+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0026p21c started at 14:07:03 on 16-Jun-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0026p21c in P2(1)/c CELL 0.71073 31.3779 12.3307 7.1600 90.000 92.968 90.000 ZERR 8.00 0.0013 0.0006 0.0003 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 88 112 16 72 V = 2766.57 F(000) = 1328.0 Mu = 0.14 mm-1 Cell Wt = 2545.94 Rho = 1.528 MERG 2 OMIT -3.00 50.00 OMIT 13 8 1 SHEL 7 0.84 HTAB O4A O1B HTAB N23 O61B HTAB N23 O61A HTAB O31B O4B HTAB O34A O31A HTAB N43 O54A HTAB O51B O54A HTAB O54B O42 HTAB O61A O64A HTAB O64B O51A EQIV_$1 -x+1, -y+1, -z HTAB O1A O22_$1 HTAB N21 O1B_$1 EQIV_$2 -x, -y+1, -z+2 HTAB N41 O34B_$2 HTAB N41 O34A_$2 MPLA C61 O61A O61B MPLA C64 O64A O64B FMAP 2 PLAN 10 SIZE 0.02 0.04 0.12 ACTA BOND $H WGHT 0.00000 17.74740 L.S. 8 TEMP -153.00 FVAR 0.12079 MOLE 1 C1 1 0.372799 0.148446 -0.050722 11.00000 0.02072 0.01693 = 0.02745 -0.00034 0.00242 0.00142 C2 1 0.336478 0.098685 0.038763 11.00000 0.02124 0.01627 = 0.02902 0.00285 0.00282 -0.00064 AFIX 43 H2 2 0.336356 0.021665 0.042017 11.00000 -1.20000 AFIX 0 C3 1 0.303511 0.147227 0.116378 11.00000 0.01866 0.01907 = 0.02686 0.00143 0.00398 -0.00411 AFIX 43 H3 2 0.283549 0.098620 0.166293 11.00000 -1.20000 AFIX 0 C4 1 0.292706 0.263774 0.138055 11.00000 0.01682 0.01922 = 0.02437 -0.00259 -0.00203 -0.00140 O1A 4 0.399034 0.080708 -0.114163 11.00000 0.02108 0.02126 = 0.04189 0.00034 0.00994 0.00220 AFIX 147 H1 2 0.419474 0.114241 -0.158786 11.00000 -1.50000 AFIX 0 O1B 4 0.377380 0.250504 -0.063013 11.00000 0.02114 0.02390 = 0.03462 0.00375 0.00789 0.00333 O4A 4 0.316876 0.339675 0.078121 11.00000 0.02165 0.01656 = 0.03472 0.00230 0.01125 -0.00370 AFIX 147 H4 2 0.337918 0.311861 0.028236 11.00000 -1.50000 AFIX 0 O4B 4 0.259479 0.286222 0.217060 11.00000 0.02504 0.01971 = 0.02914 0.00135 0.00784 0.00196 MOLE 2 C22 1 0.521107 0.771802 0.259274 11.00000 0.01557 0.01894 = 0.02689 0.00204 0.00275 -0.00105 C24 1 0.477301 0.628232 0.316487 11.00000 0.01575 0.02609 = 0.03562 -0.00068 0.00236 -0.00755 AFIX 23 H24A 2 0.452097 0.603056 0.239557 11.00000 -1.20000 H24B 2 0.474620 0.604206 0.447288 11.00000 -1.20000 AFIX 0 C25 1 0.519062 0.586650 0.237751 11.00000 0.02651 0.02219 = 0.03321 -0.00428 0.00468 -0.00861 AFIX 23 H25A 2 0.533211 0.532572 0.322267 11.00000 -1.20000 H25B 2 0.513849 0.554042 0.112293 11.00000 -1.20000 AFIX 0 N21 3 0.544238 0.685226 0.228582 11.00000 0.02017 0.01684 = 0.04231 -0.00052 0.01033 0.00067 AFIX 43 H21 2 0.571502 0.686823 0.205433 11.00000 -1.20000 AFIX 0 N23 3 0.482017 0.745244 0.305545 11.00000 0.02313 0.02228 = 0.03995 -0.00243 0.01407 -0.00039 AFIX 43 H23 2 0.461705 0.792194 0.326729 11.00000 -1.20000 AFIX 0 O22 4 0.533257 0.871079 0.244586 11.00000 0.02503 0.01823 = 0.03785 -0.00033 0.01028 0.00113 MOLE 3 C31 1 0.198594 0.491971 0.357437 11.00000 0.02500 0.02346 = 0.01954 0.00062 0.00121 -0.00007 C32 1 0.185009 0.607383 0.378293 11.00000 0.01960 0.01960 = 0.03033 0.00642 0.00469 -0.00169 AFIX 43 H32 2 0.203407 0.660590 0.330265 11.00000 -1.20000 AFIX 0 C33 1 0.150269 0.644600 0.455980 11.00000 0.02290 0.01507 = 0.03724 -0.00005 0.00058 0.00113 AFIX 43 H33 2 0.147832 0.721364 0.451697 11.00000 -1.20000 AFIX 0 C34 1 0.114592 0.591107 0.547799 11.00000 0.01658 0.02297 = 0.02882 -0.00079 0.00206 0.00021 O31A 4 0.178599 0.412876 0.406487 11.00000 0.02452 0.01615 = 0.03590 -0.00161 0.01165 -0.00163 O31B 4 0.234984 0.484931 0.274655 11.00000 0.01829 0.02348 = 0.03885 -0.00136 0.01317 0.00296 AFIX 147 H31 2 0.244330 0.421221 0.283977 11.00000 -1.50000 AFIX 0 O34A 4 0.112114 0.483706 0.553546 11.00000 0.02157 0.02067 = 0.03921 0.00102 0.01167 0.00020 AFIX 147 H34 2 0.133764 0.456705 0.507242 11.00000 -1.50000 AFIX 0 O34B 4 0.087208 0.645881 0.618175 11.00000 0.02116 0.02655 = 0.04237 -0.00207 0.01067 0.00429 MOLE 4 C42 1 0.016424 0.487699 1.218006 11.00000 0.02013 0.02427 = 0.01641 0.00491 -0.00292 -0.00228 C44 1 0.017894 0.673961 1.235458 11.00000 0.02094 0.02288 = 0.02890 0.00191 0.00737 0.00286 AFIX 23 H44A 2 0.012813 0.715311 1.117890 11.00000 -1.20000 H44B 2 0.033428 0.720474 1.328871 11.00000 -1.20000 AFIX 0 C45 1 -0.024623 0.631871 1.310311 11.00000 0.02372 0.02463 = 0.02300 -0.00426 0.00448 0.00079 AFIX 23 H45A 2 -0.026112 