+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + ssg0306 started at 16:44:19 on 05-Sep-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL ssg0306 in P2(1)/c CELL 0.67100 5.1062 18.1980 10.4320 90.000 97.060 90.000 ZERR 4.00 0.0011 0.0040 0.0020 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 28 48 8 28 V = 962.02 F(000) = 496.0 Mu = 0.15 mm-1 Cell Wt = 944.74 Rho = 1.631 MERG 2 SHEL 7 0.77 HTAB O4A O22 HTAB N23 O4B EQIV_$1 -x+1, y+1/2, -z+1/2 HTAB O1B O22_$1 EQIV_$2 x-1, y, z HTAB O2 O1A_$2 HTAB O3 O1A_$2 EQIV_$3 x, -y+1/2, z+1/2 HTAB N21 O2_$3 FMAP 2 PLAN 10 SIZE 0.01 0.05 0.10 ACTA MPLA C1 O1A O1B MPLA C4 O4A O4B BOND $H WGHT 0.06270 0.27140 L.S. 4 TEMP -153.00 FVAR 0.31469 MOLE 1 C1 1 0.636110 0.565759 0.160357 11.00000 0.01871 0.02201 = 0.01773 -0.00103 0.00794 0.00167 C2 1 0.505143 0.493260 0.187737 11.00000 0.01653 0.02229 = 0.02134 -0.00033 0.00473 0.00023 AFIX 13 H2 2 0.626665 0.452779 0.168262 11.00000 -1.20000 AFIX 0 C3 1 0.486176 0.491565 0.333740 11.00000 0.02154 0.02181 = 0.02036 0.00038 0.00577 0.00068 AFIX 13 H3 2 0.669687 0.490800 0.380003 11.00000 -1.20000 AFIX 0 C4 1 0.346254 0.422486 0.370457 11.00000 0.02133 0.02368 = 0.01755 0.00007 0.00494 0.00094 O1A 4 0.871472 0.575776 0.193274 11.00000 0.01961 0.02675 = 0.02980 0.00145 0.00573 -0.00134 O1B 4 0.475763 0.614976 0.103133 11.00000 0.02166 0.02218 = 0.02744 0.00428 0.00635 0.00010 AFIX 147 H1 2 0.559292 0.653996 0.093872 11.00000 0.04871 AFIX 0 O2 4 0.259220 0.481208 0.112050 11.00000 0.02001 0.02619 = 0.02293 -0.00221 0.00408 -0.00141 AFIX 147 H2O 2 0.152329 0.514107 0.127843 11.00000 -1.50000 AFIX 0 O3 4 0.358637 0.554939 0.373360 11.00000 0.02217 0.02365 = 0.02243 -0.00202 0.00666 0.00053 AFIX 147 H3O 2 0.194865 0.550643 0.353578 11.00000 -1.50000 AFIX 0 O4A 4 0.481241 0.362396 0.353478 11.00000 0.02438 0.02096 = 0.02647 0.00176 0.01064 -0.00056 AFIX 147 H4 2 0.397010 0.325601 0.374669 11.00000 0.02619 AFIX 0 O4B 4 0.131769 0.424347 0.408805 11.00000 0.02144 0.02517 = 0.03057 0.00253 0.01034 0.00058 MOLE 2 C22 1 0.123631 0.236734 0.513070 11.00000 0.01883 0.02282 = 0.02000 0.00061 0.00469 -0.00009 C24 1 -0.170297 0.277546 0.650030 11.00000 0.02297 0.02699 = 0.02333 0.00034 0.00865 0.00009 AFIX 23 H24A 2 -0.358234 0.292053 0.633138 11.00000 -1.20000 H24B 2 -0.086912 0.302884 0.728611 11.00000 -1.20000 AFIX 0 C25 1 -0.138801 0.193450 0.661466 11.00000 0.02217 0.02506 = 0.02373 0.00118 0.00800 -0.00022 AFIX 23 H25A 2 -0.097965 0.178014 0.752735 11.00000 -1.20000 H25B 2 -0.299915 0.167739 0.622290 11.00000 -1.20000 AFIX 0 N21 3 0.084270 0.179539 0.588703 11.00000 0.02533 0.02492 = 0.02742 0.00466 0.01310 0.00247 AFIX 43 H21 2 0.179238 0.139054 0.594111 11.00000 0.08191 AFIX 0 N23 3 -0.029818 0.292463 0.538639 11.00000 0.02978 0.02371 = 0.02817 0.00603 0.01448 0.00539 AFIX 43 H23 2 -0.045224 