H21C 0.11913 0.07158 0.68280 1.00000 0.07894 0.00000 0.00000 C22 0.25983 0.10713 0.78203 1.00000 0.04136 0.03772 0.03235 -0.00111 -0.00528 0.00392 0.03721 0.00513 0.00046 0.00010 0.00019 0.00000 0.00199 0.00206 0.00181 0.00155 0.00146 0.00158 0.00081 C23 0.22739 0.14939 0.83593 1.00000 0.03225 0.03901 0.03009 -0.00048 -0.00364 0.00063 0.03383 0.00490 0.00044 0.00010 0.00018 0.00000 0.00176 0.00205 0.00171 0.00146 0.00135 0.00150 0.00077 H23A 0.11027 0.14384 0.87390 1.00000 0.04060 0.00000 0.00000 H23B 0.34691 0.15248 0.87528 1.00000 0.04060 0.00000 0.00000 C24 0.19229 0.19433 0.79344 1.00000 0.03571 0.03609 0.02755 -0.00488 -0.00289 0.00297 0.03315 0.00487 0.00044 0.00010 0.00018 0.00000 0.00183 0.00200 0.00168 0.00146 0.00135 0.00149 0.00077 C26 0.47235 0.10464 0.74387 1.00000 0.05828 0.05035 0.04847 0.00131 0.00570 0.01413 0.05231 0.00623 0.00052 0.00012 0.00022 0.00000 0.00242 0.00245 0.00214 0.00180 0.00177 0.00190 0.00096 H26A 0.49072 0.07611 0.71548 1.00000 0.07847 0.00000 0.00000 H26B 0.57329 0.10811 0.79100 1.00000 0.07847 0.00000 0.00000 H26C 0.48895 0.12810 0.70072 1.00000 0.07847 0.00000 0.00000 C27 0.23935 0.06880 0.84716 1.00000 0.05436 0.04110 0.04698 0.00043 -0.00620 0.00298 0.04755 0.00560 0.00050 0.00011 0.00021 0.00000 0.00226 0.00220 0.00212 0.00169 0.00171 0.00179 0.00092 H27A 0.10390 0.06919 0.87219 1.00000 0.07133 0.00000 0.00000 H27B 0.34092 0.07191 0.89415 1.00000 0.07133 0.00000 0.00000 H27C 0.26022 0.04095 0.81655 1.00000 0.07133 0.00000 0.00000 C28 0.34985 0.20774 0.72661 1.00000 0.04412 0.04326 0.03748 0.00188 0.00103 0.00089 0.04161 0.00541 0.00047 0.00011 0.00019 0.00000 0.00205 0.00219 0.00188 0.00160 0.00152 0.00167 0.00085 H28A 0.48554 0.20431 0.75239 1.00000 0.06242 0.00000 0.00000 H28B 0.32858 0.23846 0.70990 1.00000 0.06242 0.00000 0.00000 H28C 0.33658 0.18906 0.67465 1.00000 0.06242 0.00000 0.00000 C29 -0.02123 0.20071 0.75595 1.00000 0.04177 0.04409 0.04044 -0.00161 -0.01202 0.00582 0.04224 0.00521 0.00046 0.00011 0.00020 0.00000 0.00201 0.00215 0.00191 0.00162 0.00151 0.00165 0.00086 H29A -0.04086 0.23157 0.73999 1.00000 0.06335 0.00000 0.00000 H29B -0.12020 0.19234 0.79997 1.00000 0.06335 0.00000 0.00000 H29C -0.03956 0.18229 0.70385 1.00000 0.06335 0.00000 0.00000 N25 0.21157 0.22657 0.86838 1.00000 0.03189 0.03602 0.03331 0.00254 -0.00254 0.00024 0.03377 0.00393 0.00037 0.00008 0.00015 0.00000 0.00158 0.00178 0.00145 0.00127 0.00128 0.00122 0.00065 H25A 0.33747 0.22454 0.89293 1.00000 0.06459 0.00000 0.01129 H25B 0.11754 0.22026 0.90934 1.00000 0.05117 0.00000 0.01032 H25C 0.19131 0.25429 0.84796 1.00000 0.04095 0.00000 0.00949 C31 1.20852 0.17435 1.24146 1.00000 0.03318 0.03854 0.03277 0.00196 -0.00753 0.00030 