+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04skc0006p21 started at 11:45:42 on 13-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04skc0006p21 in P2(1) CELL 0.71073 5.2139 11.1399 7.4889 90.000 95.315 90.000 ZERR 2.00 0.0017 0.0065 0.0029 0.000 0.033 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O UNIT 10 26 2 14 V = 433.10 F(000) = 212.0 Mu = 0.14 mm-1 Cell Wt = 398.33 Rho = 1.527 MERG 4 OMIT -3.00 55.00 SHEL 7 0.77 DFIX 0.84 0.02 O1W H1W O1W H2W DANG 1.35 0.02 H1W H2W HTAB O2 O1B HTAB N22 O1B HTAB N22 O1W HTAB O1W O4B HTAB O1W O3 EQIV_$1 x+1, y, z HTAB O2 O1A_$1 EQIV_$2 x-1, y, z HTAB O3 O1W_$2 EQIV_$3 x, y, z-1 HTAB O4A O1B_$3 HTAB O4A O1A_$3 EQIV_$4 -x, y+1/2, -z+1 HTAB N22 O1A_$4 EQIV_$5 -x+1, y+1/2, -z HTAB O1W O2_$5 FMAP 2 PLAN 5 SIZE 0.04 0.10 0.10 ACTA BOND $H WGHT 0.05760 L.S. 4 TEMP -153.00 FVAR 1.55398 MOLE 1 C1 1 -0.003625 0.658869 0.324674 11.00000 0.02069 0.01529 = 0.02216 0.00308 -0.00159 0.00332 C2 1 0.070134 0.659517 0.133948 11.00000 0.01727 0.02248 = 0.01651 -0.00112 -0.00098 -0.00004 AFIX 13 H2 2 0.018611 0.580986 0.076691 11.00000 -1.20000 AFIX 0 C3 1 -0.074288 0.759941 0.028413 11.00000 0.02146 0.01737 = 0.02010 -0.00086 0.00189 -0.00083 AFIX 13 H3 2 -0.261509 0.739409 0.009037 11.00000 -1.20000 AFIX 0 C4 1 0.035649 0.772076 -0.151450 11.00000 0.01916 0.02239 = 0.02015 0.00141 -0.00047 0.00171 O1A 4 -0.226458 0.629701 0.350445 11.00000 0.01848 0.02661 = 0.02318 0.00153 -0.00107 -0.00120 O1B 4 0.171432 0.689083 0.445545 11.00000 0.01848 0.03476 = 0.02051 0.00132 -0.00099 -0.00372 O2 4 0.338681 0.676598 0.122970 11.00000 0.01579 0.03456 = 0.01805 0.00150 0.00066 0.00236 AFIX 147 H2O 2 0.416495 0.672341 0.226128 11.00000 -1.50000 AFIX 0 O3 4 -0.042408 0.867233 0.129263 11.00000 0.02249 0.02006 = 0.02684 -0.00250 -0.00109 0.00461 AFIX 147 H3O 2 -0.174970 0.909896 0.110275 11.00000 -1.50000 AFIX 0 O4A 4 0.002391 0.674606 -0.248199 11.00000 0.03844 0.02645 = 0.01814 -0.00039 0.00390 -0.00729 AFIX 147 H4 2 0.053994 0.686487 -0.349700 11.00000 -1.50000 AFIX 0 O4B 4 0.140646 0.861984 -0.199662 11.00000 0.03216 0.02707 = 0.02336 -0.00068 0.00452 -0.00530 MOLE 2 C21 1 0.597380 0.903973 0.517465 11.00000 0.02376 0.03319 = 0.03526 -0.00673 0.00238 0.00410 AFIX 137 H21A 2 0.729380 0.966384 0.514474 11.00000 -1.50000 H21B 2 0.655392 0.830924 0.460381 11.00000 -1.50000 H21C 2 0.568217 0.886587 0.642261 11.00000 -1.50000 AFIX 0 N22 3 0.354643 0.946262 0.419798 11.00000 0.02476 0.02619 = 0.02949 -0.00499 0.00160 -0.00112 AFIX 137 H22A 2 0.236585 0.885888 0.413686 11.00000 -1.50000 H22B 2 0.384989 0.968927 0.306923 11.00000 -1.50000 H22C 2 0.292996 1.009992 0.478688 11.00000 -1.50000 AFIX 0 MOLE 3 O1W 4 0.493116 0.981491 0.061172 11.00000 0.02350 0.02276 = 0.02964 0.00288 -0.00115 -0.00103 H1W 2 0.528638 1.044188 0.006596 11.00000 0.02615 H2W 2 0.376286 0.945449 0.002191 11.00000 0.06271 HKLF 4 Covalent radii and connectivity table for 04skc0006p21 in P2(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 C21 - N22 N22 - C21 O1W - no bonds found Operators for generating equivalent atoms: $1 x+1, y, z $2 x-1, y, z $3 x, y, z-1 $4 -x, y+1/2, -z+1 $5 -x+1, y+1/2, -z Floating origin restraints generated 4139 Reflections read, of which 27 rejected -6 =< h =< 5, -14 =< k =< 12, -9 =< l =< 8, Max. 2-theta = 54.88 0 Systematic absence violations 0 Inconsistent equivalents 1040 Unique reflections, of which 0 suppressed R(int) = 0.0818 R(sigma) = 0.0844 Friedel opposites merged Maximum memory for data reduction = 1793 / 10147 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 = 2158 / 165785 wR2 = 0.1137 before cycle 1 for 1040 data and 131 / 131 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.042; Restrained GooF = 1.040 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0576 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.55367 0.00617 -0.050 OSF Mean shift/esd = 0.050 Maximum = -0.185 for tors H4 Max. shift = 0.008 A for H4 Max. dU = 0.001 for H1W Least-squares cycle 2 Maximum vector length = 511 Memory required = 2158 / 165785 wR2 = 0.1137 before cycle 2 for 1040 data and 131 / 131 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.011 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.041; Restrained GooF = 1.039 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0576 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.55358 0.00617 -0.016 OSF Mean shift/esd = 0.017 Maximum = -0.067 for y O1A Max. shift = 0.002 A for H3O Max. dU = 0.001 for H1W Least-squares cycle 3 Maximum vector length = 511 Memory required = 2158 / 165785 wR2 = 0.1137 before cycle 3 for 1040 data and 131 / 131 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.011 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.041; Restrained GooF = 1.039 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0576 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.55355 0.00617 -0.004 OSF Mean shift/esd = 0.002 Maximum = 0.014 for z H1W Max. shift = 0.001 A for H1W Max. dU = 0.000 for H2W Least-squares cycle 4 Maximum vector length = 511 Memory required = 2158 / 165785 wR2 = 0.1137 before cycle 4 for 1040 data and 131 / 131 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.011 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.041; Restrained GooF = 1.039 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0576 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.55355 0.00617 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.003 for x H1W Max. shift = 0.000 A for H1W Max. dU = 0.000 for H1W Largest correlation matrix elements -0.652 y H2W / x H2W Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0186 0.5810 0.0766 13 1.000 0.000 C2 O2 C1 C3 H3 -0.2615 0.7395 0.0091 13 1.000 0.000 C3 O3 C4 C2 H2O 0.4165 0.6721 0.2261 147 0.840 0.000 O2 C2 H2O H3O -0.1755 0.9096 0.1110 147 0.840 0.000 O3 C3 H3O H4 0.0524 0.6867 -0.3502 147 0.840 0.000 O4A C4 H4 H21A 0.7294 0.9664 0.5147 137 0.980 0.000 C21 N22 H21A H21B 0.6555 0.8309 0.4603 137 0.980 0.000 C21 N22 H21A H21C 0.5681 0.8865 0.6423 137 0.980 0.000 C21 N22 H21A H22A 0.2364 0.8860 0.4138 137 0.910 0.000 N22 C21 H22A H22B 0.3850 0.9688 0.3068 137 0.910 0.000 N22 C21 H22A H22C 0.2931 1.0101 0.4785 137 0.910 0.000 N22 C21 H22A 04skc0006p21 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.00358 0.65886 0.32473 1.00000 0.02066 0.01552 0.02211 0.00310 -0.00174 0.00333 0.01966 0.00635 0.00069 0.00033 0.00045 0.00000 0.00206 0.00197 0.00186 0.00158 0.00146 0.00162 