+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0062p21n started at 16:04:43 on 06-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0062p21n in P2(1)/n CELL 0.71073 9.2008 23.6311 10.4061 90.000 95.173 90.000 ZERR 8.00 0.0003 0.0010 0.0004 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 88 104 8 32 V = 2253.33 F(000) = 944.0 Mu = 0.10 mm-1 Cell Wt = 1785.79 Rho = 1.316 MERG 2 OMIT -3.00 55.00 OMIT 0 2 0 OMIT 0 1 1 OMIT 1 2 0 OMIT 1 1 1 OMIT -2 0 2 OMIT 0 4 0 OMIT 1 3 0 EXTI 0.00392 SHEL 7 0.77 EQIV_$6 x+1, y, z-1 HTAB O34A O1B_$6 HTAB O34A O1A_$6 HTAB N24 O4B HTAB N24 O31B HTAB O31A O4B HTAB O31A O4A HTAB N44 O4A EQIV_$1 x-1, y, z HTAB N24 O34B_$1 EQIV_$2 -x, -y, -z+1 HTAB N24 O1A_$2 EQIV_$3 -x+1, -y, -z+1 HTAB N44 O1B_$3 EQIV_$4 -x+2, -y, -z HTAB N44 O34B_$4 EQIV_$5 -x+1, -y, -z HTAB N44 O31B_$5 FMAP 2 PLAN 10 SIZE 0.04 0.18 0.32 ACTA BOND $H WGHT 0.04950 1.07770 L.S. 4 TEMP -13.00 FVAR 0.41698 MOLE 1 C1 1 0.114108 -0.003701 0.619651 11.00000 0.01490 0.02608 = 0.01369 -0.00215 -0.00155 0.00162 C2 1 0.230041 -0.000108 0.529081 11.00000 0.01589 0.02479 = 0.01652 0.00144 0.00146 -0.00174 AFIX 43 H2 2 0.274755 0.034695 0.518845 11.00000 -1.20000 AFIX 0 C3 1 0.272637 -0.043386 0.462848 11.00000 0.01811 0.02358 = 0.01900 0.00319 0.00230 -0.00196 AFIX 43 H3 2 0.226505 -0.078049 0.471028 11.00000 -1.20000 AFIX 0 C4 1 0.391405 -0.039442 0.375302 11.00000 0.01874 0.02671 = 0.01524 0.00168 -0.00215 -0.00176 O1A 4 0.047741 -0.048295 0.634364 11.00000 0.01933 0.02584 = 0.02541 0.00084 0.00495 -0.00417 O1B 4 0.090858 0.043731 0.676362 11.00000 0.01723 0.03119 = 0.02042 -0.00316 0.00924 -0.00192 AFIX 147 H1 2 0.027797 0.039267 0.726317 10.50000 -1.50000 AFIX 0 O4A 4 0.455702 -0.082685 0.344191 11.00000 0.02704 0.02491 = 0.02962 -0.00045 0.00894 0.00479 O4B 4 0.418837 0.011368 0.338958 11.00000 0.01597 0.02662 = 0.02225 0.00263 0.00992 0.00067 AFIX 147 H4 2 0.489667 0.010970 0.296454 10.50000 -1.50000 AFIX 0 MOLE 2 C21 1 0.270522 0.251170 0.307483 11.00000 0.05110 0.02502 = 0.04782 -0.00424 0.01002 -0.00359 C22 1 0.356765 0.208495 0.364752 11.00000 0.03986 0.03868 = 0.05150 -0.01649 -0.00678 -0.00804 AFIX 43 H22 2 0.436273 0.218121 0.422155 11.00000 -1.20000 AFIX 0 C23 1 0.328091 0.151902 0.339053 11.00000 0.02944 0.02771 = 0.04754 -0.00619 -0.00429 0.00029 AFIX 43 H23 2 0.387607 0.123826 0.378083 11.00000 -1.20000 AFIX 0 C24 1 0.210138 0.138103 0.254871 11.00000 0.02145 0.02084 = 0.02506 -0.00220 0.00909 -0.00385 C25 1 0.121049 0.179312 0.198385 11.00000 0.03436 0.02943 = 0.03979 -0.00029 -0.00529 0.00243 AFIX 43 H25 2 0.040716 0.169517 0.142098 11.00000 -1.20000 AFIX 0 C26 1 0.151499 0.235485 0.225701 11.00000 0.05057 0.02767 = 0.04795 -0.00084 -0.00040 0.00562 AFIX 43 H26 2 0.090205 0.263322 0.187988 11.00000 -1.20000 AFIX 0 C27 1 0.305492 0.312749 0.335673 11.00000 0.08594 0.02787 = 0.08908 -0.01299 0.00853 -0.00854 AFIX 137 H27A 2 0.286823 0.321333 0.422844 11.00000 -1.50000 H27B 2 0.245422 0.336243 0.277347 11.00000 -1.50000 H27C 2 0.406415 0.319734 0.324711 11.00000 -1.50000 AFIX 0 N24 3 0.177991 0.078445 0.225448 11.00000 0.01847 0.02486 = 0.02358 -0.00119 0.00422 -0.00063 AFIX 137 H24A 2 0.257551 0.057724 0.245659 11.00000 0.03774 H24B 2 0.150384 0.074739 0.141681 11.00000 0.04665 H24C 2 0.106536 0.066683 0.271154 11.00000 0.04675 AFIX 0 MOLE 3 C31 1 0.571500 0.048887 0.090910 11.00000 0.02089 0.01656 = 0.01676 -0.00283 0.00261 -0.00574 C32 1 0.681511 0.053869 -0.004370 11.00000 0.02136 0.01960 = 0.01614 0.00141 0.00204 0.00118 AFIX 43 