0.03491 0.00524 0.00049 0.00010 0.00020 0.00000 0.00202 0.00208 0.00185 0.00155 0.00154 0.00161 0.00078 C32 1.10146 0.15176 1.16763 1.00000 0.03257 0.04749 0.03548 -0.00298 -0.00542 0.00527 0.03858 0.00525 0.00044 0.00011 0.00019 0.00000 0.00184 0.00236 0.00184 0.00163 0.00143 0.00162 0.00082 H32 1.03615 0.17003 1.12550 1.00000 0.04629 0.00000 0.00000 C33 1.08781 0.10873 1.15458 1.00000 0.03919 0.04997 0.04467 -0.00759 -0.01397 0.00285 0.04477 0.00559 0.00047 0.00012 0.00021 0.00000 0.00205 0.00251 0.00205 0.00181 0.00159 0.00177 0.00089 H33 1.01734 0.09871 1.10374 1.00000 0.05372 0.00000 0.00000 C34 1.17446 0.07611 1.21362 1.00000 0.03021 0.04429 0.04774 -0.01098 -0.00825 0.00036 0.04084 0.00558 0.00045 0.00011 0.00022 0.00000 0.00187 0.00239 0.00219 0.00180 0.00164 0.00158 0.00086 C35 1.23023 0.00044 1.23622 1.00000 0.06702 0.03795 0.07376 -0.00134 -0.02229 0.00753 0.05983 0.00600 0.00053 0.00011 0.00024 0.00000 0.00263 0.00234 0.00263 0.00200 0.00211 0.00201 0.00109 H35A 1.37804 0.00170 1.23366 1.00000 0.08974 0.00000 0.00000 H35B 1.18307 -0.02804 1.21424 1.00000 0.08974 0.00000 0.00000 H35C 1.18797 0.00418 1.29694 1.00000 0.08974 0.00000 0.00000 O31A 1.10118 0.19026 1.30139 1.00000 0.03642 0.04084 0.03710 -0.00635 0.00322 -0.00118 0.03809 0.00330 0.00030 0.00007 0.00013 0.00000 0.00129 0.00143 0.00127 0.00105 0.00102 0.00104 0.00057 O31B 1.39523 0.17892 1.23579 1.00000 0.03209 0.04958 0.03045 -0.00156 -0.00233 -0.00381 0.03740 0.00337 0.00031 0.00007 0.00012 0.00000 0.00134 0.00148 0.00118 0.00099 0.00091 0.00106 0.00056 O34A 1.26414 0.08358 1.28146 1.00000 0.04963 0.04504 0.04863 -0.00324 -0.01552 -0.00229 0.04794 0.00370 0.00033 0.00007 0.00014 0.00000 0.00143 0.00150 0.00148 0.00115 0.00118 0.00115 0.00062 O34B 1.14423 0.03503 1.18295 1.00000 0.05154 0.04201 0.06077 -0.00838 -0.01622 0.00150 0.05162 0.00365 0.00032 0.00008 0.00014 0.00000 0.00152 0.00159 0.00157 0.00124 0.00120 0.00121 0.00066 C41 0.73544 0.03387 1.36757 1.00000 0.05498 0.03937 0.05607 0.00117 -0.01235 0.00322 0.05028 0.00544 0.00051 0.00011 0.00022 0.00000 0.00231 0.00220 0.00227 0.00179 0.00179 0.00176 0.00095 H41A 0.77353 0.00581 1.39444 1.00000 0.07542 0.00000 0.00000 H41B 0.82109 0.03944 1.31704 1.00000 0.07542 0.00000 0.00000 H41C 0.59349 0.03273 1.34836 1.00000 0.07542 0.00000 0.00000 C42 0.76401 0.07093 1.43483 1.00000 0.04403 0.03506 0.03458 0.00054 -0.00494 -0.00272 0.03795 0.00510 0.00047 0.00010 0.00019 0.00000 0.00199 0.00203 0.00185 0.00153 0.00152 0.00157 0.00081 C43 0.72280 0.11402 1.38462 1.00000 0.03364 0.03920 0.03165 -0.00033 -0.00665 -0.00187 0.03491 0.00492 0.00045 0.00010 0.00018 0.00000 0.00182 0.00206 0.00175 0.00151 0.00139 0.00149 0.00078 H43A 0.83686 