0.645985 1.445931 11.00000 -1.20000 H45B 2 -0.049612 0.665336 1.242710 11.00000 -1.20000 AFIX 0 N41 3 -0.022069 0.515357 1.271289 11.00000 0.01766 0.02674 = 0.03720 0.00013 0.01022 -0.00357 AFIX 43 H41 2 -0.043317 0.469552 1.281803 11.00000 -1.20000 AFIX 0 N43 3 0.041193 0.574097 1.203563 11.00000 0.01510 0.01597 = 0.03399 0.00223 0.00809 0.00227 AFIX 43 H43 2 0.068300 0.571423 1.177930 11.00000 -1.20000 AFIX 0 O42 4 0.026771 0.389232 1.187234 11.00000 0.02242 0.01650 = 0.03628 -0.00221 0.00853 -0.00074 MOLE 5 C51 1 0.205317 0.516725 0.844001 11.00000 0.01744 0.02732 = 0.01853 0.00003 0.00090 0.00389 C52 1 0.194948 0.400337 0.871914 11.00000 0.02694 0.01558 = 0.03112 0.00008 0.01188 0.00703 AFIX 43 H52 2 0.215594 0.350912 0.829748 11.00000 -1.20000 AFIX 0 C53 1 0.161430 0.354166 0.946397 11.00000 0.03018 0.01224 = 0.02774 -0.00050 0.00624 0.00636 AFIX 43 H53 2 0.162200 0.277173 0.949977 11.00000 -1.20000 AFIX 0 C54 1 0.122928 0.403578 1.025012 11.00000 0.01963 0.02303 = 0.02473 -0.00078 -0.00072 -0.00168 O51A 4 0.238295 0.539590 0.767699 11.00000 0.01896 0.02844 = 0.03188 0.00036 0.00728 0.00225 O51B 4 0.179646 0.593772 0.896956 11.00000 0.02000 0.01364 = 0.03333 -0.00170 0.00899 0.00054 AFIX 147 H51 2 0.157566 0.565846 0.937910 11.00000 -1.50000 AFIX 0 O54A 4 0.118341 0.505389 1.033496 11.00000 0.02156 0.01817 = 0.03395 0.00003 0.00787 0.00306 O54B 4 0.096136 0.336537 1.081927 11.00000 0.02017 0.01969 = 0.04867 0.00331 0.01103 0.00122 AFIX 147 H54 2 0.073518 0.369212 1.105064 11.00000 -1.50000 AFIX 0 MOLE 6 C61 1 0.385518 0.844846 0.455486 11.00000 0.01906 0.02515 = 0.02562 0.00212 -0.00461 0.00219 C62 1 0.347735 0.898752 0.532520 11.00000 0.02135 0.02071 = 0.03417 -0.00002 0.00706 0.00343 AFIX 43 H62 2 0.349223 0.975698 0.531488 11.00000 -1.20000 AFIX 0 C63 1 0.312407 0.860274 0.602298 11.00000 0.02828 0.01745 = 0.02312 -0.00683 0.00522 0.00931 AFIX 43 H63 2 0.292515 0.913269 0.638967 11.00000 -1.20000 AFIX 0 C64 1 0.299677 0.745288 0.630991 11.00000 0.01308 0.02867 = 0.02373 0.00344 0.00366 -0.00145 O61A 4 0.388469 0.738167 0.449343 11.00000 0.02485 0.02620 = 0.05356 -0.00360 0.01543 0.00311 AFIX 147 H61 2 0.365141 0.710516 0.476800 11.00000 -1.50000 AFIX 0 O61B 4 0.413909 0.901352 0.398481 11.00000 0.02965 0.03006 = 0.05249 -0.00113 0.01710 -0.00826 O64A 4 0.321004 0.666203 0.586917 11.00000 0.02380 0.02157 = 0.04455 -0.00384 0.01235 0.00110 O64B 4 0.262793 0.736818 0.705276 11.00000 0.02066 0.01829 = 0.03961 -0.00180 0.00896 0.00077 AFIX 147 H64 2 0.257511 0.671150 0.725052 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 07skc0026p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C3 C1 C3 - C2 C4 C4 - O4B O4A C3 O1A - C1 O1B - C1 O4A - C4 O4B - C4 C22 - O22 N21 N23 C24 - N23 C25 C25 - N21 C24 N21 - C22 C25 N23 - C22 C24 O22 - C22 C31 - O31A O31B C32 C32 - C33 C31 C33 - C32 C34 C34 - O34B O34A C33 O31A - C31 O31B - C31 O34A - C34 O34B - C34 C42 - O42 N43 N41 C44 - N43 C45 C45 - N41 C44 N41 - C42 C45 N43 - C42 C44 O42 - C42 C51 - O51A O51B C52 C52 - C53 C51 C53 - C52 C54 C54 - O54B O54A C53 O51A - C51 O51B - C51 O54A - C54 O54B - C54 C61 - O61B O61A C62 C62 - C63 C61 C63 - C62 C64 C64 - O64A O64B C63 O61A - C61 O61B - C61 O64A - C64 O64B - C64 Operators for generating equivalent atoms: $1 -x+1, -y+1, -z $2 -x, -y+1, -z+2 21783 Reflections read, of which 4359 rejected -37 =< h =< 37, -14 =< k =< 14, -8 =< l =< 8, Max. 2-theta = 50.00 0 Systematic absence violations 0 Inconsistent equivalents 4829 Unique reflections, of which 0 suppressed R(int) = 0.0788 R(sigma) = 0.0819 Friedel opposites merged Maximum memory for data reduction = 3854 / 48044 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 = 4952 / 519930 wR2 = 0.2044 before cycle 1 for 4829 data and 405 / 405 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 17.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12079 0.00033 0.004 OSF Mean shift/esd = 0.013 Maximum = -0.050 for z C64 Max. shift = 0.002 A for H31 Max. dU = 0.000 for C33 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4952 / 519930 wR2 = 0.2044 before cycle 2 for 4829 data and 405 / 405 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 17.