+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0013 started at 16:45:29 on 06-May-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0013 in P2(1)/n CELL 0.71073 8.8691 13.2988 12.1250 90.000 109.500 90.000 ZERR 4.00 0.0007 0.0017 0.0014 0.000 0.007 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 48 80 8 16 V = 1348.09 F(000) = 552.0 Mu = 0.09 mm-1 Cell Wt = 1025.20 Rho = 1.263 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB N21 O8B EQIV_$1 x-1, y, z-1 HTAB O1A O8A_$1 EQIV_$2 x+1, y, z HTAB N23 O8A_$2 FMAP 2 PLAN 10 SIZE 0.01 0.07 0.10 ACTA CONF BOND $H WGHT 0.00000 1.95540 L.S. 4 TEMP -153.00 FVAR 0.55370 MOLE 1 C1 1 -0.064328 0.098743 -0.230352 11.00000 0.01811 0.02495 = 0.01749 -0.00072 0.00595 0.00180 C2 1 0.062168 0.129663 -0.118154 11.00000 0.02728 0.02400 = 0.01952 -0.00528 0.00366 -0.00392 AFIX 23 H2A 2 0.009530 0.159715 -0.065717 11.00000 -1.20000 H2B 2 0.129986 0.182184 -0.135677 11.00000 -1.20000 AFIX 0 C3 1 0.168387 0.043747 -0.054373 11.00000 0.02526 0.02792 = 0.01686 -0.00215 0.00538 0.00107 AFIX 23 H3B 2 0.219970 0.012892 -0.107018 11.00000 -1.20000 H3A 2 0.101142 -0.008274 -0.035278 11.00000 -1.20000 AFIX 0 C4 1 0.297548 0.076941 0.057975 11.00000 0.02507 0.02531 = 0.02040 -0.00253 0.00121 -0.00174 AFIX 23 H4A 2 0.365954 0.128089 0.038696 11.00000 -1.20000 H4B 2 0.246035 0.108894 0.110026 11.00000 -1.20000 AFIX 0 C5 1 0.402305 -0.009479 0.123082 11.00000 0.02387 0.02643 = 0.01911 0.00205 0.00731 0.00134 AFIX 23 H5B 2 0.439610 -0.047989 0.067223 11.00000 -1.20000 H5A 2 0.336598 -0.055229 0.152821 11.00000 -1.20000 AFIX 0 C6 1 0.547974 0.023704 0.225676 11.00000 0.02222 0.02568 = 0.01730 0.00340 0.00532 0.00216 AFIX 23 H6B 2 0.615608 -0.035846 0.257220 11.00000 -1.20000 H6A 2 0.611862 0.071203 0.196421 11.00000 -1.20000 AFIX 0 C7 1 0.506012 0.073982 0.324799 11.00000 0.01714 0.02259 = 0.02050 0.00148 0.00338 0.00127 AFIX 23 H7B 2 0.438429 0.133542 0.293211 11.00000 -1.20000 H7A 2 0.441967 0.026492 0.353921 11.00000 -1.20000 AFIX 0 C8 1 0.650221 0.106920 0.426836 11.00000 0.02024 0.02107 = 0.01851 0.00195 0.00546 -0.00243 O1A 4 -0.141979 0.176856 -0.291659 11.00000 0.02354 0.02430 = 0.02423 -0.00177 -0.00341 -0.00013 AFIX 147 H1 2 -0.210929 0.156364 -0.353595 11.00000 0.06002 AFIX 0 O1B 4 -0.094047 0.012814 -0.260698 11.00000 0.03422 0.02281 = 0.02842 -0.00623 -0.00501 0.00022 O8A 4 0.625412 0.128152 0.522011 11.00000 0.01771 0.03365 = 0.01606 -0.00060 0.00360 0.00020 O8B 4 0.782423 0.112481 0.413337 11.00000 0.01649 0.04895 = 0.02575 -0.00709 0.00700 -0.00794 MOLE 2 C22 1 1.196378 0.120877 0.482449 11.00000 0.02232 0.02154 = 0.01457 -0.00276 0.00002 -0.00016 AFIX 43 H22 2 1.176124 0.075225 0.418882 11.00000 -1.20000 AFIX 0 C24 1 1.319312 0.223317 0.627474 11.00000 0.01980 