+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0071p-1 started at 14:59:00 on 14-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0071p-1 in P-1 CELL 0.71073 9.3001 11.9247 15.4496 76.199 74.813 89.758 ZERR 4.00 0.0024 0.0031 0.0044 0.019 0.013 0.017 LATT 1 SFAC C H N O S UNIT 56 104 8 12 4 V = 1602.69 F(000) = 656.0 Mu = 0.21 mm-1 Cell Wt = 1209.71 Rho = 1.253 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB N1 O2C HTAB N1 O32C HTAB N21 O2A HTAB N21 O32A HTAB N31 O32B EQIV_$1 -x, -y, -z+1 HTAB N1 O2A_$1 HTAB N21 O2C_$1 EQIV_$2 x, y+1, z HTAB N31 O2A_$2 EQIV_$3 x+1, y, z HTAB N41 O32C_$3 EQIV_$4 x+1, y+1, z HTAB N41 O2B_$4 EQIV_$5 -x+1, -y+1, -z+1 HTAB N41 O32B_$5 HTAB N41 S32_$5 FMAP 2 PLAN 10 SIZE 0.03 0.13 0.19 ACTA BOND $H WGHT 0.00000 16.81670 L.S. 4 TEMP -153.00 FVAR 0.52397 MOLE 1 C1 1 -0.213876 0.063373 0.695651 11.00000 0.04310 0.05115 = 0.06191 -0.01465 -0.03501 0.01367 C2 1 -0.245814 -0.056141 0.716304 11.00000 0.04400 0.02953 = 0.05490 -0.00271 -0.02352 -0.00425 C3 1 -0.311585 -0.119381 0.804865 11.00000 0.04450 0.03633 = 0.06516 -0.01853 -0.03695 0.00255 AFIX 43 H3 2 -0.326786 -0.201078 0.817818 11.00000 -1.20000 AFIX 0 C4 1 -0.356069 -0.061621 0.876024 11.00000 0.03955 0.04655 = 0.04978 0.00846 -0.02380 -0.01630 AFIX 43 H4 2 -0.406297 -0.103439 0.937039 11.00000 -1.20000 AFIX 0 C5 1 -0.326440 0.055335 0.856700 11.00000 0.03590 0.05319 = 0.05326 -0.00550 -0.02511 0.00685 AFIX 43 H5 2 -0.354058 0.093581 0.905437 11.00000 -1.20000 AFIX 0 C6 1 -0.258845 0.118062 0.770032 11.00000 0.04049 0.04229 = 0.07367 -0.02813 -0.02651 0.00848 AFIX 43 H6 2 -0.241275 0.199345 0.758775 11.00000 -1.20000 AFIX 0 N1 3 -0.141449 0.128530 0.607756 11.00000 0.06213 0.02879 = 0.06185 -0.01937 -0.02624 0.00216 AFIX 93 H1A 2 -0.113203 0.094847 0.561691 11.00000 -1.20000 H1B 2 -0.123737 0.203558 0.598047 11.00000 -1.20000 AFIX 0 O2A 4 -0.019229 -0.129339 0.607719 11.00000 0.04405 0.04657 = 0.06273 -0.02105 -0.01813 0.00477 O2B 4 -0.251074 -0.248815 0.668574 11.00000 0.04769 0.04847 = 0.07842 -0.02736 -0.02353 -0.00207 O2C 4 -0.231880 -0.070092 0.548517 11.00000 0.04827 0.04833 = 0.05915 -0.01561 -0.02856 0.00566 S2 5 -0.182472 -0.132315 0.628357 11.00000 0.03942 0.04071 = 0.05336 -0.01837 -0.01823 0.00341 MOLE 2 C22 1 0.307692 0.004970 0.667919 11.00000 0.03227 0.05243 = 0.04977 -0.01227 -0.02786 -0.00111 C23 1 0.299925 0.014186 0.765994 11.00000 0.03346 0.03789 = 0.06589 -0.01987 -0.03204 0.00548 AFIX 23 H23A 2 0.270535 0.093427 0.768704 11.00000 -1.20000 H23B 2 0.403674 0.010431 0.771407 11.00000 -1.20000 AFIX 0 C24 1 0.202824 -0.067168 0.854997 11.00000 0.03670 0.04129 = 0.04606 -0.00473 -0.02112 0.00120 C25 1 0.259676 -0.189370 0.876028 11.00000 0.04739 0.06138 = 0.04765 0.00283 -0.01599 -0.00844 AFIX 137 H25A 2 0.366747 -0.183660 0.871111 11.00000 -1.50000 H25B 2 0.242587 -0.230688 0.831523 11.00000 -1.50000 H25C 2 0.205915 -0.231614 0.938850 11.00000 -1.50000 AFIX 0 C26 1 0.430999 0.092391 0.599459 11.00000 0.05400 0.05546 = 0.04971 -0.01831 -0.02686 -0.00417 AFIX 137 H26A 2 0.428500 0.094969 0.535996 11.00000 -1.50000 H26B 2 0.528543 0.068576 0.607646 11.00000 -1.50000 H26C 2 0.414464 0.169289 0.611145 11.00000 -1.50000 AFIX 0 C27 1 0.332599 -0.116272 0.649218 11.00000 0.02840 0.04240 = 0.08005 -0.02183 -0.02341 0.00999 AFIX 137 H27A 2 0.244424 -0.168204 0.684190 11.00000 -1.50000 H27B 2 0.420145 -0.147014 0.668646 11.00000 -1.50000 H27C 2 0.349019 -0.110473 0.582961 11.00000 -1.50000 AFIX 0 C28 1 0.202071 -0.010502 0.933552 11.00000 0.05822 0.08678 = 0.05136 -0.02604 -0.01991 -0.00408 AFIX 137 H28A 2 0.304831 0.002063 0.936034 11.00000 -1.50000 H28B 2 0.144604 -0.061031 0.992312 11.00000 -1.50000 H28C 2 0.156291 0.063948 0.922890 11.00000 -1.50000 AFIX 0 C29 1 0.039313 -0.078495 0.851714 11.00000 0.04332 0.05478 = 0.05525 -0.00989 -0.01227 -0.00713 AFIX 137 H29A 2 -0.024275 -0.111908 0.914225 11.00000 -1.50000 H29B 2 0.031554 -0.128922 0.811275 11.00000 -1.50000 H29C 2 0.006762 -0.001852 0.827554 11.00000 -1.50000 AFIX 0 N21 3 0.166924 0.042106 0.642681 11.00000 0.03313 0.03847 = 0.05253 -0.00650 -0.01488 0.00036 AFIX 137 H21A 2 0.096103 -0.017608 0.666303 11.00000 -1.50000 H21B 2 0.185225 0.063191 0.579991 11.00000 -1.50000 H21C 2 0.133897 0.103303 0.666412 11.00000 -1.50000 AFIX 0 MOLE 3 C31 1 0.034709 0.564642 0.710964 11.00000 0.03712 0.03202 = 0.05341 -0.00398 -0.02295 0.00620 C32 1 0.036542 0.444790 0.740772 11.00000 0.03147 0.04736 = 0.04882 -0.01380 -0.01464 0.00370 C33 1 -0.006382 0.386087 0.834258 