+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 15:57:34 on 13-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1)/n CELL 0.71073 5.1010 18.7081 13.7459 90.000 90.676 90.000 ZERR 4.00 0.0002 0.0008 0.0007 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N BR O UNIT 48 76 8 4 4 V = 1311.68 F(000) = 592.0 Mu = 3.12 mm-1 Cell Wt = 1148.81 Rho = 1.454 MERG 2 ACTA SHEL 7 0.84 TEMP -153 SIZE 0.2 0.2 0.2 FMAP 2 PLAN 20 BOND WGHT 0.05290 0.32650 L.S. 8 BOND $H FVAR 0.64325 BR1 4 0.219476 0.835347 0.470685 11.00000 0.02520 0.03283 = 0.03008 -0.00092 -0.00149 0.00152 C7 1 -0.747988 0.663321 0.144129 11.00000 0.02495 0.02311 = 0.02133 0.00057 0.00196 -0.00163 N1 3 -0.641490 0.599503 0.163046 11.00000 0.02127 0.01699 = 0.03010 -0.00244 -0.00108 -0.00158 N2 3 -0.630518 0.713432 0.196894 11.00000 0.02267 0.01832 = 0.02521 -0.00055 0.00140 -0.00167 C4 1 -0.077511 0.662699 0.359724 11.00000 0.02572 0.02435 = 0.02565 -0.00239 -0.00101 -0.00324 C5 1 -0.254775 0.709840 0.318885 11.00000 0.02581 0.01984 = 0.02463 -0.00099 0.00160 -0.00292 C3 1 -0.083702 0.589250 0.336518 11.00000 0.02624 0.02337 = 0.02835 0.00400 -0.00045 0.00462 C2 1 -0.262992 0.561247 0.271670 11.00000 0.02663 0.01742 = 0.03124 -0.00075 0.00334 -0.00153 C9 1 -0.690236 0.790373 0.198451 11.00000 0.03036 0.01583 = 0.02886 -0.00269 -0.00349 0.00193 C12 1 -1.134456 0.912908 0.042428 11.00000 0.03103 0.02524 = 0.04036 0.00237 -0.00278 0.00503 C1 1 -0.440317 0.608723 0.230044 11.00000 0.02375 0.01939 = 0.02395 0.00032 0.00064 -0.00397 C8 1 -0.714187 0.532175 0.114891 11.00000 0.03421 0.01985 = 0.03584 -0.00664 -0.00228 -0.00512 C6 1 -0.433710 0.681523 0.252828 11.00000 0.02223 0.01857 = 0.02284 0.00137 0.00469 0.00120 C10 1 -0.879364 0.811413 0.117937 11.00000 0.02987 0.02008 = 0.02777 -0.00296 -0.00022 -0.00065 C11 1 -0.935805 0.891669 0.119763 11.00000 0.03089 0.02022 = 0.03131 -0.00176 -0.00125 0.00183 O1W 5 0.716254 0.904102 0.345816 11.00000 0.02995 0.03237 = 0.05635 0.01661 -0.00280 -0.00371 H9A 2 -0.753004 0.803900 0.263054 11.00000 0.01979 H7 2 -0.886410 0.668916 0.096836 11.00000 0.01657 H12A 2 -1.065058 0.903201 -0.022177 11.00000 0.01608 H11B 2 -1.004731 0.899732 0.181708 11.00000 0.01130 H3 2 0.047261 0.559524 0.368007 11.00000 0.03194 H10A 2 -0.816697 0.798772 0.051492 11.00000 0.03159 H12C 2 -1.299299 0.887580 0.049954 11.00000 0.01864 H5 2 -0.251609 0.756877 0.338435 11.00000 0.03270 H4 2 0.049645 0.678528 0.402700 11.00000 0.03117 H10B 2 -1.041064 0.785241 0.123357 11.00000 0.02557 H9B 2 -0.528026 0.816285 0.193781 11.00000 0.03945 H11A 2 -0.772924 0.916907 0.112021 