0.333546 0.493851 11.00000 0.04525 AFIX 0 O22 4 0.286413 0.238106 0.430465 11.00000 0.02367 0.02335 = 0.02442 0.00059 0.00963 -0.00027 HKLF 4 Covalent radii and connectivity table for ssg0306 in P2(1)/c 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 N23 N21 C24 - N23 C25 C25 - N21 C24 N21 - C22 C25 N23 - C22 C24 O22 - C22 Operators for generating equivalent atoms: $1 -x+1, y+1/2, -z+1/2 $2 x-1, y, z $3 x, -y+1/2, z+1/2 7990 Reflections read, of which 158 rejected -6 =< h =< 6, -22 =< k =< 22, -13 =< l =< 13, Max. 2-theta = 49.58 0 Systematic absence violations 0 Inconsistent equivalents 1961 Unique reflections, of which 0 suppressed R(int) = 0.0531 R(sigma) = 0.0474 Friedel opposites merged Maximum memory for data reduction = 1765 / 19594 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 = 2182 / 191448 wR2 = 0.1202 before cycle 1 for 1961 data and 153 / 153 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31452 0.00092 -0.179 OSF Mean shift/esd = 0.050 Maximum = -0.179 for OSF Max. shift = 0.003 A for H2O Max. dU =-0.001 for H23 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2182 / 191448 wR2 = 0.1202 before cycle 2 for 1961 data and 153 / 153 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31449 0.00092 -0.036 OSF Mean shift/esd = 0.016 Maximum = -0.055 for y C4 Max. shift = 0.001 A for H3O Max. dU = 0.000 for H23 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2182 / 191448 wR2 = 0.1202 before cycle 3 for 1961 data and 153 / 153 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31449 0.00092 -0.004 OSF Mean shift/esd = 0.001 Maximum = -0.007 for U33 N21 Max. shift = 0.000 A for H3O Max. dU = 0.000 for H23 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2182 / 191448 wR2 = 0.1202 before cycle 4 for 1961 data and 153 / 153 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31449 0.00092 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U33 N23 Max. shift = 0.000 A for H2O Max. dU = 0.000 for H21 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 0.6266 0.4528 0.1682 13 1.000 0.000 C2 O2 C1 C3 H3 0.6697 0.4908 0.3800 13 1.000 0.000 C3 O3 C4 C2 H1 0.5593 0.6540 0.0940 147 0.840 0.000 O1B C1 H1 H2O 0.1521 0.5140 0.1281 147 0.840 0.000 O2 C2 H2O H3O 0.1948 0.5506 0.3538 147 0.840 0.000 O3 C3 H3O H4 0.3971 0.3256 0.3748 147 0.840 0.000 O4A C4 H4 H24A -0.3583 0.2920 0.6331 23 0.990 0.000 C24 N23 C25 H24B -0.0870 0.3029 0.7286 23 0.990 0.000 C24 N23 C25 H25A -0.0980 0.1780 0.7528 23 0.990 0.000 C25 N21 C24 H25B -0.2999 0.1677 0.6223 23 0.990 0.000 C25 N21 C24 H21 0.1793 0.1390 0.5942 43 0.880 0.000 N21 C22 C25 H23 -0.0453 0.3336 0.4938 43 0.880 0.000 N23 C22 C24 ssg0306 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.63610 0.56576 0.16034 1.00000 0.01866 0.02199 0.01773 -0.00094 0.00790 0.00156 0.01899 0.00382 0.00039 0.00011 0.00020 