11.00000 0.02554 0.04502 = 0.07126 -0.02381 -0.01320 0.00268 AFIX 43 H33 2 -0.002737 0.304368 0.851610 11.00000 -1.20000 AFIX 0 C34 1 -0.054284 0.446744 0.901782 11.00000 0.04756 0.04381 = 0.05132 -0.00445 -0.01535 0.00666 AFIX 43 H34 2 -0.084331 0.408168 0.965612 11.00000 -1.20000 AFIX 0 C35 1 -0.056626 0.567904 0.871959 11.00000 0.03081 0.04296 = 0.05528 -0.02059 -0.00095 -0.00405 AFIX 43 H35 2 -0.089658 0.610991 0.917115 11.00000 -1.20000 AFIX 0 C36 1 -0.013607 0.625428 0.781375 11.00000 0.04310 0.03717 = 0.06340 -0.01504 -0.02071 0.00153 AFIX 43 H36 2 -0.015739 0.707301 0.764696 11.00000 -1.20000 AFIX 0 N31 3 0.071992 0.623694 0.619809 11.00000 0.05846 0.03708 = 0.05704 -0.02064 -0.02317 0.00237 AFIX 93 H31A 2 0.099015 0.585894 0.576252 11.00000 -1.20000 H31B 2 0.068943 0.699469 0.604748 11.00000 -1.20000 AFIX 0 O32A 4 0.094239 0.244031 0.706890 11.00000 0.06160 0.03637 = 0.05590 -0.01368 -0.02364 0.01165 O32B 4 0.223773 0.414511 0.590771 11.00000 0.05360 0.05449 = 0.05050 -0.01124 -0.02802 -0.00544 O32C 4 -0.038776 0.370176 0.613954 11.00000 0.04231 0.04920 = 0.05689 -0.01931 -0.02174 0.00452 S32 5 0.083525 0.360369 0.656708 11.00000 0.04189 0.04154 = 0.06123 -0.01852 -0.02418 0.00646 MOLE 4 C42 1 0.599279 0.491840 0.658749 11.00000 0.03902 0.03420 = 0.05994 -0.01555 -0.03030 0.00131 C43 1 0.610962 0.460656 0.759291 11.00000 0.04047 0.04618 = 0.05859 -0.01265 -0.02280 -0.00030 AFIX 23 H43A 2 0.654493 0.530550 0.769331 11.00000 -1.20000 H43B 2 0.685459 0.401372 0.762857 11.00000 -1.20000 AFIX 0 C44 1 0.470322 0.414770 0.845374 11.00000 0.04811 0.03380 = 0.07292 -0.01717 -0.02928 0.00946 C45 1 0.534338 0.374332 0.928722 11.00000 0.06498 0.06123 = 0.06192 -0.00970 -0.01920 -0.00972 AFIX 137 H45A 2 0.589696 0.439470 0.936295 11.00000 -1.50000 H45B 2 0.601673 0.312506 0.918521 11.00000 -1.50000 H45C 2 0.452585 0.345160 0.984654 11.00000 -1.50000 AFIX 0 C46 1 0.577950 0.390646 0.619793 11.00000 0.04186 0.04708 = 0.08571 -0.01345 -0.03317 0.00010 AFIX 137 H46A 2 0.603397 0.415904 0.552127 11.00000 -1.50000 H46B 2 0.473597 0.360322 0.643643 11.00000 -1.50000 H46C 2 0.642977 0.329874 0.638263 11.00000 -1.50000 AFIX 0 C47 1 0.489813 0.583286 0.639041 11.00000 0.04562 0.03863 = 0.07137 -0.01249 -0.02888 -0.00019 AFIX 137 H47A 2 0.505830 0.611214 0.572020 11.00000 -1.50000 H47B 2 0.505611 0.648041 0.665107 11.00000 -1.50000 H47C 2 0.387459 0.549528 0.667297 11.00000 -1.50000 AFIX 0 C48 1 0.378603 0.313700 0.836040 11.00000 0.04401 0.05961 = 0.06655 -0.01430 -0.01802 -0.00276 AFIX 137 H48A 2 0.304984 0.280875 0.895164 11.00000 -1.50000 H48B 2 0.445289 0.254018 0.819022 11.00000 -1.50000 H48C 2 0.326992 0.341693 0.787975 11.00000 -1.50000 AFIX 0 C49 1 0.369805 0.511769 0.861833 11.00000 0.05712 0.05981 = 0.07142 -0.01668 -0.01447 0.00885 AFIX 137 H49A 2 0.312674 0.528245 0.815670 11.00000 -1.50000 H49B 2 0.430626 0.581235 0.856558 11.00000 -1.50000 H49C 2 0.300922 0.488737 0.923947 11.00000 -1.50000 AFIX 0 N41 3 0.752724 0.548989 0.603934 11.00000 0.04420 0.04550 = 0.05914 -0.01119 -0.03504 0.00313 AFIX 137 H41A 2 0.823985 0.498749 0.613927 11.00000 -1.50000 H41B 2 0.768436 0.613685 0.622549 11.00000 -1.50000 H41C 2 0.757470 0.568693 0.542562 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0071p-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - N1 C2 C6 C2 - C3 C1 S2 C3 - C2 C4 C4 - C5 C3 C5 - C6 C4 C6 - C5 C1 N1 - C1 O2A - S2 O2B - S2 O2C - S2 S2 - O2B O2C O2A C2 C22 - N21 C23 C26 C27 C23 - C22 C24 C24 - C28 C25 C23 C29 C25 - C24 C26 - C22 C27 - C22 C28 - C24 C29 - C24 N21 - C22 C31 - N31 C32 C36 C32 - C31 C33 S32 C33 - C34 C32 C34 - C33 C35 C35 - C36 C34 C36 - C35 C31 N31 - C31 O32A - S32 O32B - S32 O32C - S32 S32 - O32A O32C O32B C32 C42 - C46 C47 N41 C43 C43 - C42 C44 C44 - C49 C45 C48 C43 C45 - C44 C46 - C42 C47 - C42 C48 - C44 C49 - C44 N41 - C42 Operators for generating equivalent atoms: $1 -x, -y, -z+1 $2 x, y+1, z $3 x+1, y, z $4 x+1, y+1, z $5 -x+1, -y+1, -z+1 24587 Reflections read, of which 140 rejected -12 =< h =< 12, -15 =< k =< 15, -19 =< l =< 19, Max. 2-theta = 54.95 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 -10 5 -2.02 1.99 3 12.06 9 1 7 2.68 1.82 4 9.41 8 -4 8 -0.22 0.20 5 2.01 -3 2 9 -9.16 4.01 3 23.20 -5 9 9 -12.87 11.42 2 66.57 -3 8 11 -2.78 2.42 4 26.44 -2 0 12 -0.46 0.35 4 11.32 -4 1 12 0.38 2.99 3 24.61 -3 4 12 -18.84 10.05 2 67.15 -1 9 14 25.36 18.03 2 101.64 -1 9 16 38.49 17.57 2 121.07 11 Inconsistent equivalents 7102 Unique reflections, of which 0 suppressed R(int) = 0.2315 