+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0008c2c started at 12:06:08 on 06-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0008c2c in C2/c CELL 0.71073 24.5889 4.5855 18.7275 90.000 123.022 90.000 ZERR 4.00 0.0015 0.0003 0.0014 0.000 0.004 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O UNIT 52 128 8 24 V = 1770.47 F(000) = 688.0 Mu = 0.09 mm-1 Cell Wt = 1249.62 Rho = 1.172 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 DFIX 0.84 0.02 O1W H1W O1W H2W DANG 1.35 0.02 H1W H2W HTAB O1W O1A EQIV_$1 x, -y+1, z+1/2 HTAB N21 O1B_$1 EQIV_$2 -x+3/2, y+1/2, -z+1/2 HTAB N21 O1A_$2 HTAB O1W O1W_$2 EQIV_$3 x, -y+2, z+1/2 HTAB N21 O1B_$3 FMAP 2 PLAN 10 SIZE 0.01 0.09 0.19 ACTA BOND $H WGHT 0.00000 12.58720 L.S. 4 TEMP -153.00 FVAR 0.60464 C1 1 0.847757 0.406550 0.147272 11.00000 0.01798 0.02236 = 0.02231 -0.00212 0.00978 -0.00497 C2 1 0.888881 0.242783 0.230555 11.00000 0.02174 0.02683 = 0.02633 0.00170 0.01447 0.00099 AFIX 23 H2A 2 0.860253 0.109892 0.237320 11.00000 -1.20000 H2B 2 0.907049 0.385656 0.277770 11.00000 -1.20000 AFIX 0 C3 1 0.944643 0.064461 0.239704 11.00000 0.02069 0.01960 = 0.02127 0.00256 0.00709 0.00319 AFIX 23 H3A 2 0.961801 -0.065126 0.289809 11.00000 -1.20000 H3B 2 0.927631 -0.060818 0.188765 11.00000 -1.20000 AFIX 0 C4 1 1.000000 0.247135 0.250000 10.50000 0.02236 0.02010 = 0.02630 0.00000 0.01006 0.00000 AFIX 23 H4A 2 0.983185 0.374384 0.199484 10.50000 -1.20000 H4B 2 1.016815 0.374385 0.300516 10.50000 -1.20000 AFIX 0 O1A 4 0.811005 0.605009 0.144395 11.00000 0.02131 0.02657 = 0.02795 0.00060 0.01336 0.00376 O1B 4 0.851406 0.341576 0.084310 11.00000 0.02805 0.02660 = 0.01994 -0.00203 0.01390 -0.00013 MOLE 2 C22 1 0.854803 1.128841 0.444719 11.00000 0.02543 0.03019 = 0.02320 0.00399 0.01533 0.00257 AFIX 23 H22A 2 0.847670 1.303297 0.409478 11.00000 -1.20000 H22B 2 0.838508 0.956850 0.406615 11.00000 -1.20000 AFIX 0 C23 1 0.926632 1.092874 0.509795 11.00000 0.02360 0.03686 = 0.02441 -0.00330 0.01398 -0.00160 AFIX 23 H23A 2 0.933400 0.930690 0.548726 11.00000 -1.20000 H23B 2 0.943768 1.273222 0.544161 11.00000 -1.20000 AFIX 0 C24 1 0.964116 1.029900 0.468001 11.00000 0.02292 0.03790 = 0.01881 0.00284 0.01091 0.00262 AFIX 23 H24A 2 0.944509 0.858784 0.430030 11.00000 -1.20000 H24B 2 0.959781 1.198911 0.432353 11.00000 -1.20000 AFIX 0 N21 3 0.817857 1.160592 0.485773 11.00000 0.02269 0.02291 = 0.02127 0.00223 0.01236 0.00184 AFIX 137 H21A 2 0.828366 1.012332 0.523450 11.00000 -1.20000 H21B 2 0.774596 1.154795 0.445283 11.00000 -1.20000 H21C 2 0.827936 1.334133 0.513780 11.00000 -1.20000 AFIX 0 MOLE 3 O1W 4 0.788007 0.647835 0.272000 11.00000 0.03516 0.02600 = 0.03132 0.00291 0.01978 0.00597 H1W 2 0.762856 0.792821 0.256847 11.00000 0.02584 H2W 2 0.800090 0.634820 0.238364 11.00000 0.07375 HKLF 4 Covalent radii and connectivity table for 07skc0008c2c in