0.02374 = 0.01721 0.00016 0.00282 -0.00007 C25 1 1.163803 0.219876 0.616944 11.00000 0.02438 0.02476 = 0.02054 -0.00449 0.00876 -0.00038 AFIX 43 H25 2 1.114442 0.255403 0.663731 11.00000 -1.20000 AFIX 0 C26 1 1.456489 0.278530 0.711943 11.00000 0.02511 0.03144 = 0.02676 -0.00680 0.00337 -0.00149 AFIX 137 H26A 2 1.417641 0.319293 0.764232 11.00000 -1.50000 H26B 2 1.505972 0.322386 0.668756 11.00000 -1.50000 H26C 2 1.535747 0.230092 0.758193 11.00000 -1.50000 AFIX 0 N21 3 1.088683 0.155584 0.526119 11.00000 0.01671 0.03065 = 0.02314 -0.00119 0.00512 0.00124 AFIX 43 H21 2 0.986292 0.140248 0.501399 11.00000 0.05669 AFIX 0 N23 3 1.337975 0.160408 0.542185 11.00000 0.01720 0.02695 = 0.01970 -0.00128 0.00627 0.00069 AFIX 43 H23 2 1.428411 0.148491 0.529508 11.00000 0.06163 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0013 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C1 C3 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C7 C5 C7 - C8 C6 C8 - O8B O8A C7 O1A - C1 O1B - C1 O8A - C8 O8B - C8 C22 - N21 N23 C24 - C25 N23 C26 C25 - C24 N21 C26 - C24 N21 - C22 C25 N23 - C22 C24 Operators for generating equivalent atoms: $1 x-1, y, z-1 $2 x+1, y, z 18518 Reflections read, of which 538 rejected -11 =< h =< 11, -17 =< k =< 17, -15 =< l =< 15, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -7 1 3 9.29 1.51 9 8.95 3 12 5 105.62 46.38 2 257.85 2 Inconsistent equivalents 3079 Unique reflections, of which 0 suppressed R(int) = 0.1667 R(sigma) = 0.1643 Friedel opposites merged Maximum memory for data reduction = 2160 / 30691 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 = 2664 / 209223 wR2 = 0.1494 before cycle 1 for 3079 data and 168 / 168 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55370 0.00130 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.003 for U12 O8A Max. shift = 0.000 A for O8B Max. dU = 0.000 for H1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2664 / 209223 wR2 = 0.1494 before cycle 2 for 3079 data and 168 / 168 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55370 0.00130 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U12 O8A Max. shift = 0.000 A for H1 Max. dU = 0.000 for H23 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2664 / 209223 wR2 = 0.1494 before cycle 3 for 3079 data and 168 / 168 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55370 0.00130 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U13 C3 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H23 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2664 / 209223 wR2 = 0.1494 before cycle 4 for 3079 data and 168 / 168 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55370 0.00130 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C24 Max. dU = 0.000 for H23 