R(sigma) = 0.3039 Friedel opposites merged Maximum memory for data reduction = 4663 / 71040 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 = 5828 / 475720 wR2 = 0.3708 before cycle 1 for 7102 data and 373 / 373 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 16.82 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52398 0.00208 0.005 OSF Mean shift/esd = 0.000 Maximum = 0.005 for OSF Max. shift = 0.000 A for H29C Max. dU = 0.000 for C5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5828 / 475720 wR2 = 0.3708 before cycle 2 for 7102 data and 373 / 373 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 16.82 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52398 0.00208 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U33 S2 Max. shift = 0.000 A for H27B Max. dU = 0.000 for C42 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5828 / 475720 wR2 = 0.3708 before cycle 3 for 7102 data and 373 / 373 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 16.82 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52398 0.00208 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U11 S32 Max. shift = 0.000 A for H27C Max. dU = 0.000 for C32 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5828 / 475720 wR2 = 0.3708 before cycle 4 for 7102 data and 373 / 373 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 16.82 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52398 0.00208 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H27C Max. dU = 0.000 for C32 Largest correlation matrix elements -0.612 U13 C1 / U33 C1 -0.561 U13 C3 / U11 C3 -0.544 U13 C4 / U33 C4 -0.611 U13 C3 / U33 C3 -0.558 U13 C46 / U33 C46 -0.541 U13 C26 / U33 C26 -0.594 U13 C23 / U33 C23 -0.557 U13 N41 / U11 N41 -0.540 U12 C3 / U23 C3 -0.584 U13 N41 / U33 N41 -0.553 U13 C23 / U11 C23 -0.539 U13 C2 / U33 C2 -0.572 U13 C22 / U33 C22 -0.551 U13 C6 / U33 C6 -0.539 z C1 / x C1 -0.567 U13 C42 / U33 C42 -0.545 U13 C22 / U11 C22 -0.533 U13 S32 / U33 S32 -0.562 U13 C5 / U33 C5 -0.545 U12 C1 / U23 C1 -0.532 U13 C42 / U11 C42 -0.561 U13 C1 / U11 C1 -0.544 U13 C31 / U33 C31 -0.531 U13 C24 / U33 C24 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 -0.3268 -0.2011 0.8178 43 0.950 0.000 C3 C2 C4 H4 -0.4063 -0.1034 0.9370 43 0.950 0.000 C4 C5 C3 H5 -0.3541 0.0936 0.9054 43 0.950 0.000 C5 C6 C4 H6 -0.2413 0.1993 0.7588 43 0.950 0.000 C6 C5 C1 H1A -0.1132 0.0948 0.5617 93 0.880 0.000 N1 C1 C2 H1B -0.1237 0.2036 0.5980 93 0.880 0.000 N1 C1 C2 H23A 0.2705 0.0934 0.7687 23 0.990 0.000 C23 C22 C24 H23B 0.4037 0.0104 0.7714 23 0.990 0.000 C23 C22 C24 H25A 0.3667 -0.1837 0.8711 137 0.980 0.000 C25 C24 H25A H25B 0.2426 -0.2307 0.8315 137 0.980 0.000 C25 C24 H25A H25C 0.2059 -0.2316 0.9389 137 0.980 0.000 C25 C24 H25A H26A 0.4285 0.0950 0.5360 137 0.980 0.000 C26 C22 H26A H26B 0.5285 0.0686 0.6076 137 0.980 0.000 C26 C22 H26A H26C 0.4145 0.1693 0.6111 137 0.980 0.000 C26 C22 H26A H27A 0.2444 -0.1682 0.6842 137 0.980 0.000 C27 C22 H27A H27B 0.4201 -0.1470 0.6686 137 0.980 0.000 C27 C22 H27A H27C 0.3490 -0.1105 0.5830 137 0.980 0.000 C27 C22 H27A H28A 0.3048 0.0021 0.9360 137 0.980 0.000 C28 C24 H28A H28B 0.1446 -0.0610 0.9923 137 0.980 0.000 C28 C24 H28A H28C 0.1563 0.0639 0.9229 137 0.980 0.000 C28 C24 H28A H29A -0.0243 -0.1119 0.9142 137 0.980 0.000 C29 C24 H29A H29B 0.0316 -0.1289 0.8113 137 0.980 0.000 C29 C24 H29A H29C 0.0068 -0.0019 0.8276 137 0.980 0.000 C29 C24 H29A H21A 0.0961 -0.0176 0.6663 137 0.910 0.000 N21 C22 H21A H21B 0.1852 0.0632 0.5800 137 0.910 0.000 N21 C22 H21A H21C 0.1339 0.1033 0.6664 137 0.910 0.000 N21 C22 H21A H33 -0.0027 0.3044 0.8516 43 0.950 0.000 C33 C34 C32 H34 -0.0843 0.4082 0.9656 43 0.950 0.000 C34 C33 C35 H35 -0.0897 0.6110 0.9171 43 0.950 0.000 C35 C36 C34 H36 -0.0157 0.7073 0.7647 43 0.950 0.000 C36 C35 C31 H31A 0.0990 0.5859 0.5762 93 0.880 0.000 N31 C31 C32 H31B 0.0689 0.6995 0.6047 93 0.880 0.000 N31 C31 C32 H43A 0.6545 0.5306 0.7693 23 0.990 0.000 C43 C42 C44 H43B 0.6855 0.4014 0.7629 23 0.990 0.000 C43 C42 C44 H45A 0.5897 0.4395 0.9363 137 0.980 0.000 C45 C44 H45A H45B 0.6017 0.3125 0.9185 137 0.980 0.000 C45 C44 H45A H45C 0.4526 0.3452 0.9847 137 0.980 0.000 C45 C44 H45A H46A 0.6034 0.4159 0.5521 137 0.980 0.000 C46 C42 H46A H46B 0.4736 0.3603 0.6436 137 0.980 0.000 C46 C42 H46A H46C 0.6430 0.3299 0.6383 137 0.980 0.000 C46 C42 H46A H47A 0.5058 0.6112 0.5720 137 0.980 0.000 C47 C42 H47A H47B 0.5056 0.6480 0.6651 137 0.980 0.000 C47 C42 H47A H47C 0.3875 0.5495 0.6673 137 0.980 0.000 C47 C42 H47A