0.00000 0.00101 0.00110 0.00106 0.00084 0.00080 0.00081 0.00045 C2 0.50514 0.49324 0.18771 1.00000 0.01651 0.02224 0.02129 -0.00035 0.00468 0.00020 0.01981 0.00375 0.00039 0.00011 0.00020 0.00000 0.00103 0.00107 0.00115 0.00084 0.00084 0.00081 0.00047 H2 0.62665 0.45275 0.16823 1.00000 0.02378 0.00000 0.00000 C3 0.48617 0.49157 0.33375 1.00000 0.02157 0.02178 0.02033 0.00044 0.00584 0.00060 0.02095 0.00393 0.00042 0.00011 0.00021 0.00000 0.00107 0.00107 0.00109 0.00086 0.00085 0.00084 0.00046 H3 0.66968 0.49082 0.38002 1.00000 0.02515 0.00000 0.00000 C4 0.34628 0.42246 0.37047 1.00000 0.02135 0.02355 0.01777 0.00022 0.00503 0.00095 0.02067 0.00387 0.00041 0.00012 0.00020 0.00000 0.00104 0.00110 0.00110 0.00088 0.00082 0.00088 0.00046 O1A 0.87148 0.57577 0.19328 1.00000 0.01956 0.02671 0.02977 0.00148 0.00572 -0.00132 0.02512 0.00278 0.00028 0.00008 0.00015 0.00000 0.00076 0.00083 0.00091 0.00067 0.00063 0.00063 0.00037 O1B 0.47577 0.61499 0.10315 1.00000 0.02163 0.02214 0.02737 0.00423 0.00636 0.00009 0.02344 0.00280 0.00028 0.00008 0.00015 0.00000 0.00076 0.00082 0.00087 0.00067 0.00063 0.00065 0.00037 H1 0.55926 0.65403 0.09400 1.00000 0.04783 0.00000 0.00873 O2 0.25919 0.48121 0.11204 1.00000 0.02000 0.02621 0.02287 -0.00217 0.00409 -0.00145 0.02290 0.00257 0.00027 0.00008 0.00014 0.00000 0.00076 0.00084 0.00083 0.00064 0.00062 0.00061 0.00036 H2O 0.15212 0.51400 0.12811 1.00000 0.03436 0.00000 0.00000 O3 0.35861 0.55493 0.37335 1.00000 0.02219 0.02365 0.02228 -0.00198 0.00667 0.00053 0.02238 0.00268 0.00029 0.00008 0.00014 0.00000 0.00075 0.00079 0.00084 0.00062 0.00062 0.00062 0.00036 H3O 0.19480 0.55056 0.35381 1.00000 0.03357 0.00000 0.00000 O4A 0.48123 0.36240 0.35347 1.00000 0.02432 0.02101 0.02636 0.00179 0.01064 -0.00052 0.02327 0.00279 0.00028 0.00008 0.00015 0.00000 0.00078 0.00079 0.00087 0.00065 0.00064 0.00064 0.00037 H4 0.39714 0.32561 0.37477 1.00000 0.02629 0.00000 0.00666 O4B 0.13176 0.42434 0.40880 1.00000 0.02148 0.02510 0.03057 0.00258 0.01038 0.00060 0.02512 0.00287 0.00029 0.00008 0.00015 0.00000 0.00077 0.00082 0.00091 0.00067 0.00064 0.00064 0.00037 C22 0.12368 0.23674 0.51307 1.00000 0.01882 0.02274 0.02013 0.00064 0.00476 -0.00007 0.02037 0.00385 0.00040 0.00011 0.00021 0.00000 0.00102 0.00109 0.00110 0.00086 0.00086 0.00084 0.00046 C24 -0.17033 0.27754 0.65000 1.00000 0.02295 0.02689 0.02330 0.00031 0.00866 0.00019 0.02390 0.00419 0.00043 0.00012 0.00022 0.00000 0.00108 0.00117 0.00118 0.00092 0.00090 0.00092 0.00049 H24A -0.35828 0.29203 0.63310 1.00000 0.02868 0.00000 0.00000 H24B -0.08699 0.30289 0.72858 1.00000 0.02868 0.00000 0.00000 C25 -0.13877 0.19345 0.66147 1.00000 0.02206 0.02506 0.02368 0.00116 0.00804 -0.00020 0.02317 0.00410 0.00042 0.00012 0.00022 0.00000 0.00107 0.00114 0.00116 0.00091 0.00089 0.00088 0.00048 H25A -0.09796 0.17803 