11.00000 0.04004 H8A 2 -0.842850 0.541619 0.070541 11.00000 0.05465 H2 2 -0.266288 0.517603 0.254505 11.00000 0.02566 H8B 2 -0.770346 0.497233 0.164003 11.00000 0.04621 H12B 2 -1.166943 0.964667 0.046127 11.00000 0.03862 H8C 2 -0.574690 0.512632 0.085644 11.00000 0.05285 H1WA 2 0.599785 0.888734 0.368049 11.00000 0.03755 H1WB 2 0.846022 0.891932 0.380979 11.00000 0.06280 HKLF 4 Covalent radii and connectivity table for s92 in P2(1)/n C 0.770 H 0.320 N 0.700 BR 1.140 O 0.660 Br1 - no bonds found C7 - N2 N1 N1 - C7 C1 C8 N2 - C7 C6 C9 C4 - C5 C3 C5 - C4 C6 C3 - C2 C4 C2 - C3 C1 C9 - N2 C10 C12 - C11 C1 - N1 C2 C6 C8 - N1 C6 - C5 N2 C1 C10 - C9 C11 C11 - C12 C10 O1W - no bonds found h k l Fo^2 Sigma Why rejected 2 0 3 19.11 3.83 observed but should be systematically absent 3 0 2 36.38 3.65 observed but should be systematically absent 9110 Reflections read, of which 1195 rejected -5 =< h =< 6, -22 =< k =< 21, -16 =< l =< 16, Max. 2-theta = 50.05 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 3 0 3 895.74 19.43 4 122.66 5 3 4 469.67 14.96 3 160.17 4 4 9 176.79 9.56 2 104.05 3 Inconsistent equivalents 2291 Unique reflections, of which 0 suppressed R(int) = 0.0697 R(sigma) = 0.0549 Friedel opposites merged Maximum memory for data reduction = 1813 / 23171 Least-squares cycle 1 Maximum vector length = 511 Memory required = 2340 / 274852 wR2 = 0.1009 before cycle 1 for 2291 data and 221 / 221 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.64388 0.00156 0.406 OSF Mean shift/su = 0.268 Maximum = 2.429 for U33 Br1 Max. shift = 0.023 A for H12B Max. dU =-0.008 for H8C Least-squares cycle 2 Maximum vector length = 511 Memory required = 2340 / 274852 wR2 = 0.0998 before cycle 2 for 2291 data and 221 / 221 parameters GooF = S = 1.061; Restrained GooF = 1.061 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.64461 0.00155 0.471 OSF Mean shift/su = 0.091 Maximum = 0.878 for U33 Br1 Max. shift = 0.011 A for H12B Max. dU = 0.003 for H11B Least-squares cycle 3 Maximum vector length = 511 Memory required = 2340 / 274852 wR2 = 0.0997 before cycle 3 for 2291 data and 221 / 221 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.64465 0.00155 0.024 OSF Mean shift/su = 0.008 Maximum = 0.070 for y H11B Max. shift = 0.003 A for H11B Max. dU = 0.000 for H8B Least-squares cycle 4 Maximum vector length = 511 Memory required = 2340 / 274852 wR2 = 0.0998 before cycle 4 for 2291 data and 221 / 221 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.64465 0.00155 0.002 OSF Mean shift/su = 0.002 Maximum = 0.015 for U22 C5 Max. shift = 0.001 A for