H48A 0.3050 0.2809 0.8952 137 0.980 0.000 C48 C44 H48A H48B 0.4453 0.2540 0.8190 137 0.980 0.000 C48 C44 H48A H48C 0.3270 0.3417 0.7880 137 0.980 0.000 C48 C44 H48A H49A 0.3127 0.5282 0.8157 137 0.980 0.000 C49 C44 H49A H49B 0.4306 0.5812 0.8566 137 0.980 0.000 C49 C44 H49A H49C 0.3009 0.4887 0.9239 137 0.980 0.000 C49 C44 H49A H41A 0.8240 0.4987 0.6139 137 0.910 0.000 N41 C42 H41A H41B 0.7684 0.6137 0.6225 137 0.910 0.000 N41 C42 H41A H41C 0.7575 0.5687 0.5426 137 0.910 0.000 N41 C42 H41A 06skc0071p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.21388 0.06337 0.69565 1.00000 0.04310 0.05114 0.06191 -0.01465 -0.03501 0.01367 0.04790 0.01739 0.00133 0.00107 0.00096 0.00000 0.00717 0.00803 0.00926 0.00719 0.00708 0.00595 0.00330 C2 -0.24581 -0.05614 0.71630 1.00000 0.04401 0.02953 0.05490 -0.00271 -0.02352 -0.00425 0.04215 0.01587 0.00125 0.00094 0.00088 0.00000 0.00692 0.00651 0.00855 0.00599 0.00654 0.00512 0.00302 C3 -0.31159 -0.11938 0.80486 1.00000 0.04451 0.03632 0.06515 -0.01853 -0.03695 0.00255 0.04329 0.01531 0.00125 0.00100 0.00091 0.00000 0.00703 0.00663 0.00922 0.00677 0.00697 0.00539 0.00315 H3 -0.32679 -0.20108 0.81782 1.00000 0.05195 0.00000 0.00000 C4 -0.35607 -0.06162 0.87602 1.00000 0.03956 0.04655 0.04978 0.00846 -0.02381 -0.01630 0.04651 0.01667 0.00124 0.00102 0.00088 0.00000 0.00689 0.00771 0.00823 0.00646 0.00645 0.00561 0.00334 H4 -0.40630 -0.10344 0.93704 1.00000 0.05581 0.00000 0.00000 C5 -0.32644 0.05533 0.85670 1.00000 0.03590 0.05318 0.05325 -0.00551 -0.02510 0.00685 0.04624 0.01745 0.00124 0.00105 0.00091 0.00000 0.00673 0.00834 0.00881 0.00683 0.00662 0.00573 0.00323 H5 -0.35406 0.09358 0.90544 1.00000 0.05549 0.00000 0.00000 C6 -0.25884 0.11806 0.77003 1.00000 0.04049 0.04228 0.07367 -0.02813 -0.02651 0.00848 0.04757 0.01642 0.00126 0.00106 0.00096 0.00000 0.00695 0.00725 0.01028 0.00738 0.00721 0.00556 0.00330 H6 -0.24127 0.19935 0.75877 1.00000 0.05708 0.00000 0.00000 N1 -0.14145 0.12853 0.60776 1.00000 0.06213 0.02878 0.06185 -0.01937 -0.02624 0.00217 0.04762 0.01297 0.00107 0.00077 0.00073 0.00000 0.00667 0.00541 0.00760 0.00529 0.00605 0.00468 0.00266 H1A -0.11320 0.09485 0.56169 1.00000 0.05714 0.00000 0.00000 H1B -0.12374 0.20356 0.59805 1.00000 0.05714 0.00000 0.00000 O2A -0.01923 -0.12934 0.60772 1.00000 0.04405 0.04657 0.06273 -0.02104 -0.01813 0.00477 0.04906 0.01103 0.00084 0.00065 0.00057 0.00000 0.00477 0.00493 0.00594 0.00432 0.00443 0.00375 0.00215 O2B -0.25107 -0.24882 0.66857 1.00000 0.04769 0.04846 0.07842 -0.02735 -0.02353 -0.00208 0.05484 0.01095 0.00087 0.00067 0.00062 0.00000 0.00501 0.00522 0.00665 0.00474 0.00481 0.00397 0.00235 O2C -0.23188 -0.07009 0.54852 1.00000 0.04827 0.04832 0.05915 -0.01561 -0.02856 0.00566 0.04877 0.01082 0.00085 0.00065 0.00057 0.00000 0.00484 0.00502 0.00570 0.00427 0.00452 0.00381 0.00216 S2 -0.18247 -0.13231 0.62836 1.00000 0.03942 0.04071 0.05335 -0.01837 -0.01823 0.00341 0.04219 0.00423 0.00033 0.00026 0.00023 0.00000 0.00172 0.00177 0.00211 0.00154 0.00160 0.00131 0.00080 C22 0.30769 0.00497 0.66792 1.00000 0.03227 0.05243 0.04977 -0.01226 -0.02786 -0.00111 0.04160 0.01521 0.00119 0.00099 0.00082 0.00000 0.00616 0.00746 0.00777 0.00609 0.00598 0.00528 0.00300 C23 0.29992 0.01419 0.76599 1.00000 0.03346 0.03790 0.06588 -0.01987 -0.03204 0.00549 0.04089 0.01462 0.00116 0.00092 0.00081 0.00000 0.00616 0.00651 0.00875 0.00617 0.00638 0.00494 0.00302 H23A 0.27054 0.09343 0.76870 1.00000 0.04906 0.00000 0.00000 H23B 0.40367 0.01043 0.77141 1.00000 0.04906 0.00000 0.00000 C24 0.20282 -0.06717 0.85500 1.00000 0.03671 0.04129 0.04605 -0.00473 -0.02112 0.00120 0.04046 0.01612 0.00120 0.00095 0.00081 0.00000 0.00642 0.00690 0.00770 0.00586 0.00605 0.00514 0.00294 C25 0.25968 -0.18937 0.87603 1.00000 0.04740 0.06138 0.04765 0.00283 -0.01599 -0.00844 0.05433 0.01848 0.00134 0.00105 0.00088 0.00000 0.00756 0.00866 0.00829 0.00670 0.00671 0.00623 0.00352 H25A 0.36674 -0.18366 0.87111 1.00000 0.08149 0.00000 0.00000 H25B 0.24258 -0.23069 0.83152 1.00000 0.08149 0.00000 0.00000 H25C 0.20592 -0.23161 0.93885 1.00000 0.08149 0.00000 0.00000 C26 0.43100 0.09239 0.59946 1.00000 0.05400 0.05546 0.04971 -0.01831 -0.02686 -0.00417 0.04958 0.01604 0.00132 0.00102 0.00083 0.00000 0.00767 0.00793 0.00814 0.00639 0.00681 0.00610 0.00326 H26A 0.42850 0.09497 0.53599 1.00000 0.07438 0.00000 0.00000 H26B 0.52854 0.06857 0.60765 1.00000 0.07438 0.00000 0.00000 H26C 0.41447 0.16929 0.61114 1.00000 0.07438 0.00000 0.00000 C27 0.33260 -0.11627 0.64922 1.00000 