+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04skc0009p21 started at 14:19:10 on 14-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04skc0009p21 in P2(1) CELL 0.71073 9.4109 8.7365 12.4478 90.000 102.099 90.000 ZERR 4.00 0.0012 0.0011 0.0014 0.000 0.009 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O UNIT 28 64 8 24 V = 1000.70 F(000) = 480.0 Mu = 0.13 mm-1 Cell Wt = 896.87 Rho = 1.488 MERG 4 OMIT -3.00 55.00 EXTI 0.01145 SHEL 7 0.77 DELU 0.01 N41A > N45B SIMU 0.01 N41A > N45B HTAB N21 O4A HTAB N21 O34B HTAB N45A O4A HTAB N45A O32 HTAB N45A O32 HTAB N45B O4A HTAB N45B O32 EQIV_$1 -x+2, y+1/2, -z HTAB N25 O31A_$1 HTAB N41A O31A_$1 EQIV_$2 -x+1, y+1/2, -z+1 HTAB N25 O1A_$2 HTAB N25 O2_$2 HTAB O3 O1B_$2 HTAB N41A O1A_$2 HTAB N41B O1A_$2 EQIV_$3 x-1, y, z HTAB N21 O31B_$3 EQIV_$4 -x+1, y-1/2, -z+1 HTAB N21 O3_$4 EQIV_$5 -x+1, y+1/2, -z HTAB N25 O34A_$5 EQIV_$6 -x+2, y-1/2, -z HTAB O33 O34A_$6 EQIV_$7 -x+2, y-1/2, -z+1 HTAB O32 O3_$7 HTAB N45A O4B_$7 HTAB N45B O4B_$7 EQIV_$8 -x+2, y+1/2, -z+1 HTAB O2 O31B_$8 HTAB N41B O4B_$8 EQIV_$9 x, y+1, z HTAB N41A O34B_$9 HTAB N41A O33_$9 HTAB N41B O34B_$9 HTAB N41B O33_$9 EQIV_$10 x+1, y, z HTAB N45A O1B_$10 HTAB N45B O1B_$10 FMAP 2 PLAN 10 SIZE 0.04 0.08 0.10 ACTA BOND $H WGHT 0.04430 0.11060 L.S. 8 TEMP -153.00 FVAR 0.83300 0.68613 MOLE 1 C22 1 0.566521 0.096493 0.177994 11.00000 0.02582 0.02721 = 0.02519 0.00098 0.00533 0.00185 AFIX 23 H22B 2 0.528115 0.058351 0.102606 11.00000 -1.20000 H22A 2 0.650242 0.164070 0.175592 11.00000 -1.20000 AFIX 0 C23 1 0.449687 0.188295 0.215726 11.00000 0.02662 0.02639 = 0.02090 -0.00507 0.00755 0.00155 AFIX 23 H23A 2 0.381670 0.116999 0.240912 11.00000 -1.20000 H23B 2 0.495405 0.252411 0.279168 11.00000 -1.20000 AFIX 0 C24 1 0.364958 0.290080 0.127016 11.00000 0.02791 0.02113 = 0.02874 -0.00127 0.00390 0.00013 AFIX 23 H24A 2 0.335556 0.229221 0.058886 11.00000 -1.20000 H24B 2 0.275216 0.324074 0.149607 11.00000 -1.20000 AFIX 0 N21 3 0.617368 -0.036723 0.252128 11.00000 0.02168 0.02572 = 0.02345 -0.00112 0.00611 -0.00055 AFIX 137 H21A 2 0.689953 -0.086360 0.228252 11.00000 -1.5 H21C 2 0.541962 -0.102235 0.251268 11.00000 -1.5 H21B 2 0.651038 -0.002391 0.321840 11.00000 -1.5 AFIX 0 N25 3 0.445895 0.427542 0.102407 11.00000 0.02544 0.02293 = 0.02367 -0.00098 0.00890 0.00329 AFIX 137 H25A 2 0.516254 0.398528 0.066392 11.00000 -1.5 H25B 2 0.487531 0.475051 0.166322 11.00000 -1.5 H25C 2 0.383400 0.493113 0.059458 11.00000 -1.5 AFIX 0 MOLE 2 C34 1 0.881823 -0.090839 0.086804 11.00000 0.01575 0.01733 = 0.02278 -0.00205 0.00258 -0.00229 C33 1 1.015631 -0.161417 0.052867 11.00000 0.01895 0.01639 = 0.01786 0.00221 0.00446 -0.00055 AFIX 13 H33 2 1.001316 -0.160725 -0.029035 11.00000 -1.20000 AFIX 0 C32 1 1.151088 -0.066849 0.103099 11.00000 0.01714 0.02202 = 0.01712 0.00148 -0.00011 -0.00224 AFIX 13 H32 2 1.136371 0.038874 0.071965 11.00000 -1.20000 AFIX 0 C31 1 1.284332 -0.135023 0.067830 11.00000 0.00914 0.01834 = 0.03056 -0.00391 0.00199 -0.00705 O34B 4 0.832554 -0.154700 0.161242 11.00000 0.03196 0.02495 = 0.03475 0.01101 0.02388 0.01111 O34A 4 0.829266 0.028551 0.036611 11.00000 0.01960 0.01962 = 0.02597 0.00619 0.00577 0.00295 O33 4 1.030764 -0.314054 0.091454 11.00000 0.02303 0.01684 = 0.03035 0.00262 0.01076 0.00185 AFIX 147 H33O 2 1.077438 -0.364914 0.053143 11.00000 -1.50000 AFIX 0 O32 4 1.167769 -0.055070 0.218507 11.00000 0.02284 0.03022 = 0.01698 0.00034 0.00333 0.00149 AFIX 147 H32O 2 1.214581 -0.130948 0.248734 11.00000 -1.50000 AFIX 0 O31A 4 1.300384 -0.105152 -0.026951 11.00000 0.01969 0.03663 = 0.01999 0.00684 0.00820 -0.00050 O31B 4 1.369239 -0.214795 0.138036 11.00000 0.01757 0.02799 = 0.02427 0.00532 0.00037 0.00209 MOLE 3 C4 1 0.766145 0.172132 0.517707 11.00000 0.01966 0.01558 = 0.01637 0.00809 0.00240 0.00146 C3 1 0.615890 0.191847 0.543191 11.00000 0.01894 0.01811 = 0.01515 -0.00304 0.00061 0.00129 AFIX 13 H3 2 0.542554 0.197116 0.472400 11.00000 -1.20000 AFIX 0 C2 1 0.580108 0.056194 0.608987 11.00000 0.01697 0.01564 = 0.02139 -0.00238 0.00506 -0.00400 AFIX 13 H2 2 0.596979 -0.038833 0.568648 11.00000 -1.20000 AFIX 0 C1 1 0.419091 0.058743 0.615406 11.00000 0.02356 0.01271 = 0.02929 0.00045 0.00949 -0.00369 O4A 4 0.775949 0.063922 0.450808 11.00000 0.01860 0.02609 = 0.02089 -0.00543 0.00635 -0.00150 O4B 4 0.868279 0.254038 0.563188 11.00000 0.02184 0.01985 = 0.03157 -0.00036 0.00084 -0.00228 O3 4 0.602601 0.326013 0.606043 11.00000 0.03034 0.01881 = 0.01989 0.00272 0.00782 0.00223 AFIX 147 H3O 2 0.618863 0.403915 0.570939 11.00000 -1.50000 AFIX 0 O2 4 0.673793 0.050324 0.714354 11.00000 0.02042 0.02073 = 0.01815 0.00148 0.00211 -0.00039 AFIX 147 H2O 2 0.667206 0.132502 0.748001 11.00000 -1.50000 AFIX 0 O1B 4 0.328958 0.049077 0.526678 11.00000 0.01816 0.04202 = 0.02644 -0.00834 0.00170 0.00283 O1A 4 0.388760 0.065043 0.708767 