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12079 0.00033 0.007 OSF Mean shift/esd = 0.005 Maximum = -0.023 for z C64 Max. shift = 0.001 A for H31 Max. dU = 0.000 for C64 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4952 / 519930 wR2 = 0.2044 before cycle 3 for 4829 data and 405 / 405 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 17.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12079 0.00033 0.002 OSF Mean shift/esd = 0.001 Maximum = 0.006 for U13 C51 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4952 / 519930 wR2 = 0.2044 before cycle 4 for 4829 data and 405 / 405 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 17.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12079 0.00033 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.004 for U13 C4 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C31 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4952 / 519930 wR2 = 0.2044 before cycle 5 for 4829 data and 405 / 405 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 17.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12079 0.00033 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for U13 C4 Max. shift = 0.000 A for H54 Max. dU = 0.000 for C31 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4952 / 519930 wR2 = 0.2044 before cycle 6 for 4829 data and 405 / 405 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 17.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12079 0.00033 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U13 C4 Max. shift = 0.000 A for H54 Max. dU = 0.000 for C31 Least-squares cycle 7 Maximum vector length = 511 Memory required = 4952 / 519930 wR2 = 0.2044 before cycle 7 for 4829 data and 405 / 405 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 17.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12079 0.00033 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U13 C4 Max. shift = 0.000 A for H54 Max. dU = 0.000 for C4 Least-squares cycle 8 Maximum vector length = 511 Memory required = 4952 / 519930 wR2 = 0.2044 before cycle 8 for 4829 data and 405 / 405 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 17.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12079 0.00033 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O51A Max. shift = 0.000 A for H54 Max. dU = 0.000 for C64 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.3363 0.0217 0.0420 43 0.950 0.000 C2 C3 C1 H3 0.2835 0.0986 0.1663 43 0.950 0.000 C3 C2 C4 H1 0.4195 0.1142 -0.1584 147 0.840 0.000 O1A C1 H1 H4 0.3379 0.3119 0.0282 147 0.840 0.000 O4A C4 H4 H24A 0.4521 0.6031 0.2395 23 0.990 0.000 C24 N23 C25 H24B 0.4746 0.6042 0.4473 23 0.990 0.000 C24 N23 C25 H25A 0.5332 0.5326 0.3223 23 0.990 0.000 C25 N21 C24 H25B 0.5139 0.5540 0.1123 23 0.990 0.000 C25 N21 C24 H21 0.5715 0.6868 0.2054 43 0.880 0.000 N21 C22 C25 H23 0.4617 0.7922 0.3268 43 0.880 0.000 N23 C22 C24 H32 0.2034 0.6606 0.3304 43 0.950 0.000 C32 C33 C31 H33 0.1478 0.7214 0.4516 43 0.950 0.000 C33 C32 C34 H31 0.2443 0.4212 0.2836 147 0.840 0.000 O31B C31 H31 H34 0.1338 0.4567 0.5073 147 0.840 0.000 O34A C34 H34 H44A 0.0128 0.7153 1.1179 23 0.990 0.000 C44 N43 C45 H44B 0.0334 0.7205 1.3289 23 0.990 0.000 C44 N43 C45 H45A -0.0261 0.6460 1.4459 23 0.990 0.000 C45 N41 C44 H45B -0.0496 0.6653 1.2427 23 0.990 0.000 C45 N41 C44 H41 -0.0433 0.4696 1.2818 43 0.880 0.000 N41 C42 C45 H43 0.0683 0.5714 1.1779 43 0.880 0.000 N43 C42 C44 H52 0.2156 0.3509 0.8298 43 0.950 0.000 C52 C53 C51 H53 0.1622 0.2771 0.9500 43 0.950 0.000 C53 C52 C54 H51 0.1576 0.5658 0.9381 147 0.840 0.000 O51B C51 H51 H54 0.0735 0.3692 1.1052 147 0.840 0.000 O54B C54 H54 H62 0.3492 0.9757 0.5314 43 0.950 0.000 C62 C63 C61 H63 0.2925 0.9133 0.6390 43 0.950 0.000 C63 C62 C64 H61 0.3652 0.7105 0.4771 147 0.840 0.000 O61A C61 H61 H64 0.2575 0.6712 0.7249 147 0.840 0.000 O64B C64 H64 07skc0026p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.37280 0.14846 -0.05073 1.00000 0.02067 0.01701 0.02754 -0.00041 0.00235 0.00142 0.02170 0.01000 0.00018 0.00046 0.00080 0.00000 0.00297 0.00313 0.00326 0.00250 0.00250 0.00258 0.00129 C2 0.33647 0.09869 0.03878 1.00000 0.02126 0.01612 0.02902 0.00288 0.00291 -0.00062 0.02208 0.00999 0.00017 0.00047 0.00079 0.00000 0.00299 0.00301 0.00331 0.00245 0.00255 0.00249 0.00130 H2 0.33635 0.02167 0.04204 