H32 2 0.648845 0.058418 -0.090956 11.00000 -1.20000 AFIX 0 C33 1 0.823551 0.052152 0.027925 11.00000 0.02289 0.01773 = 0.01372 0.00008 0.00231 0.00011 AFIX 43 H33 2 0.855820 0.047722 0.114631 11.00000 -1.20000 AFIX 0 C34 1 0.934591 0.056904 -0.066563 11.00000 0.02253 0.01476 = 0.01867 0.00240 0.00419 0.00382 O31A 4 0.617238 0.023367 0.196557 11.00000 0.01633 0.03208 = 0.01933 0.00653 0.00784 0.00073 AFIX 147 H31 2 0.547866 0.016629 0.238395 10.50000 -1.50000 AFIX 0 O31B 4 0.446340 0.067662 0.066900 11.00000 0.01539 0.02834 = 0.02545 0.00353 0.00284 0.00371 O34A 4 0.888572 0.043813 -0.183641 11.00000 0.01773 0.03108 = 0.01678 -0.00130 0.00479 -0.00125 AFIX 147 H34 2 0.955791 0.046703 -0.229883 10.50000 -1.50000 AFIX 0 O34B 4 1.061453 0.071412 -0.031559 11.00000 0.01513 0.03002 = 0.02465 -0.00086 0.00183 -0.00253 MOLE 4 C41 1 0.755204 -0.275142 0.211009 11.00000 0.03606 0.02436 = 0.04608 0.00304 0.00794 0.00343 C42 1 0.791993 -0.239095 0.313066 11.00000 0.05463 0.03118 = 0.04213 0.01157 -0.00603 0.00743 AFIX 43 H42 2 0.835114 -0.253743 0.390251 11.00000 -1.20000 AFIX 0 C43 1 0.765844 -0.181439 0.302638 11.00000 0.05407 0.02864 = 0.02959 -0.00033 -0.00602 0.00425 AFIX 43 H43 2 0.791413 -0.157615 0.372155 11.00000 -1.20000 AFIX 0 C44 1 0.701941 -0.159814 0.188933 11.00000 0.01940 0.01707 = 0.02921 0.00131 0.00613 0.00041 C45 1 0.664536 -0.194635 0.086049 11.00000 0.04697 0.02903 = 0.03071 -0.00006 -0.00393 0.00082 AFIX 43 H45 2 0.621445 -0.179892 0.008949 11.00000 -1.20000 AFIX 0 C46 1 0.691733 -0.252046 0.098385 11.00000 0.05875 0.02537 = 0.04371 -0.00890 0.00163 0.00209 AFIX 43 H46 2 0.666350 -0.275681 0.028490 11.00000 -1.20000 AFIX 0 C47 1 0.782471 -0.337857 0.223151 11.00000 0.05971 0.02582 = 0.07958 0.00917 0.01011 0.00464 AFIX 137 H47A 2 0.691802 -0.357825 0.206983 11.00000 -1.50000 H47B 2 0.824773 -0.346324 0.308703 11.00000 -1.50000 H47C 2 0.848214 -0.349386 0.161505 11.00000 -1.50000 AFIX 0 N44 3 0.670909 -0.099108 0.180112 11.00000 0.01912 0.02323 = 0.02575 0.00039 0.00306 0.00147 AFIX 137 H44A 2 0.751789 -0.079726 0.204025 11.00000 -1.50000 H44B 2 0.602250 -0.090414 0.231820 11.00000 -1.50000 H44C 2 0.639821 -0.090278 0.099126 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0062p21n in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C3 C1 C3 - C2 C4 C4 - O4A O4B C3 O1A - C1 O1B - C1 O4A - C4 O4B - C4 C21 - C26 C22 C27 C22 - C21 C23 C23 - C24 C22 C24 - C25 C23 N24 C25 - C24 C26 C26 - C21 C25 C27 - C21 N24 - C24 C31 - O31B O31A C32 C32 - C33 C31 C33 - C32 C34 C34 - O34B O34A C33 O31A - C31 O31B - C31 O34A - C34 O34B - C34 C41 - C46 C42 C47 C42 - C41 C43 C43 - C44 C42 C44 - C45 C43 N44 C45 - C44 C46 C46 - C41 C45 C47 - C41 N44 - C44 Operators for generating equivalent atoms: $1 x-1, y, z $2 -x, -y, -z+1 $3 -x+1, -y, -z+1 $4 -x+2, -y, -z $5 -x+1, -y, -z $6 x+1, y, z-1 h k l Fo^2 Sigma Why rejected 1 0 2 28.92 6.89 observed but should be systematically absent 22674 Reflections read, of which 430 rejected -10 =< h =< 10, -24 =< k =< 26, -11 =< l =< 11, Max. 2-theta = 46.54 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -1 23 5 71.48 16.20 2 95.50 2 9 7 17.35 3.15 6 17.69 2 10 7 46.11 16.19 2 123.36 4 9 8 32.40 21.96 2 155.12 3 13 8 11.06 5.65 4 39.07 -2 16 8 68.94 6.02 5 33.48 6 Inconsistent equivalents 3232 Unique reflections, of which 0 suppressed R(int) = 0.0796 R(sigma) = 0.0560 Friedel opposites merged Maximum memory for data reduction = 3324 / 32271 Default effective X-H distances for T = -13.