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 0.0095 0.1597 -0.0657 23 0.990 0.000 C2 C1 C3 H2B 0.1300 0.1822 -0.1357 23 0.990 0.000 C2 C1 C3 H3B 0.2200 0.0129 -0.1070 23 0.990 0.000 C3 C2 C4 H3A 0.1011 -0.0083 -0.0353 23 0.990 0.000 C3 C2 C4 H4A 0.3660 0.1281 0.0387 23 0.990 0.000 C4 C5 C3 H4B 0.2460 0.1089 0.1100 23 0.990 0.000 C4 C5 C3 H5B 0.4396 -0.0480 0.0672 23 0.990 0.000 C5 C4 C6 H5A 0.3366 -0.0552 0.1528 23 0.990 0.000 C5 C4 C6 H6B 0.6156 -0.0358 0.2572 23 0.990 0.000 C6 C7 C5 H6A 0.6119 0.0712 0.1964 23 0.990 0.000 C6 C7 C5 H7B 0.4384 0.1335 0.2932 23 0.990 0.000 C7 C8 C6 H7A 0.4420 0.0265 0.3539 23 0.990 0.000 C7 C8 C6 H1 -0.2109 0.1564 -0.3536 147 0.840 0.000 O1A C1 H1 H22 1.1761 0.0752 0.4189 43 0.950 0.000 C22 N21 N23 H25 1.1144 0.2554 0.6637 43 0.950 0.000 C25 C24 N21 H26A 1.4176 0.3193 0.7642 137 0.980 0.000 C26 C24 H26A H26B 1.5060 0.3224 0.6688 137 0.980 0.000 C26 C24 H26A H26C 1.5357 0.2301 0.7582 137 0.980 0.000 C26 C24 H26A H21 0.9863 0.1402 0.5014 43 0.880 0.000 N21 C22 C25 H23 1.4284 0.1485 0.5295 43 0.880 0.000 N23 C22 C24 06skc0013 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.06433 0.09874 -0.23035 1.00000 0.01811 0.02495 0.01749 -0.00072 0.00595 0.00180 0.02018 0.00699 0.00040 0.00029 0.00029 0.00000 0.00200 0.00233 0.00194 0.00175 0.00154 0.00165 0.00084 C2 0.06217 0.12966 -0.11815 1.00000 0.02728 0.02400 0.01952 -0.00528 0.00366 -0.00392 0.02464 0.00658 0.00042 0.00027 0.00029 0.00000 0.00213 0.00233 0.00195 0.00171 0.00162 0.00171 0.00090 H2A 0.00953 0.15972 -0.06572 1.00000 0.02957 0.00000 0.00000 H2B 0.12999 0.18218 -0.13568 1.00000 0.02957 0.00000 0.00000 C3 0.16839 0.04375 -0.05437 1.00000 0.02526 0.02792 0.01686 -0.00215 0.00538 0.00107 0.02376 0.00669 0.00042 0.00027 0.00029 0.00000 0.00209 0.00236 0.00194 0.00167 0.00156 0.00166 0.00089 H3B 0.21997 0.01289 -0.10702 1.00000 0.02851 0.00000 0.00000 H3A 0.10114 -0.00827 -0.03528 1.00000 0.02851 0.00000 0.00000 C4 0.29755 0.07694 0.05798 1.00000 0.02507 0.02531 0.02040 -0.00253 0.00121 -0.00174 0.02519 0.00662 0.00041 0.00028 0.00029 0.00000 0.00208 0.00233 0.00203 0.00170 0.00162 0.00169 0.00091 H4A 0.36595 0.12809 0.03870 1.00000 0.03023 0.00000 0.00000 H4B 0.24603 0.10889 0.11003 1.00000 0.03023 0.00000 0.00000 C5 0.40230 -0.00948 0.12308 1.00000 0.02387 0.02643 0.01911 0.00205 0.00731 0.00134 0.02310 0.00665 0.00040 0.00027 0.00029 0.00000 0.00212 0.00230 0.00193 0.00171 0.00159 0.00166 0.00088 H5B 0.43961 -0.04799 0.06722 1.00000 0.02772 0.00000 0.00000 H5A 0.33660 -0.05523 0.15282 1.00000 0.02772 0.00000 0.00000 C6 0.54797 0.02370 0.22568 1.00000 0.02222 0.02568 0.01730 0.00340 0.00532 0.00216 0.02205 0.00664 0.00040 0.00028 0.00028 0.00000 0.00203 0.00223 0.00189 0.00168 0.00152 0.00162 0.00085 H6B 0.61561 -0.03585 