0.11803 1.34424 1.00000 0.04189 0.00000 0.00000 H43B 0.60100 0.10885 1.34756 1.00000 0.04189 0.00000 0.00000 C44 0.69131 0.15838 1.43039 1.00000 0.03362 0.03600 0.02683 0.00537 -0.00385 0.00352 0.03220 0.00492 0.00043 0.00010 0.00018 0.00000 0.00183 0.00198 0.00166 0.00147 0.00138 0.00147 0.00076 C46 0.62064 0.06265 1.50963 1.00000 0.07440 0.04512 0.05800 0.01246 0.00800 -0.00162 0.05910 0.00650 0.00056 0.00012 0.00022 0.00000 0.00272 0.00241 0.00244 0.00189 0.00207 0.00202 0.00105 H46A 0.64215 0.03295 1.53251 1.00000 0.08865 0.00000 0.00000 H46B 0.48074 0.06558 1.48837 1.00000 0.08865 0.00000 0.00000 H46C 0.64649 0.08408 1.55630 1.00000 0.08865 0.00000 0.00000 C47 0.98401 0.06833 1.46940 1.00000 0.05837 0.04472 0.04841 -0.00305 -0.01770 0.00924 0.05070 0.00551 0.00050 0.00011 0.00022 0.00000 0.00233 0.00231 0.00210 0.00167 0.00175 0.00181 0.00095 H47A 1.00456 0.09004 1.51601 1.00000 0.07605 0.00000 0.00000 H47B 1.07676 0.07443 1.42153 1.00000 0.07605 0.00000 0.00000 H47C 1.01050 0.03888 1.49261 1.00000 0.07605 0.00000 0.00000 C48 0.85568 0.17070 1.49759 1.00000 0.05176 0.04331 0.03339 -0.00215 -0.00971 0.00183 0.04293 0.00499 0.00047 0.00011 0.00019 0.00000 0.00219 0.00220 0.00183 0.00157 0.00156 0.00170 0.00087 H48A 0.98891 0.16748 1.47121 1.00000 0.06440 0.00000 0.00000 H48B 0.84663 0.15131 1.54854 1.00000 0.06440 0.00000 0.00000 H48C 0.83677 0.20120 1.51607 1.00000 0.06440 0.00000 0.00000 C49 0.48031 0.16370 1.46881 1.00000 0.04293 0.04793 0.03730 0.00592 0.00303 0.00688 0.04270 0.00567 0.00046 0.00011 0.00020 0.00000 0.00207 0.00229 0.00186 0.00162 0.00150 0.00165 0.00087 H49A 0.46030 0.19431 1.48630 1.00000 0.06405 0.00000 0.00000 H49B 0.46771 0.14462 1.52006 1.00000 0.06405 0.00000 0.00000 H49C 0.37793 0.15558 1.42467 1.00000 0.06405 0.00000 0.00000 N45 0.70330 0.19173 1.35783 1.00000 0.02963 0.03814 0.03378 -0.00388 -0.00120 0.00017 0.03387 0.00423 0.00037 0.00008 0.00015 0.00000 0.00159 0.00185 0.00145 0.00129 0.00126 0.00121 0.00066 H45A 0.82455 0.18926 1.33097 1.00000 0.03271 0.00000 0.00858 H45B 0.69094 0.21919 1.38054 1.00000 0.04443 0.00000 0.00981 H45C 0.60166 0.18688 1.31817 1.00000 0.04998 0.00000 0.00982 Final Structure Factor Calculation for ssf1328 in P2(1)/c Total number of l.s. parameters = 346 Maximum vector length = 511 Memory required = 5071 / 22995 wR2 = 0.1321 before cycle 5 for 4405 data and 0 / 346 parameters GooF = S = 0.972; Restrained GooF = 0.972 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0643 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0498 for 2532 Fo > 4sig(Fo) and 0.1103 for all 4405 data wR2 = 0.1321, GooF = S = 0.972, Restrained GooF = 0.972 for all data Occupancy sum of asymmetric unit = 36.00 