+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + ssg0307 started at 20:08:19 on 09-Aug-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL ssg0307 in P2(1)2(1)2(1) CELL 0.68950 5.3880 9.9210 18.2650 90.000 90.000 90.000 ZERR 4.00 0.0013 0.0030 0.0050 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 28 48 8 28 V = 976.34 F(000) = 496.0 Mu = 0.15 mm-1 Cell Wt = 944.74 Rho = 1.607 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 EQIV_$1 -x+3/2, -y+1, z-1/2 HTAB O1B O22_$1 EQIV_$2 x-1/2, -y+1/2, -z HTAB O2 O4B_$2 EQIV_$3 x+1, y, z HTAB O3 O2_$3 HTAB O3 O1B_$3 HTAB O4A O22_$3 EQIV_$4 x-1, y, z HTAB N21 O4B_$4 EQIV_$5 -x+5/2, -y+1, z+1/2 HTAB N23 O1A_$5 FMAP 2 PLAN 10 SIZE 0.05 0.06 0.13 ACTA BOND $H WGHT 0.04640 0.19700 L.S. 4 TEMP -153.00 FVAR 0.62155 MOLE 1 C1 1 1.116049 0.606583 -0.053382 11.00000 0.01415 0.02191 = 0.01618 0.00048 0.00191 0.00396 C2 1 1.137154 0.526930 0.018211 11.00000 0.01462 0.02079 = 0.01537 -0.00013 -0.00037 0.00043 AFIX 13 H2 2 1.105794 0.591361 0.059286 11.00000 -1.20000 AFIX 0 C3 1 1.407589 0.480466 0.024347 11.00000 0.01498 0.02194 = 0.01656 -0.00003 -0.00109 -0.00027 AFIX 13 H3 2 1.519536 0.560462 0.028698 11.00000 -1.20000 AFIX 0 C4 1 1.436031 0.390403 0.091459 11.00000 0.01224 0.02413 = 0.01769 0.00022 -0.00201 -0.00080 O1A 4 1.238625 0.706617 -0.064453 11.00000 0.02427 0.02461 = 0.02241 0.00470 0.00029 -0.00243 O1B 4 0.956903 0.553010 -0.100119 11.00000 0.02436 0.02802 = 0.01638 0.00367 -0.00507 -0.00196 AFIX 147 H1 2 0.959455 0.596884 -0.139445 11.00000 0.04899 AFIX 0 O2 4 0.967355 0.420043 0.025782 11.00000 0.01573 0.02042 = 0.02073 -0.00009 0.00106 -0.00118 AFIX 147 H2O 2 1.005263 0.357833 -0.003342 11.00000 -1.50000 AFIX 0 O3 4 1.462634 0.408628 -0.040319 11.00000 0.01449 0.03371 = 0.01791 -0.00120 0.00231 0.00431 AFIX 147 H3O 2 1.617141 0.405809 -0.046264 11.00000 -1.50000 AFIX 0 O4A 4 1.416148 0.459598 0.153061 11.00000 0.02721 0.02424 = 0.01709 -0.00104 -0.00572 0.00419 AFIX 147 H4 2 1.447706 0.408990 0.188736 11.00000 0.03528 AFIX 0 O4B 4 1.473001 0.270227 0.088491 11.00000 0.02326 0.02266 = 0.02047 -0.00010 -0.00351 0.00399 MOLE 2 C22 1 0.753428 0.249732 0.263812 11.00000 0.01915 0.02109 = 0.01580 0.00236 0.00056 -0.00181 C24 1 1.094105 0.115540 0.290451 11.00000 0.01868 0.02739 = 0.02321 0.00156 -0.00259 0.00307 AFIX 23 H24A 2 1.060051 0.034206 0.320203 11.00000 -1.20000 H24B 2 1.272177 0.138987 0.294493 11.00000 -1.20000 AFIX 0 C25 1 1.016692 0.095130 0.210329 11.00000 0.03286 0.03798 = 0.02431 -0.00545 -0.00537 0.01676 AFIX 23 H25A 2 1.139615 0.134973 0.176350 11.00000 -1.20000 H25B 2 0.995876 -0.001679 0.198705 11.00000 -1.20000 AFIX 0 N21 3 0.780393 0.166541 0.206905 11.00000 0.02581 0.03045 = 0.01928 -0.00542 -0.00544 0.00892 AFIX 43 H21 2 0.669907 0.156148 0.171874 11.00000 0.06797 AFIX 0 N23 3 0.935838 0.228212 0.312298 11.00000 0.02681 