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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 = 4156 / 376670 wR2 = 0.1098 before cycle 1 for 3232 data and 301 / 301 parameters GooF = S = 1.012; Restrained GooF = 1.012 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 1.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41869 0.00102 1.684 OSF 2 0.00405 0.00084 0.156 EXTI 67 0.41944 0.00016 3.741 x O4B 190 0.61673 0.00016 -3.196 x O31A Mean shift/esd = 0.329 Maximum = 3.741 for x O4B Max. shift = 0.061 A for H31 Max. dU = 0.002 for H24B Least-squares cycle 2 Maximum vector length = 511 Memory required = 4156 / 376670 wR2 = 0.1068 before cycle 2 for 3232 data and 301 / 301 parameters GooF = S = 0.985; Restrained GooF = 0.985 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 1.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41917 0.00099 0.479 OSF 2 0.00409 0.00082 0.044 EXTI Mean shift/esd = 0.111 Maximum = 1.320 for x O4B Max. shift = 0.010 A for H31 Max. dU = 0.001 for H24B Least-squares cycle 3 Maximum vector length = 511 Memory required = 4156 / 376670 wR2 = 0.1067 before cycle 3 for 3232 data and 301 / 301 parameters GooF = S = 0.983; Restrained GooF = 0.983 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 1.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41918 0.00099 0.011 OSF 2 0.00409 0.00082 0.003 EXTI Mean shift/esd = 0.006 Maximum = -0.103 for tors H27A Max. shift = 0.002 A for H27C Max. dU = 0.000 for H24A Least-squares cycle 4 Maximum vector length = 511 Memory required = 4156 / 376670 wR2 = 0.1067 before cycle 4 for 3232 data and 301 / 301 parameters GooF = S = 0.983; Restrained GooF = 0.983 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 1.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41918 0.00099 0.002 OSF 2 0.00409 0.00082 0.000 EXTI Mean shift/esd = 0.002 Maximum = -0.046 for tors H27A Max. shift = 0.001 A for H27C Max. dU = 0.000 for H24C No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.2750 0.0346 0.5188 43 0.930 0.000 C2 C3 C1 H3 0.2263 -0.0781 0.4710 43 0.930 0.000 C3 C2 C4 H1 0.0275 0.0391 0.7270 147 0.820 0.000 O1B C1 H1 H4 0.4875 0.0106 0.2927 147 0.820 0.000 O4B C4 H4 H22 0.4365 0.2182 0.4220 43 0.930 0.000 C22 C21 C23 H23 0.3874 0.1238 0.3782 43 0.930 0.000 C23 C24 C22 H25 0.0409 0.1695 0.1420 43 0.930 0.000 C25 C24 C26 H26 0.0901 0.2633 0.1881 43 0.930 0.000 C26 C21 C25 H27A 0.2851 0.3215 0.4224 137 0.960 0.000 C27 C21 H27A H27B 0.2462 0.3362 0.2764 137 0.960 0.000 C27 C21 H27A H27C 0.4065 0.3197 0.3260 137 0.960 0.000 C27 C21 H27A H24A 0.2580 0.0578 0.2447 137 0.890 0.000 N24 C24 H24A H24B 0.1492 0.0747 0.1419 137 0.890 0.000 N24 C24 H24A H24C 0.1075 0.0665 0.2721 137 0.890 0.000 N24 C24 H24A H32 0.6488 0.0586 -0.0909 43 0.930 0.000 C32 C33 C31 H33 0.8559 0.0477 0.1146 43 0.930 0.000 C33 C32 C34 H31 0.5481 0.0192 0.2416 147 0.820 0.000 O31A C31 H31 H34 0.9571 0.0448 -0.2289 147 0.820 0.000 O34A C34 H34 H42 0.8351 -0.2538 0.3902 43 0.930 0.000 C42 C41 C43 H43 0.7915 -0.1576 0.3721 43 0.930 0.000 C43 C44 C42 H45 0.6215 -0.1798 0.0090 43 0.930 0.000 C45 C44 C46 H46 0.6663 -0.2757 0.0286 43 0.930 0.000 C46 C41 C45 H47A 0.6918 -0.3578 0.2069 137 0.960 0.000 C47 C41 H47A H47B 0.8248 -0.3464 0.3086 137 0.960 0.000 C47 C41 H47A H47C 0.8482 -0.3494 0.1614 137 0.960 0.000 C47 C41 H47A H44A 0.7520 -0.0797 0.2038 137 0.890 0.000 N44 C44 H44A H44B 0.6025 -0.0904 0.2319 137 0.890 0.000 N44 C44 H44A H44C 0.6398 -0.0903 0.0991 137 0.890 0.000 N44 C44 H44A 06skc0062p21n in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.11407 -0.00360 0.61963 1.00000 0.01483 0.02653 0.01506 -0.00023 -0.00142 0.00050 0.01897 0.00427 0.00024 0.00011 0.00023 0.00000 0.00127 0.00168 0.00143 0.00123 0.00101 0.00114 0.00059 C2 0.23005 -0.00020 0.52904 1.00000 0.01661 0.02477 0.01722 0.00096 0.00174 -0.00177 0.01952 0.00412 0.00023 0.00011 0.00022 0.00000 0.00128 0.00152 0.00142 0.00117 0.00105 0.00104 0.00058 H2 0.27496 0.03456 0.51875 1.00000 0.02342 0.00000 0.00000 C3 0.27245 -0.04347 0.46292 1.00000 0.01869 0.02343 0.01938 0.00327 0.00238 -0.00211 0.02046 0.00417 0.00023 0.00010 0.00022 0.00000 0.00130 0.00150 0.00142 0.00123 0.00106 0.00109 0.00058 H3 0.22631 -0.07813 0.47105 1.00000 0.02455 0.00000 0.00000 C4 0.39153 -0.03941 0.37527 1.00000 0.01906 0.02753 0.01565 0.00044 -0.00152 -0.00075 0.02094 0.00419 0.00024 0.00011 0.00023 0.00000 0.00133 0.00173 0.00140 0.00126 0.00105 0.00121 0.00059 O1A 0.04779 -0.04828 0.63425 1.00000 0.02009 0.02667 0.02545 0.00063 0.00537 -0.00371 0.02387 0.00287 0.00016 0.00007 0.00015 0.00000 0.00090 0.00109 0.00104 0.00081 0.00074 0.00078 0.00043 O1B 0.09033 0.04376 0.67686 1.00000 0.01840 0.02878 0.02109 -0.00394 0.00737 -0.00137 0.02242 0.00280 0.00016 0.00007 0.00016 0.00000 0.00096 0.00108 0.00104 0.00086 0.00071 0.00075 0.00042 H1 0.02751 0.03907 0.72696 0.50000 0.03362 0.00000 0.00000 O4A 0.45560 -0.08268 0.34431 1.00000 0.02754 0.02558 0.03010 -0.00051 0.00904 0.00482 0.02735 0.00295 0.00017 0.00007 0.00016 0.00000 0.00097 0.00108 0.00111 0.00084 0.00079 0.00081 0.00045 O4B 0.41965 0.01143 0.33861 1.00000 0.01837 0.02491 0.02194 0.00278 0.00805 0.00048 0.02136 0.00286 0.00016 0.00007 0.00015 0.00000 0.00093 0.00108 0.00108 0.00080 0.00072 0.00074 0.00042 H4 0.48753 0.01062 0.29270 0.50000 0.03204 0.00000 0.00000 C21 0.27045 0.25119 0.30742 1.00000 0.05151 0.02548 0.04833 -0.00433 0.01002 -0.00351 0.04144 0.00525 0.00032 0.00012 0.00029 0.00000 0.00190 0.00180 0.00205 0.00148 0.00156 0.00143 0.00077 C22 0.35693 0.20852 0.36476 1.00000 0.04013 0.03943 0.05217 -0.01690 -0.00597 -0.00800 0.04453 0.00497 0.00030 0.00013 0.00031 0.00000 0.00174 0.00204 0.00209 0.00163 0.00148 0.00144 0.00082 H22 0.43653 0.21816 0.42204 1.00000 0.05343 0.00000 0.00000 C23 0.32807 0.15188 0.33909 1.00000 0.03003 0.02801 0.04831 -0.00640 -0.00392 0.00027 0.03590 0.00456 0.00027 0.00011 0.00027 0.00000 0.00157 0.00174 0.00201 0.00145 0.00137 0.00123 0.00073 H23 0.38742 0.12378 0.37824 1.00000 0.04308 0.00000 0.00000 C24 0.21016 0.13813 0.25474 1.00000 0.02183 0.02126 0.02558 -0.00226 0.00899 -0.00385 0.02247 0.00422 0.00024 0.00010 0.00024 0.00000 0.00135 0.00151 0.00157 0.00121 0.00115 0.00114 0.00060 C25 0.12115 0.17932 0.19832 1.00000 0.03508 0.02946 0.03977 -0.00023 -0.00508 0.00231 0.03528 0.00488 0.00028 0.00011 0.00027 0.00000 0.00160 0.00176 0.00185 0.00140 0.00133 0.00128 0.00072 H25 0.04089 0.16953 0.14195 1.00000 0.04234 0.00000 0.00000 C26 0.15147 0.23548 0.22574 1.00000 0.05098 0.02870 0.04801 -0.00069 -0.00001 0.00543 0.04284 0.00524 0.00032 0.00012 0.00029 0.00000 0.00195 0.00185 0.00207 0.00152 0.00159 0.00143 0.00079 H26 0.09007 0.26330 0.18813 1.00000 0.05140 0.00000 0.00000 C27 0.30524 0.31278 0.33564 1.00000 0.08618 0.02812 0.09025 -0.01303 0.00880 -0.00877 0.06813 0.00598 0.00039 0.00013 0.00038 0.00000 0.00262 0.00203 0.00306 0.00190 0.00220 0.00175 0.00109 H27A 0.28507 0.32150 0.42237 1.00000 0.10220 0.00000 0.00000 H27B 0.24621 0.33624 0.27643 1.00000 0.10220 0.00000 0.00000 H27C 0.40651 0.31968 0.32601 1.00000 0.10220 0.00000 