H11B Max. dU = 0.000 for H11B Least-squares cycle 5 Maximum vector length = 511 Memory required = 2340 / 274852 wR2 = 0.0997 before cycle 5 for 2291 data and 221 / 221 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.64465 0.00155 0.001 OSF Mean shift/su = 0.001 Maximum = 0.005 for y H11B Max. shift = 0.000 A for H11B Max. dU = 0.000 for H11B Least-squares cycle 6 Maximum vector length = 511 Memory required = 2340 / 274852 wR2 = 0.0998 before cycle 6 for 2291 data and 221 / 221 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.64465 0.00155 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for x H11B Max. shift = 0.000 A for H11B Max. dU = 0.000 for H11B Least-squares cycle 7 Maximum vector length = 511 Memory required = 2340 / 274852 wR2 = 0.0998 before cycle 7 for 2291 data and 221 / 221 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.64465 0.00155 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for y Br1 Max. shift = 0.000 A for H11B Max. dU = 0.000 for H11B Least-squares cycle 8 Maximum vector length = 511 Memory required = 2340 / 274852 wR2 = 0.0998 before cycle 8 for 2291 data and 221 / 221 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.64465 0.00155 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for y Br1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H8B Largest correlation matrix elements 0.607 U33 Br1 / OSF 0.600 U22 Br1 / OSF 0.588 U11 Br1 / OSF s92 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Br1 0.21947 0.83535 0.47069 1.00000 0.02544 0.03273 0.03089 -0.00094 -0.00148 0.00149 0.02970 0.00056 0.00006 0.00002 0.00002 0.00000 0.00024 0.00024 0.00024 0.00015 0.00015 0.00014 0.00017 C7 -0.74761 0.66330 0.14428 1.00000 0.02344 0.02463 0.02240 0.00147 0.00123 -0.00132 0.02348 0.00580 0.00066 0.00016 0.00024 0.00000 0.00177 0.00177 0.00171 0.00140 0.00145 0.00141 0.00073 N1 -0.64140 0.59956 0.16307 1.00000 0.02168 0.01750 0.03048 -0.00185 -0.00082 -0.00136 0.02323 0.00446 0.00050 0.00014 0.00019 0.00000 0.00146 0.00136 0.00157 0.00116 0.00117 0.00113 0.00062 N2 -0.63084 0.71334 0.19675 1.00000 0.02203 0.01778 0.02590 -0.00193 0.00145 -0.00197 0.02190 0.00441 0.00050 0.00013 0.00019 0.00000 0.00139 0.00129 0.00144 0.00119 0.00112 0.00116 0.00059 C4 -0.07763 0.66251 0.35968 1.00000 0.02587 0.02541 0.02600 -0.00205 -0.00125 -0.00555 0.02577 0.00609 0.00070 0.00017 0.00026 0.00000 0.00187 0.00182 0.00181 0.00145 0.00149 0.00149 0.00077 C5 -0.25494 0.70988 0.31875 1.00000 0.02474 0.01824 0.02649 -0.00079 0.00133 -0.00322 0.02315 0.00569 0.00063 0.00018 0.00024 0.00000 0.00175 0.00169 