C2/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C1 C3 C3 - C4 C2 C4 - C3 C3_$4 O1A - C1 O1B - C1 C22 - N21 C23 C23 - C22 C24 C24 - C24_$5 C23 N21 - C22 O1W - no bonds found Operators for generating equivalent atoms: $1 x, -y+1, z+1/2 $2 -x+3/2, y+1/2, -z+1/2 $3 x, -y+2, z+1/2 $4 -x+2, y, -z+1/2 $5 -x+2, -y+2, -z+1 10152 Reflections read, of which 855 rejected -30 =< h =< 31, -5 =< k =< 5, -24 =< l =< 23, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 1999 Unique reflections, of which 0 suppressed R(int) = 0.1153 R(sigma) = 0.1119 Friedel opposites merged Maximum memory for data reduction = 1745 / 24362 Special position constraints for C4 x = 1.0000 z = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 2084 / 136080 wR2 = 0.1950 before cycle 1 for 1999 data and 105 / 105 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.006 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.128; Restrained GooF = 1.128 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 12.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60463 0.00223 -0.003 OSF Mean shift/esd = 0.004 Maximum = -0.016 for U12 O1A Max. shift = 0.000 A for H21B Max. dU = 0.000 for H1W Least-squares cycle 2 Maximum vector length = 511 Memory required = 2084 / 136080 wR2 = 0.1950 before cycle 2 for 1999 data and 105 / 105 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.006 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.128; Restrained GooF = 1.128 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 12.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60463 0.00223 -0.003 OSF Mean shift/esd = 0.001 Maximum = -0.007 for U12 O1A Max. shift = 0.000 A for H21B Max. dU = 0.000 for H2W Least-squares cycle 3 Maximum vector length = 511 Memory required = 2084 / 136080 wR2 = 0.1950 before cycle 3 for 1999 data and 105 / 105 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.006 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.128; Restrained GooF = 1.128 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 12.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60462 0.00223 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U12 O1A Max. shift = 0.000 A for H1W Max. dU = 0.000 for H2W Least-squares cycle 4 Maximum vector length = 511 Memory required = 2084 / 136080 wR2 = 0.1950 before cycle 4 for 1999 data and 105 / 105 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.006 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.128; Restrained GooF = 1.128 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 12.