0.00000 N24 0.17808 0.07839 0.22547 1.00000 0.01876 0.02529 0.02408 -0.00149 0.00466 -0.00078 0.02254 0.00354 0.00021 0.00008 0.00020 0.00000 0.00114 0.00132 0.00141 0.00098 0.00096 0.00096 0.00052 H24A 0.25803 0.05777 0.24468 1.00000 0.03770 0.00000 0.00806 H24B 0.14924 0.07471 0.14194 1.00000 0.04965 0.00000 0.00947 H24C 0.10753 0.06650 0.27207 1.00000 0.04600 0.00000 0.00876 C31 0.57165 0.04888 0.09121 1.00000 0.01958 0.01714 0.01911 -0.00383 0.00257 -0.00591 0.01856 0.00396 0.00025 0.00010 0.00023 0.00000 0.00139 0.00142 0.00150 0.00117 0.00109 0.00108 0.00057 C32 0.68155 0.05394 -0.00437 1.00000 0.02192 0.02033 0.01578 0.00158 0.00201 0.00108 0.01932 0.00415 0.00024 0.00009 0.00023 0.00000 0.00139 0.00142 0.00139 0.00109 0.00104 0.00103 0.00058 H32 0.64880 0.05857 -0.09091 1.00000 0.02319 0.00000 0.00000 C33 0.82362 0.05218 0.02793 1.00000 0.02331 0.01840 0.01391 0.00000 0.00205 -0.00009 0.01852 0.00408 0.00024 0.00009 0.00023 0.00000 0.00141 0.00141 0.00136 0.00108 0.00106 0.00103 0.00057 H33 0.85589 0.04772 0.11463 1.00000 0.02222 0.00000 0.00000 C34 0.93452 0.05693 -0.06650 1.00000 0.02227 0.01556 0.01844 0.00207 0.00384 0.00329 0.01863 0.00440 0.00025 0.00010 0.00023 0.00000 0.00142 0.00139 0.00156 0.00109 0.00112 0.00106 0.00058 O31A 0.61656 0.02330 0.19708 1.00000 0.01813 0.03078 0.01840 0.00619 0.00547 0.00187 0.02220 0.00290 0.00016 0.00007 0.00015 0.00000 0.00089 0.00104 0.00101 0.00083 0.00073 0.00077 0.00042 H31 0.54812 0.01924 0.24156 0.50000 0.03331 0.00000 0.00000 O31B 0.44639 0.06768 0.06686 1.00000 0.01590 0.02885 0.02608 0.00344 0.00338 0.00341 0.02352 0.00283 0.00016 0.00007 0.00015 0.00000 0.00092 0.00107 0.00106 0.00079 0.00073 0.00074 0.00043 O34A 0.88861 0.04386 -0.18361 1.00000 0.01813 0.03170 0.01753 -0.00140 0.00510 -0.00097 0.02224 0.00279 0.00015 0.00007 0.00015 0.00000 0.00089 0.00106 0.00100 0.00084 0.00072 0.00076 0.00042 H34 0.95705 0.04476 -0.22887 0.50000 0.03336 0.00000 0.00000 O34B 1.06137 0.07141 -0.03162 1.00000 0.01568 0.03039 0.02520 -0.00092 0.00210 -0.00225 0.02375 0.00279 0.00016 0.00007 0.00015 0.00000 0.00094 0.00108 0.00104 0.00080 0.00073 0.00072 0.00043 C41 0.75520 -0.27514 0.21108 1.00000 0.03593 0.02508 0.04660 0.00313 0.00826 0.00379 0.03559 0.00516 0.00028 0.00011 0.00029 0.00000 0.00167 0.00170 0.00204 0.00148 0.00143 0.00126 0.00073 C42 0.79198 -0.23911 0.31298 1.00000 0.05527 0.03141 0.04244 0.01150 -0.00587 0.00768 0.04366 0.00545 0.00032 0.00012 0.00029 0.00000 0.00195 0.00191 0.00203 0.00158 0.00153 0.00145 0.00080 H42 0.83512 -0.25375 0.39017 1.00000 0.05240 0.00000 0.00000 C43 0.76584 -0.18140 0.30258 1.00000 0.05420 0.02933 0.03065 -0.00042 -0.00537 0.00425 0.03862 0.00510 0.00030 0.00012 0.00027 0.00000 0.00186 0.00183 0.00183 0.00137 0.00143 0.00138 0.00075 H43 0.79146 -0.15757 0.37207 1.00000 0.04634 0.00000 0.00000 C44 0.70192 -0.15983 0.18898 1.00000 0.01992 0.01721 0.02951 0.00126 0.00597 0.00086 0.02199 0.00435 0.00024 0.00010 0.00024 0.00000 0.00133 0.00148 0.00166 0.00125 0.00112 0.00106 0.00060 C45 0.66456 -0.19458 0.08612 1.00000 0.04718 0.02959 0.03181 -0.00048 -0.00351 0.00103 0.03662 0.00477 0.00029 0.00012 0.00027 0.00000 0.00176 0.00180 0.00183 0.00142 0.00137 0.00135 0.00073 H45 0.62155 -0.17982 0.00901 1.00000 0.04395 0.00000 0.00000 C46 0.69171 -0.25208 0.09843 1.00000 0.05943 0.02594 0.04428 -0.00829 0.00185 0.00215 0.04339 0.00531 0.00032 0.00012 0.00030 0.00000 0.00200 0.00182 0.00205 0.00150 0.00157 0.00143 0.00079 H46 0.66627 -0.27573 0.02856 1.00000 0.05207 