1.00000 0.02649 0.00000 0.00000 C3 0.30351 0.14722 0.11637 1.00000 0.01866 0.01899 0.02690 0.00146 0.00394 -0.00406 0.02142 0.00983 0.00017 0.00046 0.00078 0.00000 0.00286 0.00308 0.00324 0.00247 0.00246 0.00253 0.00129 H3 0.28355 0.09861 0.16626 1.00000 0.02570 0.00000 0.00000 C4 0.29271 0.26376 0.13808 1.00000 0.01692 0.01931 0.02434 -0.00256 -0.00203 -0.00154 0.02030 0.00931 0.00017 0.00045 0.00077 0.00000 0.00290 0.00312 0.00308 0.00248 0.00243 0.00255 0.00127 O1A 0.39903 0.08071 -0.11415 1.00000 0.02102 0.02125 0.04189 0.00033 0.00993 0.00214 0.02777 0.00738 0.00012 0.00032 0.00060 0.00000 0.00213 0.00223 0.00266 0.00195 0.00194 0.00184 0.00100 H1 0.41952 0.11422 -0.15841 1.00000 0.04165 0.00000 0.00000 O1B 0.37738 0.25049 -0.06302 1.00000 0.02113 0.02388 0.03456 0.00371 0.00782 0.00324 0.02630 0.00710 0.00012 0.00032 0.00055 0.00000 0.00206 0.00235 0.00244 0.00188 0.00175 0.00184 0.00095 O4A 0.31687 0.33968 0.07813 1.00000 0.02167 0.01654 0.03473 0.00226 0.01127 -0.00367 0.02397 0.00697 0.00012 0.00030 0.00057 0.00000 0.00212 0.00211 0.00242 0.00178 0.00185 0.00177 0.00094 H4 0.33791 0.31187 0.02822 1.00000 0.03596 0.00000 0.00000 O4B 0.25948 0.28623 0.21707 1.00000 0.02499 0.01984 0.02907 0.00135 0.00787 0.00195 0.02441 0.00688 0.00012 0.00031 0.00054 0.00000 0.00221 0.00217 0.00225 0.00178 0.00183 0.00181 0.00093 C22 0.52110 0.77181 0.25923 1.00000 0.01563 0.01898 0.02685 0.00211 0.00268 -0.00106 0.02043 0.00976 0.00017 0.00045 0.00079 0.00000 0.00278 0.00318 0.00309 0.00246 0.00234 0.00247 0.00125 C24 0.47730 0.62824 0.31647 1.00000 0.01584 0.02629 0.03558 -0.00074 0.00250 -0.00761 0.02586 0.01020 0.00017 0.00047 0.00087 0.00000 0.00287 0.00346 0.00354 0.00279 0.00256 0.00263 0.00138 H24A 0.45209 0.60308 0.23951 1.00000 0.03103 0.00000 0.00000 H24B 0.47461 0.60421 0.44726 1.00000 0.03103 0.00000 0.00000 C25 0.51906 0.58664 0.23775 1.00000 0.02645 0.02227 0.03323 -0.00420 0.00467 -0.00860 0.02721 0.01019 0.00018 0.00048 0.00087 0.00000 0.00329 0.00328 0.00360 0.00276 0.00281 0.00274 0.00143 H25A 0.53321 0.53258 0.32230 1.00000 0.03265 0.00000 0.00000 H25B 0.51385 0.55401 0.11231 1.00000 0.03265 0.00000 0.00000 N21 0.54423 0.68523 0.22856 1.00000 0.02008 0.01679 0.04233 -0.00046 0.01027 0.00074 0.02610 0.00863 0.00015 0.00037 0.00071 0.00000 0.00251 0.00269 0.00315 0.00228 0.00223 0.00214 0.00117 H21 0.57150 0.68682 0.20541 1.00000 0.03132 0.00000 0.00000 N23 0.48202 0.74523 0.30555 1.00000 0.02306 0.02225 0.04001 -0.00245 0.01408 -0.00040 0.02801 0.00871 0.00015 0.00039 0.00070 0.00000 0.00264 0.00279 0.00312 0.00234 0.00227 0.00225 0.00121 H23 0.46171 0.79218 0.32677 1.00000 0.03361 0.00000 0.00000 O22 0.53326 0.87107 0.24459 1.00000 0.02497 0.01827 0.03790 -0.00036 0.01032 0.00109 0.02675 0.00714 0.00012 0.00031 0.00058 0.00000 0.00216 0.00220 0.00251 0.00185 0.00184 0.00180 0.00096 C31 0.19861 0.49196 0.35742 1.00000 0.02488 0.02351 0.01957 0.00056 0.00113 -0.00001 0.02266 0.01025 0.00019 0.00047 0.00079 0.00000 0.00314 0.00334 0.00308 0.00252 0.00248 0.00277 0.00132 C32 0.18501 0.60735 0.37834 1.00000 0.01959 0.01981 0.03026 0.00630 0.00467 -0.00171 0.02310 0.01017 0.00017 0.00047 0.00080 0.00000 0.00299 0.00320 0.00343 0.00255 0.00257 0.00255 0.00135 H32 0.20342 0.66056 0.33037 1.00000 0.02772 0.00000 0.00000 C33 0.15027 0.64460 0.45598 1.00000 0.02278 0.01504 0.03712 -0.00015 0.00059 0.00107 0.02501 0.01021 0.00018 0.00047 0.00084 0.00000 0.00309 0.00305 0.00360 0.00260 0.00269 0.00258 0.00137 H33 0.14783 0.72137 0.45164 1.00000 0.03001 0.00000 0.00000 C34 0.11459 0.59112 0.54781 1.00000 0.01669 0.02290 0.02890 -0.00066 0.00197 0.00014 0.02280 0.00991 0.00017 0.00047 0.00081 0.00000 0.00296 0.00331 0.00342 0.00261 0.00253 0.00262 0.00133 O31A 0.17860 0.41288 0.40651 1.00000 0.02456 0.01613 0.03593 -0.00161 0.01164 -0.00163 0.02519 0.00697 0.00012 0.00031 0.00056 0.00000 0.00218 0.00218 0.00249 0.00183 0.00190 0.00184 0.00096 O31B 0.23499 0.48493 0.27468 1.00000 0.01831 0.02358 0.03883 -0.00141 0.01313 0.00294 0.02651 0.00742 0.00012 0.00032 0.00060 0.00000 0.00209 0.00226 0.00255 0.00197 0.00188 0.00181 0.00098 H31 0.24428 0.42115 0.28361 1.00000 0.03976 0.00000 0.00000 O34A 0.11211 0.48371 0.55354 1.00000 0.02157 0.02070 0.03922 0.00102 0.01163 