11.00000 0.02162 0.04036 = 0.02534 0.00169 0.00906 0.00037 MOLE 4 PART 1 SAME N45A C44A C43A C42A N41A N41A 3 0.859428 0.539693 0.216346 21.00000 0.02018 0.01938 = 0.02411 0.00137 0.00626 0.00305 AFIX 137 H41A 2 0.827868 0.488496 0.152109 21.00000 -1.50000 H41B 2 0.885700 0.636480 0.201727 21.00000 -1.50000 H41C 2 0.786774 0.543713 0.254349 21.00000 -1.50000 AFIX 0 C42A 1 0.986304 0.458940 0.282847 21.00000 0.01568 0.01665 = 0.02393 0.00019 0.00209 -0.00276 AFIX 23 H42A 2 1.014405 0.509077 0.355532 21.00000 -1.20000 H42B 2 1.069459 0.466962 0.245875 21.00000 -1.20000 AFIX 0 C43A 1 0.954130 0.292650 0.298714 21.00000 0.01856 0.01946 = 0.02106 -0.00473 0.00259 -0.00027 AFIX 23 H43A 2 0.938494 0.238425 0.227364 21.00000 -1.20000 H43B 2 0.864661 0.283074 0.328192 21.00000 -1.20000 AFIX 0 C44A 1 1.080775 0.222460 0.377910 21.00000 0.01801 0.02251 = 0.02465 -0.00084 0.00211 -0.00025 AFIX 23 H44A 2 1.169414 0.230834 0.347264 21.00000 -1.20000 H44B 2 1.097847 0.279519 0.448160 21.00000 -1.20000 AFIX 0 N45A 3 1.052737 0.058038 0.398830 21.00000 0.01548 0.02495 = 0.02154 0.00552 0.01283 0.00509 AFIX 137 H45A 2 0.970515 0.050101 0.426036 21.00000 -1.50000 H45B 2 1.129271 0.019185 0.448373 21.00000 -1.50000 H45C 2 1.041339 0.004626 0.334830 21.00000 -1.50000 AFIX 0 PART 2 SAME N41A > N45A N41B 3 0.914065 0.597077 0.282150 -21.00000 0.01084 0.02483 = 0.02309 -0.00016 0.00817 0.00391 AFIX 137 H41D 2 0.827430 0.582719 0.302204 -21.00000 -1.50000 H41E 2 0.901635 0.661617 0.223540 -21.00000 -1.50000 H41F 2 0.978972 0.638453 0.339328 -21.00000 -1.50000 AFIX 0 C42B 1 0.969885 0.447453 0.251719 -21.00000 0.01819 0.01778 = 0.02080 0.00023 0.00375 -0.00395 AFIX 23 H42C 2 1.066597 0.462155 0.233762 -21.00000 -1.20000 H42D 2 0.903400 0.406460 0.185668 -21.00000 -1.20000 AFIX 0 C43B 1 0.981837 0.335054 0.344374 -21.00000 0.02062 0.01797 = 0.02258 -0.00289 0.00770 -0.00062 AFIX 23 H43C 2 1.050507 0.374180 0.409976 -21.00000 -1.20000 H43D 2 0.885731 0.321544 0.363613 -21.00000 -1.20000 AFIX 0 C44B 1 1.034205 0.186091 0.310547 -21.00000 0.01808 0.02038 = 0.02188 -0.00089 0.00762 0.00026 AFIX 23 H44C 2 1.132603 0.199358 0.295355 -21.00000 -1.20000 H44D 2 0.968803 0.151224 0.241968 -21.00000 -1.20000 AFIX 0 N45B 3 1.039244 0.067087 0.397765 -21.00000 0.00800 0.02053 = 0.02722 0.00284 0.00093 0.00783 AFIX 137 H45D 2 1.111224 0.090355 0.456567 -21.00000 -1.50000 H45E 2 1.057105 -0.026100 0.370721 -21.00000 -1.50000 H45F 2 0.952467 0.064653 0.419034 -21.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 04skc0009p21 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 C22 - N21 C23 C23 - C24 C22 C24 - N25 C23 N21 - C22 N25 - C24 C34 - O34B O34A C33 C33 - O33 C32 C34 C32 - O32 C31 C33 C31 - O31A O31B C32 O34B - C34 O34A - C34 O33 - C33 O32 - C32 O31A - C31 O31B - C31 C4 - O4B O4A C3 C3 - O3 C2 C4 C2 - O2 C3 C1 C1 - O1B O1A C2 O4A - C4 O4B - C4 O3 - C3 O2 - C2 O1B - C1 O1A - C1 N41A_a - C42A_a C42A_a - N41A_a C43A_a C43A_a - C42A_a C44A_a C44A_a - N45A_a C43A_a N45A_a - C44A_a N41B_b - C42B_b C42B_b - N41B_b C43B_b C43B_b - C44B_b C42B_b C44B_b - C43B_b N45B_b N45B_b - C44B_b Operators for generating equivalent atoms: $1 -x+2, y+1/2, -z $2 -x+1, y+1/2, -z+1 $3 x-1, y, z $4 -x+1, y-1/2, -z+1 $5 -x+1, y+1/2, -z $6 -x+2, y-1/2, -z $7 -x+2, y-1/2, -z+1 $8 -x+2, y+1/2, -z+1 $9 x, y+1, z $10 x+1, y, z Floating origin restraints generated 8284 Reflections read, of which 42 rejected -12 =< h =< 12, -11 =< k =< 10, -12 =< l =< 16, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 7 4 3 124.80 7.75 6 58.08 7 5 5 16.11 8.00 3 86.44 2 Inconsistent equivalents 2437 Unique reflections, of which 0 suppressed R(int) = 0.0830 R(sigma) = 0.1135 Friedel opposites merged Maximum memory for data reduction = 4826 / 24139 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 = 5838 / 412823 wR2 = 0.1136 before cycle 1 for 2437 data and 328 / 328 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 19. 0. 0. 0. 14. 126. 0. 0. rms sigma 0.000 0.000 0.000 0.029 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.003 0.004 0.000 0.000 GooF = S = 1.024; Restrained GooF = 0.991 for 160 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0443 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83318 0.00238 0.075 OSF 2 0.68579 0.00661 -0.051 FVAR 2 3 0.01166 0.00290 0.071 EXTI Mean shift/esd = 0.079 Maximum = -0.807 for U11 N21 Max. shift = 0.016 A for H45D_b Max. dU = 0.000 for N21 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5838 / 412823 wR2 = 0.1134 before cycle 2 for 2437 data and 328 / 328 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 19. 0. 0. 0. 14. 126. 0. 