0.00000 0.00000 C47 0.78246 -0.33789 0.22311 1.00000 0.05931 0.02628 0.08017 0.00955 0.01032 0.00515 0.05501 0.00591 0.00034 0.00012 0.00034 0.00000 0.00206 0.00185 0.00261 0.00173 0.00178 0.00149 0.00092 H47A 0.69179 -0.35785 0.20690 1.00000 0.08252 0.00000 0.00000 H47B 0.82476 -0.34639 0.30865 1.00000 0.08252 0.00000 0.00000 H47C 0.84821 -0.34940 0.16144 1.00000 0.08252 0.00000 0.00000 N44 0.67102 -0.09910 0.18009 1.00000 0.01961 0.02412 0.02592 0.00024 0.00329 0.00158 0.02314 0.00341 0.00019 0.00008 0.00019 0.00000 0.00109 0.00131 0.00128 0.00098 0.00089 0.00089 0.00052 H44A 0.75199 -0.07974 0.20382 1.00000 0.03471 0.00000 0.00000 H44B 0.60252 -0.09036 0.23193 1.00000 0.03471 0.00000 0.00000 H44C 0.63975 -0.09030 0.09914 1.00000 0.03471 0.00000 0.00000 Final Structure Factor Calculation for 06skc0062p21n in P2(1)/n Total number of l.s. parameters = 301 Maximum vector length = 511 Memory required = 3855 / 22995 wR2 = 0.1067 before cycle 5 for 3232 data and 0 / 301 parameters GooF = S = 0.983; Restrained GooF = 0.983 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 1.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0429 for 2215 Fo > 4sig(Fo) and 0.0816 for all 3232 data wR2 = 0.1067, GooF = S = 0.983, Restrained GooF = 0.983 for all data Occupancy sum of asymmetric unit = 32.00 for non-hydrogen and 26.00 for hydrogen atoms Principal mean square atomic displacements U 0.0266 0.0180 0.0124 C1 0.0253 0.0173 0.0160 C2 0.0257 0.0195 0.0161 C3 0.0277 0.0211 0.0141 C4 0.0285 0.0264 0.0168 O1A 0.0312 0.0227 0.0133 O1B 0.0356 0.0276 0.0188 O4A 0.0281 0.0231 0.0129 O4B 0.0561 0.0437 0.0245 C21 0.0652 0.0472 0.0212 C22 0.0533 0.0290 0.0255 C23 0.0318 0.0203 0.0153 C24 0.0472 0.0310 0.0277 C25 0.0556 0.0455 0.0274 C26 0.0936 0.0862 0.0246 C27 0.0268 0.0235 0.0173 N24 0.0256 0.0184 0.0117 C31 0.0225 0.0202 0.0153 C32 0.0233 0.0184 0.0138 C33 0.0245 0.0174 0.0140 C34 0.0338 0.0195 0.0134 O31A 0.0318 0.0238 0.0149 O31B 0.0319 0.0208 0.0140 O34A 0.0308 0.0251 0.0153 O34B 0.0486 0.0344 0.0238 C41 0.0620 0.0481 0.0209 C42 0.0589 0.0293 0.0276 C43 0.0306 0.0184 0.0170 C44 0.0507 0.0297 0.0295 C45 0.0607 0.0468 0.0226 C46 0.0824 0.0584 0.0242 C47 0.0262 0.0244 0.0188 N44 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.017 0.026 0.037 0.047 0.061 0.077 0.099 0.139 1.000 Number in group 345. 335. 316. 320. 309. 332. 316. 317. 319. 323. GooF 0.920 0.917 1.021 1.019 0.974 0.983 1.095 0.954 0.867 1.061 K 0.740 1.301 1.220 0.922 0.960 1.006 0.984 0.994 1.013 1.016 Resolution(A) 0.90 0.93 0.97 1.01 1.07 1.13 1.22 1.34 1.53 1.92 inf Number in group 323. 335. 316. 318. 323. 328. 322. 319. 323. 325. GooF 0.990 0.956 0.928 0.889 0.891 0.915 0.889 0.939 1.075 1.282 K 1.102 0.993 1.023 0.981 1.005 1.006 1.018 1.018 1.030 1.004 R1 0.245 0.168 0.147 0.095 0.071 0.066 0.064 0.049 0.039 0.033 Recommended weighting scheme: WGHT 0.0450 0.7232 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) 2 5 1 168.14 256.84 4.75 0.068 3.08 -1 1 2 29.33 68.86 4.36 0.035 4.61 8 2 6 2899.53 29.18 4.34 0.023 0.91 6 17 5 36.72 328.64 4.30 0.077 0.90 -1 2 2 1383.24 1731.60 4.08 0.177 4.36 3 14 2 26.11 72.02 3.68 0.036 1.40 -5 1 3 9.31 43.63 3.58 0.028 1.68 -2 1 1 1318.07 1610.52 3.55 0.170 4.27 2 1 1 199.41 148.08 3.36 0.052 4.00 0 4 2 179.61 238.99 3.27 0.066 3.90 3 12 0 29.12 56.71 3.23 0.032 1.66 -5 5 1 -5.82 7.90 3.21 0.012 1.71 -5 15 7 149.41 258.68 3.21 0.068 0.96 7 6 6 111.27 211.14 3.21 0.062 0.97 -6 1 2 320.61 234.78 3.13 0.065 1.50 0 10 2 33.77 12.30 3.13 0.015 2.15 2 4 0 