0.00177 0.00142 0.00136 0.00140 0.00072 C3 -0.08409 0.58935 0.33640 1.00000 0.02593 0.02300 0.02936 0.00507 -0.00027 0.00465 0.02610 0.00598 0.00068 0.00018 0.00025 0.00000 0.00179 0.00169 0.00184 0.00151 0.00149 0.00153 0.00075 C2 -0.26314 0.56116 0.27179 1.00000 0.02587 0.01801 0.03108 -0.00058 0.00355 -0.00133 0.02496 0.00599 0.00064 0.00019 0.00025 0.00000 0.00178 0.00171 0.00192 0.00150 0.00143 0.00140 0.00074 C9 -0.69087 0.79033 0.19836 1.00000 0.03170 0.01542 0.02836 -0.00164 -0.00293 0.00257 0.02519 0.00589 0.00073 0.00017 0.00026 0.00000 0.00193 0.00162 0.00199 0.00145 0.00152 0.00146 0.00075 C12 -1.13418 0.91290 0.04243 1.00000 0.03306 0.02355 0.04118 0.00259 -0.00283 0.00502 0.03262 0.00710 0.00078 0.00021 0.00030 0.00000 0.00215 0.00187 0.00241 0.00172 0.00171 0.00171 0.00083 C1 -0.44062 0.60881 0.23001 1.00000 0.02477 0.01843 0.02393 -0.00033 0.00098 -0.00455 0.02237 0.00527 0.00061 0.00016 0.00022 0.00000 0.00171 0.00158 0.00174 0.00136 0.00134 0.00136 0.00071 C8 -0.71445 0.53227 0.11511 1.00000 0.03445 0.01991 0.03692 -0.00617 -0.00209 -0.00533 0.03045 0.00603 0.00083 0.00019 0.00030 0.00000 0.00214 0.00181 0.00217 0.00169 0.00184 0.00165 0.00082 C6 -0.43361 0.68164 0.25276 1.00000 0.02343 0.01919 0.02305 0.00156 0.00545 0.00110 0.02185 0.00565 0.00063 0.00017 0.00023 0.00000 0.00172 0.00161 0.00167 0.00135 0.00134 0.00135 0.00070 C10 -0.87927 0.81132 0.11804 1.00000 0.02965 0.02006 0.02930 -0.00231 0.00059 0.00064 0.02633 0.00621 0.00071 0.00019 0.00026 0.00000 0.00196 0.00166 0.00196 0.00150 0.00152 0.00155 0.00075 C11 -0.93606 0.89163 0.11976 1.00000 0.03116 0.02062 0.03252 -0.00138 -0.00060 0.00196 0.02811 0.00619 0.00074 0.00018 0.00028 0.00000 0.00199 0.00176 0.00215 0.00153 0.00159 0.00153 0.00080 O1W 0.71654 0.90407 0.34585 1.00000 0.02950 0.03339 0.05715 0.01608 -0.00267 -0.00297 0.04004 0.00545 0.00064 0.00015 0.00022 0.00000 0.00156 0.00154 0.00191 0.00138 0.00150 0.00130 0.00070 H9A -0.75118 0.80254 0.26317 1.00000 0.02201 0.05723 0.00602 0.00177 0.00251 0.00000 0.00843 H7 -0.88356 0.66875 0.09775 1.00000 0.01355 0.05594 0.00646 0.00143 0.00231 0.00000 0.00781 H12A -1.06659 0.90202 -0.02296 1.00000 0.02193 0.05753 0.00618 0.00170 0.00259 0.00000 0.00859 H11B -1.00265 0.89981 0.18117 1.00000 0.02162 0.05539 0.00624 0.00170 0.00252 0.00000 0.00886 H3 0.04469 0.55991 0.36693 1.00000 0.02760 0.05916 0.00705 0.00182 0.00245 0.00000 0.00899 H10A -0.81442 0.79906 0.05081 1.00000 0.02774 0.05885 0.00668 0.00184 0.00258 0.00000 0.00880 H12C -1.29913 0.88726 0.05044 1.00000 0.01862 0.05651 0.00665 0.00166 0.00222 0.00000 