0. rms sigma 0.000 0.000 0.000 0.029 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.003 0.004 0.000 0.000 GooF = S = 1.022; Restrained GooF = 0.989 for 160 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0443 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83327 0.00237 0.041 OSF 2 0.68576 0.00661 -0.005 FVAR 2 3 0.01175 0.00291 0.032 EXTI Mean shift/esd = 0.028 Maximum = -0.265 for U11 N21 Max. shift = 0.007 A for H45F_b Max. dU = 0.000 for N45B_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 5838 / 412823 wR2 = 0.1134 before cycle 3 for 2437 data and 328 / 328 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 19. 0. 0. 0. 14. 126. 0. 0. rms sigma 0.000 0.000 0.000 0.029 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.003 0.004 0.000 0.000 GooF = S = 1.022; Restrained GooF = 0.988 for 160 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0443 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83327 0.00237 -0.001 OSF 2 0.68577 0.00661 0.002 FVAR 2 3 0.01175 0.00291 0.000 EXTI Mean shift/esd = 0.003 Maximum = -0.022 for tors H41D_b Max. shift = 0.002 A for H41F_b Max. dU = 0.000 for N45B_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 5838 / 412823 wR2 = 0.1134 before cycle 4 for 2437 data and 328 / 328 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 19. 0. 0. 0. 14. 126. 0. 0. rms sigma 0.000 0.000 0.000 0.029 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.003 0.004 0.000 0.000 GooF = S = 1.022; Restrained GooF = 0.988 for 160 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0443 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83327 0.00237 0.000 OSF 2 0.68578 0.00661 0.002 FVAR 2 3 0.01175 0.00291 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.012 for tors H41D_b Max. shift = 0.001 A for H41F_b Max. dU = 0.000 for N45B_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 5838 / 412823 wR2 = 0.1134 before cycle 5 for 2437 data and 328 / 328 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 19. 0. 0. 0. 14. 126. 0. 0. rms sigma 0.000 0.000 0.000 0.029 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.003 0.004 0.000 0.000 GooF = S = 1.022; Restrained GooF = 0.988 for 160 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0443 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83327 0.00237 -0.001 OSF 2 0.68578 0.00661 0.000 FVAR 2 3 0.01175 0.00291 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.007 for tors H41D_b Max. shift = 0.001 A for H41F_b Max. dU = 0.000 for N45B_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 5838 / 412823 wR2 = 0.1134 before cycle 6 for 2437 data and 328 / 328 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 19. 0. 0. 0. 14. 126. 0. 0. rms sigma 0.000 0.000 0.000 0.029 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.003 0.004 0.000 0.000 GooF = S = 1.022; Restrained GooF = 0.988 for 160 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0443 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83327 0.00237 -0.001 OSF 2 0.68578 0.00661 0.000 FVAR 2 3 0.01174 0.00291 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.004 for tors H41D_b Max. shift = 0.000 A for H41F_b Max. dU = 0.000 for N45B_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 5838 / 412823 wR2 = 0.1134 before cycle 7 for 2437 data and 328 / 328 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 19. 0. 0. 0. 14. 126. 0. 0. rms sigma 0.000 0.000 0.000 0.029 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.003 0.004 0.000 0.000 GooF = S = 1.022; Restrained GooF = 0.988 for 160 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0443 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83327 0.00237 0.000 OSF 2 0.68578 0.00661 0.000 FVAR 2 3 0.01174 0.00291 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for tors H41D_b Max. shift = 0.000 A for H41F_b Max. dU = 0.000 for N45B_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 5838 / 412823 wR2 = 0.1134 before cycle 8 for 2437 data and 328 / 328 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 19. 0. 0. 0. 14. 126. 0. 0. rms sigma 0.000 0.000 0.000 0.029 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.003 0.004 0.000 0.000 GooF = S = 1.022; Restrained GooF = 0.988 for 160 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0443 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83327 0.00237 0.001 OSF 2 0.68578 0.00661 0.000 FVAR 2 3 0.01175 0.00291 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for tors H41D_b Max. shift = 0.000 A for H41F_b Max. dU = 0.000 for N45B_b Largest correlation matrix elements -0.977 x N45B_b / x N45A_a 0.750 z N45A_a / y N45A_a -0.597 U13 C42A_a / x C42A_a -0.967 z N45B_b / z N45A_a -0.724 U11 N45A_a / x N45A_a 0.562 EXTI / OSF -0.913 y N45B_b / y N45A_a -0.707 U33 N45B_b / U33 N45A_a 0.549 z N45B_b / U13 N45A_a -0.804 x C42B_b / x C42A_a 0.706 x C42B_b / U13 C42A_a -0.548 U13 N45B_b / U13 N45A_a 0.803 z N45B_b / y N45B_b -0.697 U23 N45B_b / U23 N45A_a -0.545 U13 C42B_b / x C42A_a 0.793 x N45B_b / U11 N45A_a -0.617 U12 N45B_b / U12 N45A_a -0.535 y C42B_b / y C42A_a -0.785 y N45B_b / z N45A_a 0.613 z C42B_b / U33 C42A_a 0.532 y C42B_b / U23 C42A_a -0.762 z N45B_b / y N45A_a 0.605 x C42B_b / U11 C42A_a -0.523 y N45B_b / U22 N45A_a Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H22B 0.5281 0.0581 0.1026 23 0.990 0.000 C22 N21 C23 H22A 0.6503 0.1639 0.1755 23 0.990 0.000 C22 N21 C23 H23A 0.3816 0.1172 0.2410 23 0.990 0.000 C23 C24 C22 H23B 0.4954 0.2526 0.2791 23 0.990 0.000 C23 C24 C22 H24A 0.3356 0.2292 0.0589 23 0.990 0.000 C24 N25 C23 H24B 0.2752 0.3242 0.1495 23 0.990 0.000 C24 N25 C23 H21A 0.6899 -0.0862 0.2283 137 0.910 0.000 N21 C22 H21A H21C 0.5419 -0.1020 0.2513 137 0.910 0.000 N21 C22 H21A H21B 0.6509 -0.0021 0.3218 137 0.910 0.000 N21 C22 H21A H25A 0.5163 0.3984 0.0663 137 0.910 0.000 N25 C24 H25A H25B 0.4878 0.4749 0.1663 137 0.910 0.000 N25 C24 H25A H25C 0.3836 0.4932 0.0595 137 0.910 0.000 N25 C24 H25A H33 1.0013 -0.1608 -0.0291 13 1.000 0.000 C33 O33 C32 C34 H32 1.1364 0.0390 0.0720 13 1.000 0.000 C32 O32 C31 C33 H33O 1.0769 -0.3651 0.0528 147 0.840 0.000 O33 C33 H33O H32O 1.2145 -0.1311 0.2487 147 0.840 0.000 O32 C32 H32O H3 0.5427 0.1971 0.4724 13 1.000 0.000 C3 O3 C2 C4 H2 0.5970 -0.0388 0.5687 13 1.000 0.000 C2 O2 C3 C1 H3O 0.6185 0.4040 0.5708 147 0.840 0.000 O3 C3 H3O H2O 0.6666 0.1321 0.7483 147 0.840 0.000 O2 C2 H2O H41A 0.8285 0.4896 0.1518 137 0.910 0.000 N41A_a C42A_a H41A_a H41B 0.8855 0.6371 0.2027 137 0.910 0.000 N41A_a C42A_a H41A_a H41C 0.7864 0.5428 0.2541 137 0.910 0.000 N41A_a C42A_a H41A_a H42A 1.0144 0.5088 0.3556 23 0.990 0.000 C42A_a N41A_a C43A_a H42B 1.0694 0.4669 0.2459 23 0.990 0.000 C42A_a N41A_a C43A_a H43A 0.9387 0.2385 0.2272 23 0.990 0.000 C43A_a C42A_a C44A_a H43B 0.8646 0.2830 0.3279 23 0.990 0.000 C43A_a C42A_a C44A_a H44A 1.1693 0.2308 0.3472 23 0.990 0.000 C44A_a N45A_a C43A_a H44B 1.0976 0.2797 0.4480 23 0.990 0.000 C44A_a N45A_a C43A_a H45A 0.9701 0.0502 0.4258 137 0.910 0.000 N45A_a C44A_a H45A_a H45B 1.1289 0.0195 0.4488 137 0.910 0.000 N45A_a C44A_a H45A_a H45C 1.0417 0.0045 0.3350 137 0.910 0.000 N45A_a C44A_a H45A_a H41D 0.8269 0.5829 0.3016 137 0.910 0.000 N41B_b C42B_b H41D_b H41E 0.9026 0.6621 0.2240 137 0.910 0.000 N41B_b C42B_b H41D_b H41F 0.9785 0.6378 0.3400 137 0.910 0.000 N41B_b C42B_b H41D_b H42C 1.0663 0.4622 0.2336 23 0.990 0.000 C42B_b N41B_b C43B_b H42D 0.9030 0.4066 0.1857 23 0.990 0.000 C42B_b N41B_b C43B_b H43C 1.0506 0.3742 0.4098 23 0.990 0.000 C43B_b C44B_b C42B_b H43D 0.8859 0.3214 0.3636 23 0.990 0.000 C43B_b C44B_b C42B_b H44C 1.1328 0.1996 0.2954 23 0.990 0.000 C44B_b C43B_b N45B_b H44D 0.9691 0.1514 0.2419 23 0.990 0.000 C44B_b C43B_b N45B_b H45D 1.1122 0.0895 0.4560 137 0.910 0.000 N45B_b C44B_b H45D_b H45E 1.0563 -0.0263 0.3701 137 0.910 0.000 N45B_b C44B_b H45D_b H45F 0.9531 0.0651 0.4194 137 0.910 0.000 N45B_b C44B_b H45D_b 04skc0009p21 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C22 0.56654 0.09639 0.17795 1.00000 0.02574 0.02685 0.02531 0.00047 0.00552 0.00220 0.02594 0.00890 0.00048 0.00052 0.00040 0.00000 0.00232 0.00250 0.00281 0.00206 0.00211 0.00203 0.00109 H22B 0.52805 0.05813 0.10261 1.00000 0.03113 0.00000 0.00000 H22A 0.65027 0.16390 0.17545 1.00000 0.03113 0.00000 0.00000 C23 0.44966 0.18840 0.21575 1.00000 0.02562 0.02752 0.02080 -0.00527 0.00714 0.00128 0.02432 0.00835 0.00045 0.00054 0.00036 0.00000 0.00233 0.00237 0.00256 0.00213 0.00196 0.00216 0.00102 H23A 0.38162 0.11719 0.24099 1.00000 0.02918 0.00000 0.00000 H23B 0.49544 0.25257 0.27915 1.00000 0.02918 0.00000 0.00000 C24 0.36500 0.29011 0.12698 1.00000 0.02742 0.02112 0.02905 -0.00161 0.00384 0.00042 0.02617 0.00822 0.00047 0.00049 0.00040 0.00000 0.00238 0.00253 0.00298 0.00214 0.00224 0.00210 0.00112 H24A 0.33563 0.22921 0.05887 1.00000 0.03140 0.00000 0.00000 H24B 0.27524 0.32416 0.14952 1.00000 0.03140 0.00000 0.00000 N21 0.61728 -0.03653 0.25212 1.00000 0.01961 0.02523 0.02522 -0.00193 0.00738 -0.00028 0.02296 0.00678 0.00035 0.00043 0.00031 0.00000 0.00187 0.00202 0.00231 0.00168 0.00168 0.00170 0.00089 H21A 0.68988 -0.08624 0.22831 1.00000 0.03444 0.00000 0.00000 H21C 0.54187 -0.10202 0.25130 1.00000 0.03444 0.00000 0.00000 H21B 0.65092 -0.00208 0.32180 1.00000 0.03444 0.00000 0.00000 N25 0.44603 0.42746 0.10241 1.00000 0.02565 0.02301 0.02306 -0.00088 0.00750 0.00332 0.02356 0.00672 0.00037 0.00041 0.00031 0.00000 0.00192 0.00204 0.00233 0.00173 0.00170 0.00170 0.00089 H25A 0.51628 0.39841 0.06631 1.00000 0.03534 0.00000 0.00000 H25B 0.48780 0.47486 0.16634 1.00000 0.03534 0.00000 0.00000 H25C 0.38356 0.49316 0.05955 1.00000 0.03534 0.00000 0.00000 C34 0.88180 -0.09071 0.08684 1.00000 0.01592 0.01773 0.02220 -0.00140 0.00262 -0.00195 0.01882 0.00771 0.00042 0.00048 0.00038 0.00000 0.00213 0.00225 0.00268 0.00198 0.00196 0.00188 0.00099 C33 1.01559 -0.16144 