65.70 41.51 3.11 0.027 3.62 -3 3 6 4.10 32.76 3.09 0.024 1.54 2 11 2 151.11 104.94 3.08 0.043 1.80 5 19 5 -29.19 28.21 3.07 0.023 0.90 1 2 1 168.07 225.92 3.06 0.064 5.75 1 1 5 178.93 123.69 3.00 0.047 1.98 -2 5 1 59.65 89.73 2.98 0.040 3.20 3 2 0 5.41 21.07 2.98 0.019 2.96 4 9 1 115.12 80.01 2.94 0.038 1.68 -8 7 6 128.51 3.58 2.93 0.008 0.96 -1 7 4 1362.79 1160.05 2.93 0.145 2.04 -5 8 6 320.29 408.63 2.89 0.086 1.20 0 11 2 260.98 204.82 2.74 0.061 1.98 0 5 4 239.57 304.53 2.73 0.074 2.27 3 15 6 -4.41 38.66 2.72 0.026 1.07 9 5 3 303.58 388.66 2.69 0.084 0.93 3 5 1 28.26 48.63 2.68 0.030 2.45 8 12 4 -24.95 21.73 2.66 0.020 0.90 -8 7 2 148.52 204.63 2.64 0.061 1.08 3 3 1 92.50 124.58 2.64 0.047 2.69 -10 5 1 186.08 270.19 2.62 0.070 0.90 -1 15 6 64.39 11.48 2.62 0.014 1.16 -2 2 1 22.95 39.47 2.61 0.027 4.07 1 11 8 183.73 122.16 2.61 0.047 1.09 -6 2 8 199.97 267.28 2.56 0.069 1.03 3 10 0 266.67 330.16 2.55 0.077 1.87 6 1 0 25.41 0.13 2.54 0.002 1.52 0 24 0 226.47 333.94 2.54 0.078 0.98 8 5 4 517.17 705.42 2.52 0.113 0.99 4 5 8 258.60 341.80 2.52 0.078 1.06 -1 0 3 1920.11 2198.27 2.50 0.199 3.33 -1 24 3 54.37 132.87 2.50 0.049 0.94 -2 5 2 19.90 37.51 2.47 0.026 2.86 -2 7 1 221.66 273.56 2.44 0.070 2.66 Bond lengths and angles C1 - Distance Angles O1A 1.2356 (0.0027) O1B 1.2955 (0.0028) 125.18 (0.21) C2 1.4884 (0.0031) 120.94 (0.22) 113.88 (0.21) C1 - O1A O1B C2 - Distance Angles C3 1.3114 (0.0032) C1 1.4884 (0.0031) 123.67 (0.23) H2 0.9300 118.16 118.16 C2 - C3 C1 C3 - Distance Angles C2 1.3114 (0.0032) C4 1.4905 (0.0032) 122.74 (0.23) H3 0.9300 118.63 118.63 C3 - C2 C4 C4 - Distance Angles O4A 1.2373 (0.0028) O4B 1.2936 (0.0028) 125.31 (0.22) C3 1.4905 (0.0032) 119.99 (0.23) 114.70 (0.22) C4 - O4A O4B O1A - Distance Angles C1 1.2356 (0.0027) O1A - O1B - Distance Angles C1 1.2955 (0.0028) H1 0.8200 109.47 O1B - C1 O4A - Distance Angles C4 1.2373 (0.0028) O4A - O4B - Distance Angles C4 1.2936 (0.0028) H4 0.8200 109.47 O4B - C4 C21 - Distance Angles C26 1.3750 (0.0039) C22 1.3857 (0.0040) 117.64 (0.26) C27 1.5134 (0.0040) 121.48 (0.28) 120.87 (0.28) C21 - C26 C22 C22 - Distance Angles C21 1.3857 (0.0040) C23 1.3857 (0.0038) 121.82 (0.26) H22 0.9300 119.09 119.09 C22 - C21 C23 C23 - Distance Angles C24 1.3716 (0.0034) C22 1.3857 (0.0038) 118.61 (0.25) H23 0.9300 120.70 120.70 C23 - C24 C22 C24 - Distance Angles C25 1.3697 (0.0034) C23 1.3716 (0.0034) 120.92 (0.24) N24 1.4686 (0.0029) 119.54 (0.22) 119.54 (0.22) C24 - C25 C23 C25 - Distance Angles C24 1.3697 (0.0034) C26 1.3805 (0.0037) 119.51 (0.25) H25 0.9300 120.24 120.24 C25 - C24 C26 C26 - Distance Angles C21 1.3750 (0.0039) C25 1.3805 (0.0037) 121.47 (0.27) H26 0.9300 119.27 119.27 C26 - C21 C25 C27 - Distance Angles C21 1.5134 (0.0040) H27A 0.9600 109.47 H27B 0.9600 109.47 109.47 H27C 0.9600 109.47 109.47 109.47 C27 - C21 H27A H27B N24 - Distance Angles C24 1.4686 (0.0029) H24A 0.8900 109.47 H24B 0.8900 109.47 109.47 H24C 0.8900 109.47 109.47 109.47 N24 - C24 H24A H24B C31 - Distance Angles O31B 1.2398 (0.0026) O31A 1.2914 (0.0027) 124.20 (0.21) C32 1.4857 (0.0032) 120.70 (0.22) 115.09 (0.20) C31 - O31B O31A C32 - Distance Angles C33 1.3206 (0.0031) C31 1.4857 (0.0032) 123.01 (0.23) H32 0.9300 118.49 118.49 C32 - C33 C31 C33 - Distance Angles C32 1.3206 (0.0031) C34 1.4833 (0.0031) 123.59 (0.23) H33 0.9300 118.21 118.21 C33 - C32 C34 C34 - Distance Angles O34B 1.2388 (0.0026) O34A 1.2908 (0.0027) 124.20 (0.21) C33 1.4833 (0.0031) 120.87 (0.22) 114.91 (0.20) C34 - O34B O34A O31A - Distance Angles C31 