0.02640 = 0.02031 -0.00372 -0.00662 0.00416 AFIX 43 H23 2 0.957641 0.276038 0.352361 11.00000 0.03813 AFIX 0 O22 4 0.582138 0.335695 0.270974 11.00000 0.02253 0.02770 = 0.01646 -0.00105 -0.00048 0.00552 HKLF 4 Covalent radii and connectivity table for ssg0307 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - O2 C1 C3 C3 - O3 C4 C2 C4 - O4B O4A C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C22 - O22 N21 N23 C24 - N23 C25 C25 - N21 C24 N21 - C22 C25 N23 - C22 C24 O22 - C22 Operators for generating equivalent atoms: $1 -x+3/2, -y+1, z-1/2 $2 x-1/2, -y+1/2, -z $3 x+1, y, z $4 x-1, y, z $5 -x+5/2, -y+1, z+1/2 9884 Reflections read, of which 1555 rejected -6 =< h =< 6, -12 =< k =< 12, -23 =< l =< 23, Max. 2-theta = 53.19 0 Systematic absence violations 0 Inconsistent equivalents 2167 Unique reflections, of which 0 suppressed R(int) = 0.0397 R(sigma) = 0.0323 Friedel opposites not merged Maximum memory for data reduction = 1852 / 21269 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 = 2269 / 191448 wR2 = 0.0823 before cycle 1 for 2167 data and 153 / 153 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0464 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62155 0.00135 0.003 OSF Mean shift/esd = 0.003 Maximum = 0.009 for U23 O2 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H21 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2269 / 191448 wR2 = 0.0823 before cycle 2 for 2167 data and 153 / 153 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0464 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62156 0.00135 0.002 OSF Mean shift/esd = 0.001 Maximum = 0.003 for U23 O2 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H21 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2269 / 191448 wR2 = 0.0823 before cycle 3 for 2167 data and 153 / 153 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0464 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62156 0.00135 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O4B Max. shift = 0.000 A for H3O Max. dU = 0.000 for H1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2269 / 191448 wR2 = 0.0823 before cycle 4 for 2167 data and 153 / 153 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0464 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62156 0.00135 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O4B Max. shift = 0.000 A for H3O Max. dU = 0.000 for H1 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 1.1058 0.5914 0.0593 13 1.000 0.000 C2 O2 C1 C3 H3 1.5195 0.5605 0.0287 13 1.000 0.000 C3 O3 C4 C2 H1 0.9595 0.5969 -0.1394 147 0.840 0.000 O1B C1 H1 H2O 1.0053 0.3578 -0.0033 147 0.840 0.000 O2 C2 H2O H3O 1.6171 0.4058 -0.0463 147 0.840 0.000 O3 C3 H3O H4 1.4477 0.4090 0.1887 147 0.840 0.000 O4A C4 H4 H24A 1.0601 0.0342 0.3202 23 0.990 0.000 C24 N23 C25 H24B 1.2722 0.1390 0.2945 23 0.990 