+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + ssg0304 started at 15:47:38 on 02-Jul-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL ssg0304 in P2(1)2(1)2(1) CELL 0.67100 7.5842 8.2124 32.3630 90.000 90.000 90.000 ZERR 8.00 0.0014 0.0016 0.0060 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O UNIT 64 96 16 48 V = 2015.71 F(000) = 976.0 Mu = 0.13 mm-1 Cell Wt = 1857.57 Rho = 1.530 MERG 4 SHEL 7 0.77 FMAP 2 SIZE 0.01 0.01 0.01 ACTA HTAB O2 O31A HTAB N23 O3 HTAB N23 O2 HTAB O32 O1B EQIV_$1 x-1, y, z HTAB O1A O4A_$1 HTAB O34B O31A_$1 HTAB N41 O4A_$1 HTAB N41 O3_$1 EQIV_$2 -x+1, y-1/2, -z+1/2 HTAB O3 O4B_$2 EQIV_$3 x+1/2, -y+3/2, -z HTAB N21 O34A_$3 EQIV_$4 x-1/2, -y+3/2, -z HTAB O33 O31B_$4 HTAB N43 O31B_$4 PLAN 10 BOND $H WGHT 0.04650 L.S. 4 TEMP -153.00 FVAR 0.23107 MOLE 1 C1 1 0.060870 0.996293 0.168413 11.00000 0.01497 0.01766 = 0.02032 0.00191 -0.00085 0.00075 C2 1 0.259403 1.031106 0.169860 11.00000 0.01607 0.01952 = 0.01695 0.00284 -0.00012 -0.00017 AFIX 13 H2 2 0.278172 1.151387 0.167906 11.00000 -1.20000 AFIX 0 C3 1 0.345531 0.969163 0.209346 11.00000 0.01457 0.01889 = 0.01703 -0.00030 -0.00118 0.00017 AFIX 13 H3 2 0.279751 1.014212 0.233563 11.00000 -1.20000 AFIX 0 C4 1 0.537779 1.029660 0.211319 11.00000 0.01686 0.02289 = 0.01228 -0.00058 -0.00173 -0.00124 O1A 4 -0.019850 1.030169 0.203002 11.00000 0.01455 0.04050 = 0.02099 -0.00589 0.00213 -0.00271 AFIX 147 H1 2 -0.144742 1.002392 0.203912 11.00000 0.05981 AFIX 0 O1B 4 -0.011032 0.946577 0.137430 11.00000 0.01920 0.03715 = 0.01991 -0.00286 -0.00346 -0.00276 O2 4 0.347797 0.954691 0.136526 11.00000 0.01810 0.02608 = 0.01519 0.00037 -0.00014 0.00422 AFIX 147 H2O 2 0.305773 0.988326 0.114079 11.00000 -1.50000 AFIX 0 O3 4 0.327143 0.797935 0.209279 11.00000 0.02424 0.01884 = 0.01863 0.00261 -0.00473 -0.00401 AFIX 147 H3O 2 0.357311 0.760769 0.232404 11.00000 -1.50000 AFIX 0 O4A 4 0.660586 0.927725 0.205853 11.00000 0.01313 0.02461 = 0.02585 -0.00226 0.00040 0.00046 O4B 4 0.557105 1.177153 0.218513 11.00000 0.02420 0.01900 = 0.02548 -0.00166 -0.00556 -0.00288 MOLE 2 C22 1 0.203659 0.603159 0.103057 11.00000 0.02079 0.02763 = 0.02548 0.00357 0.00054 0.00287 AFIX 43 H22 2 0.258843 0.680248 0.085400 11.00000 -1.20000 AFIX 0 C24 1 0.102378 0.480017 0.158860 11.00000 0.02244 0.02127 = 0.02193 -0.00141 -0.00236 0.00276 C25 1 0.058037 0.389674 0.125519 11.00000 0.02557 0.02184 = 0.02441 0.00103 -0.00375 0.00085 AFIX 43 H25 2 -0.006060 0.290293 0.125777 11.00000 -1.20000 AFIX 0 C26 1 0.067409 0.456105 0.203727 11.00000 0.04820 0.03696 = 0.02070 0.00110 -0.00098 -0.00330 AFIX 137 H26A 2 -0.017192 0.367076 0.207402 11.00000 -1.50000 H26B 2 0.018581 0.556497 0.215434 11.00000 -1.50000 H26C 2 0.177823 0.429006 0.217875 11.00000 -1.50000 AFIX 0 N21 3 0.122570 0.467825 0.091260 11.00000 0.02983 0.02757 = 0.01743 -0.00286 -0.00367 0.00587 AFIX 43 H21 2 0.113837 0.433333 0.066184 11.00000 0.04471 AFIX 0 N23 3 0.193931 0.611565 0.143809 11.00000 0.02145 0.02206 = 0.02500 -0.00395 -0.00357 0.00027 AFIX 43 H23 2 0.237069 0.687659 0.158437 11.00000 0.04568 AFIX 0 MOLE 3 C31 1 0.246817 1.006017 0.018505 11.00000 0.01375 0.01685 = 0.01977 -0.00082 -0.00063 -0.00421 C32 1 0.056672 1.061851 0.023082 11.00000 0.01449 0.02018 = 0.01459 -0.00277 0.00158 -0.00018 AFIX 13 H32 