0.75275 1.00000 0.02780 0.00000 0.00000 H25B -0.29986 0.16772 0.62230 1.00000 0.02780 0.00000 0.00000 N21 0.08432 0.17953 0.58874 1.00000 0.02531 0.02475 0.02742 0.00453 0.01304 0.00245 0.02501 0.00356 0.00036 0.00011 0.00018 0.00000 0.00095 0.00098 0.00105 0.00079 0.00078 0.00080 0.00044 H21 0.17931 0.13905 0.59417 1.00000 0.08120 0.00000 0.01221 N23 -0.02988 0.29248 0.53861 1.00000 0.02978 0.02366 0.02833 0.00596 0.01448 0.00533 0.02635 0.00367 0.00037 0.00010 0.00019 0.00000 0.00104 0.00099 0.00107 0.00085 0.00083 0.00081 0.00045 H23 -0.04533 0.33356 0.49382 1.00000 0.04413 0.00000 0.00808 O22 0.28644 0.23810 0.43048 1.00000 0.02370 0.02330 0.02441 0.00064 0.00965 -0.00020 0.02325 0.00278 0.00029 0.00008 0.00015 0.00000 0.00079 0.00079 0.00084 0.00063 0.00065 0.00061 0.00037 Final Structure Factor Calculation for ssg0306 in P2(1)/c Total number of l.s. parameters = 153 Maximum vector length = 511 Memory required = 2029 / 22995 wR2 = 0.1202 before cycle 5 for 1961 data and 0 / 153 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0439 for 1444 Fo > 4sig(Fo) and 0.0668 for all 1961 data wR2 = 0.1202, GooF = S = 1.029, Restrained GooF = 1.029 for all data Occupancy sum of asymmetric unit = 16.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0235 0.0221 0.0114 C1 0.0224 0.0218 0.0152 C2 0.0241 0.0216 0.0172 C3 0.0241 0.0219 0.0160 C4 0.0305 0.0267 0.0181 O1A 0.0304 0.0218 0.0182 O1B 0.0276 0.0219 0.0192 O2 0.0262 0.0238 0.0172 O3 0.0322 0.0215 0.0161 O4A 0.0344 0.0245 0.0164 O4B 0.0229 0.0215 0.0167 C22 0.0284 0.0268 0.0165 C24 0.0278 0.0250 0.0167 C25 0.0370 0.0231 0.0149 N21 0.0419 0.0207 0.0165 N23 0.0300 0.0233 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 0.013 0.026 0.038 0.053 0.070 0.090 0.113 0.147 0.212 1.000 Number in group 209. 194. 187. 205. 188. 193. 196. 198. 195. 196. GooF 0.765 0.923 0.981 1.072 1.106 1.231 1.050 1.006 0.963 1.141 K 1.205 0.775 0.877 1.017 1.057 1.040 1.034 0.994 0.997 0.975 Resolution(A) 0.80 0.83 0.86 0.90 0.95 1.01 1.09 1.19 1.37 1.69 inf Number in group 208. 187. 193. 196. 198. 201. 190. 202. 191. 195. GooF 0.819 0.924 0.919 1.006 0.900 1.013 0.961 1.047 1.080 1.486 K 0.978 0.989 0.967 0.968 1.005 1.007 1.015 1.015 1.016 0.957 R1 0.133 0.116 0.116 0.111 0.075 0.059 0.053 0.047 0.033 0.043 Recommended weighting scheme: WGHT 0.0630 0.2636 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) 1 0 0 488.22 700.43 4.79 0.246 5.07 2 1 2 56.04 32.53 4.03 0.053 2.16 3 5 0 99.33 64.94 3.98 0.075 1.53 0 13 4 70.74 44.02 3.60 0.062 1.23 0 1 6 84.32 57.54 3.48 0.070 1.72 -1 4 2 812.66 1032.53 3.47 0.298 2.95 0 6 5 50.82 73.86 3.32 0.080 1.71 -2 2 2 133.17 100.30 3.28 0.093 2.32 0 19 1 255.60 194.38 3.26 0.130 0.95 1 5 4 20.93 35.26 3.09 0.055 1.88 -2 10 1 63.76 42.80 3.04 0.061 1.48 0 4 1 1316.88 1637.55 3.00 0.376 4.17 0 13 1 110.43 80.03 