1.2914 (0.0027) H31 0.8200 109.47 O31A - C31 O31B - Distance Angles C31 1.2398 (0.0026) O31B - O34A - Distance Angles C34 1.2908 (0.0027) H34 0.8200 109.47 O34A - C34 O34B - Distance Angles C34 1.2388 (0.0026) O34B - C41 - Distance Angles C46 1.3743 (0.0038) C42 1.3782 (0.0039) 117.86 (0.26) C47 1.5072 (0.0038) 121.04 (0.28) 121.10 (0.28) C41 - C46 C42 C42 - Distance Angles C41 1.3782 (0.0039) C43 1.3873 (0.0038) 121.23 (0.27) H42 0.9300 119.38 119.38 C42 - C41 C43 C43 - Distance Angles C44 1.3703 (0.0035) C42 1.3873 (0.0038) 119.40 (0.26) H43 0.9300 120.30 120.30 C43 - C44 C42 C44 - Distance Angles C45 1.3683 (0.0035) C43 1.3703 (0.0035) 120.63 (0.24) N44 1.4641 (0.0030) 120.35 (0.23) 119.01 (0.23) C44 - C45 C43 C45 - Distance Angles C44 1.3683 (0.0035) C46 1.3854 (0.0038) 119.07 (0.26) H45 0.9300 120.47 120.46 C45 - C44 C46 C46 - Distance Angles C41 1.3743 (0.0038) C45 1.3854 (0.0038) 121.80 (0.28) H46 0.9300 119.10 119.10 C46 - C41 C45 C47 - Distance Angles C41 1.5072 (0.0038) H47A 0.9600 109.47 H47B 0.9600 109.47 109.47 H47C 0.9600 109.47 109.47 109.47 C47 - C41 H47A H47B N44 - Distance Angles C44 1.4641 (0.0030) H44A 0.8900 109.47 H44B 0.8900 109.47 109.47 H44C 0.8900 109.47 109.47 109.47 N44 - C44 H44A H44B Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.82 1.64 2.457(2) 177.1 O34A-H34...O1B_$6 0.82 2.79 3.314(2) 123.6 O34A-H34...O1A_$6 0.89 2.03 2.891(3) 163.8 N24-H24A...O4B 0.89 2.66 3.101(3) 111.9 N24-H24A...O31B 0.82 1.63 2.452(2) 176.2 O31A-H31...O4B 0.82 2.80 3.350(2) 126.3 O31A-H31...O4A 0.89 1.87 2.759(2) 172.1 N44-H44B...O4A 0.89 1.91 2.796(3) 171.8 N24-H24B...O34B_$1 0.89 1.85 2.739(2) 174.6 N24-H24C...O1A_$2 0.89 2.01 2.856(2) 158.1 N44-H44A...O1B_$3 0.89 2.60 3.093(2) 115.9 N44-H44A...O34B_$4 0.89 1.91 2.797(3) 173.5 N44-H44C...O31B_$5 FMAP and GRID set by program FMAP 2 2 25 GRID -1.136 -2 -2 1.136 2 2 R1 = 0.0815 for 3232 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.20 at 0.7860 0.1364 0.1974 [ 1.01 A from H47A ] Deepest hole -0.20 at 0.8626 0.0463 0.9169 [ 0.71 A from C34 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3579 / 17907 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7140 -0.3636 0.3026 1.00000 0.05 0.20 1.01 H47A 1.09 H47B 1.24 C47 2.03 H47C Q2 1 0.9155 -0.3419 0.2948 1.00000 0.05 0.19 0.87 H47B 1.38 C47 1.48 H47C 2.21 H47A Q3 1 0.7657 -0.2607 0.4712 1.00000 0.05 0.18 1.11 H42 1.76 C42 1.90 H27A 2.37 C21 Q4 1 0.2214 0.3288 0.3526 1.00000 0.05 0.18 0.86 H27B 0.89 C27 0.91 H27A 1.76 H27C Q5 1 0.2953 0.1444 0.2567 1.00000 0.05 0.17 0.80 C24 0.90 C23 1.54 H23 1.86 C25 Q6 1 0.3455 0.0645 0.5383 1.00000 0.05 0.16 0.97 H2 1.86 C2 2.15 O4A 2.24 H23 Q7 1 0.1422 0.0811 0.6439 1.00000 0.05 0.16 1.07 O1B 1.74 H1 1.78 H44A 1.92 H43 Q8 1 0.3632 0.3185 0.4244 1.00000 0.05 0.16 0.72 H27A 1.03 C27 1.13 H27C 1.85 H27B Q9 1 0.8849 -0.1427 0.3679 1.00000 0.05 0.16 0.93 H43 1.54 C43 2.40 O1B 2.43 C44 Q10 1 0.2729 0.2351 0.3745 1.00000 0.05 0.15 0.79 C21 1.01 C22 1.59 H22 1.83 C26 Shortest distances between peaks (including symmetry equivalents) 4 8 1.46 7 9 1.48 3 10 1.78 1 2 1.93 3 8 2.16 8 10 2.18 4 10 2.27 6 7 2.29 3 4 2.43 5 10 2.49 2 5 2.78 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.03: 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 1.02: Structure factors and derivatives 1.88: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.30: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0062p21n finished at 16:04:48 Total CPU time: 4.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++