2 0.034707 1.151655 0.002859 11.00000 -1.20000 AFIX 0 C33 1 -0.061106 0.917328 0.011665 11.00000 0.01370 0.01796 = 0.01486 -0.00033 -0.00084 0.00013 AFIX 13 H33 2 -0.035691 0.883884 -0.017443 11.00000 -1.20000 AFIX 0 C34 1 -0.252440 0.973750 0.014733 11.00000 0.01472 0.01765 = 0.01407 -0.00215 -0.00200 -0.00162 O31A 4 0.338996 0.990095 0.050783 11.00000 0.01231 0.03408 = 0.01817 -0.00028 -0.00157 0.00025 O31B 4 0.297919 0.974000 -0.017397 11.00000 0.01455 0.02512 = 0.01679 -0.00271 0.00014 0.00101 O32 4 0.015140 1.119352 0.063174 11.00000 0.01893 0.02399 = 0.02002 -0.00679 0.00403 -0.00213 AFIX 147 H32O 2 0.010202 1.040383 0.079630 11.00000 -1.50000 AFIX 0 O33 4 -0.014677 0.789256 0.038521 11.00000 0.01708 0.01589 = 0.02503 0.00174 -0.00395 0.00009 AFIX 147 H33O 2 -0.060636 0.702196 0.030178 11.00000 -1.50000 AFIX 0 O34A 4 -0.305557 1.080170 -0.008538 11.00000 0.01684 0.02205 = 0.02097 0.00243 -0.00246 0.00108 O34B 4 -0.346000 0.901902 0.043145 11.00000 0.01317 0.02716 = 0.02200 0.00393 0.00073 0.00113 AFIX 147 H34 2 -0.470629 0.948525 0.043207 11.00000 0.07531 AFIX 0 MOLE 4 C42 1 -0.312244 0.692234 0.119536 11.00000 0.01859 0.02283 = 0.02171 0.00252 -0.00119 -0.00197 AFIX 43 H42 2 -0.276981 0.796993 0.110223 11.00000 -1.20000 AFIX 0 C44 1 -0.377925 0.429577 0.120564 11.00000 0.01477 0.02222 = 0.02507 -0.00097 0.00341 -0.00123 C45 1 -0.398340 0.489630 0.159286 11.00000 0.02196 0.02255 = 0.02201 0.00235 0.00199 0.00105 AFIX 43 H45 2 -0.434496 0.430227 0.183007 11.00000 -1.20000 AFIX 0 C46 1 -0.402856 0.264334 0.102714 11.00000 0.02867 0.02485 = 0.04052 -0.01113 0.00683 -0.00315 AFIX 137 H46A 2 -0.410423 0.184201 0.125082 11.00000 -1.50000 H46B 2 -0.302656 0.237890 0.084810 11.00000 -1.50000 H46C 2 -0.511921 0.262006 0.086486 11.00000 -1.50000 AFIX 0 N41 3 -0.356626 0.653878 0.157822 11.00000 0.02277 0.02125 = 0.02077 -0.00021 -0.00070 0.00216 AFIX 43 H41 2 -0.362809 0.732272 0.180449 11.00000 0.05513 AFIX 0 N43 3 -0.325312 0.559496 0.096303 11.00000 0.01829 0.02536 = 0.01749 -0.00096 0.00168 -0.00307 AFIX 43 H43 2 -0.294105 0.548622 0.069802 11.00000 0.03182 AFIX 0 HKLF 4 Covalent radii and connectivity table for ssg0304 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - O2 C3 C1 C3 - O3 C2 C4 C4 - O4B O4A C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C22 - N23 N21 C24 - C25 N23 C26 C25 - C24 N21 C26 - C24 N21 - C22 C25 N23 - C22 C24 C31 - O31B O31A C32 C32 - O32 C31 C33 C33 - O33 C34 C32 C34 - O34A O34B C33 O31A - C31 O31B - C31 O32 - C32 O33 - C33 O34A - C34 O34B - C34 C42 - N41 N43 C44 - C45 N43 C46 C45 - C44 N41 C46 - C44 N41 - C42 C45 N43 - C42 C44 Operators for generating equivalent atoms: $1 x-1, y, z $2 -x+1, y-1/2, -z+1/2 $3 x+1/2, -y+3/2, -z $4 x-1/2, -y+3/2, -z 17039 Reflections read, of which 78 rejected -9 =< h =< 9, -10 =< k =< 10, -40 =< l =< 40, Max. 2-theta = 49.60 0 Systematic absence violations 0 Inconsistent equivalents 2392 Unique reflections, of which 0 suppressed R(int) = 0.0595 R(sigma) = 0.0350 Friedel opposites merged Maximum memory for data reduction = 3151 / 23548 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 = 3982 / 379323 wR2 = 0.0792 before cycle 1 for 2392 data and 303 / 303 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23078 0.00043 -0.663 OSF Mean shift/esd = 