0.000 C24 N23 C25 H25A 1.1396 0.1350 0.1763 23 0.990 0.000 C25 N21 C24 H25B 0.9959 -0.0017 0.1987 23 0.990 0.000 C25 N21 C24 H21 0.6699 0.1561 0.1719 43 0.880 0.000 N21 C22 C25 H23 0.9576 0.2760 0.3524 43 0.880 0.000 N23 C22 C24 ssg0307 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 1.11605 0.60658 -0.05338 1.00000 0.01415 0.02191 0.01618 0.00048 0.00191 0.00396 0.01741 0.00247 0.00026 0.00015 0.00007 0.00000 0.00061 0.00064 0.00061 0.00051 0.00049 0.00055 0.00028 C2 1.13715 0.52693 0.01821 1.00000 0.01462 0.02079 0.01537 -0.00013 -0.00037 0.00043 0.01693 0.00241 0.00026 0.00014 0.00007 0.00000 0.00063 0.00063 0.00061 0.00051 0.00047 0.00052 0.00028 H2 1.10579 0.59136 0.05929 1.00000 0.02031 0.00000 0.00000 C3 1.40759 0.48047 0.02435 1.00000 0.01498 0.02194 0.01656 -0.00003 -0.00109 -0.00027 0.01783 0.00244 0.00027 0.00014 0.00007 0.00000 0.00065 0.00063 0.00061 0.00052 0.00051 0.00054 0.00028 H3 1.51954 0.56046 0.02870 1.00000 0.02139 0.00000 0.00000 C4 1.43603 0.39040 0.09146 1.00000 0.01224 0.02413 0.01769 0.00022 -0.00201 -0.00080 0.01802 0.00233 0.00025 0.00014 0.00007 0.00000 0.00059 0.00064 0.00059 0.00051 0.00050 0.00055 0.00027 O1A 1.23863 0.70662 -0.06445 1.00000 0.02427 0.02461 0.02241 0.00470 0.00029 -0.00243 0.02376 0.00194 0.00022 0.00011 0.00006 0.00000 0.00055 0.00051 0.00048 0.00041 0.00043 0.00043 0.00024 O1B 0.95690 0.55301 -0.10012 1.00000 0.02436 0.02802 0.01638 0.00367 -0.00507 -0.00196 0.02292 0.00177 0.00021 0.00011 0.00005 0.00000 0.00054 0.00053 0.00046 0.00040 0.00039 0.00045 0.00023 H1 0.95945 0.59689 -0.13944 1.00000 0.04897 0.00000 0.00643 O2 0.96735 0.42004 0.02578 1.00000 0.01573 0.02042 0.02073 -0.00009 0.00106 -0.00118 0.01896 0.00169 0.00019 0.00010 0.00005 0.00000 0.00049 0.00046 0.00045 0.00038 0.00037 0.00041 0.00022 H2O 1.00526 0.35783 -0.00334 1.00000 0.02844 0.00000 0.00000 O3 1.46263 0.40863 -0.04032 1.00000 0.01449 0.03371 0.01791 -0.00120 0.00231 0.00431 0.02204 0.00180 0.00019 0.00012 0.00005 0.00000 0.00049 0.00055 0.00045 0.00039 0.00036 0.00046 0.00023 H3O 1.61714 0.40581 -0.04626 1.00000 0.03306 0.00000 0.00000 O4A 1.41615 0.45960 0.15306 1.00000 0.02721 0.02424 0.01709 -0.00104 -0.00572 0.00419 0.02285 0.00180 0.00022 0.00010 0.00005 0.00000 0.00055 0.00049 0.00046 0.00040 0.00042 0.00046 0.00024 H4 1.44770 0.40899 0.18874 1.00000 0.03528 0.00000 0.00538 O4B 1.47300 0.27023 0.08849 1.00000 0.02326 0.02266 0.02047 -0.00010 -0.00351 0.00399 0.02213 0.00173 0.00020 0.00010 0.00005 0.00000 0.00052 0.00050 0.00046 0.00039 0.00041 0.00043 0.00023 C22 0.75343 0.24973 0.26381 1.00000 0.01915 0.02109 0.01580 0.00236 0.00056 -0.00181 0.01868 0.00239 0.00026 0.00014 0.00007 0.00000 0.00065 0.00064 0.00058 0.00051 0.00052 0.00058 0.00028 C24 1.09411 0.11554 0.29045 1.00000 0.01868 0.02739 0.02321 0.00156 -0.00259 0.00307 0.02309 0.00264 0.00029 0.00015 