0.00082 C2 0.07017 0.65951 0.13391 1.00000 0.01767 0.02243 0.01635 -0.00118 -0.00083 -0.00002 0.01897 0.00613 0.00065 0.00035 0.00042 0.00000 0.00200 0.00214 0.00176 0.00158 0.00137 0.00168 0.00081 H2 0.01863 0.58099 0.07662 1.00000 0.02276 0.00000 0.00000 C3 -0.07424 0.75999 0.02843 1.00000 0.02111 0.01740 0.02014 -0.00076 0.00195 -0.00100 0.01955 0.00657 0.00074 0.00033 0.00044 0.00000 0.00235 0.00199 0.00182 0.00156 0.00145 0.00160 0.00086 H3 -0.26147 0.73946 0.00909 1.00000 0.02346 0.00000 0.00000 C4 0.03559 0.77211 -0.15155 1.00000 0.01919 0.02223 0.02018 0.00163 -0.00042 0.00173 0.02067 0.00665 0.00075 0.00036 0.00045 0.00000 0.00226 0.00212 0.00186 0.00171 0.00145 0.00173 0.00085 O1A -0.22647 0.62964 0.35044 1.00000 0.01864 0.02659 0.02324 0.00168 -0.00104 -0.00117 0.02301 0.00417 0.00048 0.00023 0.00031 0.00000 0.00152 0.00157 0.00125 0.00113 0.00097 0.00121 0.00064 O1B 0.17143 0.68908 0.44553 1.00000 0.01875 0.03456 0.02049 0.00128 -0.00083 -0.00373 0.02477 0.00450 0.00048 0.00027 0.00030 0.00000 0.00144 0.00168 0.00132 0.00119 0.00100 0.00118 0.00065 O2 0.33865 0.67659 0.12299 1.00000 0.01577 0.03456 0.01794 0.00129 0.00068 0.00251 0.02281 0.00451 0.00045 0.00026 0.00030 0.00000 0.00138 0.00156 0.00119 0.00126 0.00096 0.00124 0.00063 H2O 0.41647 0.67214 0.22613 1.00000 0.03422 0.00000 0.00000 O3 -0.04241 0.86724 0.12926 1.00000 0.02249 0.02003 0.02661 -0.00247 -0.00115 0.00456 0.02325 0.00454 0.00053 0.00022 0.00034 0.00000 0.00156 0.00146 0.00134 0.00110 0.00110 0.00118 0.00063 H3O -0.17549 0.90963 0.11097 1.00000 0.03488 0.00000 0.00000 O4A 0.00243 0.67461 -0.24823 1.00000 0.03839 0.02627 0.01823 -0.00032 0.00377 -0.00736 0.02756 0.00455 0.00052 0.00024 0.00031 0.00000 0.00172 0.00167 0.00131 0.00122 0.00113 0.00133 0.00068 H4 0.05240 0.68673 -0.35016 1.00000 0.04134 0.00000 0.00000 O4B 0.14058 0.86198 -0.19965 1.00000 0.03223 0.02711 0.02340 -0.00081 0.00445 -0.00528 0.02746 0.00484 0.00056 0.00024 0.00035 0.00000 0.00176 0.00165 0.00139 0.00123 0.00117 0.00137 0.00069 C21 0.59739 0.90394 0.51752 1.00000 0.02392 0.03304 0.03515 -0.00666 0.00257 0.00389 0.03071 0.00771 0.00080 0.00040 0.00055 0.00000 0.00222 0.00250 0.00226 0.00195 0.00180 0.00186 0.00101 H21A 0.72937 0.96637 0.51470 1.00000 0.04607 0.00000 0.00000 H21B 0.65551 0.83094 0.46035 1.00000 0.04607 0.00000 0.00000 H21C 0.56810 0.88645 0.64226 1.00000 0.04607 0.00000 0.00000 N22 0.35462 0.94628 0.41976 1.00000 0.02482 0.02611 0.02952 -0.00491 0.00153 -0.00105 0.02688 0.00622 0.00067 0.00032 0.00046 0.00000 0.00192 0.00192 0.00164 0.00148 0.00136 0.00150 0.00079 H22A 0.23643 0.88597 0.41379 1.00000 0.04032 0.00000 0.00000 H22B 0.38498 0.96882 0.30684 1.00000 0.04032 0.00000 0.00000 H22C 0.29314 1.01010 0.47854 1.00000 0.04032 0.00000 0.00000 O1W 0.49302 0.98150 0.06111 1.00000 0.02354 0.02268 0.02950 0.00284 -0.00090 -0.00080 0.02545 0.00499 0.00056 0.00026 0.00035 0.00000 0.00164 0.00170 0.00142 0.00127 0.00118 0.00127 0.00069 H1W 0.52770 1.04438 0.00666 1.00000 0.02811 0.06516 0.00833 0.00259 0.00499 0.00000 0.01226 H2W 0.37590 0.94546 0.00189 1.00000 0.06247 0.03937 0.00818 0.00388 0.00603 0.00000 0.01946 Final Structure Factor Calculation for 04skc0006p21 in P2(1) Total number of l.s. parameters = 131 Maximum vector length = 511 Memory required = 2029 / 25046 wR2 = 0.1137 before cycle 5 for 1040 data and 2 / 131 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.011 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.041; Restrained GooF = 1.039 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0576 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0558 for 802 Fo > 4sig(Fo) and 0.0826 for all 1040 data wR2 = 0.1137, GooF = S = 1.041, Restrained GooF = 1.039 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0256 0.0212 0.0122 C1 0.0227 0.0196 0.0146 C2 0.0214 0.0202 0.0170 C3 0.0232 0.0222 0.0167 C4 0.0281 0.0235 0.0174 O1A 0.0357 0.0218 0.0168 O1B 0.0349 0.0183 0.0151 O2 0.0310 0.0222 0.0165 O3 0.0419 0.0228 0.0180 O4A 0.0357 0.0240 0.0227 O4B 0.0415 0.0289 0.0217 C21 0.0331 0.0254 0.0221 N22 0.0323 0.0225 0.0216 O1W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.031 0.044 0.057 0.069 0.085 0.103 0.129 0.163 0.230 1.000 Number in group 108. 104. 101. 107. 100. 105. 105. 104. 102. 104. GooF 0.955 0.971 1.215 1.116 1.033 1.020 1.004 1.002 1.035 1.042 K 1.251 1.379 1.554 1.207 1.102 0.985 1.023 1.013 1.009 1.007 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.17 1.33 1.69 inf Number in group 105. 103. 104. 106. 102. 105. 104. 103. 104. 104. GooF 1.086 1.042 0.926 1.085 1.032 1.100 0.876 0.917 1.075 1.221 K 1.180 1.146 1.194 1.059 1.019 1.067 0.997 1.014 1.018 1.001 R1 0.235 0.208 0.172 0.126 0.094 0.090 0.040 0.033 0.033 0.033 Recommended weighting scheme: WGHT 0.0590 0.0000 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 1 4 7.66 1.71 4.39 0.021 1.57 -2 1 9 1.84 12.45 3.96 0.057 0.81 -2 0 1 44.32 26.37 3.40 0.083 2.53 -4 7 4 178.77 139.45 3.40 0.191 0.91 -5 2 1 20.65 36.45 3.34 0.098 1.02 -2 2 7 24.67 31.78 2.84 0.091 1.00 -3 4 7 35.59 18.01 2.82 0.069 0.90 0 1 2 87.06 71.96 2.82 0.137 3.54 4 11 0 27.46 10.07 2.81 0.051 0.80 -3 7 6 28.78 12.15 2.74 0.056 0.88 2 1 3 125.72 106.38 2.70 0.167 1.70 -1 0 7 17.48 8.18 2.68 0.046 1.06 -3 5 7 50.17 33.49 2.64 0.093 0.87 -3 0 3 0.87 6.01 2.58 0.040 1.49 5 7 3 95.19 59.25 2.57 0.124 0.80 -5 1 2 17.21 24.90 2.55 0.081 1.02 -1 3 8 27.77 13.34 2.47 0.059 0.90 2 1 4 308.83 267.84 2.34 0.264 1.44 5 9 1 25.43 10.01 2.33 0.051 0.79 -2 2 3 63.15 73.44 2.30 0.138 1.79 -2 5 6 23.29 29.53 2.27 0.088 1.03 1 0 0 1505.65 1771.99 2.26 0.680 5.19 2 10 5 -2.18 12.55 2.26 0.057 0.83 0 10 5 30.56 15.01 2.25 0.063 0.89 2 0 3 14.41 10.37 2.22 0.052 1.72 6 1 0 -7.70 4.75 2.21 0.035 0.86 -2 1 8 31.36 40.21 2.21 0.102 0.90 0 12 4 27.14 12.53 2.20 0.057 0.83 2 1 2 71.32 62.29 2.17 0.127 2.01 4 7 2 99.40 79.24 2.17 0.144 0.95 4 2 5 165.91 139.52 2.17 0.191 0.92 -3 5 8 23.65 7.63 2.15 0.045 0.80 3 2 8 14.01 27.06 2.11 0.084 0.78 -2 0 3 81.79 68.85 2.11 0.134 1.88 -4 8 2 13.05 20.05 2.11 0.072 0.94 -1 4 7 3.87 10.17 2.10 0.052 0.99 -4 1 8 82.41 66.13 2.10 0.131 0.79 2 12 2 -1.77 6.74 2.08 0.042 0.85 1 1 6 103.88 118.74 2.08 0.176 1.18 -3 2 7 51.84 41.90 2.06 0.105 0.93 1 2 7 216.88 10.29 2.06 0.052 1.01 -1 3 4 48.96 56.38 2.05 0.121 1.63 -3 6 4 2.72 6.44 2.05 0.041 1.08 -1 0 1 135.39 158.88 2.03 0.204 4.46 4 5 4 12.49 5.52 2.02 0.038 0.93 -5 0 2 16.54 7.63 1.99 0.045 1.03 -4 6 7 37.08 24.70 1.99 0.080 0.78 5 1 3 6.52 