0.199 Maximum = 1.102 for x O1A Max. shift = 0.007 A for H33O Max. dU = 0.005 for H34 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3982 / 379323 wR2 = 0.0786 before cycle 2 for 2392 data and 303 / 303 parameters GooF = S = 1.108; Restrained GooF = 1.108 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23064 0.00043 -0.342 OSF Mean shift/esd = 0.069 Maximum = 0.372 for x O1A Max. shift = 0.005 A for H33O Max. dU = 0.003 for H34 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3982 / 379323 wR2 = 0.0785 before cycle 3 for 2392 data and 303 / 303 parameters GooF = S = 1.108; Restrained GooF = 1.108 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23064 0.00043 -0.004 OSF Mean shift/esd = 0.004 Maximum = 0.071 for tors H33O Max. shift = 0.002 A for H33O Max. dU = 0.001 for H34 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3982 / 379323 wR2 = 0.0785 before cycle 4 for 2392 data and 303 / 303 parameters GooF = S = 1.108; Restrained GooF = 1.108 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23064 0.00043 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.030 for tors H33O Max. shift = 0.001 A for H33O Max. dU = 0.000 for H34 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 0.2783 1.1514 0.1678 13 1.000 0.000 C2 O2 C3 C1 H3 0.2798 1.0142 0.2336 13 1.000 0.000 C3 O3 C2 C4 H1 -0.1258 1.0019 0.2014 147 0.840 0.000 O1A C1 H1 H2O 0.3049 0.9876 0.1141 147 0.840 0.000 O2 C2 H2O H3O 0.3570 0.7607 0.2324 147 0.840 0.000 O3 C3 H3O H22 0.2588 0.6800 0.0853 43 0.950 0.000 C22 N23 N21 H25 -0.0062 0.2903 0.1258 43 0.950 0.000 C25 C24 N21 H26A -0.0168 0.3664 0.2074 137 0.980 0.000 C26 C24 H26A H26B 0.0176 0.5560 0.2154 137 0.980 0.000 C26 C24 H26A H26C 0.1777 0.4294 0.2179 137 0.980 0.000 C26 C24 H26A H21 0.1122 0.4335 0.0656 43 0.880 0.000 N21 C22 C25 H23 0.2393 0.6900 0.1591 43 0.880 0.000 N23 C22 C24 H32 0.0348 1.1517 0.0029 13 1.000 0.000 C32 O32 C31 C33 H33 -0.0356 0.8838 -0.0175 13 1.000 0.000 C33 O33 C34 C32 H32O 0.0111 1.0405 0.0797 147 0.840 0.000 O32 C32 H32O H33O -0.0589 0.7017 0.0300 147 0.840 0.000 O33 C33 H33O H34 -0.4485 0.9400 0.0431 147 0.840 0.000 O34B C34 H34 H42 -0.2773 0.7971 0.1102 43 0.950 0.000 C42 N41 N43 H45 -0.4343 0.4303 0.1830 43 0.950 0.000 C45 C44 N41 H46A -0.4103 0.1842 0.1251 137 0.980 0.000 C46 C44 H46A H46B -0.3026 0.2377 0.0848 137 0.980 0.000 C46 C44 H46A H46C -0.5119 0.2619 0.0865 137 0.980 0.000 C46 C44 H46A H41 -0.3591 0.7212 0.1789 43 0.880 0.000 N41 C42 C45 H43 -0.3034 0.5547 0.0697 43 0.880 0.000 N43 C42 C44 ssg0304 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.06069 0.99639 0.16838 1.00000 0.01423 0.01758 0.02018 0.00180 -0.00064 0.00076 0.01733 0.00378 0.00028 0.00026 0.00007 0.00000 0.00099 0.00111 0.00107 0.00090 0.00083 0.00092 0.00045 C2 0.25947 1.03111 0.16983 1.00000 0.01540 0.01945 0.01688 0.00299 -0.00037 -0.00036 0.01724 0.00386 0.00028 0.00028 0.00006 0.00000 0.00101 0.00104 0.00102 0.00088 0.00082 0.00094 0.00044 H2 0.27834 1.15137 0.16785 1.00000 0.02069 0.00000 0.00000 C3 0.34559 0.96919 0.20937 1.00000 0.01471 0.01883 0.01640 -0.00022 -0.00133 0.00020 0.01665 0.00370 0.00028 0.00027 0.00007 0.00000 0.00102 0.00109 0.00098 0.00087 0.00084 0.00092 0.00044 H3 0.27980 1.01424 0.23358 1.00000 0.01998 0.00000 0.00000 C4 0.53771 1.02966 0.21131 