0.00012 0.02681 0.00727 0.00012 0.00031 0.00059 0.00000 0.00218 0.00227 0.00268 0.00188 0.00195 0.00180 0.00100 H34 0.13377 0.45672 0.50731 1.00000 0.04022 0.00000 0.00000 O34B 0.08721 0.64588 0.61819 1.00000 0.02118 0.02653 0.04239 -0.00218 0.01073 0.00434 0.02972 0.00738 0.00012 0.00033 0.00060 0.00000 0.00216 0.00235 0.00263 0.00199 0.00193 0.00193 0.00101 C42 0.01642 0.48770 1.21804 1.00000 0.02018 0.02430 0.01641 0.00500 -0.00286 -0.00231 0.02043 0.00962 0.00017 0.00046 0.00075 0.00000 0.00309 0.00339 0.00302 0.00240 0.00240 0.00260 0.00130 C44 0.01789 0.67397 1.23548 1.00000 0.02095 0.02287 0.02893 0.00193 0.00736 0.00282 0.02404 0.01060 0.00017 0.00046 0.00084 0.00000 0.00305 0.00328 0.00328 0.00259 0.00256 0.00256 0.00134 H44A 0.01281 0.71533 1.11792 1.00000 0.02885 0.00000 0.00000 H44B 0.03342 0.72048 1.32890 1.00000 0.02885 0.00000 0.00000 C45 -0.02461 0.63186 1.31031 1.00000 0.02378 0.02451 0.02305 -0.00433 0.00442 0.00080 0.02367 0.01000 0.00018 0.00046 0.00081 0.00000 0.00308 0.00333 0.00311 0.00256 0.00250 0.00268 0.00133 H45A -0.02610 0.64597 1.44593 1.00000 0.02841 0.00000 0.00000 H45B -0.04961 0.66533 1.24271 1.00000 0.02841 0.00000 0.00000 N41 -0.02207 0.51536 1.27128 1.00000 0.01763 0.02686 0.03722 0.00005 0.01024 -0.00353 0.02693 0.00883 0.00015 0.00040 0.00070 0.00000 0.00251 0.00291 0.00314 0.00233 0.00224 0.00221 0.00120 H41 -0.04332 0.46956 1.28177 1.00000 0.03232 0.00000 0.00000 N43 0.04119 0.57409 1.20355 1.00000 0.01515 0.01591 0.03398 0.00221 0.00808 0.00216 0.02144 0.00827 0.00014 0.00035 0.00067 0.00000 0.00231 0.00257 0.00289 0.00213 0.00204 0.00204 0.00110 H43 0.06830 0.57141 1.17789 1.00000 0.02573 0.00000 0.00000 O42 0.02677 0.38923 1.18723 1.00000 0.02253 0.01642 0.03632 -0.00225 0.00852 -0.00079 0.02485 0.00674 0.00012 0.00030 0.00055 0.00000 0.00210 0.00216 0.00248 0.00178 0.00183 0.00175 0.00095 C51 0.20532 0.51671 0.84400 1.00000 0.01740 0.02725 0.01846 0.00010 0.00098 0.00395 0.02103 0.01002 0.00017 0.00047 0.00078 0.00000 0.00302 0.00335 0.00296 0.00252 0.00241 0.00264 0.00129 C52 0.19495 0.40035 0.87192 1.00000 0.02696 0.01573 0.03099 0.00006 0.01178 0.00706 0.02420 0.01054 0.00019 0.00046 0.00081 0.00000 0.00321 0.00307 0.00345 0.00250 0.00269 0.00262 0.00137 H52 0.21560 0.35093 0.82976 1.00000 0.02904 0.00000 0.00000 C53 0.16143 0.35414 0.94640 1.00000 0.03004 0.01234 0.02783 -0.00049 0.00620 0.00637 0.02324 0.01031 0.00018 0.00046 0.00079 0.00000 0.00334 0.00289 0.00330 0.00242 0.00270 0.00260 0.00134 H53 0.16220 0.27714 0.94997 1.00000 0.02789 0.00000 0.00000 C54 0.12293 0.40358 1.02502 1.00000 0.01963 0.02314 0.02465 -0.00078 -0.00077 -0.00172 0.02254 0.01000 0.00018 0.00048 0.00081 0.00000 0.00294 0.00341 0.00315 0.00252 0.00246 0.00264 0.00132 O51A 0.23829 0.53961 0.76772 1.00000 0.01899 0.02840 0.03199 0.00040 0.00726 0.00229 0.02625 0.00711 0.00012 0.00032 0.00057 0.00000 0.00214 0.00235 0.00242 0.00191 0.00185 0.00186 0.00096 O51B 0.17965 0.59377 0.89695 1.00000 0.02003 0.01366 0.03335 -0.00176 0.00900 0.00050 0.02208 0.00680 0.00012 0.00029 0.00056 0.00000 0.00207 0.00203 0.00240 0.00173 0.00180 0.00171 0.00092 H51 0.15759 0.56585 0.93814 1.00000 0.03312 0.00000 0.00000 O54A 0.11834 0.50539 1.03351 1.00000 0.02162 0.01807 0.03401 0.00002 0.00796 0.00306 0.02434 0.00692 0.00012 0.00031 0.00056 0.00000 0.00214 0.00223 0.00248 0.00177 0.00181 0.00174 0.00095 O54B 0.09614 0.33652 1.08190 1.00000 0.02016 0.01962 0.04863 0.00331 0.01111 0.00122 0.02915 0.00753 0.00012 0.00032 0.00062 0.00000 0.00213 0.00224 0.00279 0.00198 0.00201 0.00184 0.00103 H54 0.07353 0.36919 1.10516 1.00000 0.04372 0.00000 0.00000 C61 0.38551 0.84485 0.45547 1.00000 0.01907 0.02507 0.02561 0.00214 -0.00458 0.00222 0.02345 0.01007 0.00018 0.00049 0.00080 0.00000 0.00305 0.00337 0.00328 0.00261 0.00251 0.00272 0.00135 C62 0.34773 0.89876 0.53249 1.00000 0.02135 0.02073 0.03415 -0.00005 0.00697 0.00351 0.02522 0.01058 0.00018 0.00049 0.00083 0.00000 0.00308 0.00325 0.00353 0.00264 0.00266 0.00263 0.00138 H62 0.34922 0.97571 0.53144 1.00000 0.03026 0.00000 0.00000 C63 0.31241 0.86026 0.60230 1.00000 0.02829 0.01744 0.02310 -0.00682 0.00519 0.00935 0.02281 0.00998 0.00018 0.00046 0.00077 0.00000 0.00330 0.00310 0.00313 0.00242 0.00259 0.00261 