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60462 0.00223 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H2W Max. dU = 0.000 for H2W Largest correlation matrix elements 0.918 z H2W / x H2W 0.628 U13 C23 / U33 C23 0.606 U13 C2 / U11 C2 0.668 y H1W / x H1W 0.628 U13 N21 / U33 N21 0.588 U12 C22 / U23 C22 0.654 U13 C22 / U33 C22 0.625 U13 O1A / U11 O1A 0.587 U13 C24 / U33 C24 0.644 U13 C24 / U11 C24 0.625 U13 O1A / U33 O1A 0.584 U13 C1 / U33 C1 0.643 U13 C22 / U11 C22 0.625 U13 O1B / U11 O1B 0.584 U13 C4 / U33 C4 0.639 U13 C2 / U33 C2 0.621 U13 N21 / U11 N21 0.582 U13 O1W / U33 O1W 0.633 U13 O1W / U11 O1W 0.618 U13 O1B / U33 O1B 0.575 z H1W / x H1W 0.632 U13 C23 / U11 C23 0.615 U13 C1 / U11 C1 0.575 U13 C3 / U11 C3 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.8603 0.1099 0.2373 23 0.990 0.000 C2 C1 C3 H2B 0.9071 0.3857 0.2778 23 0.990 0.000 C2 C1 C3 H3A 0.9618 -0.0651 0.2898 23 0.990 0.000 C3 C4 C2 H3B 0.9276 -0.0608 0.1888 23 0.990 0.000 C3 C4 C2 H4A 1.0168 0.3744 0.3005 23 0.990 0.000 C4 C3 C3_$4 H4B 0.9832 0.3744 0.1995 23 0.990 0.000 C4 C3 C3_$4 H22A 0.8477 1.3033 0.4095 23 0.990 0.000 C22 N21 C23 H22B 0.8385 0.9569 0.4066 23 0.990 0.000 C22 N21 C23 H23A 0.9334 0.9307 0.5487 23 0.990 0.000 C23 C22 C24 H23B 0.9438 1.2732 0.5442 23 0.990 0.000 C23 C22 C24 H24A 0.9445 0.8588 0.4300 23 0.990 0.000 C24 C24_$5 C23 H24B 0.9598 1.1989 0.4323 23 0.990 0.000 C24 C24_$5 C23 H21A 0.8284 1.0123 0.5234 137 0.910 0.000 N21 C22 H21A H21B 0.7746 1.1548 0.4453 137 0.910 0.000 N21 C22 H21A H21C 0.8279 1.3341 0.5138 137 0.910 0.000 N21 C22 H21A 07skc0008c2c in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.84776 0.40655 0.14727 1.00000 0.01799 0.02237 0.02230 -0.00210 0.00980 -0.00493 0.02150 0.00893 0.00018 0.00093 0.00025 0.00000 0.00189 0.00231 0.00215 0.00189 0.00170 0.00181 0.00092 C2 0.88888 0.24278 0.23056 1.00000 0.02174 0.02682 0.02634 0.00171 0.01447 0.00101 0.02426 0.00978 0.00019 0.00096 0.00026 0.00000 0.00200 0.00237 0.00234 0.00197 0.00187 0.00184 0.00098 H2A 0.86025 0.10989 0.23732 1.00000 0.02911 0.00000 0.00000 H2B 0.90705 0.38566 0.27777 1.00000 0.02911 0.00000 0.00000 C3 0.94464 0.06446 0.23971 1.00000 0.02067 0.01959 0.02128 0.00257 0.00708 0.00320 0.02277 0.00938 0.00018 0.00091 0.00027 0.00000 0.00190 0.00225 0.00209 0.00183 0.00169 0.00180 0.00094 H3A 0.96180 -0.06513 0.28981 1.00000 0.02732 0.00000 0.00000 H3B 0.92763 -0.06082 0.18877 1.00000 0.02732 0.00000 0.00000 C4 1.00000 0.24713 0.25000 0.50000 0.02235 0.02011 0.02628 0.00000 0.01005 0.00000 0.02457 0.00605 0.00000 0.00132 0.00000 0.00000 0.00293 0.00316 0.00329 0.00000 0.00262 0.00000 0.00137 H4A 1.01682 0.37438 0.30052 0.50000 0.02948 0.00000 0.00000 H4B 0.98318 0.37438 0.19948 0.50000 0.02948 0.00000 0.00000 O1A 0.81101 0.60501 0.14440 1.00000 0.02130 0.02657 0.02794 0.00060 0.01335 0.00373 0.02530 0.00638 0.00013 0.00065 0.00018 0.00000 0.00139 0.00171 0.00163 0.00142 0.00128 0.00137 0.00071 O1B 0.85141 0.34158 0.08431 1.00000 0.02804 0.02662 0.01992 -0.00204 0.01388 -0.00013 0.02444 0.00633 0.00013 0.00065 0.00017 0.00000 0.00146 0.00170 0.00147 0.00138 0.00125 0.00138 0.00069 C22 0.85480 1.12885 0.44472 