1.00000 0.01667 0.02249 0.01240 -0.00030 -0.00154 -0.00091 0.01719 0.00374 0.00028 0.00028 0.00006 0.00000 0.00109 0.00119 0.00094 0.00084 0.00079 0.00095 0.00046 O1A -0.01954 1.03013 0.20304 1.00000 0.01400 0.04079 0.02109 -0.00615 0.00168 -0.00320 0.02529 0.00285 0.00021 0.00023 0.00005 0.00000 0.00078 0.00103 0.00079 0.00075 0.00064 0.00077 0.00038 H1 -0.12575 1.00187 0.20138 1.00000 0.06315 0.00000 0.01137 O1B -0.01100 0.94665 0.13744 1.00000 0.01868 0.03727 0.01992 -0.00276 -0.00333 -0.00275 0.02529 0.00279 0.00021 0.00022 0.00005 0.00000 0.00079 0.00099 0.00078 0.00072 0.00066 0.00077 0.00038 O2 0.34762 0.95461 0.13653 1.00000 0.01768 0.02581 0.01527 0.00029 -0.00029 0.00418 0.01959 0.00272 0.00020 0.00020 0.00004 0.00000 0.00075 0.00085 0.00071 0.00063 0.00061 0.00071 0.00034 H2O 0.30494 0.98756 0.11409 1.00000 0.02938 0.00000 0.00000 O3 0.32714 0.79799 0.20926 1.00000 0.02394 0.01846 0.01872 0.00275 -0.00470 -0.00392 0.02038 0.00262 0.00022 0.00019 0.00005 0.00000 0.00084 0.00079 0.00074 0.00063 0.00071 0.00071 0.00035 H3O 0.35705 0.76074 0.23239 1.00000 0.03056 0.00000 0.00000 O4A 0.66065 0.92768 0.20585 1.00000 0.01306 0.02483 0.02547 -0.00231 0.00038 0.00050 0.02112 0.00270 0.00020 0.00020 0.00005 0.00000 0.00074 0.00085 0.00080 0.00068 0.00066 0.00068 0.00035 O4B 0.55722 1.17717 0.21850 1.00000 0.02389 0.01888 0.02527 -0.00167 -0.00550 -0.00286 0.02268 0.00266 0.00022 0.00019 0.00005 0.00000 0.00086 0.00084 0.00085 0.00066 0.00068 0.00071 0.00037 C22 0.20369 0.60299 0.10302 1.00000 0.02067 0.02744 0.02552 0.00388 0.00044 0.00305 0.02454 0.00434 0.00031 0.00031 0.00007 0.00000 0.00116 0.00130 0.00121 0.00105 0.00094 0.00104 0.00052 H22 0.25884 0.68002 0.08535 1.00000 0.02945 0.00000 0.00000 C24 0.10242 0.48001 0.15885 1.00000 0.02266 0.02090 0.02163 -0.00137 -0.00250 0.00251 0.02173 0.00399 0.00030 0.00029 0.00007 0.00000 0.00113 0.00116 0.00112 0.00094 0.00090 0.00097 0.00049 C25 0.05800 0.38962 0.12555 1.00000 0.02539 0.02128 0.02384 0.00131 -0.00364 0.00082 0.02350 0.00414 0.00032 0.00029 0.00007 0.00000 0.00121 0.00118 0.00117 0.00099 0.00098 0.00103 0.00051 H25 -0.00622 0.29031 0.12582 1.00000 0.02821 0.00000 0.00000 C26 0.06720 0.45588 0.20372 1.00000 0.04764 0.03693 0.02052 0.00106 -0.00073 -0.00382 0.03503 0.00478 0.00041 0.00036 0.00007 0.00000 0.00164 0.00149 0.00120 0.00110 0.00114 0.00136 0.00063 H26A -0.01682 0.36636 0.20736 1.00000 0.05255 0.00000 0.00000 H26B 0.01759 0.55598 0.21541 1.00000 0.05255 0.00000 0.00000 H26C 0.17767 0.42942 0.21793 1.00000 0.05255 0.00000 0.00000 N21 0.12277 0.46774 0.09126 1.00000 0.02929 0.02726 0.01731 -0.00284 -0.00353 0.00589 0.02462 0.00352 0.00027 0.00025 0.00006 0.00000 0.00108 0.00110 0.00094 0.00083 0.00080 0.00095 0.00045 H21 0.11224 0.43352 0.06561 1.00000 0.04146 0.00000 0.00837 N23 0.19397 0.61166 0.14386 1.00000 0.02124 0.02224 0.02464 -0.00370 -0.00339 0.00059 0.02271 0.00341 0.00025 0.00025 0.00006 0.00000 0.00099 0.00101 0.00099 0.00083 0.00082 0.00088 0.00043 H23 0.23934 0.68997 0.15907 1.00000 0.04812 0.00000 0.00945 C31 0.24691 1.00595 0.01852 1.00000 0.01327 0.01674 0.01969 -0.00097 -0.00059 -0.00404 0.01657 0.00360 0.00028 0.00026 0.00006 0.00000 0.00097 0.00104 0.00106 0.00088 0.00082 0.00087 0.00044 C32 0.05672 1.06191 0.02308 1.00000 0.01386 