0.00008 0.00000 0.00068 0.00070 0.00068 0.00057 0.00057 0.00062 0.00031 H24A 1.06005 0.03421 0.32020 1.00000 0.02771 0.00000 0.00000 H24B 1.27218 0.13899 0.29449 1.00000 0.02771 0.00000 0.00000 C25 1.01669 0.09513 0.21033 1.00000 0.03286 0.03798 0.02431 -0.00545 -0.00537 0.01676 0.03172 0.00302 0.00033 0.00018 0.00009 0.00000 0.00089 0.00085 0.00074 0.00064 0.00064 0.00078 0.00038 H25A 1.13962 0.13497 0.17635 1.00000 0.03806 0.00000 0.00000 H25B 0.99588 -0.00168 0.19871 1.00000 0.03806 0.00000 0.00000 N21 0.78039 0.16654 0.20690 1.00000 0.02582 0.03045 0.01928 -0.00541 -0.00545 0.00892 0.02518 0.00232 0.00026 0.00014 0.00007 0.00000 0.00066 0.00065 0.00056 0.00051 0.00050 0.00058 0.00028 H21 0.66991 0.15615 0.17187 1.00000 0.06800 0.00000 0.00837 N23 0.93584 0.22821 0.31230 1.00000 0.02681 0.02640 0.02031 -0.00373 -0.00662 0.00416 0.02451 0.00224 0.00026 0.00013 0.00007 0.00000 0.00065 0.00060 0.00057 0.00049 0.00051 0.00054 0.00028 H23 0.95764 0.27604 0.35236 1.00000 0.03812 0.00000 0.00540 O22 0.58214 0.33569 0.27097 1.00000 0.02253 0.02770 0.01646 -0.00105 -0.00048 0.00552 0.02223 0.00179 0.00019 0.00011 0.00005 0.00000 0.00051 0.00051 0.00043 0.00039 0.00040 0.00045 0.00023 Final Structure Factor Calculation for ssg0307 in P2(1)2(1)2(1) Total number of l.s. parameters = 153 Maximum vector length = 511 Memory required = 2118 / 25046 wR2 = 0.0823 before cycle 5 for 2167 data and 2 / 153 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0464 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0311 for 2085 Fo > 4sig(Fo) and 0.0322 for all 2167 data wR2 = 0.0823, GooF = S = 1.043, Restrained GooF = 1.043 for all data Flack x parameter = 0.7643 with esd 0.8981 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 16.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0238 0.0166 0.0119 C1 0.0208 0.0155 0.0144 C2 0.0220 0.0171 0.0144 C3 0.0242 0.0183 0.0115 C4 0.0290 0.0241 0.0182 O1A 0.0310 0.0242 0.0135 O1B 0.0211 0.0205 0.0153 O2 0.0347 0.0190 0.0124 O3 0.0321 0.0220 0.0144 O4A 0.0280 0.0214 0.0170 O4B 0.0227 0.0188 0.0146 C22 0.0285 0.0244 0.0164 C24 0.0543 0.0224 0.0184 C25 0.0401 0.0192 0.0162 N21 0.0346 0.0228 0.0161 N23 0.0313 0.0190 0.0164 O22 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.061 0.090 0.117 0.142 0.172 0.214 0.258 0.320 0.445 1.000 Number in group 229. 205. 227. 213. 212. 218. 215. 213. 217. 218. GooF 1.035 1.097 1.005 0.959 1.027 1.083 1.059 1.113 1.065 0.983 K 1.069 1.054 1.041 1.016 1.013 1.003 1.004 0.995 0.991 1.015 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.13 1.29 1.58 inf Number in group 222. 214. 218. 214. 216. 222. 210. 216. 220. 