1.00000 0.02541 0.03019 0.02320 0.00400 0.01532 0.00258 0.02519 0.00976 0.00018 0.00105 0.00026 0.00000 0.00210 0.00253 0.00216 0.00207 0.00183 0.00198 0.00097 H22A 0.84767 1.30331 0.40948 1.00000 0.03023 0.00000 0.00000 H22B 0.83851 0.95686 0.40661 1.00000 0.03023 0.00000 0.00000 C23 0.92663 1.09287 0.50980 1.00000 0.02359 0.03685 0.02440 -0.00330 0.01397 -0.00160 0.02782 0.00968 0.00019 0.00109 0.00027 0.00000 0.00208 0.00277 0.00223 0.00211 0.00185 0.00204 0.00104 H23A 0.93340 0.93068 0.54872 1.00000 0.03338 0.00000 0.00000 H23B 0.94377 1.27321 0.54416 1.00000 0.03338 0.00000 0.00000 C24 0.96412 1.02989 0.46800 1.00000 0.02292 0.03784 0.01880 0.00284 0.01091 0.00264 0.02676 0.00969 0.00018 0.00109 0.00026 0.00000 0.00210 0.00275 0.00210 0.00199 0.00180 0.00199 0.00103 H24A 0.94451 0.85877 0.43003 1.00000 0.03211 0.00000 0.00000 H24B 0.95978 1.19890 0.43235 1.00000 0.03211 0.00000 0.00000 N21 0.81786 1.16060 0.48577 1.00000 0.02268 0.02291 0.02126 0.00224 0.01236 0.00184 0.02209 0.00758 0.00015 0.00078 0.00020 0.00000 0.00171 0.00189 0.00178 0.00162 0.00150 0.00157 0.00079 H21A 0.82836 1.01233 0.52344 1.00000 0.02650 0.00000 0.00000 H21B 0.77459 1.15482 0.44528 1.00000 0.02650 0.00000 0.00000 H21C 0.82794 1.33413 0.51378 1.00000 0.02650 0.00000 0.00000 O1W 0.78801 0.64784 0.27200 1.00000 0.03515 0.02600 0.03132 0.00292 0.01978 0.00597 0.02996 0.00746 0.00015 0.00073 0.00020 0.00000 0.00179 0.00187 0.00180 0.00155 0.00156 0.00158 0.00077 H1W 0.76286 0.79282 0.25685 1.00000 0.02583 0.10137 0.00174 0.00693 0.00263 0.00000 0.01314 H2W 0.80009 0.63482 0.23837 1.00000 0.07378 0.13751 0.00253 0.01183 0.00286 0.00000 0.02213 Final Structure Factor Calculation for 07skc0008c2c in C2/c Total number of l.s. parameters = 105 Maximum vector length = 511 Memory required = 1979 / 22995 wR2 = 0.1950 before cycle 5 for 1999 data and 0 / 105 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.006 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.128; Restrained GooF = 1.128 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 12.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1036 for 1148 Fo > 4sig(Fo) and 0.1843 for all 1999 data wR2 = 0.1950, GooF = S = 1.128, Restrained GooF = 1.128 for all data Occupancy sum of asymmetric unit = 10.50 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0258 0.0239 0.0148 C1 0.0283 0.0248 0.0196 C2 0.0306 0.0222 0.0155 C3 0.0319 0.0217 0.0201 C4 0.0292 0.0281 0.0186 O1A 0.0284 0.0272 0.0178 O1B 0.0323 0.0243 0.0189 C22 0.0377 0.0240 0.0218 C23 0.0384 0.0236 0.0183 C24 0.0249 0.0217 0.0197 N21 0.0381 0.0288 0.0230 O1W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.024 0.035 0.049 0.065 0.081 0.106 0.142 0.204 1.000 Number in group 203. 213. 203. 190. 194. 200. 196. 203. 196. 