0.03 1.96 0.003 0.92 -1 9 4 230.12 16.95 1.95 0.066 1.02 3 2 1 579.78 508.43 1.93 0.364 1.58 Bond lengths and angles C1 - Distance Angles O1A 1.2389 (0.0041) O1B 1.2694 (0.0040) 125.56 (0.31) C2 1.5139 (0.0047) 118.16 (0.30) 116.28 (0.30) C1 - O1A O1B C2 - Distance Angles O2 1.4225 (0.0040) C1 1.5139 (0.0047) 113.09 (0.26) C3 1.5276 (0.0050) 108.23 (0.29) 109.60 (0.28) H2 1.0000 108.61 108.61 108.61 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4149 (0.0045) C4 1.5185 (0.0053) 111.31 (0.29) C2 1.5276 (0.0050) 108.36 (0.26) 108.41 (0.29) H3 1.0000 109.58 109.58 109.58 C3 - O3 C4 C2 C4 - Distance Angles O4B 1.2117 (0.0046) O4A 1.3079 (0.0048) 124.18 (0.33) C3 1.5185 (0.0053) 123.72 (0.33) 112.10 (0.31) C4 - O4B O4A O1A - Distance Angles C1 1.2389 (0.0042) O1A - O1B - Distance Angles C1 1.2694 (0.0040) O1B - O2 - Distance Angles C2 1.4225 (0.0040) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4149 (0.0045) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.3079 (0.0048) H4 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2117 (0.0046) O4B - C21 - Distance Angles N22 1.4795 (0.0056) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - N22 H21A H21B N22 - Distance Angles C21 1.4795 (0.0056) H22A 0.9100 109.47 H22B 0.9100 109.47 109.47 H22C 0.9100 109.47 109.47 109.47 N22 - C21 H22A H22B O1W - Distance Angles H1W 0.8386 (0.0191) H2W 0.8250 (0.0195) 109.10 (3.04) O1W - H1W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.18 2.646(3) 114.9 O2-H2O...O1B 0.91 2.24 3.032(5) 145.9 N22-H22A...O1B 0.91 1.98 2.872(4) 166.6 N22-H22B...O1W 0.82(2) 2.07(3) 2.881(4) 165(5) O1W-H2W...O4B 0.82(2) 2.61(4) 3.152(4) 125(4) O1W-H2W...O3 0.84 2.06 2.757(3) 140.3 O2-H2O...O1A_$1 0.84 1.91 2.742(4) 170.5 O3-H3O...O1W_$2 0.84 1.70 2.537(4) 171.1 O4A-H4...O1B_$3 0.84 2.63 3.169(4) 122.8 O4A-H4...O1A_$3 0.91 1.90 2.792(4) 165.3 N22-H22C...O1A_$4 0.839(19) 1.93(2) 2.760(4) 171(5) O1W-H1W...O2_$5 FMAP and GRID set by program FMAP 2 1 15 GRID -4.167 -2 -2 4.167 2 2 R1 = 0.0826 for 1040 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.25 at 0.4159 0.8464 0.7717 [ 1.38 A from H21C ] Deepest hole -0.30 at 0.0082 0.1412 0.5785 [ 0.75 A from C1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2103 / 15165 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4159 0.8464 0.7717 1.00000 0.05 0.25 1.38 H21C 1.48 O4B 2.07 H2W 2.27 C4 Q2 1 -0.3578 0.7260 0.0543 1.00000 0.05 0.25 0.65 H3 1.56 C3 1.80 O2 1.92 H2O Q3 1 0.4974 1.1363 0.5053 1.00000 0.05 0.25 1.76 H22C 1.83 O1B 1.86 O1A 2.06 H2O Q4 1 0.5822 1.1197 -0.0444 1.00000 0.05 0.25 0.98 H1W 0.98 O2 1.48 H2O 1.81 O1W Q5 1 0.3012 0.7481 0.1892 1.00000 0.05 0.24 0.97 O2 1.06 H2O 1.58 C2 2.19 O1B Shortest distances between peaks (including symmetry equivalents) 2 4 1.66 4 5 1.93 2 5 2.14 1 2 2.68 3 5 2.73 Time profile in seconds ----------------------- 0.08: 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. 0.20: 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 0.16: Structure factors and derivatives 0.14: 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 0.02: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04skc0006p21 finished at 11:45:43 Total CPU time: 0.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++