215. GooF 0.964 0.985 0.929 0.908 0.905 0.967 1.015 0.902 1.026 1.631 K 1.074 1.043 1.023 1.001 0.989 0.977 0.969 0.983 1.015 1.033 R1 0.049 0.050 0.043 0.038 0.035 0.028 0.028 0.024 0.022 0.032 Recommended weighting scheme: WGHT 0.0463 0.1969 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 3 3 6.00 1.08 5.52 0.022 2.91 2 4 1 32.69 18.23 5.37 0.091 1.82 0 6 5 18.57 8.82 4.91 0.063 1.51 2 0 7 116.61 79.86 4.78 0.191 1.87 -2 4 1 29.78 18.19 4.43 0.091 1.82 0 4 6 113.32 84.06 4.41 0.196 1.92 0 5 16 21.41 33.12 3.75 0.123 0.99 0 2 0 244.36 308.59 3.74 0.375 4.96 1 3 9 65.19 48.80 3.57 0.149 1.65 0 2 1 3.78 1.02 3.51 0.022 4.79 1 0 2 9.33 15.89 3.47 0.085 4.64 0 2 4 8.94 4.57 3.47 0.046 3.36 0 4 0 0.81 4.77 3.37 0.047 2.48 -1 2 7 217.68 178.88 3.33 0.285 2.12 2 0 1 1261.02 1039.94 3.30 0.688 2.67 2 0 6 56.43 73.34 3.30 0.183 2.02 0 2 5 235.79 194.83 3.29 0.298 2.94 0 7 17 38.19 25.43 3.28 0.108 0.86 -1 9 15 290.57 232.97 3.25 0.326 0.81 0 4 2 137.89 112.20 3.13 0.226 2.39 1 2 7 215.61 178.94 3.11 0.285 2.12 1 0 8 27.15 19.35 3.10 0.094 2.10 0 9 14 216.23 177.74 2.97 0.284 0.84 -1 3 9 61.73 48.87 2.94 0.149 1.65 2 3 1 494.31 423.43 2.92 0.439 2.08 0 4 7 89.31 71.68 2.91 0.181 1.80 0 5 15 43.94 56.88 2.89 0.161 1.04 0 6 7 31.94 23.57 2.89 0.104 1.40 3 0 13 193.91 231.66 2.83 0.325 1.11 0 2 19 34.04 24.53 2.82 0.106 0.94 -3 8 12 274.92 221.73 2.78 0.318 0.85 3 11 6 52.75 40.36 2.76 0.136 0.78 0 5 17 96.39 118.72 2.74 0.232 0.94 0 4 20 61.49 46.59 2.73 0.146 0.86 0 5 10 11.74 7.30 2.69 0.058 1.34 1 4 3 529.71 458.81 2.69 0.457 2.11 0 7 1 275.41 322.60 2.67 0.383 1.41 0 4 16 59.00 73.58 2.66 0.183 1.04 5 0 8 647.91 752.06 2.64 0.585 0.97 3 7 2 449.12 521.57 2.63 0.487 1.10 0 2 23 383.50 315.30 2.61 0.379 0.78 2 3 2 2588.44 2197.18 2.60 1.000 2.04 0 5 2 41.91 52.57 2.59 0.155 1.94 1 1 4 252.95 294.03 2.59 0.366 3.29 3 9 4 4.76 9.20 2.58 0.065 0.92 2 0 19 9.47 4.89 2.57 0.047 0.91 5 8 5 153.21 127.16 2.57 0.241 0.79 -3 1 1 73.50 60.55 2.56 0.166 1.76 0 7 14 46.99 59.21 2.55 0.164 0.96 2 8 15 11.82 6.61 2.53 0.055 0.83 Bond lengths and angles C1 - Distance Angles O1A 1.2091 (0.0018) O1B 1.3215 (0.0017) 125.20 (0.13) C2 1.5321 (0.0019) 121.70 (0.13) 113.08 (0.12) C1 - O1A O1B C2 - Distance Angles O2 1.4074 (0.0017) C1 1.5321 (0.0019) 115.10 (0.11) C3 1.5324 (0.0019) 112.60 (0.12) 106.75 (0.11) H2 1.0000 107.34 107.34 107.34 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4110 (0.0017) C4 1.5246 (0.0019) 110.85 (0.12) C2 1.5324 (0.0019) 106.89 (0.11) 109.31 (0.11) H3 1.0000 109.91 109.91 109.91 C3 - O3 C4 C2 C4 - Distance Angles O4B 1.2100 (0.0018) O4A 1.3224 (0.0017) 124.26 (0.13) C3 1.5246 (0.0019) 123.92 (0.13) 111.82 (0.12) C4 - O4B O4A O1A - Distance Angles C1 1.2091 (0.0018) O1A - O1B - Distance Angles C1 1.3215 (0.0017) H1 0.8400 109.47 O1B - C1 O2 - Distance Angles C2 1.4074 (0.0017) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4110 (0.0017) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.3224 (0.0017) H4 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2100 (0.0018) O4B - C22 - Distance Angles