0.02841 0.04240 0.08004 -0.02183 -0.02341 0.00999 0.04741 0.01621 0.00119 0.00094 0.00092 0.00000 0.00604 0.00700 0.00991 0.00672 0.00651 0.00500 0.00328 H27A 0.24443 -0.16821 0.68419 1.00000 0.07111 0.00000 0.00000 H27B 0.42015 -0.14701 0.66864 1.00000 0.07111 0.00000 0.00000 H27C 0.34902 -0.11047 0.58296 1.00000 0.07111 0.00000 0.00000 C28 0.20207 -0.01050 0.93355 1.00000 0.05822 0.08677 0.05136 -0.02603 -0.01991 -0.00408 0.06284 0.01805 0.00148 0.00123 0.00090 0.00000 0.00864 0.01064 0.00898 0.00788 0.00743 0.00751 0.00389 H28A 0.30483 0.00206 0.93603 1.00000 0.09425 0.00000 0.00000 H28B 0.14461 -0.06103 0.99231 1.00000 0.09425 0.00000 0.00000 H28C 0.15629 0.06395 0.92289 1.00000 0.09425 0.00000 0.00000 C29 0.03931 -0.07849 0.85171 1.00000 0.04333 0.05477 0.05525 -0.00989 -0.01227 -0.00712 0.05191 0.01725 0.00124 0.00105 0.00089 0.00000 0.00721 0.00818 0.00871 0.00675 0.00662 0.00603 0.00337 H29A -0.02427 -0.11191 0.91423 1.00000 0.07787 0.00000 0.00000 H29B 0.03155 -0.12893 0.81128 1.00000 0.07787 0.00000 0.00000 H29C 0.00677 -0.00185 0.82755 1.00000 0.07787 0.00000 0.00000 N21 0.16692 0.04211 0.64268 1.00000 0.03313 0.03847 0.05253 -0.00650 -0.01488 0.00036 0.04154 0.01282 0.00092 0.00075 0.00065 0.00000 0.00510 0.00554 0.00663 0.00477 0.00489 0.00410 0.00243 H21A 0.09610 -0.01761 0.66630 1.00000 0.06231 0.00000 0.00000 H21B 0.18522 0.06319 0.57999 1.00000 0.06231 0.00000 0.00000 H21C 0.13390 0.10331 0.66641 1.00000 0.06231 0.00000 0.00000 C31 0.03471 0.56464 0.71096 1.00000 0.03712 0.03202 0.05340 -0.00398 -0.02295 0.00621 0.03991 0.01663 0.00122 0.00094 0.00088 0.00000 0.00638 0.00655 0.00835 0.00616 0.00624 0.00497 0.00292 C32 0.03654 0.44479 0.74077 1.00000 0.03148 0.04736 0.04882 -0.01379 -0.01464 0.00370 0.04146 0.01613 0.00118 0.00101 0.00086 0.00000 0.00621 0.00744 0.00831 0.00635 0.00602 0.00520 0.00294 C33 -0.00638 0.38609 0.83426 1.00000 0.02554 0.04502 0.07126 -0.02381 -0.01320 0.00268 0.04557 0.01668 0.00116 0.00106 0.00095 0.00000 0.00593 0.00722 0.00983 0.00724 0.00634 0.00509 0.00317 H33 -0.00274 0.30437 0.85161 1.00000 0.05469 0.00000 0.00000 C34 -0.05428 0.44674 0.90178 1.00000 0.04757 0.04381 0.05132 -0.00445 -0.01536 0.00665 0.04845 0.01820 0.00129 0.00102 0.00091 0.00000 0.00747 0.00767 0.00855 0.00658 0.00674 0.00580 0.00325 H34 -0.08433 0.40817 0.96561 1.00000 0.05814 0.00000 0.00000 C35 -0.05663 0.56790 0.87196 1.00000 0.03081 0.04296 0.05528 -0.02058 -0.00096 -0.00405 0.04356 0.01644 0.00117 0.00099 0.00090 0.00000 0.00626 0.00743 0.00888 0.00663 0.00611 0.00522 0.00304 H35 -0.08966 0.61099 0.91712 1.00000 0.05228 0.00000 0.00000 C36 -0.01361 0.62543 0.78137 1.00000 0.04310 0.03717 0.06340 -0.01504 -0.02070 0.00152 0.04618 0.01660 0.00127 0.00103 0.00094 0.00000 0.00705 0.00690 0.00934 0.00685 0.00690 0.00542 0.00314 H36 -0.01574 0.70730 0.76469 1.00000 0.05541 0.00000 0.00000 N31 0.07199 0.62369 0.61981 1.00000 0.05846 0.03708 0.05703 -0.02064 -0.02317 0.00237 0.04779 0.01303 0.00103 0.00080 0.00070 0.00000 0.00664 0.00573 0.00735 0.00537 0.00584 0.00479 0.00265 H31A 0.09902 0.58589 0.57625 1.00000 0.05734 0.00000 0.00000 H31B 0.06894 0.69947 0.60475 1.00000 0.05734 0.00000 0.00000 O32A 0.09424 0.24403 0.70689 1.00000 0.06161 0.03636 0.05590 -0.01368 -0.02364 0.01165 0.04938 0.01142 0.00090 0.00063 0.00056 0.00000 0.00537 0.00469 0.00566 0.00414 0.00466 0.00384 0.00216 O32B 0.22377 0.41451 0.59077 1.00000 0.05360 0.05448 0.05050 -0.01124 -0.02802 -0.00543 0.05041 0.01066 0.00088 0.00068 0.00055 0.00000 0.00530 0.00527 0.00548 0.00427 0.00465 0.00412 0.00223 O32C -0.03878 0.37018 0.61395 1.00000 0.04231 0.04920 0.05689 -0.01931 -0.02174 0.00452 0.04674 0.01075 0.00083 0.00065 0.00056 0.00000 0.00457 0.00497 0.00561 0.00421 0.00431 0.00370 0.00209 S32 0.08353 0.36037 0.65671 1.00000 0.04189 0.04154 0.06122 -0.01852 -0.02418 0.00646 0.04520 0.00435 0.00034 0.00026 0.00024 0.00000 0.00177 0.00182 0.00227 0.00163 0.00172 0.00137 0.00085 C42 0.59928 0.49184 0.65875 1.00000 0.03902 0.03420 0.05994 -0.01555 -0.03030 0.00131 0.04040 0.01479 0.00120 0.00091 0.00083 0.00000 0.00660 0.00632 0.00843 0.00583 0.00637 0.00494 0.00297 C43 0.61096 0.46066 0.75929 1.00000 0.04047 0.04618 0.05859 -0.01265 -0.02280 -0.00030 0.04660 0.01643 0.00124 0.00101 0.00082 0.00000 0.00691 0.00733 0.00875 0.00636 0.00670 0.00547 0.00318 H43A 0.65449 0.53055 0.76933 1.00000 0.05593 0.00000 0.00000 H43B 0.68546 0.40137 0.76286 1.00000 0.05593 0.00000 0.00000 C44 0.47032 0.41477 0.84537 1.00000 0.04811 0.03380 0.07291 -0.01717 -0.02928 0.00946 0.04840 0.01708 0.00133 0.00096 0.00093 0.00000 0.00734 0.00669 0.00963 0.00649 0.00727 0.00548 0.00330 C45 0.53434 0.37433 0.92872 1.00000 0.06499 0.06123 0.06192 -0.00971 -0.01920 -0.00972 0.06321 0.01894 0.00152 0.00114 0.00093 0.00000 0.00902 0.00893 0.00959 0.00739 0.00786 0.00701 0.00385 H45A 0.58969 0.43947 0.93630 1.00000 0.09481 0.00000 0.00000 H45B 0.60167 0.31251 0.91852 1.00000 0.09481 0.00000 0.00000 H45C 0.45259 0.34516 0.98466 1.00000 0.09481 0.00000 0.00000 C46 0.57795 0.39065 0.61979 1.00000 0.04187 0.04707 0.08570 -0.01345 -0.03318 0.00011 0.05560 0.01664 0.00131 0.00100 0.00096 0.00000 0.00720 0.00767 0.01070 0.00720 0.00752 0.00573 0.00369 H46A 0.60339 0.41590 0.55213 1.00000 0.08341 0.00000 0.00000 H46B 0.47360 0.36032 0.64365 1.00000 0.08341 0.00000 0.00000 H46C 0.64298 0.32987 0.63826 1.00000 0.08341 0.00000 0.00000 C47 0.48981 0.58329 0.63904 1.00000 0.04562 0.03863 0.07137 -0.01250 -0.02888 -0.00019 0.04949 0.01666 0.00128 0.00095 0.00090 0.00000 0.00719 0.00700 0.00947 0.00648 0.00705 0.00537 0.00334 H47A 0.50583 0.61121 0.57202 1.00000 0.07424 0.00000 0.00000 H47B 0.50561 0.64804 0.66511 1.00000 0.07424 0.00000 0.00000 H47C 0.38746 0.54953 0.66730 1.00000 0.07424 0.00000 0.00000 C48 0.37860 0.31370 0.83604 1.00000 0.04401 0.05961 0.06655 -0.01430 -0.01802 -0.00276 0.05631 0.01734 0.00134 0.00107 0.00093 0.00000 0.00739 0.00858 0.00975 0.00724 0.00717 0.00618 0.00359 H48A 0.30498 0.28088 0.89516 1.00000 0.08446 0.00000 0.00000 H48B 0.44529 0.25401 0.81902 1.00000 0.08446 0.00000 0.00000 H48C 0.32700 0.34169 0.78797 1.00000 0.08446 0.00000 0.00000 C49 0.36980 0.51177 0.86183 1.00000 0.05713 0.05980 0.07142 -0.01668 -0.01448 0.00885 0.06325 0.02039 0.00146 0.00112 0.00100 0.00000 0.00845 0.00897 0.01038 0.00774 0.00785 0.00683 0.00385 H49A 0.31267 0.52824 0.81567 1.00000 0.09487 0.00000 0.00000 H49B 0.43062 0.58124 0.85656 1.00000 0.09487 0.00000 0.00000 H49C 0.30092 0.48873 0.92395 1.00000 0.09487 0.00000 0.00000 N41 0.75272 0.54899 0.60393 1.00000 0.04420 0.04550 0.05913 -0.01119 -0.03504 0.00313 0.04580 0.01274 0.00097 0.00077 0.00067 0.00000 0.00572 0.00589 0.00693 0.00509 0.00543 0.00452 0.00261 H41A 0.82398 0.49875 0.61393 1.00000 0.06871 0.00000 0.00000 H41B 0.76843 0.61369 0.62255 1.00000 0.06871 0.00000 0.00000 H41C 0.75747 0.56869 0.54256 1.00000 0.06871 0.00000 0.00000 Final Structure Factor Calculation for 06skc0071p-1 in P-1 Total number of l.s. parameters = 373 Maximum vector length = 511 Memory required = 5455 / 24017 wR2 = 0.3708 before cycle 5 for 7102 data and 0 / 373 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 16.82 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.2106 for 2916 Fo > 4sig(Fo) and 0.3758 for all 7102 data wR2 = 0.3708, GooF = S = 1.153, Restrained GooF = 1.153 for all data Occupancy sum of asymmetric unit = 40.00 for non-hydrogen and 52.00 for hydrogen atoms Principal mean square atomic displacements U 0.0712 0.0516 0.0209 C1 0.0645 0.0348 0.0272 C2 0.0746 0.0373 0.0179 C3 0.0833 0.0328 0.0235 C4 0.0640 0.0517 0.0230 C5 0.0773 0.0350 0.0304 C6 0.0695 0.0508 0.0225 N1 0.0643 0.0429 0.0400 O2A 0.0802 0.0531 0.0311 O2B 0.0659 0.0473 0.0331 O2C 0.0555 0.0390 0.0320 S2 0.0588 0.0518 0.0143 C22 0.0707 0.0351 0.0168 C23 0.0550 0.0397 0.0266 C24 0.0799 0.0433 0.0398 C25 0.0649 0.0575 0.0264 C26 0.0802 0.0397 0.0223 C27 0.0904 0.0598 0.0383 C28 0.0625 0.0556 0.0377 C29 0.0556 0.0381 0.0309 N21 0.0592 0.0368 0.0238 C31 0.0499 0.0454 0.0291 C32 0.0734 0.0388 0.0245 C33 0.0586 0.0493 0.0375 C34 0.0664 0.0359 0.0284 C35 0.0640 0.0410 0.0335 C36 0.0639 0.0510 0.0284 N31 0.0662 0.0488 0.0331 O32A 0.0698 0.0520 0.0294 O32B 0.0605 0.0457 0.0340 O32C 0.0640 0.0384 0.0332 S32 0.0659 0.0355 0.0198 C42 0.0614 0.0472 0.0312 C43 0.0758 0.0389 0.0305 C44 0.0795 0.0603 0.0498 C45 0.0897 0.0478 0.0293 C46 0.0754 0.0412 0.0318 C47 0.0674 0.0617 0.0398 C48 0.0738 0.0635 0.0525 C49 0.0707 0.0455 0.0212 N41 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.006 0.011 0.017 0.023 0.031 0.040 0.052 0.071 0.109 1.000 Number in group 775. 659. 727. 680. 739. 688. 704. 705. 715. 710. GooF 1.207 1.208 1.250 1.182 1.207 1.168 1.148 1.151 1.041 0.933 K 109.535 20.065 8.154 4.261 2.619 1.884 1.365 1.129 0.977 1.003 Resolution(A) 0.77 0.80 0.84 0.88 0.92 0.98 1.05 1.16 1.33 1.67 inf Number in group 729. 713. 712. 693. 708. 704. 725. 703. 702. 