for non-hydrogen and 50.00 for hydrogen atoms Principal mean square atomic displacements U 0.0383 0.0369 0.0257 C1 0.0509 0.0355 0.0293 C2 0.0527 0.0336 0.0309 C3 0.0518 0.0363 0.0280 C4 0.0794 0.0617 0.0402 C5 0.0478 0.0403 0.0274 O1A 0.0495 0.0361 0.0291 O1B 0.0586 0.0439 0.0345 O4A 0.0514 0.0449 0.0409 O4B 0.0777 0.0438 0.0363 C21 0.0463 0.0359 0.0295 C22 0.0392 0.0353 0.0270 C23 0.0415 0.0330 0.0250 C24 0.0699 0.0479 0.0392 C26 0.0590 0.0440 0.0397 C27 0.0449 0.0430 0.0369 C28 0.0564 0.0422 0.0281 C29 0.0380 0.0343 0.0290 N25 0.0416 0.0383 0.0248 C31 0.0508 0.0373 0.0277 C32 0.0621 0.0453 0.0269 C33 0.0590 0.0379 0.0256 C34 0.0951 0.0490 0.0354 C35 0.0462 0.0362 0.0318 O31A 0.0504 0.0340 0.0278 O31B 0.0657 0.0462 0.0319 O34A 0.0759 0.0433 0.0356 O34B 0.0691 0.0444 0.0374 C41 0.0473 0.0346 0.0319 C42 0.0409 0.0384 0.0254 C43 0.0390 0.0357 0.0219 C44 0.0771 0.0634 0.0368 C46 0.0757 0.0430 0.0334 C47 0.0571 0.0429 0.0288 C48 0.0549 0.0386 0.0346 C49 0.0405 0.0322 0.0289 N45 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.020 0.031 0.042 0.055 0.071 0.091 0.118 0.170 1.000 Number in group 459. 432. 447. 437. 442. 447. 425. 432. 440. 444. GooF 0.744 0.819 0.971 0.936 0.983 1.008 0.994 1.078 0.973 1.155 K -4.381 0.648 0.734 0.885 0.934 0.998 1.016 1.031 1.016 1.014 Resolution(A) 0.90 0.93 0.97 1.01 1.07 1.13 1.22 1.34 1.53 1.92 inf Number in group 452. 445. 425. 451. 434. 436. 442. 441. 437. 442. GooF 0.839 0.876 0.857 0.941 0.946 0.940 0.947 0.963 0.997 1.325 K 0.907 0.939 0.954 0.971 0.986 1.003 1.024 1.026 1.009 1.020 R1 0.291 0.240 0.192 0.165 0.114 0.106 0.088 0.077 0.048 0.045 Recommended weighting scheme: WGHT 0.0645 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 1 1737.13 2345.45 4.46 0.279 5.23 0 8 0 38815.24 30042.22 4.31 1.000 3.81 1 6 2 1303.07 1682.51 3.98 0.237 3.55 1 2 1 792.65 1061.72 3.95 0.188 5.61 -3 3 12 138.65 44.42 3.83 0.038 1.10 2 14 5 379.80 274.37 3.77 0.096 1.56 -1 1 3 30081.63 24317.60 3.59 0.900 4.03 -3 15 13 182.12 49.86 3.53 0.041 0.93 1 2 2 791.49 994.98 3.53 0.182 4.72 0 4 3 272.15 197.63 3.49 0.081 4.23 -1 6 1 28.08 83.75 3.48 0.053 3.91 -1 11 4 266.43 198.23 3.46 0.081 2.13 1 1 1 71.04 39.61 3.46 0.036 5.92 1 3 1 2904.46 3603.54 3.43 0.346 5.19 0 3 2 671.65 842.81 3.42 0.167 6.11 1 8 2 201.10 141.72 3.36 0.069 3.02 1 6 3 592.03 755.45 3.32 0.159 3.14 -1 0 12 331.92 190.76 3.28 0.080 1.25 2 0 4 682.19 534.40 3.26 0.133 2.48 4 2 8 81.26 8.95 3.26 0.017 1.24 0 5 2 1719.45 2109.77 3.24 0.265 4.76 1 17 3 384.89 289.36 3.16 0.098 1.64 -1 13 13 37.97 125.26 3.15 0.065 1.04 6 2 3 -14.17 58.58 3.12 0.044 1.07 -1 4 1 1039.44 1294.34 3.11 0.208 4.76 0 11 4 68.44 22.02 3.10 0.027 2.24 0 26 0 2109.12 1704.58 3.06 0.238 