O22 1.2634 (0.0018) N21 1.3352 (0.0019) 125.27 (0.13) N23 1.3401 (0.0018) 125.09 (0.13) 109.64 (0.13) C22 - O22 N21 C24 - Distance Angles N23 1.4615 (0.0020) C25 1.5351 (0.0021) 101.69 (0.12) H24A 0.9900 111.43 111.43 H24B 0.9900 111.43 111.43 109.28 C24 - N23 C25 H24A C25 - Distance Angles N21 1.4584 (0.0020) C24 1.5351 (0.0021) 102.36 (0.12) H25A 0.9900 111.30 111.30 H25B 0.9900 111.30 111.30 109.19 C25 - N21 C24 H25A N21 - Distance Angles C22 1.3352 (0.0019) C25 1.4584 (0.0020) 111.22 (0.12) H21 0.8800 124.39 124.39 N21 - C22 C25 N23 - Distance Angles C22 1.3401 (0.0018) C24 1.4615 (0.0020) 111.68 (0.12) H23 0.8800 124.16 124.16 N23 - C22 C24 O22 - Distance Angles C22 1.2634 (0.0018) O22 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.78 2.6090(15) 167.9 O1B-H1...O22_$1 0.84 2.02 2.8143(15) 158.5 O2-H2O...O4B_$2 0.84 2.30 2.9775(16) 137.4 O3-H3O...O2_$3 0.84 2.54 3.2151(16) 138.2 O3-H3O...O1B_$3 0.84 1.82 2.6362(15) 163.7 O4A-H4...O22_$3 0.88 2.17 2.9119(16) 141.1 N21-H21...O4B_$4 0.88 2.24 2.9261(18) 134.7 N23-H23...O1A_$5 FMAP and GRID set by program FMAP 2 1 9 GRID -4.167 -2 -2 4.167 2 2 R1 = 0.0318 for 1290 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.33 at 0.0721 0.5611 0.5594 [ 0.76 A from C4 ] Deepest hole -0.18 at 0.1536 0.1173 0.0623 [ 0.42 A from H3O ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 2474 / 17043 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.4279 0.4389 0.0594 1.00000 0.05 0.33 0.76 C4 0.77 C3 1.42 H3 1.72 O4A Q2 1 1.1151 0.5613 -0.0179 1.00000 0.05 0.32 0.75 C2 0.79 C1 1.44 H2 1.73 O1B Q3 1 0.7289 0.1962 0.1601 1.00000 0.05 0.22 0.55 H21 0.95 N21 1.97 C22 2.04 O4B Q4 1 1.2690 0.5031 0.0226 1.00000 0.05 0.20 0.75 C2 0.78 C3 1.41 H2 1.47 H3 Q5 1 1.4257 0.4411 -0.0065 1.00000 0.05 0.19 0.69 C3 0.73 O3 1.31 H3O 1.44 H3 Q6 1 1.0488 0.0790 0.2569 1.00000 0.05 0.19 0.75 C24 0.88 C25 1.24 H24A 1.36 H25B Q7 1 1.4202 0.4434 -0.0792 1.00000 0.05 0.17 0.82 O3 1.28 H3O 1.93 C3 2.27 H25A Q8 1 1.5361 0.3419 0.0814 1.00000 0.05 0.16 0.75 C4 0.80 O4B 1.86 C3 1.87 O4A Q9 1 1.0431 0.0355 0.1780 1.00000 0.05 0.15 0.59 H25B 0.85 C25 1.12 H25A 1.99 N21 Q10 1 0.5779 0.3890 0.2382 1.00000 0.05 0.14 0.80 O22 1.16 H4 1.74 C22 1.92 O4A Shortest distances between peaks (including symmetry equivalents) 4 5 1.17 1 8 1.19 1 5 1.20 2 4 1.25 1 4 1.26 5 7 1.33 6 9 1.50 7 9 1.93 5 8 1.97 2 5 2.07 4 7 2.11 3 7 2.27 3 8 2.29 2 7 2.31 3 9 2.35 4 8 2.40 1 2 2.51 3 10 2.52 1 7 2.53 3 6 2.73 6 10 2.76 8 10 2.91 9 10 2.94 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 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.44: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.55: Structure factors and derivatives 0.39: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + ssg0307 finished at 20:08:20 Total CPU time: 1.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++