0.01965 0.01462 -0.00255 0.00173 -0.00054 0.01604 0.00364 0.00028 0.00027 0.00006 0.00000 0.00102 0.00108 0.00098 0.00082 0.00080 0.00088 0.00044 H32 0.03480 1.15173 0.00286 1.00000 0.01925 0.00000 0.00000 C33 -0.06106 0.91726 0.01165 1.00000 0.01352 0.01784 0.01467 -0.00042 -0.00084 0.00027 0.01534 0.00364 0.00028 0.00026 0.00006 0.00000 0.00100 0.00103 0.00096 0.00085 0.00078 0.00086 0.00043 H33 -0.03564 0.88379 -0.01746 1.00000 0.01841 0.00000 0.00000 C34 -0.25248 0.97381 0.01473 1.00000 0.01416 0.01731 0.01420 -0.00175 -0.00202 -0.00146 0.01522 0.00353 0.00028 0.00026 0.00006 0.00000 0.00097 0.00102 0.00097 0.00087 0.00079 0.00091 0.00043 O31A 0.33912 0.99004 0.05078 1.00000 0.01242 0.03410 0.01790 -0.00026 -0.00137 0.00015 0.02147 0.00256 0.00019 0.00020 0.00004 0.00000 0.00071 0.00094 0.00075 0.00070 0.00060 0.00073 0.00036 O31B 0.29795 0.97397 -0.01741 1.00000 0.01431 0.02474 0.01669 -0.00282 0.00015 0.00111 0.01858 0.00254 0.00019 0.00019 0.00004 0.00000 0.00072 0.00081 0.00073 0.00066 0.00057 0.00067 0.00033 O32 0.01521 1.11938 0.06320 1.00000 0.01841 0.02373 0.01988 -0.00681 0.00390 -0.00206 0.02067 0.00260 0.00021 0.00020 0.00004 0.00000 0.00076 0.00082 0.00076 0.00065 0.00069 0.00071 0.00035 H32O 0.01114 1.04047 0.07969 1.00000 0.03101 0.00000 0.00000 O33 -0.01459 0.78915 0.03855 1.00000 0.01657 0.01556 0.02519 0.00141 -0.00434 0.00021 0.01911 0.00265 0.00021 0.00018 0.00005 0.00000 0.00075 0.00075 0.00082 0.00063 0.00066 0.00067 0.00034 H33O -0.05893 0.70174 0.02997 1.00000 0.02866 0.00000 0.00000 O34A -0.30563 1.08019 -0.00855 1.00000 0.01636 0.02171 0.02098 0.00210 -0.00250 0.00098 0.01968 0.00266 0.00020 0.00019 0.00005 0.00000 0.00079 0.00078 0.00075 0.00067 0.00062 0.00065 0.00034 O34B -0.34575 0.90181 0.04315 1.00000 0.01300 0.02721 0.02232 0.00392 0.00072 0.00170 0.02084 0.00281 0.00020 0.00020 0.00005 0.00000 0.00076 0.00087 0.00077 0.00069 0.00066 0.00071 0.00034 H34 -0.44847 0.94005 0.04312 1.00000 0.08387 0.00000 0.01388 C42 -0.31230 0.69230 0.11954 1.00000 0.01862 0.02291 0.02149 0.00214 -0.00147 -0.00192 0.02101 0.00392 0.00029 0.00029 0.00007 0.00000 0.00111 0.00114 0.00112 0.00095 0.00092 0.00096 0.00048 H42 -0.27732 0.79714 0.11022 1.00000 0.02521 0.00000 0.00000 C44 -0.37786 0.42946 0.12054 1.00000 0.01459 0.02186 0.02528 -0.00080 0.00352 -0.00134 0.02058 0.00397 0.00029 0.00028 0.00007 0.00000 0.00105 0.00117 0.00114 0.00096 0.00089 0.00092 0.00048 C45 -0.39820 0.48961 0.15927 1.00000 0.02175 0.02255 0.02177 0.00223 0.00179 0.00139 0.02202 0.00406 0.00030 0.00029 0.00007 0.00000 0.00112 0.00123 0.00112 0.00095 0.00089 0.00097 0.00050 H45 -0.43430 0.43027 0.18301 1.00000 0.02643 0.00000 0.00000 C46 -0.40279 0.26426 0.10275 1.00000 0.02835 0.02468 0.04008 -0.01089 0.00680 -0.00288 0.03103 0.00449 0.00037 0.00030 0.00009 0.00000 0.00139 0.00134 0.00152 0.00113 0.00119 0.00110 0.00062 H46A -0.41033 0.18422 0.12514 1.00000 0.04655 0.00000 0.00000 H46B -0.30261 0.23774 0.08485 1.00000 0.04655 0.00000 0.00000 H46C -0.51187 0.26186 0.08653 1.00000 0.04655 0.00000 0.00000 N41 -0.35650 0.65369 0.15777 1.00000 0.02267 0.02103 0.02058 -0.00083 -0.00084 0.00180 0.02143 0.00340 0.00026 0.00024 0.00006 0.00000 0.00098 0.00101 0.00096 0.00080 0.00083 0.00083 0.00043 H41 -0.35905 0.72125 0.17887 1.00000 0.05049 