0.25722 1.00000 0.02646 0.00000 0.00000 H6A 0.61186 0.07120 0.19642 1.00000 0.02646 0.00000 0.00000 C7 0.50601 0.07398 0.32480 1.00000 0.01714 0.02259 0.02050 0.00148 0.00338 0.00127 0.02080 0.00645 0.00039 0.00027 0.00029 0.00000 0.00191 0.00221 0.00190 0.00165 0.00148 0.00156 0.00084 H7B 0.43843 0.13354 0.29321 1.00000 0.02497 0.00000 0.00000 H7A 0.44197 0.02649 0.35392 1.00000 0.02497 0.00000 0.00000 C8 0.65022 0.10692 0.42684 1.00000 0.02024 0.02107 0.01851 0.00195 0.00546 -0.00243 0.02019 0.00678 0.00042 0.00026 0.00030 0.00000 0.00208 0.00212 0.00196 0.00168 0.00158 0.00160 0.00082 O1A -0.14198 0.17686 -0.29166 1.00000 0.02354 0.02430 0.02423 -0.00177 -0.00341 -0.00013 0.02687 0.00485 0.00030 0.00018 0.00022 0.00000 0.00149 0.00156 0.00150 0.00125 0.00118 0.00118 0.00064 H1 -0.21093 0.15636 -0.35360 1.00000 0.06002 0.00000 0.01525 O1B -0.09405 0.01281 -0.26070 1.00000 0.03422 0.02281 0.02842 -0.00623 -0.00501 0.00022 0.03236 0.00479 0.00030 0.00020 0.00021 0.00000 0.00160 0.00163 0.00150 0.00129 0.00117 0.00124 0.00069 O8A 0.62541 0.12815 0.52201 1.00000 0.01771 0.03365 0.01606 -0.00060 0.00360 0.00020 0.02298 0.00443 0.00026 0.00018 0.00019 0.00000 0.00133 0.00167 0.00129 0.00116 0.00103 0.00109 0.00061 O8B 0.78242 0.11248 0.41334 1.00000 0.01649 0.04895 0.02575 -0.00709 0.00700 -0.00794 0.03041 0.00465 0.00028 0.00020 0.00020 0.00000 0.00143 0.00191 0.00146 0.00130 0.00112 0.00123 0.00069 C22 1.19638 0.12088 0.48245 1.00000 0.02232 0.02154 0.01457 -0.00276 0.00002 -0.00016 0.02102 0.00664 0.00040 0.00027 0.00029 0.00000 0.00207 0.00216 0.00183 0.00161 0.00158 0.00161 0.00085 H22 1.17612 0.07522 0.41888 1.00000 0.02522 0.00000 0.00000 C24 1.31931 0.22332 0.62747 1.00000 0.01980 0.02374 0.01721 0.00016 0.00282 -0.00007 0.02109 0.00681 0.00040 0.00027 0.00029 0.00000 0.00209 0.00217 0.00186 0.00171 0.00151 0.00164 0.00084 C25 1.16380 0.21988 0.61694 1.00000 0.02438 0.02476 0.02054 -0.00449 0.00876 -0.00038 0.02291 0.00671 0.00040 0.00028 0.00029 0.00000 0.00216 0.00221 0.00199 0.00177 0.00159 0.00171 0.00086 H25 1.11444 0.25540 0.66373 1.00000 0.02749 0.00000 0.00000 C26 1.45649 0.27853 0.71194 1.00000 0.02511 0.03144 0.02676 -0.00680 0.00337 -0.00149 0.02909 0.00663 0.00041 0.00029 0.00031 0.00000 0.00222 0.00242 0.00216 0.00190 0.00170 0.00177 0.00096 H26A 1.41764 0.31929 0.76423 1.00000 0.04364 0.00000 0.00000 H26B 1.50597 0.32239 0.66876 1.00000 0.04364 0.00000 0.00000 H26C 1.53575 0.23009 0.75819 1.00000 0.04364 0.00000 0.00000 N21 1.08868 0.15558 0.52612 1.00000 0.01671 0.03065 0.02314 -0.00119 0.00512 0.00124 0.02389 0.00583 0.00035 0.00023 0.00024 0.00000 0.00181 0.00192 0.00169 0.00151 0.00136 0.00139 0.00074 H21 0.98629 0.14025 0.50140 1.00000 0.05669 0.00000 0.01449 N23 1.33797 0.16041 0.54218 