0.00134 H63 0.29252 0.91325 0.63904 1.00000 0.02737 0.00000 0.00000 C64 0.29968 0.74530 0.63093 1.00000 0.01317 0.02891 0.02365 0.00339 0.00361 -0.00142 0.02182 0.00990 0.00017 0.00048 0.00077 0.00000 0.00271 0.00348 0.00310 0.00263 0.00229 0.00271 0.00130 O61A 0.38847 0.73816 0.44933 1.00000 0.02489 0.02615 0.05356 -0.00348 0.01544 0.00308 0.03440 0.00785 0.00013 0.00033 0.00065 0.00000 0.00228 0.00249 0.00301 0.00216 0.00218 0.00197 0.00110 H61 0.36517 0.71050 0.47712 1.00000 0.05161 0.00000 0.00000 O61B 0.41391 0.90136 0.39847 1.00000 0.02957 0.03009 0.05256 -0.00119 0.01707 -0.00814 0.03689 0.00789 0.00014 0.00035 0.00065 0.00000 0.00244 0.00256 0.00303 0.00222 0.00220 0.00213 0.00114 O64A 0.32100 0.66620 0.58692 1.00000 0.02379 0.02156 0.04448 -0.00383 0.01231 0.00108 0.02958 0.00728 0.00012 0.00032 0.00060 0.00000 0.00222 0.00233 0.00274 0.00196 0.00200 0.00192 0.00103 O64B 0.26279 0.73683 0.70529 1.00000 0.02067 0.01828 0.03958 -0.00183 0.00899 0.00075 0.02592 0.00722 0.00012 0.00031 0.00060 0.00000 0.00209 0.00213 0.00250 0.00194 0.00182 0.00179 0.00095 H64 0.25749 0.67116 0.72493 1.00000 0.03888 0.00000 0.00000 Final Structure Factor Calculation for 07skc0026p21c in P2(1)/c Total number of l.s. parameters = 405 Maximum vector length = 511 Memory required = 4547 / 22995 wR2 = 0.2044 before cycle 9 for 4829 data and 0 / 405 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 17.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0990 for 2884 Fo > 4sig(Fo) and 0.1648 for all 4829 data wR2 = 0.2044, GooF = S = 1.058, Restrained GooF = 1.058 for all data Occupancy sum of asymmetric unit = 44.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0277 0.0210 0.0165 C1 0.0298 0.0211 0.0153 C2 0.0276 0.0227 0.0139 C3 0.0262 0.0200 0.0148 C4 0.0444 0.0221 0.0168 O1A 0.0382 0.0229 0.0177 O1B 0.0395 0.0206 0.0118 O4A 0.0338 0.0205 0.0189 O4B 0.0275 0.0190 0.0148 C22 0.0357 0.0301 0.0118 C24 0.0380 0.0282 0.0155 C25 0.0449 0.0176 0.0158 N21 0.0462 0.0221 0.0157 N23 0.0418 0.0207 0.0177 O22 0.0249 0.0236 0.0195 C31 0.0335 0.0212 0.0146 C32 0.0372 0.0229 0.0149 C33 0.0290 0.0228 0.0166 C34 0.0415 0.0183 0.0158 O31A 0.0435 0.0245 0.0115 O31B 0.0433 0.0207 0.0164 O34A 0.0453 0.0286 0.0152 O34B 0.0287 0.0194 0.0132 C42 0.0328 0.0224 0.0169 C44 0.0286 0.0248 0.0177 C45 0.0403 0.0276 0.0130 N41 0.0362 0.0161 0.0121 N43 0.0391 0.0192 0.0162 O42 0.0286 0.0185 0.0160 C51 0.0398 0.0220 0.0108 C52 0.0346 0.0252 0.0100 C53 0.0254 0.0238 0.0184 C54 0.0342 0.0285 0.0160 O51A 0.0365 0.0167 0.0131 O51B 0.0366 0.0211 0.0154 O54A 0.0513 0.0192 0.0168 O54B 0.0294 0.0258 0.0152 C61 0.0360 0.0233 0.0164 C62 0.0337 0.0271 0.0076 C63 0.0306 0.0228 0.0121 C64 0.0583 0.0280 0.0169 O61A 0.0599 0.0333 0.0175 O61B 0.0487 0.0228 0.0172 O64A 0.0419 0.0193 0.0166 O64B Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.002 0.004 0.007 0.009 0.012 0.015 0.020 0.027 0.042 1.000 Number in group 492. 486. 685. 394. 485. 375. 530. 441. 460. 481. GooF 1.143 1.093 1.107 1.083 1.071 0.961 1.034 1.002 1.032 0.997 K 25.197 3.947 1.801 1.258 1.188 1.044 1.017 1.012 0.994 1.001 Resolution(A) 0.84 0.87 0.90 0.95 1.00 1.06 1.14 1.26 1.43 1.79 inf Number in group 489. 480. 481. 490. 479. 482. 483. 477. 484. 484. GooF 1.135 1.187 1.140 1.062 1.091 1.155 0.953 0.933 0.975 0.902 K 1.162 1.180 1.123 1.019 1.034 0.996 0.991 1.021 1.015 0.996 R1 0.344 0.325 0.270 0.207 0.172 0.153 0.136 0.116 0.079 0.053 Recommended weighting scheme: WGHT 0.0000 17.6961 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) -18 8 2 3033.30 5711.83 6.07 0.090 1.11 13 4 5 395.42 1135.35 5.20 0.040 1.12 11 6 2 653.81 1473.33 4.65 0.046 1.49 -14 12 2 34.27 479.87 4.22 0.026 0.91 -18 9 2 552.38 1215.26 4.11 0.042 1.04 14 11 2 252.06 694.46 3.95 0.032 0.96 16 0 6 322.11 1001.50 3.49 0.038 1.00 21 9 2 283.06 20.90 3.46 0.005 0.96 -28 2 5 253.52 16.73 3.43 0.005 0.89 33 0 0 396.13 113.94 3.18 0.013 0.95 27 10 0 -32.58 137.32 3.14 0.014 0.85 30 6 0 268.95 5.12 3.13 0.003 0.93 6 3 8 223.57 3.24 3.09 0.002 0.85 -6 1 7 214.12 20.98 3.08 0.005 1.01 -15 10 4 443.41 862.81 3.07 0.035 0.92 0 8 0 20300.01 16980.83 3.06 0.156 1.54 -20 7 2 511.95 952.96 3.05 0.037 1.13 -14 0 6 453.01 863.85 3.04 0.035 1.08 -16 9 4 195.96 0.09 3.02 0.000 0.96 21 