0.05282 1.00000 0.01952 0.01703 0.01736 0.00266 0.00431 -0.00050 0.01791 0.00783 0.00044 0.00047 0.00036 0.00000 0.00213 0.00216 0.00241 0.00191 0.00181 0.00192 0.00094 H33 1.00128 -0.16076 -0.02908 1.00000 0.02149 0.00000 0.00000 C32 1.15106 -0.06678 0.10313 1.00000 0.01762 0.02172 0.01762 0.00158 -0.00012 -0.00227 0.01954 0.00757 0.00041 0.00051 0.00036 0.00000 0.00210 0.00225 0.00267 0.00195 0.00186 0.00190 0.00098 H32 1.13638 0.03896 0.07202 1.00000 0.02345 0.00000 0.00000 C31 1.28427 -0.13511 0.06783 1.00000 0.00881 0.01845 0.03089 -0.00390 0.00174 -0.00677 0.01974 0.00752 0.00042 0.00046 0.00039 0.00000 0.00202 0.00225 0.00302 0.00209 0.00200 0.00185 0.00103 O34B 0.83253 -0.15476 0.16121 1.00000 0.03192 0.02548 0.03482 0.01097 0.02328 0.01134 0.02836 0.00615 0.00032 0.00035 0.00026 0.00000 0.00172 0.00163 0.00207 0.00155 0.00157 0.00142 0.00078 O34A 0.82922 0.02855 0.03661 1.00000 0.01999 0.01946 0.02580 0.00595 0.00576 0.00287 0.02161 0.00531 0.00028 0.00033 0.00024 0.00000 0.00145 0.00159 0.00181 0.00138 0.00125 0.00133 0.00070 O33 1.03079 -0.31406 0.09148 1.00000 0.02275 0.01682 0.03047 0.00264 0.01084 0.00202 0.02258 0.00575 0.00031 0.00033 0.00025 0.00000 0.00157 0.00147 0.00193 0.00147 0.00134 0.00139 0.00071 H33O 1.07685 -0.36512 0.05285 1.00000 0.03387 0.00000 0.00000 O32 1.16780 -0.05512 0.21850 1.00000 0.02291 0.03036 0.01689 0.00011 0.00328 0.00148 0.02352 0.00531 0.00030 0.00035 0.00023 0.00000 0.00166 0.00184 0.00187 0.00147 0.00132 0.00145 0.00074 H32O 1.21453 -0.13109 0.24867 1.00000 0.03527 0.00000 0.00000 O31A 1.30040 -0.10524 -0.02693 1.00000 0.01985 0.03648 0.02008 0.00686 0.00833 -0.00044 0.02486 0.00561 0.00030 0.00035 0.00026 0.00000 0.00156 0.00190 0.00191 0.00145 0.00140 0.00142 0.00078 O31B 1.36926 -0.21479 0.13807 1.00000 0.01743 0.02813 0.02456 0.00536 0.00039 0.00204 0.02396 0.00530 0.00029 0.00033 0.00026 0.00000 0.00151 0.00178 0.00191 0.00144 0.00139 0.00141 0.00076 C4 0.76615 0.17214 0.51778 1.00000 0.02000 0.01534 0.01630 0.00790 0.00275 0.00185 0.01737 0.00794 0.00043 0.00046 0.00035 0.00000 0.00215 0.00225 0.00249 0.00198 0.00188 0.00203 0.00095 C3 0.61600 0.19186 0.54321 1.00000 0.01901 0.01834 0.01536 -0.00311 0.00098 0.00119 0.01795 0.00747 0.00042 0.00049 0.00034 0.00000 0.00212 0.00211 0.00240 0.00196 0.00183 0.00191 0.00094 H3 0.54270 0.19711 0.47240 1.00000 0.02154 0.00000 0.00000 C2 0.58013 0.05621 0.60898 1.00000 0.01651 0.01588 0.02187 -0.00233 0.00524 -0.00342 0.01791 0.00746 0.00039 0.00050 0.00034 0.00000 0.00201 0.00213 0.00249 0.00202 0.00182 0.00192 0.00093 H2 0.59701 -0.03882 0.56865 1.00000 0.02149 0.00000 0.00000 C1 0.41909 0.05871 0.61540 1.00000 0.02324 0.01278 0.02923 0.00052 0.00923 -0.00345 0.02120 0.00818 0.00043 0.00049 0.00038 0.00000 0.00223 0.00214 0.00286 0.00211 0.00214 0.00209 0.00099 O4A 0.77591 0.06384 0.45082 1.00000 0.01883 0.02631 0.02104 -0.00549 0.00653 -0.00143 0.02172 0.00506 0.00027 0.00035 0.00023 0.00000 0.00146 0.00165 0.00174 0.00152 0.00125 0.00138 0.00069 O4B 0.86827 0.25406 0.56324 1.00000 0.02206 0.01967 0.03184 -0.00051 0.00103 -0.00227 0.02520 0.00545 0.00030 0.00033 0.00026 0.00000 0.00153 0.00153 0.00204 0.00144 0.00140 0.00151 0.00076 O3 0.60259 0.32604 0.60602 1.00000 0.03010 0.01859 0.02010 0.00288 0.00783 0.00226 0.02255 0.00554 0.00033 0.00032 0.00025 0.00000 0.00173 0.00155 0.00175 0.00137 0.00138 0.00142 0.00072 H3O 0.61848 0.40396 0.57079 1.00000 0.03383 0.00000 0.00000 O2 0.67379 0.05031 0.71439 1.00000 0.02062 0.02072 0.01781 0.00166 0.00202 -0.00054 0.02001 0.00503 0.00028 0.00033 0.00023 0.00000 0.00145 0.00156 0.00165 0.00139 0.00126 0.00140 0.00066 H2O 0.66659 0.13214 0.74827 1.00000 0.03001 0.00000 0.00000 O1B 0.32897 0.04910 0.52669 1.00000 0.01818 0.04217 0.02670 -0.00849 0.00189 0.00299 0.02943 0.00570 0.00029 0.00040 0.00026 0.00000 0.00147 0.00192 0.00195 0.00169 0.00139 0.00158 0.00076 O1A 0.38882 0.06509 0.70875 1.00000 0.02163 0.04010 0.02548 0.00172 0.00910 0.00043 0.02846 0.00572 0.00029 0.00039 0.00026 0.00000 0.00157 0.00198 0.00198 0.00164 0.00140 0.00155 0.00077 N41A_a 0.85941 0.53988 0.21644 0.68578 0.02057 0.01963 0.02388 0.00111 0.00631 0.00297 0.02112 0.01171 0.00053 0.00066 0.00049 0.00661 0.00276 0.00283 0.00361 0.00266 0.00248 0.00251 0.00140 H41A_a 0.82847 0.48955 0.15175 0.68578 0.03168 0.00661 0.00000 H41B_a 0.88552 0.63706 0.20269 0.68578 0.03168 0.00661 0.00000 H41C_a 0.78636 0.54284 0.25409 0.68578 0.03168 0.00661 0.00000 C42A_a 0.98622 0.45877 0.28284 0.68578 0.01569 0.01658 0.02394 0.00034 0.00204 -0.00262 0.01904 0.01676 0.00111 0.00083 0.00073 0.00661 0.00346 0.00294 0.00440 0.00295 0.00358 0.00268 0.00193 H42A_a 1.01440 0.50877 0.35557 0.68578 0.02285 0.00661 0.00000 H42B_a 1.06936 0.46685 0.24585 0.68578 0.02285 0.00661 0.00000 C43A_a 0.95418 0.29264 0.29860 0.68578 0.01855 0.01962 