1.00000 0.01720 0.02695 0.01970 -0.00128 0.00627 0.00069 0.02125 0.00555 0.00034 0.00022 0.00023 0.00000 0.00173 0.00187 0.00162 0.00144 0.00130 0.00136 0.00071 H23 1.42841 0.14849 0.52951 1.00000 0.06163 0.00000 0.01528 Final Structure Factor Calculation for 06skc0013 in P2(1)/n Total number of l.s. parameters = 168 Maximum vector length = 511 Memory required = 2496 / 22995 wR2 = 0.1494 before cycle 5 for 3079 data and 0 / 168 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1082 for 1700 Fo > 4sig(Fo) and 0.2045 for all 3079 data wR2 = 0.1494, GooF = S = 1.094, Restrained GooF = 1.094 for all data Occupancy sum of asymmetric unit = 18.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0256 0.0178 0.0171 C1 0.0314 0.0275 0.0151 C2 0.0295 0.0253 0.0165 C3 0.0327 0.0261 0.0167 C4 0.0272 0.0236 0.0185 C5 0.0271 0.0231 0.0160 C6 0.0240 0.0226 0.0158 C7 0.0249 0.0186 0.0170 C8 0.0411 0.0243 0.0152 O1A 0.0557 0.0250 0.0164 O1B 0.0337 0.0201 0.0152 O8A 0.0517 0.0249 0.0146 O8B 0.0292 0.0217 0.0121 C22 0.0240 0.0236 0.0157 C24 0.0276 0.0243 0.0169 C25 0.0384 0.0292 0.0197 C26 0.0312 0.0239 0.0166 N21 0.0273 0.0195 0.0170 N23 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.014 0.022 0.030 0.039 0.049 0.063 0.083 0.122 1.000 Number in group 319. 299. 319. 323. 289. 302. 320. 290. 313. 305. GooF 1.279 1.235 1.123 1.096 1.058 1.037 1.089 0.986 0.989 0.998 K 53.390 9.098 3.319 2.060 1.733 1.499 1.262 1.041 0.996 0.996 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.65 inf Number in group 314. 307. 302. 315. 300. 311. 305. 310. 305. 310. GooF 1.097 1.055 1.131 1.214 1.101 1.172 1.017 1.052 1.040 1.042 K 1.432 1.679 1.459 1.987 1.232 1.194 1.024 0.987 0.990 1.007 R1 0.508 0.445 0.371 0.369 0.263 0.205 0.119 0.112 0.073 0.033 Recommended weighting scheme: WGHT 0.0000 1.9553 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 2 11 128.28 1.01 3.82 0.006 0.87 -3 13 6 2170.05 42.05 3.70 0.037 0.90 -4 14 3 268.79 0.43 3.61 0.004 0.87 3 9 6 124.90 19.40 3.22 0.025 1.01 6 5 0 48.04 10.44 3.16 0.018 1.23 -7 2 9 39.28 1.81 3.11 0.008 1.05 1 2 12 2135.57 97.61 3.11 0.056 0.90 -7 7 13 263.38 91.87 3.09 0.055 0.78 -11 4 4 -14.51 168.21 3.06 0.074 0.78 1 13 3 284.65 97.85 3.02 0.056 0.97 -1 2 2 3561.21 3923.74 3.00 0.356 4.32 2 15 1 157.46 34.16 2.96 0.033 0.86 -1 1 3 43.95 11.12 2.96 0.019 3.84 -4 1 9 52.07 0.65 2.89 0.005 1.29 -4 12 3 196.28 111.72 2.83 0.060 0.99 -2 7 14 138.77 6.30 2.79 0.014 0.78 5 4 6 59.78 10.19 2.79 0.018 1.04 -7 4 5 30.32 0.05 2.78 0.001 1.16 8 4 0 174.75 19.00 2.75 0.025 1.00 -6 7 12 139.43 5.25 2.73 0.013 0.85 -7 4 14 165.05 21.05 2.64 0.026 0.79 4 3 3 32.25 1.00 2.60 0.006 1.52 6 2 7 121.93 34.85 2.59 0.034 0.91 5 2 8 56.00 0.08 2.59 0.002 0.93 -1 13 5 315.00 193.53 2.58 0.079 0.94 0 10 0 