1.17 -3 5 3 504.60 403.00 3.04 0.116 1.93 -2 11 7 538.94 426.72 3.04 0.119 1.53 -2 10 6 404.17 301.46 3.01 0.100 1.69 -1 7 1 2034.96 2466.51 3.00 0.287 3.55 -1 7 4 252.27 190.39 3.00 0.080 2.65 -3 23 2 780.69 1059.26 2.98 0.188 1.12 0 24 5 511.25 400.11 2.97 0.115 1.17 0 24 11 -25.54 61.24 2.97 0.045 0.94 0 5 3 1371.95 1654.72 2.96 0.235 3.91 0 1 5 748.65 952.61 2.96 0.178 3.04 0 8 3 86.70 41.19 2.93 0.037 3.05 1 5 2 810.33 995.37 2.91 0.182 3.85 0 6 6 260.05 205.59 2.83 0.083 2.28 3 9 8 350.63 268.72 2.81 0.095 1.32 -6 4 8 412.37 297.23 2.80 0.099 0.95 -1 26 4 189.93 275.12 2.78 0.096 1.11 -7 0 4 292.96 136.97 2.77 0.068 0.92 6 14 2 149.08 235.00 2.77 0.088 0.97 -5 7 4 42.91 115.86 2.76 0.062 1.21 -1 21 2 230.30 155.85 2.75 0.072 1.39 4 1 11 462.79 358.94 2.75 0.109 1.05 2 8 6 315.62 253.40 2.74 0.092 1.77 -4 5 11 572.66 707.86 2.73 0.153 1.06 Bond lengths and angles C1 - Distance Angles O1B 1.2470 (0.0034) O1A 1.2728 (0.0033) 125.77 (0.28) C2 1.4904 (0.0043) 117.94 (0.26) 116.01 (0.27) C1 - O1B O1A C2 - Distance Angles C3 1.3342 (0.0042) C1 1.4904 (0.0044) 128.66 (0.30) H2 0.9500 115.67 115.67 C2 - C3 C1 C3 - Distance Angles C2 1.3342 (0.0042) C4 1.4506 (0.0045) 124.20 (0.31) H3 0.9500 117.90 117.90 C3 - C2 C4 C4 - Distance Angles O4B 1.2152 (0.0036) O4A 1.3524 (0.0037) 122.58 (0.31) C3 1.4506 (0.0045) 126.90 (0.31) 110.51 (0.30) C4 - O4B O4A C5 - Distance Angles O4A 1.4377 (0.0040) H5A 0.9800 109.47 H5B 0.9800 109.47 109.47 H5C 0.9800 109.47 109.47 109.47 C5 - O4A H5A H5B O1A - Distance Angles C1 1.2728 (0.0033) O1A - O1B - Distance Angles C1 1.2470 (0.0034) O1B - O4A - Distance Angles C4 1.3524 (0.0037) C5 1.4377 (0.0040) 116.02 (0.27) O4A - C4 O4B - Distance Angles C4 1.2152 (0.0036) O4B - C21 - Distance Angles C22 1.5281 (0.0041) 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 C21 1.5281 (0.0041) C26 1.5326 (0.0044) 109.35 (0.26) C27 1.5420 (0.0042) 108.16 (0.27) 107.39 (0.26) C23 1.5458 (0.0041) 113.47 (0.25) 112.34 (0.26) 105.83 (0.24) C22 - C21 C26 C27 C23 - Distance Angles C24 1.5319 (0.0040) C22 1.5458 (0.0041) 122.72 (0.24) H23A 0.9900 106.65 106.65 H23B 0.9900 106.65 106.65 106.58 C23 - C24 C22 H23A C24 - Distance Angles N25 1.5127 (0.0035) C28 1.5267 (0.0042) 106.40 (0.24) C29 1.5281 (0.0040) 105.51 (0.23) 110.62 (0.24) C23 1.5319 (0.0040) 104.45 (0.22) 114.99 (0.25) 113.92 (0.26) C24 - N25 C28 C29 C26 - Distance Angles C22 1.5326 (0.0044) 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 1.5420 (0.0042) 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 1.5267 (0.0042) 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 1.5281 (0.0040) 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 1.5127 (0.0035) 