0.02080 -0.00478 0.00259 -0.00019 0.01988 0.01302 0.00069 0.00071 0.00063 0.00661 0.00300 0.00293 0.00369 0.00264 0.00274 0.00251 0.00154 H43A_a 0.93873 0.23847 0.22724 0.68578 0.02386 0.00661 0.00000 H43B_a 0.86462 0.28296 0.32794 0.68578 0.02386 0.00661 0.00000 C44A_a 1.08060 0.22249 0.37784 0.68578 0.01810 0.02302 0.02437 -0.00087 0.00202 -0.00012 0.02219 0.01321 0.00065 0.00071 0.00062 0.00661 0.00291 0.00307 0.00386 0.00281 0.00272 0.00253 0.00154 H44A_a 1.16928 0.23076 0.34724 0.68578 0.02662 0.00661 0.00000 H44B_a 1.09763 0.27967 0.44804 0.68578 0.02662 0.00661 0.00000 N45A_a 1.05259 0.05816 0.39892 0.68578 0.01575 0.02503 0.02136 0.00607 0.01282 0.00497 0.01941 0.05278 0.00304 0.00161 0.00188 0.00661 0.00608 0.00436 0.00455 0.00371 0.00429 0.00407 0.00259 H45A_a 0.97011 0.05025 0.42580 0.68578 0.02911 0.00661 0.00000 H45B_a 1.12892 0.01953 0.44877 0.68578 0.02911 0.00661 0.00000 H45C_a 1.04166 0.00453 0.33504 0.68578 0.02911 0.00661 0.00000 N41B_b 0.91400 0.59711 0.28230 0.31422 0.01062 0.02486 0.02278 -0.00081 0.00844 0.00406 0.01870 0.02656 0.00123 0.00124 0.00115 0.00661 0.00536 0.00522 0.00685 0.00500 0.00499 0.00465 0.00276 H41D_b 0.82686 0.58294 0.30160 0.31422 0.02805 0.00661 0.00000 H41E_b 0.90261 0.66210 0.22399 0.31422 0.02805 0.00661 0.00000 H41F_b 0.97847 0.63783 0.34001 0.31422 0.02805 0.00661 0.00000 C42B_b 0.96967 0.44749 0.25173 0.31422 0.01826 0.01792 0.02080 -0.00040 0.00454 -0.00353 0.01893 0.04723 0.00299 0.00179 0.00152 0.00661 0.00505 0.00436 0.00591 0.00444 0.00511 0.00441 0.00286 H42C_b 1.06628 0.46220 0.23359 0.31422 0.02272 0.00661 0.00000 H42D_b 0.90301 0.40656 0.18574 0.31422 0.02272 0.00661 0.00000 C43B_b 0.98190 0.33504 0.34425 0.31422 0.02065 0.01828 0.02248 -0.00327 0.00808 -0.00018 0.01995 0.03230 0.00181 0.00138 0.00127 0.00661 0.00439 0.00400 0.00502 0.00403 0.00431 0.00399 0.00235 H43C_b 1.05057 0.37425 0.40983 0.31422 0.02394 0.00661 0.00000 H43D_b 0.88586 0.32138 0.36355 0.31422 0.02394 0.00661 0.00000 C44B_b 1.03439 0.18621 0.31052 0.31422 0.01788 0.02097 0.02181 -0.00157 0.00780 0.00059 0.01969 0.02950 0.00155 0.00143 0.00130 0.00661 0.00473 0.00431 0.00517 0.00436 0.00441 0.00428 0.00235 H44C_b 1.13280 0.19961 0.29539 0.31422 0.02363 0.00661 0.00000 H44D_b 0.96910 0.15138 0.24188 0.31422 0.02363 0.00661 0.00000 N45B_b 1.03949 0.06693 0.39753 0.31422 0.00900 0.02068 0.02788 0.00240 0.00096 0.00828 0.01961 0.11665 0.00667 0.00374 0.00410 0.00661 0.00846 0.00721 0.00900 0.00698 0.00774 0.00752 0.00482 H45D_b 1.11218 0.08946 0.45603 0.31422 0.02942 0.00661 0.00000 H45E_b 1.05631 -0.02631 0.37008 0.31422 0.02942 0.00661 0.00000 H45F_b 0.95310 0.06513 0.41939 0.31422 0.02942 0.00661 0.00000 Final Structure Factor Calculation for 04skc0009p21 in P2(1) Total number of l.s. parameters = 328 Maximum vector length = 511 Memory required = 5512 / 25046 wR2 = 0.1134 before cycle 9 for 2437 data and 2 / 328 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 19. 0. 0. 0. 14. 126. 0. 0. rms sigma 0.000 0.000 0.000 0.029 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.003 0.004 0.000 0.000 GooF = S = 1.022; Restrained GooF = 0.988 for 160 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0443 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0575 for 1591 Fo > 4sig(Fo) and 0.1122 for all 2437 data wR2 = 0.1134, GooF = S = 1.022, Restrained GooF = 0.988 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 30.00 for non-hydrogen and 32.00 for hydrogen atoms Principal mean square atomic displacements U 0.0286 0.0252 0.0240 C22 0.0305 0.0261 0.0163 C23 0.0313 0.0264 0.0208 C24 0.0274 0.0237 0.0178 N21 0.0281 0.0239 0.0187 N25 0.0230 0.0189 0.0145 C34 0.0200 0.0195 0.0142 C33 0.0252 0.0190 0.0144 C32 0.0325 0.0215 0.0053 C31 0.0541 0.0184 0.0126 O34B 0.0295 0.0198 0.0155 O34A 0.0328 0.0188 0.0162 O33 0.0307 0.0230 0.0169 O32 0.0390 0.0224 0.0132 O31A 0.0324 0.0243 0.0152 O31B 0.0238 0.0205 0.0079 C4 0.0231 0.0175 0.0133 C3 0.0231 0.0179 0.0128 C2 0.0304 0.0219 0.0113 C1 0.0299 0.0193 0.0159 O4A 0.0349 0.0226 0.0180 O4B 0.0309 0.0205 0.0163 O3 0.0232 0.0202 0.0167 O2 0.0472 0.0234 0.0177 O1B 0.0403 0.0272 0.0178 O1A 0.0251 0.0214 0.0169 N41A_a 0.0252 0.0184 0.0135 C42A_a 0.0256 0.0187 0.0153 C43A_a 0.0261 0.0228 0.0177 C44A_a 0.0329 0.0185 0.0068 N45A_a 0.0259 0.0237 0.0065 N41B_b 0.0217 0.0206 0.0145 C42B_b 0.0256 0.0192 0.0151 C43B_b 0.0238 0.0209 0.0144 C44B_b 0.0292 0.0250 0.0047 N45B_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.023 0.034 0.044 0.054 0.065 0.078 0.095 0.119 0.168 1.000 Number in group 250. 271. 219. 235. 248. 243. 251. 233. 243. 244. GooF 0.809 1.037 0.921 1.078 1.043 1.124 1.077 1.035 1.028 1.025 K 1.714 1.149 1.125 1.056 1.008 1.053 1.028 0.999 1.014 1.015 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.16 1.34 1.69 inf Number in group 253. 243. 245. 240. 