201. GooF 1.197 1.149 1.128 1.206 1.193 1.197 1.211 1.039 0.993 0.938 K 38.774 3.298 2.395 1.547 1.238 1.080 1.030 1.009 1.011 1.004 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.67 inf Number in group 206. 195. 207. 193. 198. 202. 198. 199. 200. 201. GooF 1.278 1.202 1.315 1.217 1.184 1.095 0.983 0.961 0.950 1.018 K 1.462 1.360 1.228 1.121 1.139 1.043 0.991 0.988 1.017 1.005 R1 0.486 0.379 0.372 0.287 0.240 0.180 0.117 0.099 0.074 0.041 Recommended weighting scheme: WGHT 0.0000 12.6019 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) 10 2 13 483.55 0.17 3.94 0.002 0.80 20 2 0 233.60 17.41 3.73 0.025 0.94 0 2 19 472.90 77.73 3.63 0.053 0.78 -31 1 13 421.48 0.54 3.42 0.004 0.78 3 3 12 1179.49 625.44 3.11 0.149 0.93 -15 5 6 273.10 12.14 3.09 0.021 0.80 -15 5 2 353.98 38.95 3.00 0.037 0.78 -18 0 10 911.45 1419.52 2.93 0.225 1.33 -16 4 17 -109.28 149.26 2.91 0.073 0.79 14 2 9 -140.49 183.42 2.90 0.081 0.84 -25 3 10 364.41 0.63 2.87 0.005 0.83 -11 5 9 491.86 121.86 2.86 0.066 0.83 -12 4 11 220.88 7.51 2.85 0.016 0.93 -18 0 16 756.96 1212.51 2.80 0.208 1.10 11 1 1 128.18 7.37 2.78 0.016 1.64 -18 4 10 306.54 42.38 2.76 0.039 0.87 -22 2 10 -30.69 142.56 2.74 0.071 1.00 7 3 9 317.26 70.86 2.73 0.050 0.96 12 2 10 283.10 44.72 2.70 0.040 0.86 -23 1 13 150.84 0.89 2.69 0.006 1.01 -24 2 14 460.02 197.25 2.66 0.084 0.91 -5 1 19 327.65 58.16 2.65 0.046 0.89 -12 4 12 -39.55 82.29 2.63 0.054 0.91 -19 1 5 111.16 0.31 2.63 0.003 1.21 -22 2 14 171.58 5.22 2.62 0.014 0.96 -12 2 22 572.10 177.72 2.61 0.080 0.79 -5 3 8 202.93 64.96 2.59 0.048 1.28 16 2 2 151.88 13.92 2.57 0.022 1.04 -7 5 2 -40.09 98.44 2.56 0.059 0.89 -22 2 19 422.13 104.83 2.53 0.061 0.85 -7 3 18 1103.10 701.13 2.52 0.158 0.84 -25 3 5 209.98 0.54 2.50 0.004 0.80 -6 2 19 125.45 373.06 2.43 0.115 0.86 8 4 7 -237.52 243.95 2.40 0.093 0.88 -3 5 6 -10.71 191.17 2.40 0.083 0.88 16 0 6 81.82 0.02 2.39 0.001 0.97 -17 1 19 1070.58 695.09 2.38 0.158 0.95 -10 4 8 103.25 0.15 2.37 0.002 1.01 -13 5 3 -73.46 67.06 2.35 0.049 0.82 -1 3 13 204.12 10.20 2.34 0.019 0.97 12 4 6 -56.04 103.50 2.34 0.061 0.82 15 3 7 605.49 206.31 2.32 0.086 0.81 -17 1 22 -30.09 127.64 2.32 0.068 0.84 13 3 6 190.15 10.35 2.32 0.019 0.90 -14 0 22 114.92 419.30 2.32 0.122 0.85 11 3 9 828.44 395.89 2.31 0.119 0.85 -9 5 9 167.53 12.96 2.29 0.022 0.83 -10 0 20 77.59 346.80 2.29 0.111 0.92 -18 2 18 138.26 15.16 2.29 0.023 0.92 -22 4 7 371.50 24.48 2.28 0.030 0.80 Bond lengths and angles C1 - Distance Angles O1A 1.2628 (0.0048) O1B 1.2659 (0.0047) 122.83 (0.38) C2 1.5166 (0.0056) 117.47 (0.36) 119.70 (0.36) C1 - O1A O1B C2 - Distance Angles C1 1.5166 (0.0056) C3 1.5238 (0.0055) 115.86 (0.35) H2A 0.9900 108.32 108.32 H2B 0.9900 108.32 108.32 107.41 C2 - C1 C3 H2A C3 - Distance Angles C4 1.5184 (0.0051) C2 1.5238 (0.0055) 114.06 (0.36) H3A 0.9900 108.74 108.74 H3B 0.9900 108.74 108.74 107.64 C3 - C4 C2 H3A C4 - Distance Angles C3 1.5184 (0.0051) C3_$4 1.5184 (0.0051) 113.04 (0.49) H4A 0.9900 108.97 108.97 H4B 0.9900 108.97 108.97 107.77 C4 - C3 C3_$4 H4A O1A - Distance Angles C1 1.2628 (0.0048) O1A - O1B - Distance Angles C1 1.2659 (0.0047) O1B - C22 - Distance Angles N21 1.4829 (0.0048) C23 1.5119 (0.0053) 111.68 (0.33) H22A 0.9900 109.28 109.28 H22B 0.9900 109.28 109.28 107.95 C22 - N21 C23 H22A C23 - Distance Angles C22 1.5119 (0.0053) C24 1.5270 (0.0056) 111.95 (0.34) H23A 0.9900 109.22 109.22 H23B 0.9900 109.22 109.22 107.91 C23 - C22 C24 H23A C24 - Distance Angles C24_$5 1.5233 (0.0075) C23 1.5270 (0.0055) 113.25 (0.43) H24A 0.9900 108.93 108.93 H24B 0.9900 108.93 108.93 107.74 C24 - C24_$5 C23 H24A N21 - Distance Angles C22 1.4829 (0.0048) 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 O1W - Distance Angles H1W 0.8447 (0.0183) H2W 0.8323 (0.0187) 107.47 (2.92) O1W - H1W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.832(19) 1.92(2) 2.746(4) 169(5) O1W-H2W...O1A 0.91 1.88 2.780(5) 167.8 N21-H21A...O1B_$1 0.91 1.86 2.762(4) 172.3 N21-H21B...O1A_$2 0.845(18) 1.94(2) 2.784(4) 175(5) O1W-H1W...O1W_$2 0.91 1.86 2.764(5) 172.0 N21-H21C...O1B_$3 FMAP and GRID set by program FMAP 2 1 39 GRID -0.694 -2 -1 0.694 2 1 R1 = 0.1843 for 1999 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.38 at 0.0888 0.5015 0.1474 [ 1.45 A from H2B ] Deepest hole -0.38 at 0.1369 0.6577 0.4003 [ 1.35 A from H21C ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 2049 / 25047 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9112 0.5015 0.3526 1.00000 0.05 0.38 1.45 H2B 1.91 H24B 2.04 H24A 2.36 C2 Q2 1 0.9173 1.4504 0.5198 1.00000 0.05 0.30 0.98 H23B 1.68 C23 1.95 H22A 2.04 C22 Q3 1 0.9015 0.5773 0.2803 1.00000 0.05 0.30 0.89 H2B 1.73 C2 2.15 H3A 2.18 H2W Q4 1 0.8775 0.4798 0.1163 1.00000 0.05 0.29 0.87 O1B 1.20 C1 1.83 H21C 2.05 O1A Q5 1 0.8679 0.9948 0.5884 1.00000 0.05 0.28 1.07 H21A 1.59 O1B 1.67 H3B 1.79 N21 Q6 1 0.9364 1.4976 0.4314 1.00000 0.05 0.28 1.48 H24B 1.67 H24A 2.18 H22A 2.24 C24 Q7 1 0.7556 1.4485 0.4535 1.00000 0.05 0.28 1.46 H21B 1.59 H21C 1.86 N21 2.29 O1A Q8 1 0.7500 0.7500 0.5000 0.50000 0.05 0.27 2.10 H21A 2.14 O1B 2.35 H21B 2.58 C1 Q9 1 0.7379 0.9322 0.4516 1.00000 0.05 0.26 1.41 H21B 1.72 O1A 1.91 H21A 1.91 C1 Q10 1 0.7269 0.8063 0.1620 1.00000 0.05 0.26 1.49 H1W 1.57 H22A 1.76 H2W 1.91 O1W Shortest distances between peaks (including symmetry equivalents) 8 9 1.15 1 6 1.25 1 3 1.29 7 8 1.68 7 9 1.78 2 6 1.96 4 5 2.22 7 9 2.26 9 9 2.29 4 9 2.40 3 6 2.49 2 4 2.50 7 10 2.51 7 7 2.64 5 8 2.68 5 7 2.70 6 6 2.76 5 9 2.82 3 4 2.83 4 8 2.87 4 7 2.90 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.47: 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 0.27: Structure factors and derivatives 0.20: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0008c2c finished at 12:06:09 Total CPU time: 1.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++