+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - MSDOS 32-BIT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-1 + + s92 started at 10:54:10 on 16-Sep-1999 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 7.879 9.393 10.085 90.01 108.24 103.77 ZERR 2.00 0.002 0.002 0.002 0.03 0.03 0.03 LATT 1 SFAC C H N O S CL UNIT 26 24 6 6 2 2 V = 686.23 F(000) = 336.0 Mu = 0.44 mm-1 Cell Wt = 651.53 Rho = 1.577 ACTA FMAP 2 PLAN 10 L.S. 4 BOND WGHT 0.027500 0.458100 FVAR 0.99373 CL1 6 0.88284 0.78609 0.87616 11.00000 0.03572 0.01622 = 0.03396 0.00113 0.01144 0.00229 S1 5 0.50478 0.03384 0.77324 11.00000 0.01647 0.01424 = 0.01772 0.00091 0.00706 0.00320 O1 4 0.59593 0.02968 0.67199 11.00000 0.02116 0.02179 = 0.02176 0.00054 0.01084 0.00681 O2 4 0.45651 -0.09752 0.84142 11.00000 0.02603 0.01418 = 0.02471 0.00336 0.01138 0.00410 O3 4 -0.10151 0.38464 0.35352 11.00000 0.02818 0.03549 = 0.02554 0.00997 0.01235 0.01101 N1 3 -0.16057 0.25735 0.53337 11.00000 0.01772 0.02233 = 0.02098 0.00337 0.00946 0.00641 N2 3 0.63751 0.15327 0.90559 11.00000 0.01991 0.01651 = 0.01527 0.00191 0.00497 0.00101 N3 3 0.71888 0.35464 0.78035 11.00000 0.02195 0.01871 = 0.02026 0.00140 0.00935 0.00260 C1 1 -0.37868 0.38821 0.39996 11.00000 0.02511 0.02648 = 0.02700 0.00272 0.00629 0.01034 C2 1 -0.20012 0.34513 0.42554 11.00000 0.02145 0.01703 = 0.01761 -0.00163 0.00377 0.00317 C3 1 -0.00249 0.20379 0.58397 11.00000 0.01632 0.01236 = 0.01953 -0.00105 0.00523 0.00046 C4 1 0.11166 0.19324 0.50475 11.00000 0.02299 0.01796 = 0.01547 0.00213 0.00763 0.00435 C5 1 0.26591 0.13978 0.56191 11.00000 0.02022 0.01570 = 0.01919 -0.00042 0.01055 0.00196 C6 1 0.30656 0.09707 0.69728 11.00000 0.01449 0.01269 = 0.01882 -0.00106 0.00522 0.00036 C7 1 0.19101 0.10333 0.77621 11.00000 0.02089 0.02050 = 0.01553 0.00197 0.00692 0.00354 C8 1 0.03685 0.15560 0.71883 11.00000 0.01748 0.01992 = 0.01937 -0.00047 0.00992 0.00272 C9 1 0.69205 0.30641 0.89752 11.00000 0.01335 0.01788 = 0.01763 0.00135 0.00354 0.00369 C10 1 0.72036 0.39728 1.01547 11.00000 0.03233 0.02547 = 0.01774 0.00153 0.01000 0.00369 C11 1 0.77954 0.54650 1.01033 11.00000 0.03481 0.02223 = 0.02158 -0.00383 0.00852 0.00366 C12 1 0.80772 0.59886 0.88901 11.00000 0.01695 0.01666 = 0.02541 0.00197 0.00460 0.00325 C13 1 0.77795 0.50118 0.77739 11.00000 0.02402 0.01879 = 0.02115 0.00298 0.00917 0.00285 H1A 2 -0.22660 0.24516 0.58601 11.00000 0.03007 H1B 2 -0.42768 0.37527 0.47782 11.00000 0.04350 H1C 2 -0.46751 0.33357 0.31844 11.00000 0.04962 H1D 2 -0.36400 0.48533 0.37543 11.00000 0.05689 H2A 2 0.61361 0.12964 0.98174 11.00000 0.03200 H4 2 0.08452 0.22207 0.41398 11.00000 0.02699 H5 2 0.33675 0.13130 0.50603 11.00000 0.01851 H7 2 0.21865 0.07524 0.87009 11.00000 0.02805 H8 2 -0.04061 0.15873 0.76973 11.00000 0.02220 H10 2 0.70139 0.35749 1.09624 11.00000 0.02771 H11 2 0.80003 0.61261 1.09043 11.00000 0.04355 H13 2 0.79611 0.53347 0.69333 11.00000 0.02358 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 CL 0.990 Cl1 - C12 S1 - O1 O2 N2 C6 O1 - S1 O2 - S1 O3 - C2 N1 - C2 C3 N2 - C9 S1 N3 - C9 C13 C1 - C2 C2 - O3 N1 C1 C3 - C4 C8 N1 C4 - C5 C3 C5 - C4 C6 C6 - C5 C7 S1 C7 - C8 C6 C8 - C7 C3 C9 - N3 C10 N2 C10 - C11 C9 C11 - C10 C12 C12 - C13 C11 Cl1 C13 - N3 C12 8309 