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 C31 - Distance Angles O31B 1.2474 (0.0035) O31A 1.2646 (0.0035) 125.14 (0.28) C32 1.4908 (0.0041) 117.25 (0.28) 117.37 (0.28) C31 - O31B O31A C32 - Distance Angles C33 1.3294 (0.0043) C31 1.4908 (0.0041) 126.83 (0.29) H32 0.9500 116.58 116.58 C32 - C33 C31 C33 - Distance Angles C32 1.3294 (0.0043) C34 1.4540 (0.0044) 123.80 (0.29) H33 0.9500 118.10 118.10 C33 - C32 C34 C34 - Distance Angles O34A 1.2078 (0.0033) O34B 1.3505 (0.0036) 122.72 (0.30) C33 1.4540 (0.0044) 125.94 (0.31) 111.33 (0.27) C34 - O34A O34B C35 - Distance Angles O34B 1.4432 (0.0037) H35A 0.9800 109.47 H35B 0.9800 109.47 109.47 H35C 0.9800 109.47 109.47 109.47 C35 - O34B H35A H35B O31A - Distance Angles C31 1.2646 (0.0035) O31A - O31B - Distance Angles C31 1.2474 (0.0035) O31B - O34A - Distance Angles C34 1.2078 (0.0033) O34A - O34B - Distance Angles C34 1.3505 (0.0036) C35 1.4432 (0.0037) 115.25 (0.25) O34B - C34 C41 - Distance Angles C42 1.5368 (0.0042) H41A 0.9800 109.47 H41B 0.9800 109.47 109.47 H41C 0.9800 109.47 109.47 109.47 C41 - C42 H41A H41B C42 - Distance Angles C46 1.5181 (0.0044) C41 1.5368 (0.0042) 108.05 (0.28) C47 1.5423 (0.0043) 109.34 (0.26) 107.25 (0.27) C43 1.5429 (0.0041) 114.10 (0.27) 105.91 (0.24) 111.85 (0.26) C42 - C46 C41 C47 C43 - Distance Angles C44 1.5381 (0.0041) C42 1.5429 (0.0041) 123.11 (0.23) H43A 0.9900 106.55 106.55 H43B 0.9900 106.55 106.55 106.53 C43 - C44 C42 H43A C44 - Distance Angles N45 1.5072 (0.0035) C48 1.5304 (0.0038) 106.44 (0.24) C49 1.5316 (0.0041) 105.65 (0.23) 111.03 (0.24) C43 1.5381 (0.0041) 104.43 (0.22) 114.89 (0.24) 113.48 (0.25) C44 - N45 C48 C49 C46 - Distance Angles C42 1.5181 (0.0044) H46A 0.9800 109.47 H46B 0.9800 109.47 109.47 H46C 0.9800 109.47 109.47 109.47 C46 - C42 H46A H46B C47 - Distance Angles C42 1.5423 (0.0043) H47A 0.9800 109.47 H47B 0.9800 109.47 109.47 H47C 0.9800 109.47 109.47 109.47 C47 - C42 H47A H47B C48 - Distance Angles C44 1.5304 (0.0038) H48A 0.9800 109.47 H48B 0.9800 109.47 109.47 H48C 0.9800 109.47 109.47 109.47 C48 - C44 H48A H48B C49 - Distance Angles C44 1.5316 (0.0041) H49A 0.9800 109.47 H49B 0.9800 109.47 109.47 H49C 0.9800 109.47 109.47 109.47 C49 - C44 H49A H49B N45 - Distance Angles C44 1.5072 (0.0035) H45A 0.9100 109.47 H45B 0.9100 109.47 109.47 H45C 0.9100 109.47 109.47 109.47 N45 - C44 H45A H45B Selected torsion angles -79.44 ( 0.42) O1B - C1 - C2 - C3 106.31 ( 0.37) O1A - C1 - C2 - C3 -0.80 ( 0.51) C1 - C2 - C3 - C4 -7.42 ( 0.51) C2 - C3 - C4 - O4B 171.66 ( 0.27) C2 - C3 - C4 - O4A 2.54 ( 0.42) O4B - C4 - O4A - C5 -176.59 ( 0.26) C3 - C4 - O4A - C5 -48.70 ( 0.40) C21 - C22 - C23 - C24 75.96 ( 0.34) C26 - C22 - C23 - C24 -167.15 ( 0.26) C27 - C22 - C23 - C24 -168.75 ( 0.25) C22 - C23 - C24 - N25 -52.53 ( 0.37) C22 - C23 - C24 - C28 76.65 ( 0.36) C22 - C23 - C24 - C29 81.13 ( 0.43) O31B - C31 - C32 - C33 -104.15 ( 0.38) O31A - C31 - C32 - C33 1.54 ( 0.54) C31 - C32 - C33 - C34 1.66 ( 0.55) C32 - C33 - C34 - O34A -177.81 ( 0.30) C32 - C33 - C34 - O34B -1.14 ( 0.45) O34A - C34 - O34B - C35 178.36 ( 0.28) C33 - C34 - O34B - C35 48.15 ( 0.39) C46 - C42 - C43 - C44 166.86 ( 0.27) C41 - C42 - C43 - C44 -76.62 ( 0.36) C47 - C42 - C43 - C44 167.73 ( 0.25) C42 - C43 - C44 - N45 51.53 ( 0.39) C42 - C43 - C44 - C48 -77.72 ( 0.34) C42 - C43 - C44 - C49 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.89 2.783(3) 165.8 N45-H45A...O31A 0.91 1.92 2.818(3) 168.7 N25-H25A...O1A 0.91 1.89 2.795(3) 170.8 N45-H45B...O1A_$1 0.91 1.86 2.768(3) 178.0 N45-H45C...O31B_$2 0.91 1.88 2.791(3) 177.3 N25-H25B...O1B_$2 0.91 1.92 2.825(3) 170.1 N25-H25C...O31A_$3 FMAP and GRID set by program FMAP 2 1 15 GRID -4.167 24 -2 4.167 1 2 R1 = 0.1103 for 4405 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.19 at 0.0370 0.4234 0.1186 [ 1.12 A from H21C ] Deepest hole -0.18 at 0.1337 0.3687 0.5957 [ 1.18 A from C33 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 5479 / 35265 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0370 0.0766 0.6186 1.00000 0.05 0.19 1.12 H21C 1.61 C21 1.63 H47A 1.67 H21A Q2 1 0.8633 0.0683 1.4467 1.00000 0.05 0.19 0.68 C42 0.87 C47 1.48 H47B 1.49 H47C Q3 1 1.2694 0.1676 1.3422 1.00000 0.05 0.18 1.44 O31A 1.49 H49C 1.60 C31 1.87 O31B Q4 1 0.8310 0.0714 1.0630 1.00000 0.05 0.16 1.24 O4A 1.60 H33 1.64 H5C 1.70 C4 Q5 1 1.0050 0.0333 1.1378 1.00000 0.05 0.16 1.14 O34B 2.06 H33 2.06 C34 2.33 C35 Q6 1 0.7836 0.0105 1.0632 1.00000 0.05 0.16 0.63 H5B 1.23 C5 1.60 H5C 1.93 O4A Q7 1 0.9548 0.0354 1.5167 1.00000 0.05 0.15 0.54 H47C 1.25 C47 1.70 H47A 2.05 H47B Q8 1 0.7093 0.0658 1.4599 1.00000 0.05 0.15 0.55 C42 0.97 C46 1.56 H46A 1.58 H46B Q9 1 0.0811 0.1989 0.7846 1.00000 0.05 0.15 0.76 C24 0.80 C29 1.37 H29B 1.45 H29A Q10 1 -0.2137 0.2092 0.7003 1.00000 0.05 0.15 1.41 H29C 1.46 H29A 1.54 C29 1.71 H29B Shortest distances between peaks (including symmetry equivalents) 2 8 1.04 2 7 1.58 4 6 1.88 5 6 1.97 4 5 1.98 7 8 2.05 1 7 2.07 7 7 2.30 9 10 2.34 1 2 2.86 Time profile in seconds ----------------------- 0.09: 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 0.02: Analyse other restraints etc. 0.88: 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 1.88: Structure factors and derivatives 3.31: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.38: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + ssf1328 finished at 12:57:10 Total CPU time: 6.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++