74.74 150.14 2.57 0.070 1.33 5 2 7 94.55 27.56 2.56 0.030 1.00 1 9 10 102.35 20.89 2.54 0.026 0.87 2 12 8 108.59 7.53 2.53 0.016 0.82 -10 4 2 198.65 57.57 2.53 0.043 0.84 -1 11 9 117.40 20.26 2.52 0.026 0.89 -6 0 6 215.60 87.06 2.50 0.053 1.36 8 8 4 -30.35 74.94 2.48 0.049 0.78 9 3 2 36.54 186.28 2.48 0.078 0.86 2 16 0 120.47 1.13 2.48 0.006 0.82 1 3 1 54.93 23.39 2.48 0.028 3.54 0 5 10 78.72 12.12 2.47 0.020 1.05 8 3 0 178.30 302.69 2.47 0.099 1.02 3 8 9 78.68 0.38 2.46 0.003 0.88 -6 5 14 147.93 28.77 2.46 0.031 0.80 -9 0 3 92.86 0.16 2.45 0.002 0.98 -7 0 7 135.04 36.32 2.44 0.034 1.17 2 10 8 72.64 1.85 2.44 0.008 0.90 -5 13 5 119.59 25.27 2.43 0.029 0.87 -5 13 4 250.80 107.71 2.43 0.059 0.88 -6 5 1 45.77 18.02 2.41 0.024 1.27 -3 1 8 320.38 407.13 2.41 0.115 1.48 -8 12 5 102.92 1.91 2.41 0.008 0.78 3 12 0 156.57 237.14 2.40 0.088 1.03 -10 2 9 236.09 22.89 2.39 0.027 0.83 Bond lengths and angles C1 - Distance Angles O1B 1.2025 (0.0041) O1A 1.3282 (0.0040) 123.52 (0.31) C2 1.5032 (0.0045) 123.92 (0.33) 112.55 (0.32) C1 - O1B O1A C2 - Distance Angles C1 1.5032 (0.0045) C3 1.5181 (0.0047) 113.82 (0.30) H2A 0.9900 108.79 108.79 H2B 0.9900 108.79 108.79 107.67 C2 - C1 C3 H2A C3 - Distance Angles C2 1.5181 (0.0047) C4 1.5235 (0.0044) 113.01 (0.29) H3B 0.9900 108.98 108.98 H3A 0.9900 108.98 108.98 107.77 C3 - C2 C4 H3B C4 - Distance Angles C5 1.5224 (0.0047) C3 1.5235 (0.0044) 113.05 (0.30) H4A 0.9900 108.97 108.97 H4B 0.9900 108.97 108.97 107.77 C4 - C5 C3 H4A C5 - Distance Angles C4 1.5224 (0.0047) C6 1.5292 (0.0045) 114.06 (0.30) H5B 0.9900 108.74 108.74 H5A 0.9900 108.74 108.74 107.64 C5 - C4 C6 H5B C6 - Distance Angles C7 1.5260 (0.0046) C5 1.5292 (0.0045) 113.90 (0.28) H6B 0.9900 108.78 108.77 H6A 0.9900 108.77 108.78 107.66 C6 - C7 C5 H6B C7 - Distance Angles C8 1.5172 (0.0044) C6 1.5260 (0.0046) 114.07 (0.28) H7B 0.9900 108.74 108.74 H7A 0.9900 108.74 108.74 107.64 C7 - C8 C6 H7B C8 - Distance Angles O8B 1.2390 (0.0039) O8A 1.2765 (0.0039) 124.23 (0.31) C7 1.5172 (0.0044) 119.13 (0.31) 116.63 (0.30) C8 - O8B O8A O1A - Distance Angles C1 1.3282 (0.0040) H1 0.8400 109.47 O1A - C1 O1B - Distance Angles C1 1.2025 (0.0041) O1B - O8A - Distance Angles C8 1.2765 (0.0039) O8A - O8B - Distance Angles C8 1.2390 (0.0039) O8B - C22 - Distance Angles N21 1.3204 (0.0043) N23 1.3307 (0.0041) 108.74 (0.31) H22 0.9500 125.63 125.63 C22 - N21 N23 C24 - Distance Angles C25 1.3428 (0.0046) N23 1.3824 (0.0042) 106.49 (0.30) C26 1.4955 (0.0046) 131.06 (0.34) 122.43 (0.31) C24 - C25 N23 C25 - Distance Angles C24 1.3428 (0.0046) N21 1.3776 (0.0042) 107.73 (0.31) H25 0.9500 126.14 126.14 C25 - C24 N21 C26 - Distance Angles C24 1.4955 (0.0046) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C24 H26A H26B N21 - Distance Angles C22 