4 4 173.99 28.94 3.01 0.006 1.05 20 4 4 41.32 215.05 2.98 0.018 1.08 10 8 6 431.66 161.03 2.94 0.015 0.89 9 2 7 229.83 24.70 2.92 0.006 0.96 19 11 3 213.75 0.00 2.92 0.000 0.86 29 6 2 330.41 82.43 2.92 0.011 0.91 10 9 0 610.64 1032.14 2.91 0.038 1.26 -6 2 7 1131.03 670.75 2.90 0.031 1.00 -29 0 4 440.67 7.04 2.90 0.003 0.95 -9 7 7 193.72 2.10 2.87 0.002 0.87 -7 9 4 104.90 4.85 2.85 0.003 1.06 -7 2 6 -44.87 104.37 2.83 0.012 1.15 -10 8 6 422.85 800.44 2.81 0.034 0.91 14 13 0 32.21 269.06 2.79 0.020 0.87 22 4 6 463.05 195.29 2.79 0.017 0.86 9 13 0 347.47 4.84 2.79 0.003 0.92 14 10 2 160.36 1.38 2.78 0.001 1.03 7 1 8 187.97 18.18 2.77 0.005 0.87 -21 10 2 -2.16 199.32 2.76 0.017 0.93 -16 9 3 358.43 708.49 2.76 0.032 1.03 6 14 2 166.46 6.02 2.74 0.003 0.84 -22 2 7 62.23 329.55 2.71 0.022 0.84 -13 1 6 455.59 211.60 2.69 0.017 1.09 -28 1 2 302.21 6.75 2.66 0.003 1.08 -10 6 3 78.58 0.31 2.65 0.001 1.41 14 9 3 134.84 8.77 2.65 0.004 1.04 13 2 6 -58.40 71.90 2.65 0.010 1.03 7 3 8 277.78 74.08 2.64 0.010 0.85 17 4 3 125.27 387.17 2.63 0.024 1.29 3 8 7 184.18 446.79 2.63 0.025 0.85 -5 10 5 187.72 16.28 2.63 0.005 0.93 Bond lengths and angles C1 - Distance Angles O1B 1.2699 (0.0066) O1A 1.2729 (0.0066) 123.23 (0.51) C2 1.4706 (0.0077) 122.46 (0.51) 114.32 (0.50) C1 - O1B O1A C2 - Distance Angles C3 1.3401 (0.0077) C1 1.4706 (0.0077) 128.81 (0.54) H2 0.9500 115.60 115.60 C2 - C3 C1 C3 - Distance Angles C2 1.3401 (0.0077) C4 1.4865 (0.0078) 131.31 (0.53) H3 0.9500 114.35 114.35 C3 - C2 C4 C4 - Distance Angles O4B 1.2428 (0.0063) O4A 1.2920 (0.0064) 120.69 (0.51) C3 1.4865 (0.0078) 117.66 (0.49) 121.65 (0.49) C4 - O4B O4A O1A - Distance Angles C1 1.2729 (0.0066) H1 0.8400 109.47 O1A - C1 O1B - Distance Angles C1 1.2699 (0.0066) O1B - O4A - Distance Angles C4 1.2920 (0.0064) H4 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2428 (0.0063) O4B - C22 - Distance Angles O22 1.2879 (0.0065) N21 1.3158 (0.0070) 126.11 (0.49) N23 1.3280 (0.0070) 122.41 (0.51) 111.46 (0.49) C22 - O22 N21 C24 - Distance Angles N23 1.4527 (0.0074) C25 1.5411 (0.0076) 102.70 (0.43) H24A 0.9900 111.23 111.23 H24B 0.9900 111.23 111.23 109.14 C24 - N23 C25 H24A C25 - Distance Angles N21 1.4530 (0.0071) C24 1.5411 (0.0076) 102.28 (0.46) H25A 0.9900 111.31 111.31 H25B 0.9900 111.31 111.31 109.20 C25 - N21 C24 H25A N21 - Distance Angles C22 1.3158 (0.0070) C25 1.4530 (0.0071) 111.44 (0.46) H21 0.8800 124.28 124.28 N21 - C22 C25 N23 - Distance Angles C22 1.3280 (0.0070) C24 1.4527 (0.0074) 110.89 (0.46) H23 0.8800 124.55 124.55 N23 - C22 C24 O22 - Distance Angles C22 1.2879 (0.0065) O22 - C31 - Distance Angles O31A 1.2213 (0.0066) O31B 1.3159 (0.0068) 123.21 (0.53) C32 1.4951 (0.0080) 125.27 (0.52) 111.50 (0.49) C31 - O31A O31B C32 - Distance Angles C33 1.3310 (0.0078) C31 1.4951 (0.0080) 127.91 (0.54) H32 0.9500 116.05 116.05 C32 - C33 C31 C33 - Distance Angles C32 1.3310 (0.0078) C34 1.4821 (0.0079) 133.28 (0.56) H33 0.9500 113.36 113.36 C33 - C32 C34 C34 - Distance Angles O34B 1.2219 (0.0066) O34A 1.3274 (0.0067) 119.68 (0.51) C33 1.4821 (0.0079) 120.03 (0.53) 120.30 (0.50) C34 - O34B O34A O31A - Distance Angles C31 1.2213 (0.0066) O31A - O31B - Distance Angles C31 1.3159 (0.0068) H31 0.8400 109.47 O31B - C31 O34A - Distance Angles C34 1.3274 (0.0067) H34 0.8400 109.47 O34A - C34 O34B - Distance Angles C34 1.2219 (0.0066) O34B - C42 - Distance Angles O42 1.2791 (0.0067) N43 1.3259 (0.0070) 126.45 (0.50) N41 1.3295 (0.0071) 122.37 (0.51) 111.18 (0.51) C42 - O42 N43 C44 - Distance Angles N43 1.4564 (0.0070) C45 1.5523 (0.0073) 102.63 (0.44) H44A 0.9900 111.24 111.24 H44B 0.9900 111.24 111.24 109.15 C44 - N43 C45 H44A C45 - Distance Angles N41 1.4664 (0.0073) C44 1.5523 (0.0073) 101.86 (0.43) H45A 0.9900 111.40 111.40 H45B 0.9900 111.40 111.40 109.26 C45 - N41 C44 H45A N41 - Distance Angles C42 1.3295 (0.0071) C45 1.4664 (0.0073) 111.42 (0.46) H41 0.8800 124.29 124.29 N41 - C42 C45 N43 - Distance Angles C42 1.3259 (0.0070) C44 1.4564 (0.0070) 111.47 (0.45) H43 0.8800 124.27 124.27 N43 - C42 C44 O42 - Distance Angles C42 1.2791 (0.0067) O42 - C51 - Distance Angles O51A 1.2276 (0.0065) O51B 1.3142 (0.0065) 120.35 (0.52) C52 1.4870 (0.0080) 118.50 (0.50) 121.14 (0.49) C51 - O51A O51B C52 - Distance Angles C53 