0.00000 0.00988 N43 -0.32514 0.55935 0.09634 1.00000 0.01820 0.02567 0.01739 -0.00063 0.00136 -0.00358 0.02042 0.00327 0.00025 0.00024 0.00006 0.00000 0.00094 0.00106 0.00090 0.00077 0.00077 0.00084 0.00042 H43 -0.30342 0.55469 0.06965 1.00000 0.03386 0.00000 0.00763 Final Structure Factor Calculation for ssg0304 in P2(1)2(1)2(1) Total number of l.s. parameters = 303 Maximum vector length = 511 Memory required = 3681 / 25046 wR2 = 0.0785 before cycle 5 for 2392 data and 2 / 303 parameters GooF = S = 1.108; Restrained GooF = 1.108 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0316 for 2175 Fo > 4sig(Fo) and 0.0372 for all 2392 data wR2 = 0.0785, GooF = S = 1.108, Restrained GooF = 1.108 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 32.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0211 0.0170 0.0139 C1 0.0215 0.0154 0.0149 C2 0.0189 0.0171 0.0140 C3 0.0226 0.0171 0.0119 C4 0.0430 0.0194 0.0135 O1A 0.0380 0.0227 0.0152 O1B 0.0276 0.0161 0.0151 O2 0.0289 0.0165 0.0157 O3 0.0275 0.0229 0.0130 O4A 0.0302 0.0222 0.0157 O4B 0.0312 0.0232 0.0193 C22 0.0262 0.0200 0.0190 C24 0.0283 0.0226 0.0195 C25 0.0489 0.0357 0.0204 C26 0.0354 0.0223 0.0162 N21 0.0287 0.0211 0.0183 N23 0.0201 0.0191 0.0105 C31 0.0209 0.0150 0.0122 C32 0.0179 0.0150 0.0131 C33 0.0182 0.0162 0.0113 C34 0.0341 0.0182 0.0121 O31A 0.0257 0.0159 0.0141 O31B 0.0303 0.0180 0.0138 O32 0.0271 0.0159 0.0143 O33 0.0236 0.0206 0.0148 O34A 0.0296 0.0201 0.0128 O34B 0.0253 0.0200 0.0177 C42 0.0266 0.0217 0.0134 C44 0.0257 0.0207 0.0197 C45 0.0484 0.0257 0.0190 C46 0.0242 0.0203 0.0198 N41 0.0272 0.0181 0.0160 N43 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.035 0.053 0.070 0.086 0.105 0.126 0.156 0.197 0.268 1.000 Number in group 244. 250. 231. 240. 246. 224. 245. 234. 237. 241. GooF 1.048 1.002 1.183 1.036 1.044 1.221 1.169 1.108 1.122 1.139 K 1.071 0.968 1.030 1.017 1.016 1.009 0.994 1.004 1.000 1.006 Resolution(A) 0.80 0.83 0.86 0.90 0.95 1.02 1.10 1.22 1.40 1.79 inf Number in group 247. 236. 234. 240. 242. 235. 244. 236. 240. 238. GooF 0.968 1.025 1.003 0.994 1.017 0.957 1.094 1.160 1.298 1.454 K 1.030 1.000 0.999 0.997 0.999 1.003 0.997 1.000 1.021 1.003 R1 0.077 0.063 0.054 0.049 0.034 0.031 0.028 0.032 0.027 0.027 Recommended weighting scheme: WGHT 0.0540 0.0251 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) 0 2 16 108.98 69.54 5.11 0.069 1.81 0 2 6 18799.41 14456.46 4.33 0.988 3.27 0 1 8 1206.07 1489.78 3.84 0.317 3.63 0 7 19 173.53 233.50 3.38 0.126 0.97 9 1 7 469.66 377.23 3.32 0.160 0.82 0 2 4 351.24 424.26 3.28 0.169 3.66 2 2 1 292.81 347.94 3.18 0.153 2.78 3 2 15 263.08 217.69 3.16 0.121 1.52 1 6 13 223.10 179.14 3.14 0.110 1.18 0 2 3 57.73 75.47 3.09 0.071 3.84 1 4 15 107.10 82.13 3.08 0.074 1.46 2 7 22 58.83 87.56 3.07 0.077 0.89 0 3 2 2530.02 2968.17 3.05 0.448 2.70 2 4 34 138.50 180.06 3.05 0.110 0.84 0 4 8 510.26 429.53 3.03 0.170 1.83 1 3 13 1908.51 1636.19 3.03 0.332 1.79 0 3 15 178.13 140.83 3.02 0.097 1.69 1 3 19 329.42 275.38 2.99 0.136 1.42 1 7 0 334.86 272.76 2.97 0.136 1.16 3 4 19 493.15 395.38 2.95 0.163 1.16 2 4 9 43.21 29.80 2.91 0.045 1.61 2 4 14 226.68 190.06 2.85 0.113 1.42 8 1 0 33.76 6.21 2.84 0.020 0.94 0 6 0 43.77 17.38 2.81 0.034 1.37 0 2 5 142.99 178.74 2.79 0.110 3.47 2 3 4 590.19 684.31 2.78 