1.3204 (0.0043) C25 1.3776 (0.0042) 108.42 (0.30) H21 0.8800 125.79 125.79 N21 - C22 C25 N23 - Distance Angles C22 1.3307 (0.0041) C24 1.3824 (0.0042) 108.62 (0.29) H23 0.8800 125.69 125.69 N23 - C22 C24 Selected torsion angles 9.18 ( 0.51) O1B - C1 - C2 - C3 -171.93 ( 0.30) O1A - C1 - C2 - C3 179.01 ( 0.31) C1 - C2 - C3 - C4 179.00 ( 0.31) C2 - C3 - C4 - C5 171.19 ( 0.30) C3 - C4 - C5 - C6 64.86 ( 0.40) C4 - C5 - C6 - C7 179.94 ( 0.30) C5 - C6 - C7 - C8 15.95 ( 0.47) C6 - C7 - C8 - O8B -164.66 ( 0.31) C6 - C7 - C8 - O8A -0.04 ( 0.39) N23 - C24 - C25 - N21 -178.58 ( 0.36) C26 - C24 - C25 - N21 0.15 ( 0.39) N23 - C22 - N21 - C25 -0.06 ( 0.40) C24 - C25 - N21 - C22 -0.18 ( 0.39) N21 - C22 - N23 - C24 0.13 ( 0.39) C25 - C24 - N23 - C22 178.83 ( 0.33) C26 - C24 - N23 - C22 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.80 2.664(4) 164.8 N21-H21...O8B 0.84 1.75 2.582(3) 170.8 O1A-H1...O8A_$1 0.88 1.80 2.676(4) 173.0 N23-H23...O8A_$2 FMAP and GRID set by program FMAP 2 2 19 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.2044 for 3079 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.30 at 0.0804 0.2025 0.8948 [ 0.72 A from H2B ] Deepest hole -0.26 at 0.8622 0.2350 0.0842 [ 0.93 A from C24 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2551 / 18725 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0804 0.2025 -0.1052 1.00000 0.05 0.30 0.72 H2B 0.99 C2 1.07 H2A 2.13 C1 Q2 1 -0.0613 -0.0578 -0.2143 1.00000 0.05 0.28 1.08 O1B 1.70 H26B 2.09 C1 2.27 H3A Q3 1 -0.0547 0.1467 -0.0043 1.00000 0.05 0.26 1.09 H2A 1.98 H3A 2.00 C2 2.03 H26B Q4 1 -0.0931 -0.0365 -0.3275 1.00000 0.05 0.25 1.04 O1B 1.22 H22 2.12 C22 2.12 C1 Q5 1 0.5075 0.0157 0.2948 1.00000 0.05 0.25 0.86 C7 1.02 C6 1.07 H7A 1.37 H6B Q6 1 0.8325 0.1222 0.5030 1.00000 0.05 0.23 1.04 O8B 1.39 H21 1.58 C8 1.93 O8A Q7 1 -0.0201 0.0528 -0.2808 1.00000 0.05 0.23 0.94 O1B 1.03 C1 1.95 O1A 2.12 C2 Q8 1 -0.2952 0.1429 -0.3855 1.00000 0.05 0.23 0.74 H1 1.12 O8A 1.52 O1A 2.22 C8 Q9 1 0.3669 0.1317 -0.0820 1.00000 0.05 0.23 1.47 H4A 2.00 H5B 2.01 H3B 2.09 H2B Q10 1 1.2910 0.1512 0.4640 1.00000 0.05 0.22 0.91 N23 1.02 C22 1.21 H23 1.41 H22 Shortest distances between peaks (including symmetry equivalents) 2 4 1.34 4 7 1.38 2 7 1.77 6 8 2.05 1 3 2.11 4 10 2.49 7 8 2.63 1 9 2.63 6 7 2.67 2 3 2.77 1 7 2.83 4 6 2.86 4 8 2.93 3 10 2.98 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.02: 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. 0.92: 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 0.69: Structure factors and derivatives 0.58: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.08: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0013 finished at 16:45:31 Total CPU time: 2.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++