248. 232. 247. 244. 241. 244. GooF 1.035 1.062 0.952 1.049 1.053 0.973 0.934 1.008 0.978 1.153 K 1.159 1.123 1.144 1.026 1.015 0.993 1.009 1.019 1.022 1.006 R1 0.289 0.282 0.235 0.193 0.140 0.094 0.058 0.045 0.033 0.026 Recommended weighting scheme: WGHT 0.0469 0.0745 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) -5 7 12 688.56 83.56 5.42 0.075 0.77 2 1 0 279.73 359.86 4.98 0.155 4.07 2 0 0 455.92 581.65 4.74 0.198 4.60 -2 1 1 826.94 1021.96 4.37 0.262 4.10 -3 1 1 79.16 103.46 3.69 0.083 2.95 -7 7 6 348.10 213.55 3.68 0.120 0.87 -4 9 7 147.60 15.42 3.66 0.032 0.82 3 8 6 71.21 144.30 3.21 0.098 0.89 1 0 15 220.84 67.16 3.13 0.067 0.79 -10 0 1 76.44 14.21 3.12 0.031 0.93 -3 2 9 234.23 179.22 3.09 0.110 1.29 7 1 7 19.81 66.71 3.08 0.067 0.95 4 2 5 51.58 32.92 3.05 0.047 1.44 10 5 2 -20.60 45.98 3.01 0.056 0.79 0 9 4 103.88 68.65 2.97 0.068 0.92 6 8 5 240.90 81.00 2.97 0.074 0.80 -9 2 8 112.50 16.75 2.95 0.034 0.92 3 6 9 83.95 166.04 2.91 0.106 0.90 -8 1 3 11.49 31.96 2.87 0.046 1.16 2 10 0 -1.37 16.30 2.84 0.033 0.86 -9 4 6 53.66 24.65 2.81 0.041 0.91 0 5 3 1256.44 1093.78 2.77 0.271 1.60 0 2 11 73.29 111.55 2.77 0.087 1.07 0 7 9 82.98 28.58 2.72 0.044 0.92 -10 3 9 88.70 34.47 2.69 0.048 0.81 -1 1 2 1201.81 1367.17 2.64 0.303 4.74 8 2 6 203.65 147.68 2.63 0.100 0.90 -11 3 2 137.89 86.57 2.61 0.076 0.82 10 4 2 237.41 13.16 2.57 0.030 0.82 6 8 3 257.81 143.24 2.56 0.098 0.85 -4 3 13 18.37 51.36 2.56 0.059 0.89 1 0 3 7.74 21.82 2.56 0.038 3.45 0 5 2 334.05 292.07 2.50 0.140 1.68 8 2 1 -0.39 19.92 2.50 0.037 1.09 -6 2 10 49.36 90.70 2.50 0.078 1.04 0 3 6 97.97 76.98 2.49 0.072 1.66 6 5 6 88.68 56.18 2.48 0.061 0.94 -7 5 3 14.27 51.08 2.46 0.059 1.06 0 2 0 2084.27 2344.80 2.45 0.397 4.37 -5 5 3 80.31 119.32 2.45 0.090 1.26 2 8 7 -12.83 16.65 2.44 0.033 0.89 6 1 2 153.28 128.48 2.43 0.093 1.40 -2 7 4 31.79 46.44 2.42 0.056 1.14 -1 2 1 174.33 198.55 2.41 0.115 3.86 -11 4 2 237.66 133.15 2.38 0.095 0.79 4 10 0 -42.77 21.58 2.37 0.038 0.82 -1 2 9 300.78 248.62 2.35 0.129 1.32 -7 2 8 1010.70 848.64 2.34 0.239 1.08 -1 5 11 56.44 91.30 2.34 0.078 0.95 2 11 2 -25.08 14.99 2.33 0.032 0.77 Bond lengths and angles C22 - Distance Angles N21 1.4980 (0.0057) C23 1.5147 (0.0061) 112.24 (0.37) H22B 0.9900 109.16 109.16 H22A 0.9900 109.16 109.16 107.88 C22 - N21 C23 H22B C23 - Distance Angles C24 1.5087 (0.0062) C22 1.5147 (0.0061) 113.05 (0.38) H23A 0.9900 108.97 108.97 H23B 0.9900 108.97 108.97 107.77 C23 - C24 C22 H23A C24 - Distance Angles N25 1.4876 (0.0055) C23 1.5087 (0.0062) 114.26 (0.35) H24A 0.9900 108.69 108.69 H24B 0.9900 108.69 108.69 107.62 C24 - N25 C23 H24A N21 - Distance Angles C22 1.4980 (0.0058) H21A 0.9100 109.47 H21C 0.9100 109.47 109.47 H21B 0.9100 109.47 109.47 109.47 N21 - C22 H21A H21C N25 - Distance Angles C24 1.4876 (0.0055) 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 C34 - Distance Angles O34B 1.2510 (0.0050) O34A 1.2616 (0.0050) 124.65 (0.38) C33 1.5396 (0.0058) 118.38 (0.36) 116.97 (0.39) C34 - O34B O34A C33 - Distance Angles O33 1.4146 (0.0049) C32 1.5385 (0.0056) 110.62 (0.34) C34 1.5396 (0.0058) 108.36 (0.34) 109.14 (0.35) H33 1.0000 109.57 109.57 109.57 C33 - O33 C32 C34 C32 - Distance Angles O32 1.4152 (0.0051) C31 1.5336 (0.0059) 113.26 (0.33) C33 1.5385 (0.0056) 110.99 (0.34) 109.36 (0.34) H32 1.0000 107.67 107.67 107.67 C32 - O32 C31 C33 C31 - Distance Angles O31A 1.2480 (0.0052) O31B 1.2631 (0.0050) 125.78 (0.38) C32 1.5336 (0.0059) 117.26 (0.37) 116.95 (0.40) C31 - O31A O31B O34B - Distance Angles C34 1.2510 (0.0050) O34B - O34A - Distance Angles C34 1.2616 (0.0050) O34A - O33 - Distance Angles C33 1.4146 (0.0049) H33O 0.8400 109.47 O33 - C33 O32 - Distance Angles C32 1.4152 (0.0051) H32O 0.8400 109.47 O32 - C32 O31A - Distance Angles C31 1.2480 (0.0052) O31A - O31B - Distance Angles C31 1.2631 (0.0050) O31B - C4 - Distance Angles O4B 1.2362 (0.0046) O4A 1.2769 (0.0051) 124.92 (0.38) C3 1.5212 (0.0055) 120.40 (0.38) 114.63 (0.36) C4 - O4B O4A C3 - Distance Angles O3 1.4292 (0.0049) C2 1.5181 (0.0060) 106.87 (0.32) C4 1.5212 (0.0055) 113.52 (0.33) 110.19 (0.34) H3 1.0000 108.72 108.72 108.72 C3 - O3 C2 C4 C2 - Distance Angles O2 1.4199 (0.0047) C3 1.5181 (0.0060) 111.19 (0.32) C1 1.5343 (0.0053) 112.40 (0.33) 110.53 (0.33) H2 1.0000 107.49 107.49 107.49 C2 - O2 C3 C1 C1 - Distance Angles O1B 1.2462 (0.0050) O1A 1.2543 (0.0050) 125.40 (0.37) C2 1.5343 (0.0053) 116.69 (0.37) 117.87 (0.37) C1 - O1B O1A O4A - Distance Angles C4 1.2769 (0.0051) O4A - O4B - Distance Angles C4 1.2362 (0.0047) O4B - O3 - Distance Angles C3 1.4292 (0.0049) H3O 0.8400 109.47 O3 - C3 O2 - Distance Angles C2 1.4199 (0.0047) H2O 0.8400 109.47 O2 - C2 O1B - Distance Angles C1 1.2462 (0.0050) O1B - O1A - Distance Angles C1 1.2543 (0.0050) O1A - N41A_a - Distance Angles C42A_a 1.4819 (0.0086) H41A_a 0.9100 109.47 H41B_a 0.9100 