713. GooF 1.219 1.199 1.193 1.226 1.252 1.182 1.138 1.067 1.005 1.020 K 3.394 3.061 2.860 1.994 1.608 1.342 1.124 1.001 1.013 1.020 R1 0.666 0.650 0.616 0.538 0.491 0.403 0.277 0.203 0.167 0.085 Recommended weighting scheme: WGHT 0.0000 16.8143 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 -12 8 709.33 42.68 3.65 0.035 0.78 2 1 1 992.99 517.63 3.61 0.121 4.33 9 5 12 471.48 8.57 3.60 0.016 0.87 -1 6 7 545.40 1086.97 3.53 0.175 1.55 -2 2 1 269.39 10.58 3.52 0.017 3.49 -8 8 2 674.76 279.90 3.50 0.089 0.90 2 -12 4 386.84 18.53 3.47 0.023 0.88 7 -4 6 438.71 934.71 3.47 0.162 1.14 -9 8 6 407.97 10.13 3.40 0.017 0.78 5 3 16 370.50 21.16 3.40 0.024 0.93 7 -10 2 307.43 4.15 3.38 0.011 0.88 9 -7 1 380.81 107.77 3.28 0.055 0.88 3 -7 7 205.47 5.43 3.28 0.012 1.16 8 10 5 289.75 21.96 3.13 0.025 0.83 -1 7 7 82.11 395.22 3.12 0.106 1.43 0 13 5 325.39 0.62 3.12 0.004 0.92 -4 10 14 373.51 8.17 3.07 0.015 0.78 9 -2 8 -18.40 165.06 3.05 0.068 0.97 5 -1 13 315.26 85.87 3.05 0.049 1.06 1 1 5 182.18 27.42 3.05 0.028 3.08 -7 11 3 243.05 14.66 3.01 0.020 0.83 -10 4 5 311.69 0.02 3.00 0.001 0.79 -7 9 2 169.25 0.23 3.00 0.003 0.93 -2 11 7 471.93 22.41 3.00 0.025 1.00 0 -12 6 313.65 5.13 2.99 0.012 0.83 3 7 8 408.59 122.04 2.98 0.059 1.35 -2 2 3 547.32 39.97 2.97 0.034 2.82 0 -4 2 -50.06 110.10 2.94 0.056 2.48 -5 3 9 575.42 142.52 2.93 0.063 1.08 11 0 1 527.40 10.96 2.88 0.018 0.83 5 -5 1 143.75 7.10 2.88 0.014 1.46 10 -4 1 176.75 2.73 2.85 0.009 0.88 5 9 2 723.21 374.90 2.84 0.103 1.06 3 4 3 118.99 0.82 2.83 0.005 2.15 6 0 15 154.89 0.18 2.83 0.002 0.93 -8 8 0 183.62 1.56 2.83 0.007 0.91 8 6 10 147.19 0.98 2.82 0.005 0.96 -6 1 7 -58.05 142.56 2.82 0.063 1.09 1 -8 8 342.60 49.67 2.79 0.037 1.03 11 -4 3 281.12 31.26 2.79 0.030 0.81 1 6 17 -43.52 91.87 2.79 0.051 0.88 9 -1 7 74.28 351.90 2.79 0.100 1.00 -7 4 12 361.86 0.28 2.78 0.003 0.79 0 9 8 354.12 92.69 2.76 0.051 1.19 1 10 6 260.78 57.52 2.76 0.040 1.16 -8 1 4 236.80 14.57 2.76 0.020 1.00 6 4 17 274.71 31.33 2.74 0.030 0.86 10 2 5 -59.06 107.25 2.73 0.055 0.92 5 -9 2 893.31 512.24 2.73 0.120 1.06 -10 7 2 277.15 59.03 2.73 0.041 0.79 Bond lengths and angles C1 - Distance Angles N1 1.3868 (0.0154) C2 1.3993 (0.0155) 123.21 (1.20) C6 1.4227 (0.0171) 119.84 (1.14) 116.95 (1.25) C1 - N1 C2 C2 - Distance Angles C3 1.3741 (0.0159) C1 1.3993 (0.0155) 121.95 (1.20) S2 1.7842 (0.0130) 118.16 (0.87) 119.55 (1.00) C2 - C3 C1 C3 - Distance Angles C2 1.3741 (0.0159) C4 1.4053 (0.0170) 119.13 (1.08) H3 0.9500 120.43 120.43 C3 - C2 C4 C4 - Distance Angles C5 1.3681 (0.0154) C3 1.4053 (0.0170) 119.45 (1.18) H4 0.9500 120.28 120.28 C4 - C5 C3 C5 - Distance Angles C6 1.3538 (0.0162) C4 1.3681 (0.0154) 121.81 (1.28) H5 0.9500 119.10 119.10 C5 - C6 C4 C6 - Distance Angles C5 1.3538 (0.0162) C1 1.4227 (0.0171) 120.61 (1.19) H6 0.9500 119.70 119.70 C6 - C5 C1 N1 - Distance Angles C1 1.3868 (0.0154) H1A 0.8800 120.00 H1B 0.8800 120.00 120.00 N1 - C1 H1A O2A - Distance Angles S2 1.4660 (0.0079) O2A - O2B - Distance Angles S2 1.4529 (0.0081) O2B - O2C - Distance Angles S2 1.4631 (0.0077) O2C - S2 - Distance Angles O2B 1.4529 (0.0081) O2C 1.4631 (0.0077) 113.66 (0.46) O2A 1.4660 (0.0079) 112.46 (0.47) 111.68 (0.50) C2 1.7842 (0.0130) 105.20 (0.54) 106.35 (0.51) 106.84 (0.49) S2 - O2B O2C O2A C22 - Distance Angles N21 1.4974 (0.0122) C23 1.5282 (0.0154) 110.75 (0.95) C26 1.5392 (0.0157) 104.93 (0.86) 108.50 (0.85) C27 1.5456 (0.0152) 106.13 (0.80) 116.28 (0.93) 109.65 (1.01) C22 - N21 C23 C26 C23 - Distance Angles C22 1.5282 (0.0154) C24 1.5388 (0.0155) 124.83 (0.89) H23A 0.9900 106.12 106.12 H23B 0.9900 106.12 106.12 106.33 C23 - C22 C24 H23A C24 - Distance Angles C28 1.5219 (0.0162) C25 1.5382 (0.0156) 109.84 (0.98) C23 1.5388 (0.0155) 106.58 (0.94) 113.58 (0.99) C29 1.5423 (0.0145) 106.77 (1.03) 108.27 (0.92) 111.58 (0.87) C24 - C28 C25 C23 C25 - Distance Angles C24 1.5382 (0.0156) H25A 0.9800 109.47 H25B 0.9800 109.47 109.47 H25C 0.9800 109.47 109.47 109.47 C25 - C24 H25A H25B C26 - Distance Angles C22 1.5392 (0.0156) 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 1.5456 (0.0152) 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 1.5219 (0.0162) 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 1.5423 (0.0145) 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 N21 - Distance Angles C22 1.4974 (0.0122) H21A 0.9100 109.47 H21B 0.9100 109.47 109.47 H21C 0.9100 109.47 109.47 109.47 N21 - C22 H21A H21B C31 - Distance Angles N31 1.3684 (0.0141) C32 1.3946 (0.0149) 123.67 (1.16) C36 1.4241 (0.0167) 119.98 (1.03) 116.32 (1.13) C31 - N31 C32 C32 - Distance Angles C31 1.3946 (0.0150) C33 1.3976 (0.0159) 122.60 (1.15) S32 1.7927 (0.0124) 119.33 (0.97) 117.94 (0.91) C32 - C31 C33 C33 - Distance Angles C34 1.3870 (0.0167) C32 1.3976 (0.0159) 120.22 (1.14) H33 0.9500 119.89 119.89 C33 - C34 C32 C34 - Distance Angles C33 1.3870 (0.0167) C35 1.4098 (0.0155) 117.38 (1.20) H34 0.9500 121.31 121.31 C34 - C33 C35 C35 - Distance Angles C36 1.3565 (0.0160) C34 1.4098 (0.0155) 122.64 (1.20) H35 0.9500 118.68 118.68 C35 - C36 C34 C36 - Distance Angles C35 1.3565 (0.0160) C31 1.4241 (0.0167) 120.84 (1.12) H36 0.9500 119.58 119.58 C36 - C35 C31 N31 - Distance Angles C31 1.3684 (0.0141) H31A 0.8800 120.00 H31B 0.8800 120.00 120.00 N31 - C31 H31A O32A - Distance Angles S32 1.4359 (0.0077) O32A - O32B - Distance Angles S32 1.4673 (0.0085) O32B - O32C - Distance Angles S32 1.4489 (0.0073) O32C - S32 - Distance Angles O32A 1.4359 (0.0077) O32C 1.4489 (0.0074) 112.29 (0.47) O32B 1.4673 (0.0085) 114.33 (0.50) 111.81 (0.47) C32 1.7927 (0.0124) 106.44 (0.55) 105.22 (0.49) 105.95 (0.51) S32 - O32A O32C O32B C42 - Distance Angles C46 1.5063 (0.0151) C47 1.5208 (0.0141) 110.95 (0.87) N41 1.5224 (0.0138) 106.17 (0.98) 105.17 (0.86) C43 1.5412 (0.0153) 115.50 (0.97) 114.68 (1.03) 103.09 (0.77) C42 - C46 C47 N41 C43 - Distance Angles C42 1.5412 (0.0153) C44 1.5895 (0.0169) 122.43 (0.90) H43A 0.9900 106.72 106.72 H43B 0.9900 106.72 106.72 106.61 C43 - C42 C44 H43A C44 - Distance Angles C49 1.5110 (0.0163) C45 1.5324 (0.0160) 108.42 (1.14) C48 1.5353 (0.0153) 109.31 (1.02) 109.30 (1.00) C43 1.5895 (0.0169) 110.59 (1.00) 105.34 (0.94) 113.70 (1.05) C44 - C49 C45 C48 C45 - Distance Angles C44 1.5324 (0.0160) H45A 0.9800 109.47 H45B 0.9800 109.47 109.47 H45C 0.9800 109.47 109.47 109.47 C45 - C44 H45A H45B C46 - Distance Angles C42 1.5063 (0.0151) 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 1.5208 (0.0141) 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 1.5353 (0.0153) 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 1.5110 (0.0163) 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 N41 - Distance Angles C42 1.5224 (0.0138) H41A 0.9100 109.47 H41B 0.9100 109.47 109.47 H41C 0.9100 109.47 109.47 109.47 N41 - C42 H41A H41B Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.34 2.934(12) 125.4 N1-H1A...O2C 0.88 2.23 3.070(11) 159.2 N1-H1B...O32C 0.91 2.20 2.918(11) 135.3 N21-H21A...O2A 0.91 1.93 2.831(12) 171.2 N21-H21C...O32A 0.88 2.34 2.931(13) 124.7 N31-H31A...O32B 0.88 2.52 3.270(14) 143.9 N1-H1A...O2A_$1 0.91 1.90 2.793(13) 166.6 N21-H21B...O2C_$1 0.88 2.20 3.038(12) 158.2 N31-H31B...O2A_$2 0.91 1.99 2.880(12) 165.3 N41-H41A...O32C_$3 0.91 1.93 2.818(12) 165.8 N41-H41B...O2B_$4 0.91 1.98 2.884(12) 170.7 N41-H41C...O32B_$5 0.91 2.96 3.798(10) 153.8 N41-H41C...S32_$5 FMAP and GRID set by program FMAP 2 3 38 GRID -1.429 -2 -2 1.429 2 2 R1 = 0.3744 for 7102 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.49 at 0.8259 0.5929 0.4711 [ 1.09 A from H41C ] Deepest hole -0.41 at 0.9826 0.6425 0.2718 [ 1.11 A from S32 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 5085 / 31123 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8259 0.5929 0.4711 1.00000 0.05 0.49 1.09 H41C 1.19 O32B 1.88 S32 1.93 N41 Q2 1 0.0092 0.3975 0.6810 1.00000 0.05 0.45 0.87 S32 1.27 C32 1.34 O32C 1.98 O32A Q3 1 0.6448 0.5365 0.7918 1.00000 0.05 0.39 0.36 H43A 1.21 C43 1.79 H43B 2.04 C44 Q4 1 -0.2627 -0.1084 0.6526 1.00000 0.05 0.39 0.83 S2 1.33 C2 1.51 O2C 1.64 O2B Q5 1 0.1610 0.1941 0.6988 1.00000 0.05 0.39 0.86 O32A 1.35 H21C 1.90 H23A 2.12 S32 Q6 1 0.0260 -0.0378 0.5638 1.00000 0.05 0.38 1.15 O2A 1.93 H21A 2.01 H21B 2.04 H1A Q7 1 0.2894 0.1077 0.7927 1.00000 0.05 0.37 0.51 H23A 1.27 C23 1.60 H23B 2.01 H28C Q8 1 -0.2392 -0.2156 0.6032 1.00000 0.05 0.37 0.97 O2B 1.31 S2 1.73 O2C 1.99 H41B Q9 1 -0.0050 0.7014 0.5855 1.00000 0.05 0.37 0.82 H31B 1.27 N31 1.69 H31A 2.12 O2A Q10 1 -0.0430 0.2229 0.8816 1.00000 0.05 0.37 1.00 H33 1.91 C33 2.38 H28B 2.62 O32A Shortest distances between peaks (including symmetry equivalents) 4 8 1.63 6 6 2.14 5 7 2.19 8 9 2.37 1 2 2.42 4 6 2.71 2 5 2.79 Time profile in seconds ----------------------- 0.06: 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. 1.13: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.22: Structure factors and derivatives 6.28: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.45: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.44: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0071p-1 finished at 14:59:11 Total CPU time: 10.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++