1.3316 (0.0078) C51 1.4870 (0.0080) 130.51 (0.53) H52 0.9500 114.74 114.74 C52 - C53 C51 C53 - Distance Angles C52 1.3316 (0.0078) C54 1.4895 (0.0078) 130.47 (0.55) H53 0.9500 114.76 114.76 C53 - C52 C54 C54 - Distance Angles O54B 1.2616 (0.0068) O54A 1.2654 (0.0067) 123.74 (0.53) C53 1.4895 (0.0078) 114.88 (0.52) 121.38 (0.52) C54 - O54B O54A O51A - Distance Angles C51 1.2276 (0.0065) O51A - O51B - Distance Angles C51 1.3142 (0.0065) H51 0.8400 109.47 O51B - C51 O54A - Distance Angles C54 1.2654 (0.0067) O54A - O54B - Distance Angles C54 1.2616 (0.0068) H54 0.8400 109.47 O54B - C54 C61 - Distance Angles O61B 1.2182 (0.0068) O61A 1.3197 (0.0069) 120.34 (0.54) C62 1.4897 (0.0079) 118.60 (0.55) 121.06 (0.52) C61 - O61B O61A C62 - Distance Angles C63 1.3271 (0.0078) C61 1.4897 (0.0079) 132.53 (0.57) H62 0.9500 113.73 113.73 C62 - C63 C61 C63 - Distance Angles C62 1.3271 (0.0079) C64 1.4899 (0.0080) 128.85 (0.53) H63 0.9500 115.58 115.58 C63 - C62 C64 C64 - Distance Angles O64A 1.2328 (0.0066) O64B 1.3030 (0.0063) 123.12 (0.52) C63 1.4899 (0.0080) 124.38 (0.49) 112.49 (0.49) C64 - O64A O64B O61A - Distance Angles C61 1.3197 (0.0069) H61 0.8400 109.47 O61A - C61 O61B - Distance Angles C61 1.2182 (0.0068) O61B - O64A - Distance Angles C64 1.2328 (0.0066) O64A - O64B - Distance Angles C64 1.3030 (0.0064) H64 0.8400 109.47 O64B - C64 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.62 2.456(5) 176.2 O4A-H4...O1B 0.88 2.10 2.977(6) 175.8 N23-H23...O61B 0.88 2.59 3.162(6) 123.6 N23-H23...O61A 0.84 1.80 2.607(5) 160.0 O31B-H31...O4B 0.84 1.70 2.540(5) 175.1 O34A-H34...O31A 0.88 2.09 2.892(6) 151.3 N43-H43...O54A 0.84 1.62 2.457(5) 174.0 O51B-H51...O54A 0.84 1.63 2.429(5) 158.6 O54B-H54...O42 0.84 1.72 2.541(6) 166.0 O61A-H61...O64A 0.84 1.76 2.596(6) 171.4 O64B-H64...O51A 0.84 1.64 2.438(5) 156.6 O1A-H1...O22_$1 0.88 2.09 2.896(6) 151.3 N21-H21...O1B_$1 0.88 2.13 2.987(6) 164.5 N41-H41...O34B_$2 0.88 2.58 3.150(6) 123.5 N41-H41...O34A_$2 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 12.8165 (0.2800) x - 0.0114 (0.0626) y + 6.3753 (0.0320) z = 7.8350 (0.0669) * 0.0000 (0.0000) C61 * 0.0000 (0.0000) O61A * 0.0000 (0.0000) O61B Rms deviation of fitted atoms = 0.0000 12.8592 (0.1363) x - 0.0782 (0.1211) y + 6.3703 (0.0151) z = 7.8145 (0.1117) Angle to previous plane (with approximate esd) = 0.32 ( 0.86 ) * 0.0000 (0.0000) C64 * 0.0000 (0.0000) O64A * 0.0000 (0.0000) O64B Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 3 17 GRID -3.571 -1 -2 3.571 1 2 R1 = 0.1647 for 4829 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.35 at 0.0623 0.5456 0.1231 [ 0.53 A from H43 ] Deepest hole -0.36 at 0.4955 0.1733 0.2426 [ 1.12 A from C24 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 4973 / 37951 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0623 0.5456 1.1231 1.00000 0.05 0.35 0.53 H43 0.97 N43 1.77 C42 1.97 O54A Q2 1 0.1702 0.3725 0.8560 1.00000 0.05 0.33 0.75 C53 0.85 C52 1.38 H53 1.47 H52 Q3 1 0.3174 0.7953 0.6650 1.00000 0.05 0.33 0.86 C64 0.93 C63 1.66 H63 1.69 O64A Q4 1 0.0995 0.2049 0.9473 1.00000 0.05 0.32 1.89 O54B 2.16 H53 2.29 H34 2.47 O34A Q5 1 0.5600 0.6925 0.1130 1.00000 0.05 0.31 0.74 H21 0.99 N21 1.92 C22 2.07 C25 Q6 1 -0.0066 0.3810 1.1332 1.00000 0.05 0.30 1.10 O42 1.60 C42 1.94 H41 2.00 N41 Q7 1 0.5402 0.5965 0.4246 1.00000 0.05 0.30 1.09 H25A 1.47 C25 1.79 N21 2.06 H1 Q8 1 0.0695 0.6632 1.1328 1.00000 0.05 0.30 1.18 H43 1.52 N43 1.82 C44 1.89 H44A Q9 1 0.3973 1.0796 0.4825 1.00000 0.05 0.30 2.02 H62 2.16 H21 2.21 O1B 2.33 H4 Q10 1 0.0625 0.5960 0.4996 1.00000 0.05 0.30 1.28 O34B 1.65 C34 1.89 H41 2.11 O34A Shortest distances between peaks (including symmetry equivalents) 1 8 1.47 5 9 2.07 1 6 2.63 5 7 2.63 6 8 2.73 1 10 2.77 8 10 2.77 1 6 2.97 5 7 2.98 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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. 0.97: 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 3.47: Structure factors and derivatives 10.34: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 1.13: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.23: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0026p21c finished at 14:07:20 Total CPU time: 16.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++