109.47 109.47 H41C_a 0.9100 109.47 109.47 109.47 N41A_a - C42A_a H41A_a H41B_a C42A_a - Distance Angles N41A_a 1.4819 (0.0085) C43A_a 1.5037 (0.0090) 111.98 (0.72) H42A_a 0.9900 109.22 109.22 H42B_a 0.9900 109.22 109.22 107.91 C42A_a - N41A_a C43A_a H42A_a C43A_a - Distance Angles C42A_a 1.5037 (0.0090) C44A_a 1.5073 (0.0080) 109.00 (0.59) H43A_a 0.9900 109.88 109.88 H43B_a 0.9900 109.88 109.88 108.30 C43A_a - C42A_a C44A_a H43A_a C44A_a - Distance Angles N45A_a 1.4928 (0.0128) C43A_a 1.5073 (0.0080) 111.21 (1.14) H44A_a 0.9900 109.39 109.39 H44B_a 0.9900 109.39 109.39 108.01 C44A_a - N45A_a C43A_a H44A_a N45A_a - Distance Angles C44A_a 1.4928 (0.0127) H45A_a 0.9100 109.47 H45B_a 0.9100 109.47 109.47 H45C_a 0.9100 109.47 109.47 109.47 N45A_a - C44A_a H45A_a H45B_a N41B_b - Distance Angles C42B_b 1.4871 (0.0145) H41D_b 0.9100 109.47 H41E_b 0.9100 109.47 109.47 H41F_b 0.9100 109.47 109.47 109.47 N41B_b - C42B_b H41D_b H41E_b C42B_b - Distance Angles N41B_b 1.4871 (0.0145) C43B_b 1.4997 (0.0142) 110.72 (1.31) H42C_b 0.9900 109.50 109.50 H42D_b 0.9900 109.50 109.50 108.07 C42B_b - N41B_b C43B_b H42C_b C43B_b - Distance Angles C44B_b 1.4825 (0.0129) C42B_b 1.4997 (0.0142) 109.49 (1.23) H43C_b 0.9900 109.78 109.78 H43D_b 0.9900 109.78 109.78 108.23 C43B_b - C44B_b C42B_b H43C_b C44B_b - Distance Angles C43B_b 1.4825 (0.0129) N45B_b 1.4965 (0.0170) 111.58 (1.98) H44C_b 0.9900 109.31 109.31 H44D_b 0.9900 109.31 109.31 107.96 C44B_b - C43B_b N45B_b H44C_b N45B_b - Distance Angles C44B_b 1.4965 (0.0170) H45D_b 0.9100 109.47 H45E_b 0.9100 109.47 109.47 H45F_b 0.9100 109.47 109.47 109.47 N45B_b - C44B_b H45D_b H45E_b Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.87 2.751(5) 161.9 N21-H21B...O4A 0.91 1.82 2.722(5) 168.7 N21-H21A...O34B 0.91 1.92 2.81(3) 165.6 N45A_a-H45A_a...O4A 0.91 2.12 2.87(2) 138.3 N45A_a-H45C_a...O32 0.91 2.12 2.87(2) 138.3 N45A_a-H45C_a...O32 0.91 1.79 2.70(6) 175.3 N45B_b-H45F_b...O4A 0.91 2.36 2.95(5) 122.5 N45B_b-H45E_b...O32 0.91 1.89 2.757(5) 158.4 N25-H25A...O31A_$1 0.91 1.94 2.819(7) 160.6 N41A_a-H41A_a...O31A_$1 0.91 1.91 2.803(5) 168.4 N25-H25B...O1A_$2 0.91 2.43 2.950(5) 116.6 N25-H25B...O2_$2 0.84 1.89 2.718(5) 167.8 O3-H3O...O1B_$2 0.91 1.81 2.699(6) 163.7 N41A_a-H41C_a...O1A_$2 0.91 2.01 2.889(11) 161.1 N41B_b-H41D_b...O1A_$2 0.91 2.15 2.915(4) 140.8 N21-H21C...O31B_$3 0.91 2.53 3.221(5) 132.9 N21-H21C...O3_$4 0.91 2.13 2.933(4) 146.8 N25-H25C...O34A_$5 0.84 1.82 2.655(4) 177.2 O33-H33O...O34A_$6 0.84 2.25 2.922(4) 137.0 O32-H32O...O3_$7 0.91 2.32 2.773(13) 110.1 N45A_a-H45B_a...O4B_$7 0.91 2.15 2.88(3) 136.3 N45B_b-H45E_b...O4B_$7 0.84 2.03 2.839(4) 162.8 O2-H2O...O31B_$8 0.91 1.96 2.850(14) 166.3 N41B_b-H41F_b...O4B_$8 0.91 1.93 2.753(6) 150.0 N41A_a-H41B_a...O34B_$9 0.91 2.18 2.775(6) 122.1 N41A_a-H41B_a...O33_$9 0.91 1.84 2.660(11) 148.5 N41B_b-H41E_b...O34B_$9 0.91 2.25 2.923(12) 130.6 N41B_b-H41E_b...O33_$9 0.91 1.95 2.75(3) 146.5 N45A_a-H45B_a...O1B_$10 0.91 2.08 2.86(6) 144.1 N45B_b-H45D_b...O1B_$10 FMAP and GRID set by program FMAP 2 2 23 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.1122 for 2437 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.8497 0.3506 0.6372 [ 1.29 A from O4B ] Deepest hole -0.27 at 0.5136 0.0711 0.0634 [ 0.49 A from H22B ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 5273 / 22740 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8497 0.3506 0.6372 1.00000 0.05 0.28 1.29 O4B 1.41 H45E 1.66 H32O 1.68 H45C Q2 1 0.7809 0.3196 0.3792 1.00000 0.05 0.26 1.05 H43D 1.16 H43B 2.03 C43B 2.10 C43A Q3 1 0.5567 -0.2531 0.2748 1.00000 0.05 0.25 1.35 H21C 1.67 O1A 2.01 N21 2.08 H21A Q4 1 1.1610 -0.0431 0.3418 1.00000 0.05 0.25 1.12 H45E 1.18 H45C 1.53 H45B 1.55 O32 Q5 1 0.5465 -0.0523 0.3583 1.00000 0.05 0.24 1.25 H21B 1.39 H21C 1.61 N21 1.89 O3 Q6 1 1.1005 -0.1418 0.2805 1.00000 0.05 0.24 1.22 H32O 1.33 O32 1.60 H45C 1.62 H45E Q7 1 0.9202 0.0650 0.1438 1.00000 0.05 0.24 1.43 H44D 1.46 O34A 1.54 C34 1.83 H43A Q8 1 1.1851 0.2023 0.2149 1.00000 0.05 0.23 1.21 H44C 1.67 H24B 1.70 H44A 1.96 H23A Q9 1 1.1708 -0.3195 0.1207 1.00000 0.05 0.23 1.16 H33O 1.29 O33 2.03 H2O 2.05 O31B Q10 1 0.7852 0.7776 0.3706 1.00000 0.05 0.23 1.98 H41D 2.17 H21A 2.29 H41F 2.30 H44B Shortest distances between peaks (including symmetry equivalents) 1 4 0.98 1 6 1.04 4 6 1.21 3 5 2.05 3 10 2.25 5 10 2.67 4 8 2.70 6 9 2.71 7 8 2.74 6 7 2.80 Time profile in seconds ----------------------- 0.13: 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. 0.39: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.78: Structure factors and derivatives 3.33: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.11: Apply other restraints 0.67: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04skc0009p21 finished at 14:19:17 Total CPU time: 6.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++