0.00804 H5 -0.25045 0.75817 0.33869 1.00000 0.03028 0.06402 0.00655 0.00204 0.00246 0.00000 0.00947 H4 0.04732 0.67909 0.40110 1.00000 0.02803 0.06586 0.00750 0.00179 0.00268 0.00000 0.00954 H10B -1.04404 0.78478 0.12194 1.00000 0.02523 0.05962 0.00668 0.00175 0.00232 0.00000 0.00887 H9B -0.52644 0.81662 0.19404 1.00000 0.04069 0.07234 0.00820 0.00205 0.00274 0.00000 0.01093 H11A -0.77267 0.91635 0.11129 1.00000 0.04006 0.07065 0.00796 0.00199 0.00275 0.00000 0.01048 H8A -0.84387 0.54052 0.06974 1.00000 0.05973 0.08210 0.00958 0.00240 0.00325 0.00000 0.01346 H2 -0.26633 0.51638 0.25349 1.00000 0.02330 0.05983 0.00651 0.00185 0.00236 0.00000 0.00889 H8B -0.77009 0.49697 0.16336 1.00000 0.04130 0.06415 0.00746 0.00214 0.00267 0.00000 0.01088 H12B -1.16943 0.96298 0.04515 1.00000 0.03727 0.06636 0.00733 0.00225 0.00258 0.00000 0.01026 H8C -0.57381 0.51279 0.08535 1.00000 0.04359 0.06627 0.00855 0.00210 0.00282 0.00000 0.01156 H1WA 0.59996 0.88852 0.36845 1.00000 0.03835 0.07740 0.00861 0.00224 0.00309 0.00000 0.01387 H1WB 0.84580 0.89222 0.38180 1.00000 0.06176 0.08499 0.00958 0.00252 0.00351 0.00000 0.01500 Final Structure Factor Calculation for s92 in P2(1)/n Total number of l.s. parameters = 221 Maximum vector length = 511 Memory required = 2119 / 24017 wR2 = 0.0998 before cycle 9 for 2291 data and 0 / 221 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0529 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0387 for 1857 Fo > 4sig(Fo) and 0.0527 for all 2291 data wR2 = 0.0998, GooF = S = 1.060, Restrained GooF = 1.060 for all data Occupancy sum of asymmetric unit = 16.00 for non-hydrogen and 19.00 for hydrogen atoms Principal mean square atomic displacements U 0.0337 0.0307 0.0247 Br1 0.0257 0.0239 0.0208 C7 0.0308 0.0221 0.0168 N1 0.0269 0.0220 0.0168 N2 0.0312 0.0269 0.0192 C4 0.0275 0.0250 0.0169 C5 0.0327 0.0278 0.0178 C3 0.0327 0.0244 0.0178 C2 0.0342 0.0264 0.0149 C9 0.0424 0.0347 0.0207 C12 0.0273 0.0238 0.0161 C1 0.0391 0.0361 0.0161 C8 0.0287 0.0190 0.0179 C6 0.0299 0.0297 0.0195 C10 0.0334 0.0308 0.0202 C11 0.0658 0.0294 0.0249 O1W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.025 0.039 0.053 0.069 0.087 0.109 0.136 0.184 1.000 Number in group 243. 230. 214. 229. 230. 239. 225. 222. 230. 229. GooF 0.874 1.026 1.133 1.004 1.243 1.030 0.937 1.008 1.109 1.193 K 0.906 0.872 0.942 0.965 0.962 0.977 1.013 1.031 1.035 1.008 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.44 1.81 inf Number in group 238. 229. 223. 228. 227. 230. 231. 226. 230. 