0.215 2.14 3 4 2 262.37 224.27 2.78 0.123 1.59 3 1 12 403.55 469.22 2.77 0.178 1.80 0 2 1 26.68 15.25 2.74 0.032 4.07 0 2 8 26.04 11.53 2.73 0.028 2.88 2 0 9 334.80 275.68 2.67 0.136 2.61 1 2 19 385.66 334.34 2.67 0.150 1.54 2 2 8 666.37 765.14 2.64 0.227 2.29 2 3 19 529.07 445.01 2.61 0.173 1.35 7 1 1 32.62 15.31 2.60 0.032 1.07 0 2 10 749.06 864.47 2.59 0.242 2.54 1 5 19 111.66 84.84 2.57 0.076 1.17 2 2 15 1092.12 949.90 2.53 0.253 1.71 1 8 9 121.74 149.81 2.49 0.101 0.98 7 5 0 248.91 304.22 2.47 0.143 0.90 4 2 12 233.12 270.10 2.44 0.135 1.45 1 8 18 34.06 54.72 2.44 0.061 0.89 2 4 19 74.41 56.57 2.42 0.062 1.24 1 6 12 26.84 13.15 2.42 0.030 1.21 2 4 18 266.29 229.20 2.40 0.124 1.27 1 1 8 20.41 11.75 2.40 0.028 3.27 2 5 22 1847.05 1610.58 2.39 0.330 1.05 2 2 14 2166.77 1923.71 2.35 0.360 1.78 0 2 24 38.46 56.65 2.34 0.062 1.28 0 2 12 209.38 178.11 2.34 0.110 2.25 Bond lengths and angles C1 - Distance Angles O1B 1.2103 (0.0027) O1A 1.3060 (0.0026) 124.95 (0.20) C2 1.5350 (0.0030) 121.95 (0.20) 113.07 (0.19) C1 - O1B O1A C2 - Distance Angles O2 1.4153 (0.0026) C3 1.5240 (0.0029) 106.78 (0.17) C1 1.5350 (0.0030) 110.99 (0.18) 112.62 (0.18) H2 1.0000 108.78 108.78 108.78 C2 - O2 C3 C1 C3 - Distance Angles O3 1.4129 (0.0027) C2 1.5240 (0.0029) 106.70 (0.18) C4 1.5407 (0.0029) 114.49 (0.18) 109.39 (0.17) H3 1.0000 108.71 108.71 108.71 C3 - O3 C2 C4 C4 - Distance Angles O4B 1.2425 (0.0028) O4A 1.2657 (0.0027) 125.70 (0.21) C3 1.5407 (0.0029) 115.76 (0.20) 118.54 (0.19) C4 - O4B O4A O1A - Distance Angles C1 1.3060 (0.0026) H1 0.8400 109.47 O1A - C1 O1B - Distance Angles C1 1.2103 (0.0027) O1B - O2 - Distance Angles C2 1.4153 (0.0026) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4129 (0.0027) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2657 (0.0027) O4A - O4B - Distance Angles C4 1.2425 (0.0028) O4B - C22 - Distance Angles N23 1.3255 (0.0031) N21 1.3249 (0.0033) 107.81 (0.22) H22 0.9500 126.09 126.09 C22 - N23 N21 C24 - Distance Angles C25 1.3513 (0.0031) N23 1.3734 (0.0031) 106.06 (0.20) C26 1.4899 (0.0033) 131.27 (0.23) 122.66 (0.22) C24 - C25 N23 C25 - Distance Angles C24 1.3513 (0.0031) N21 1.3728 (0.0030) 107.39 (0.21) H25 0.9500 126.30 126.30 C25 - C24 N21 C26 - Distance Angles C24 1.4899 (0.0033) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C24 H26A H26B N21 - Distance Angles C22 1.3249 (0.0033) C25 1.3728 (0.0029) 108.97 (0.19) H21 0.8800 125.51 125.51 N21 - C22 C25 N23 - Distance Angles C22 1.3255 (0.0031) C24 1.3734 (0.0031) 109.76 (0.21) H23 0.8800 125.12 125.12 N23 - C22 C24 C31 - Distance Angles O31B 1.2533 (0.0025) O31A 1.2634 (0.0026) 125.03 (0.20) C32 1.5210 (0.0030) 116.50 (0.18) 118.43 (0.18) C31 - O31B O31A C32 - Distance Angles O32 1.4170 (0.0025) C31 1.5210 (0.0030) 113.59 (0.17) C33 1.5317 (0.0030) 110.49 (0.17) 107.18 (0.18) H32 1.0000 108.49 108.49 108.49 C32 - O32 C31 C33 C33 - Distance Angles O33 1.4103 (0.0025) C34 1.5275 (0.0029) 115.09 (0.18) C32 1.5317 (0.0030) 106.48 (0.17) 107.62 (0.17) H33 1.0000 109.16 109.16 109.16 C33 - O33 C34 C32 C34 - Distance Angles O34A 1.2219 (0.0026) O34B 1.3023 (0.0026) 125.50 (0.20) C33 1.5275 (0.0029) 119.39 (0.19) 115.11 (0.18) C34 - O34A O34B O31A - Distance Angles C31 1.2634 (0.0026) O31A - O31B - Distance Angles C31 1.2533 (0.0025) O31B - O32 - Distance Angles C32 1.4170 (0.0025) H32O 0.8400 109.47 O32 - C32 O33 - Distance Angles C33 1.4103 (0.0025) H33O 0.8400 109.47 O33 - C33 O34A - Distance Angles C34 1.2219 (0.0026) O34A - O34B - Distance Angles C34 1.3023 (0.0026) H34 0.8400 109.47 O34B - C34 C42 - Distance Angles N41 1.3207 (0.0030) N43 1.3286 (0.0029) 108.27 (0.20) H42 0.9500 125.86 125.86 C42 - N41 N43 C44 - Distance Angles C45 1.3562 (0.0032) N43 1.3825 (0.0030) 105.99 (0.20) C46 1.4859 (0.0032) 132.55 (0.23) 121.45 (0.21) C44 - C45 N43 C45 - Distance Angles C44 1.3562 (0.0032) N41 1.3849 (0.0031) 107.22 (0.21) H45 0.9500 126.39 126.39 C45 - C44 N41 C46 - Distance Angles C44 1.4859 (0.0032) H46A 0.9800 109.47 H46B 0.9800 109.47 109.47 H46C 0.9800 109.47 109.47 109.47 C46 - C44 H46A H46B N41 - Distance Angles C42 1.3207 (0.0030) C45 1.3849 (0.0031) 108.93 (0.20) H41 0.8800 125.54 125.54 N41 - C42 C45 N43 - Distance Angles C42 1.3286 (0.0029) C44 1.3825 (0.0030) 109.58 (0.18) H43 0.8800 125.21 125.21 N43 - C42 C44 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.07 2.791(2) 144.4 O2-H2O...O31A 0.88 1.97 2.800(2) 157.5 N23-H23...O3 0.88 2.44 3.057(3) 128.1 N23-H23...O2 0.84 2.03 2.797(2) 151.8 O32-H32O...O1B 0.84 1.74 2.569(2) 170.4 O1A-H1...O4A_$1 0.84 1.68 2.510(2) 168.6 O34B-H34...O31A_$1 0.88 1.91 2.739(3) 155.7 N41-H41...O4A_$1 0.88 2.65 3.152(3) 117.2 N41-H41...O3_$1 0.84 1.85 2.687(2) 175.0 O3-H3O...O4B_$2 0.88 1.95 2.759(2) 151.9 N21-H21...O34A_$3 0.84 1.85 2.676(2) 166.8 O33-H33O...O31B_$4 0.88 1.87 2.733(2) 165.6 N43-H43...O31B_$4 FMAP and GRID set by program FMAP 2 3 36 GRID -0.758 -2 -2 0.758 2 2 R1 = 0.0372 for 2392 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.26 at 0.1510 0.0384 0.0201 [ 0.75 A from C32 ] Deepest hole -0.19 at 0.7930 0.7981 0.0277 [ 1.38 A from H33O ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3385 / 19683 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1510 1.0384 0.0201 1.00000 0.05 0.26 0.75 C32 0.78 C31 1.40 H32 1.73 O31B Q2 1 0.1633 1.0213 0.1706 1.00000 0.05 0.25 0.73 C2 0.81 C1 1.38 H2 1.74 O1A Q3 1 -0.1575 0.9434 0.0161 1.00000 0.05 0.24 0.76 C34 0.78 C33 1.51 H33 1.71 O34B Q4 1 0.0166 0.4734 0.1457 1.00000 0.05 0.21 0.78 C24 1.00 C25 1.64 H25 1.76 N23 Q5 1 -0.4093 1.0891 -0.0073 1.00000 0.05 0.18 0.79 O34A 1.68 C34 1.90 H21 2.06 H34 Q6 1 -0.4504 0.4359 0.1383 1.00000 0.05 0.17 0.80 C44 0.90 C45 1.45 H45 1.86 C46 Q7 1 -0.5911 0.4398 0.1508 1.00000 0.05 0.17 1.54 C45 1.58 H45 1.89 C44 2.17 N23 Q8 1 0.4030 0.9525 -0.0051 1.00000 0.05 0.17 0.91 O31B 1.48 C31 1.53 H33O 1.90 O31A Q9 1 0.2920 0.9890 0.1870 1.00000 0.05 0.17 0.70 C2 0.85 C3 1.47 H2 1.53 H3 Q10 1 0.4430 0.9997 0.2068 1.00000 0.05 0.16 0.77 C4 0.78 C3 1.52 H3 1.74 O4B Shortest distances between peaks (including symmetry equivalents) 2 9 1.14 6 7 1.14 9 10 1.32 5 8 1.81 1 8 2.19 3 5 2.38 2 10 2.43 1 3 2.47 4 7 2.99 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.02: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.75: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.23: Structure factors and derivatives 1.36: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.30: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + ssg0304 finished at 15:47:41 Total CPU time: 3.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++