2.97 0.083 1.39 3 8 2 128.26 95.92 2.96 0.091 1.28 -2 3 1 41.06 27.10 2.95 0.048 2.34 1 7 5 125.09 95.40 2.94 0.091 1.50 -6 0 4 381.07 286.24 2.89 0.157 0.83 0 9 3 51.46 32.72 2.86 0.053 1.74 1 4 0 438.54 537.27 2.85 0.215 3.39 -1 3 2 582.76 706.99 2.76 0.247 3.26 0 3 2 7421.43 8905.66 2.75 0.877 3.94 -2 2 6 116.54 88.71 2.75 0.087 1.49 -3 2 1 69.16 48.11 2.75 0.064 1.67 -1 9 4 162.04 129.97 2.67 0.106 1.55 0 8 4 92.93 71.27 2.67 0.078 1.71 2 1 10 132.37 192.14 2.66 0.129 0.92 1 1 1 604.99 728.07 2.65 0.251 4.23 -1 4 10 64.22 41.69 2.64 0.060 1.01 2 1 1 131.68 104.14 2.63 0.095 2.37 0 0 8 94.33 63.26 2.60 0.074 1.29 4 15 2 175.07 222.09 2.59 0.138 0.85 2 5 0 288.07 349.18 2.59 0.174 2.08 -2 7 2 40.55 27.61 2.58 0.049 1.76 1 3 3 18.56 29.27 2.57 0.050 2.47 -2 16 3 28.79 12.67 2.55 0.033 1.01 0 1 11 379.43 311.47 2.54 0.164 0.94 -2 14 4 23.80 39.07 2.51 0.058 1.08 -4 14 1 108.11 68.36 2.50 0.077 0.91 -1 10 11 165.79 221.13 2.47 0.138 0.84 -1 6 5 76.73 57.98 2.47 0.071 1.67 0 7 3 109.89 87.66 2.46 0.087 2.08 1 3 0 1246.40 1471.07 2.46 0.356 3.89 2 10 8 -5.65 8.43 2.46 0.027 0.94 5 8 5 -3.06 11.13 2.45 0.031 0.81 -1 5 1 514.03 609.55 2.41 0.229 2.90 -2 18 2 43.98 68.32 2.39 0.077 0.93 0 4 4 221.36 266.14 2.37 0.152 2.25 0 5 3 125.81 101.70 2.37 0.094 2.50 -5 12 1 135.56 102.13 2.34 0.094 0.85 6 5 0 155.41 196.41 2.33 0.130 0.82 Bond lengths and angles C1 - Distance Angles O1A 1.2224 (0.0025) O1B 1.3072 (0.0026) 124.41 (0.19) C2 1.5223 (0.0028) 121.06 (0.19) 114.51 (0.17) C1 - O1A O1B C2 - Distance Angles O2 1.4158 (0.0024) C1 1.5223 (0.0028) 114.17 (0.17) C3 1.5388 (0.0029) 112.93 (0.16) 106.58 (0.17) H2 1.0000 107.62 107.62 107.62 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4109 (0.0025) C4 1.5185 (0.0029) 110.77 (0.17) C2 1.5388 (0.0029) 111.18 (0.17) 110.79 (0.17) H3 1.0000 107.99 107.99 107.99 C3 - O3 C4 C2 C4 - Distance Angles O4B 1.2119 (0.0025) O4A 1.3156 (0.0025) 125.28 (0.20) C3 1.5185 (0.0029) 122.15 (0.19) 112.56 (0.17) C4 - O4B O4A O1A - Distance Angles C1 1.2224 (0.0025) O1A - O1B - Distance Angles C1 1.3072 (0.0026) H1 0.8400 109.47 O1B - C1 O2 - Distance Angles C2 1.4158 (0.0024) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4109 (0.0025) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.3156 (0.0025) H4 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2119 (0.0025) O4B - C22 - Distance Angles O22 1.2687 (0.0025) N23 1.3290 (0.0027) 124.97 (0.20) N21 1.3366 (0.0027) 125.09 (0.19) 109.93 (0.18) C22 - O22 N23 C24 - Distance Angles N23 1.4640 (0.0028) C25 1.5419 (0.0031) 100.91 (0.17) H24A 0.9900 111.59 111.59 H24B 0.9900 111.59 111.59 109.39 C24 - N23 C25 H24A C25 - Distance Angles N21 1.4663 (0.0028) C24 1.5419 (0.0031) 102.22 (0.17) H25A 0.9900 111.32 111.32 H25B 0.9900 111.32 111.32 109.21 C25 - N21 C24 H25A N21 - Distance Angles C22 1.3366 (0.0027) C25 1.4663 (0.0028) 110.72 (0.18) H21 0.8800 124.64 124.64 N21 - C22 C25 N23 - Distance Angles C22 1.3290 (0.0027) C24 1.4640 (0.0028) 112.09 (0.18) H23 0.8800 123.96 123.96 N23 - C22 C24 O22 - Distance Angles C22 1.2687 (0.0025) O22 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.81 2.636(2) 167.6 O4A-H4...O22 0.88 2.13 2.924(2) 150.0 N23-H23...O4B 0.84 1.75 2.593(2) 176.1 O1B-H1...O22_$1 0.84 2.00 2.830(2) 167.4 O2-H2O...O1A_$2 0.84 2.25 2.951(2) 141.2 O3-H3O...O1A_$2 0.88 2.23 3.059(2) 157.0 N21-H21...O2_$3 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 1.6015 (0.0093) x + 5.9685 (0.0637) y + 9.6276 (0.0102) z = 3.9017 (0.0415) * 0.0000 (0.0000) C1 * 0.0000 (0.0000) O1A * 0.0000 (0.0000) O1B Rms deviation of fitted atoms = 0.0000 1.6781 (0.0109) x + 1.1278 (0.0658) y + 9.3354 (0.0127) z = 4.5160 (0.0250) Angle to previous plane (with approximate esd) = 40.79 ( 0.17 ) * 0.0000 (0.0000) C4 * 0.0000 (0.0000) O4A * 0.0000 (0.0000) O4B Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 1 14 GRID -4.545 24 -2 4.545 1 2 R1 = 0.0667 for 1961 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.37 at 0.1061 0.3688 0.0723 [ 0.44 A from H21 ] Deepest hole -0.25 at 0.2389 0.3564 0.1226 [ 0.41 A from H21 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2407 / 21307 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1061 0.1312 0.5723 1.00000 0.05 0.37 0.44 H21 0.91 N21 2.00 C25 2.02 C22 Q2 1 0.0556 0.3492 0.5380 1.00000 0.05 0.22 0.71 H23 1.12 N23 1.99 O4B 2.10 C22 Q3 1 0.1510 0.6195 0.3911 1.00000 0.05 0.21 1.34 H3O 1.61 O3 1.62 H23 1.89 H24B Q4 1 0.0510 0.2472 0.3751 1.00000 0.05 0.21 1.28 O22 1.45 C22 1.84 H24B 1.95 H25A Q5 1 0.6229 0.4697 0.1468 1.00000 0.05 0.20 0.38 H2 0.89 C2 1.75 C1 1.86 O2 Q6 1 0.1067 0.1075 0.4882 1.00000 0.05 0.20 1.26 H21 1.69 N21 2.00 O1A 2.15 O2 Q7 1 -0.0729 0.0889 0.4922 1.00000 0.05 0.19 1.81 H21 1.86 H2O 2.05 N21 2.22 O1B Q8 1 0.4850 0.4868 0.2601 1.00000 0.05 0.19 0.77 C3 0.78 C2 1.41 H2 1.47 H3 Q9 1 0.0918 0.6306 0.0766 1.00000 0.05 0.18 1.97 O1B 2.02 O1A 2.05 N21 2.12 H21 Q10 1 0.6469 0.4984 0.3482 1.00000 0.05 0.18 0.37 H3 0.83 C3 1.74 C2 1.84 O3 Shortest distances between peaks (including symmetry equivalents) 1 6 0.98 6 7 0.98 7 9 1.04 8 10 1.18 6 9 1.22 1 7 1.39 2 3 1.47 5 8 1.48 1 9 1.75 5 10 2.15 4 9 2.32 2 4 2.51 5 7 2.60 4 6 2.80 1 4 2.94 Time profile in seconds ----------------------- 0.05: 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. 0.45: 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 0.33: Structure factors and derivatives 0.31: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: 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 0.05: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + ssg0306 finished at 16:44:21 Total CPU time: 1.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++