229. GooF 0.992 0.992 1.032 1.041 1.027 1.065 0.976 0.915 1.111 1.381 K 1.038 1.009 1.002 1.002 1.029 1.040 1.041 1.040 1.031 0.975 R1 0.112 0.100 0.092 0.057 0.059 0.042 0.039 0.034 0.032 0.035 Recommended weighting scheme: WGHT 0.0543 0.2894 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)/su Fc/Fc(max) Resolution(A) -5 0 1 4510.65 3128.64 4.62 0.211 1.02 -4 8 8 26.37 161.28 3.70 0.048 0.94 1 9 0 411.59 320.35 3.65 0.068 1.92 -4 14 2 260.51 382.87 3.50 0.074 0.92 0 3 7 176.10 244.02 3.47 0.059 1.87 2 1 6 1559.97 1912.77 3.32 0.165 1.69 -1 1 5 139.94 189.17 3.25 0.052 2.41 5 1 9 396.08 283.38 3.21 0.064 0.84 0 8 3 83.24 52.13 3.06 0.027 2.08 2 3 2 350.68 280.25 3.06 0.063 2.23 2 5 3 2169.36 1759.73 3.05 0.158 1.91 5 6 2 38.37 96.43 2.94 0.037 0.96 -1 9 1 756.72 631.77 2.87 0.095 1.91 1 3 6 4628.72 5457.84 2.75 0.279 1.97 4 1 12 281.55 200.36 2.75 0.053 0.85 -1 2 6 974.51 1163.12 2.73 0.129 2.05 -3 6 5 10.36 29.44 2.70 0.020 1.32 -2 20 3 -13.01 61.48 2.69 0.030 0.86 -4 11 4 178.71 232.60 2.67 0.058 0.98 1 2 7 1193.04 1400.85 2.64 0.141 1.79 2 9 1 7363.31 6314.03 2.63 0.300 1.60 4 15 1 228.40 306.44 2.62 0.066 0.89 4 10 4 43.63 102.66 2.62 0.038 1.00 1 9 5 348.41 273.15 2.61 0.062 1.57 4 5 10 348.11 271.57 2.61 0.062 0.90 1 1 9 360.29 432.23 2.61 0.078 1.45 3 13 5 17.28 48.33 2.61 0.026 1.02 2 6 3 71.60 51.64 2.60 0.027 1.81 2 7 14 74.20 2.55 2.59 0.006 0.86 -1 11 13 1529.93 1192.33 2.59 0.130 0.89 0 10 0 1105.32 917.61 2.58 0.114 1.87 2 8 0 2267.04 1937.14 2.57 0.166 1.72 1 4 9 675.70 796.79 2.55 0.107 1.39 0 20 3 222.88 304.22 2.53 0.066 0.92 0 9 2 23.45 3.72 2.52 0.007 1.99 2 10 0 1908.83 1639.32 2.51 0.153 1.51 1 1 6 1287.88 1496.45 2.49 0.146 2.07 2 4 1 1400.68 1171.43 2.49 0.129 2.21 2 7 3 46.58 78.26 2.48 0.033 1.71 -2 2 4 213.36 258.07 2.45 0.061 2.01 -2 14 4 6.49 43.24 2.44 0.025 1.12 0 7 11 180.15 226.58 2.42 0.057 1.13 -3 3 9 396.90 477.58 2.40 0.082 1.12 2 7 0 1585.27 1350.95 2.39 0.139 1.85 2 7 1 3821.55 3317.13 2.39 0.217 1.83 1 1 2 3300.59 3789.66 2.36 0.232 3.98 0 2 3 12344.46 14276.75 2.34 0.451 4.11 -3 15 3 134.63 183.98 2.33 0.051 0.98 -4 2 8 98.50 63.46 2.33 0.030 1.02 2 3 3 555.23 649.27 2.32 0.096 2.09 Bond lengths and angles C7 - Distance Angles N2 1.3196 (0.0042) N1 1.3338 (0.0041) 110.41 (0.29) H7 0.9433 (0.0341) 128.14 (1.69) 121.43 (1.68) C7 - N2 N1 N1 - Distance Angles C7 1.3338 (0.0041) C1 1.3797 (0.0041) 108.28 (0.26) C8 1.4671 (0.0042) 125.43 (0.29) 126.15 (0.28) N1 - C7 C1 N2 - Distance Angles C7 1.3196 (0.0042) C6 1.3922 (0.0041) 108.58 (0.26) C9 1.4727 (0.0040) 127.54 (0.28) 123.87 (0.26) N2 - C7 C6 C4 - Distance Angles C5 1.3813 (0.0048) C3 1.4059 (0.0047) 121.23 (0.33) H4 0.9045 (0.0382) 119.31 (2.22) 119.45 (2.23) C4 - C5 C3 C5 - Distance Angles C4 1.3813 (0.0048) C6 1.3832 (0.0047) 116.44 (0.31) H5 0.9443 (0.0374) 118.82 (2.18) 124.70 (2.16) C5 - C4 C6 C3 - Distance Angles C2 1.3718 (0.0049) C4 1.4059 (0.0047) 122.36 (0.33) H3 0.9510 (0.0364) 120.94 (2.09) 116.69 (2.10) C3 - C2 C4 C2 - Distance Angles C3 1.3718 (0.0049) C1 1.3899 (0.0046) 116.52 (0.32) H2 0.8748 (0.0336) 124.35 (2.25) 119.05 (2.25) C2 - C3 C1 C9 - Distance Angles N2 1.4727 (0.0040) C10 1.5073 (0.0048) 112.01 (0.28) H9A 0.9731 (0.0337) 108.15 (1.97) 113.81 (1.89) H9B 0.9748 (0.0418) 108.27 (2.25) 111.44 (2.29) 102.64 (2.91) C9 - N2 C10 H9A C12 - Distance Angles C11 1.5113 (0.0052) H12A 0.9877 (0.0345) 110.37 (1.86) H12C 0.9759 (0.0338) 111.20 (1.85) 108.18 (2.61) H12B 0.9548 (0.0409) 110.82 (2.34) 107.80 (2.82) 108.35 (2.99) C12 - C11 H12A H12C C1 - Distance Angles N1 1.3797 (0.0041) C2 1.3899 (0.0046) 132.07 (0.29) C6 1.3983 (0.0042) 106.75 (0.27) 121.18 (0.30) C1 - N1 C2 C8 - Distance Angles N1 1.4671 (0.0042) H8A 0.9159 (0.0487) 109.79 (2.84) H8B 0.9802 (0.0394) 110.38 (2.17) 111.23 (3.59) H8C 0.9065 (0.0437) 110.45 (2.50) 109.17 (3.70) 105.76 (3.24) C8 - N1 H8A H8B C6 - Distance Angles C5 1.3832 (0.0047) N2 1.3922 (0.0041) 131.77 (0.30) C1 1.3983 (0.0042) 122.26 (0.30) 105.97 (0.27) C6 - C5 N2 C10 - Distance Angles C9 1.5073 (0.0048) C11 1.5303 (0.0047) 111.33 (0.29) H10A 1.0115 (0.0356) 113.42 (1.94) 107.50 (1.98) H10B 0.9782 (0.0341) 111.62 (1.94) 109.55 (1.92) 103.03 (2.72) C10 - C9 C11 H10A C11 - Distance Angles C12 1.5113 (0.0052) C10 1.5303 (0.0047) 111.88 (0.30) H11B 0.9263 (0.0337) 110.37 (2.02) 104.34 (2.04) H11A 0.9614 (0.0405) 111.20 (2.32) 107.81 (2.22) 111.02 (3.01) C11 - C12 C10 H11B O1W - Distance Angles H1WA 0.7342 (0.0427) H1WB 0.8488 (0.0525) 106.12 (4.58) O1W - H1WA FMAP and GRID set by program FMAP 2 1 9 GRID -4.167 -2 -2 4.167 2 2 R1 = 0.0512 for 2291 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.63 at 0.2187 0.8362 0.4719 [ 0.02 A from BR1 ] Deepest hole -0.80 at 0.2270 0.8840 0.4719 [ 0.91 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 2590 / 18882 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -1.2919 1.0075 -0.0267 1.00000 0.05 0.51 1.43 H12B 1.87 H11A 2.10 H3 2.16 C12 Q2 1 -1.1664 0.6644 0.0895 1.00000 0.05 0.50 1.45 H7 1.73 BR1 2.26 C7 2.38 H10B Q3 1 0.2272 0.8401 0.3882 1.00000 0.05 0.41 1.14 BR1 1.86 H9A 2.13 H1WA 2.18 H1WB Q4 1 0.1790 0.8365 0.5532 1.00000 0.05 0.40 1.16 BR1 2.31 H7 2.52 C7 2.54 N1 Q5 1 0.3239 0.8399 0.3881 1.00000 0.05 0.36 1.26 BR1 1.70 H1WA 1.89 H9A 2.41 O1W Q6 1 -0.4094 0.6364 0.2248 1.00000 0.05 0.28 0.55 C1 0.94 C6 1.60 N1 1.72 C2 Q7 1 -0.5092 0.7082 0.1362 1.00000 0.05 0.26 1.05 N2 1.48 C7 1.72 C6 1.99 C9 Q8 1 -0.2944 0.6933 0.1568 1.00000 0.05 0.26 1.52 C6 1.85 N2 2.02 C1 2.19 H10B Q9 1 -0.2857 0.6431 0.1546 1.00000 0.05 0.25 1.46 C1 1.71 C6 1.99 N1 2.23 C2 Q10 1 0.5958 0.9052 0.4616 1.00000 0.05 0.25 1.32 H1WA 1.71 H1WB 1.71 O1W 1.82 H8A Q11 1 -0.7857 0.8178 0.3466 1.00000 0.05 0.25 1.20 H9A 1.74 BR1 2.16 C9 2.39 H1WA Q12 1 0.4928 0.8006 0.4787 1.00000 0.05 0.25 1.54 BR1 1.84 H7 2.31 H1WA 2.32 H10A Q13 1 0.5088 0.8725 0.4784 1.00000 0.05 0.24 1.62 H1WA 1.63 BR1 1.89 H7 2.18 H8A Q14 1 -1.4524 0.9804 0.0367 1.00000 0.05 0.24 1.48 H12B 1.92 H12C 2.05 H3 2.06 C12 Q15 1 -0.8282 0.9350 0.1728 1.00000 0.05 0.23 0.96 H11A 1.11 H11B 1.22 C11 2.40 C12 Q16 1 -0.4880 0.5017 0.1318 1.00000 0.05 0.23 0.80 H8C 1.31 C8 1.51 H8B 2.03 H2 Q17 1 -0.4643 0.6162 0.0579 1.00000 0.05 0.22 1.74 N1 1.78 BR1 2.05 H8C 2.08 C7 Q18 1 0.4313 0.8596 0.3374 1.00000 0.05 0.22 1.10 H1WA 1.68 O1W 1.74 H9A 2.14 H9B Q19 1 0.8520 0.9078 0.4945 1.00000 0.05 0.22 1.58 H1WB 1.74 H8A 1.97 H8C 2.03 C8 Q20 1 -0.7101 0.5236 0.0185 1.00000 0.05 0.22 1.04 H8A 1.16 H8C 1.34 C8 2.08 H8B Shortest distances between peaks (including symmetry equivalents) 3 5 0.49 3 11 0.71 10 13 0.79 5 11 0.89 2 4 0.93 8 9 0.94 5 18 0.97 4 17 1.15 2 9 1.16 7 8 1.16 6 9 1.16 2 8 1.26 1 14 1.31 3 18 1.31 1 14 1.33 14 14 1.33 12 13 1.35 17 19 1.35 11 18 1.36 19 20 1.36 10 19 1.38 4 9 1.45 4 8 1.53 6 8 1.54 5 13 1.67 5 12 1.67 9 17 1.68 7 9 1.68 4 7 1.72 2 17 1.81 10 20 1.83 2 12 1.85 6 7 1.88 13 19 1.88 2 13 1.91 16 20 1.96 3 12 1.97 3 13 1.98 13 18 1.99 4 12 2.02 10 12 2.04 2 7 2.04 7 17 2.04 10 18 2.08 4 13 2.09 5 10 2.10 8 17 2.16 17 20 2.20 12 18 2.25 1 1 2.27 4 19 2.28 3 4 2.29 2 6 2.31 11 12 2.31 6 17 2.34 16 20 2.36 1 15 2.36 16 17 2.37 20 20 2.38 4 5 2.40 3 10 2.45 4 6 2.46 13 20 2.47 11 13 2.55 16 19 2.57 2 10 2.57 10 17 2.62 16 19 2.66 3 17 2.67 13 17 2.67 12 19 2.72 3 19 2.73 2 5 2.77 4 10 2.80 2 3 2.81 14 15 2.82 19 20 2.84 6 16 2.85 9 16 2.85 4 11 2.87 8 12 2.87 9 13 2.88 5 17 2.89 17 20 2.96 15 18 2.96 10 20 2.98 10 11 2.98 7 19 3.00 10 16 3.00 Time profile in seconds ----------------------- 0.02: 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. 0.39: 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 0.59: Structure factors and derivatives 1.11: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.22: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:57:37 Total CPU time: 2.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++