Reflections read, of which 0 rejected -9 =< h =< 8, -11 =< k =< 11, -11 =< l =< 11, Max. 2-theta = 49.98 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 1 0 749.02 26.08 2 140.76 1 9 0 268.88 10.93 2 72.62 0 0 1 13.70 0.23 4 4.98 -4 4 1 222.25 3.89 5 22.23 -1 0 3 2.89 0.24 5 1.31 -3 -2 4 3.36 0.34 5 2.21 6 Inconsistent equivalents 2415 Unique reflections, of which 0 suppressed R(int) = 0.0404 R(sigma) = 0.0344 Friedel opposites merged Maximum memory for data reduction = 1708 / 24151 Least-squares cycle 1 Maximum vector length = 511 Memory required = 2270 / 297192 wR2 = 0.0806 before cycle 1 for 2415 data and 238 / 238 parameters GooF = S = 1.111; Restrained GooF = 1.111 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0275 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.99373 0.00189 -0.001 OSF Mean shift/esd = 0.005 Maximum = 0.073 for y Cl1 Max. shift = 0.000 A for H1C Max. dU = 0.000 for H2A Least-squares cycle 2 Maximum vector length = 511 Memory required = 2270 / 297192 wR2 = 0.0806 before cycle 2 for 2415 data and 238 / 238 parameters GooF = S = 1.111; Restrained GooF = 1.111 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0275 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.99373 0.00189 0.002 OSF Mean shift/esd = 0.002 Maximum = 0.025 for y Cl1 Max. shift = 0.000 A for H1A Max. dU = 0.000 for H1C Least-squares cycle 3 Maximum vector length = 511 Memory required = 2270 / 297192 wR2 = 0.0806 before cycle 3 for 2415 data and 238 / 238 parameters GooF = S = 1.111; Restrained GooF = 1.111 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0275 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.99373 0.00189 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H1C Max. dU = 0.000 for H2A Least-squares cycle 4 Maximum vector length = 511 Memory required = 2270 / 297192 wR2 = 0.0806 before cycle 4 for 2415 data and 238 / 238 parameters GooF = S = 1.111; Restrained GooF = 1.111 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0275 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.99373 0.00189 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z S1 Max. shift = 0.000 A for H1B Max. dU = 0.000 for H8 No correlation matrix elements larger than 0.500 s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Cl1 0.88284 0.78609 0.87616 1.00000 0.03572 0.01622 0.03396 0.00113 0.01144 0.00229 0.02934 0.00104 0.00007 0.00005 0.00005 0.00000 0.00029 0.00026 0.00029 0.00019 0.00021 0.00019 0.00015 S1 0.50478 0.03384 0.77324 1.00000 0.01647 0.01424 0.01772 0.00091 0.00706 0.00320 0.01589 0.00089 0.00005 0.00005 0.00004 0.00000 0.00023 0.00024 0.00023 0.00017 0.00017 0.00017 0.00014 O1 0.59593 0.02968 0.67199 1.00000 0.02116 0.02179 0.02176 0.00054 0.01084 0.00681 0.02037 0.00271 0.00016 0.00014 0.00012 0.00000 0.00063 0.00069 0.00065 0.00051 0.00051 0.00051 0.00028 O2 0.45651 -0.09752 0.84142 1.00000 0.02603 0.01418 0.02471 0.00336 0.01138 0.00410 0.02104 0.00273 0.00017 0.00013 0.00013 0.00000 0.00067 0.00065 0.00066 0.00052 0.00053 0.00051 0.00029 O3 -0.10151 0.38464 0.35352 1.00000 0.02818 0.03549 0.02554 0.00997 0.01235 0.01101 0.02831 0.00308 0.00018 0.00016 0.00014 0.00000 0.00072 0.00083 0.00071 0.00061 0.00058 0.00061 0.00033 N1 -0.16057 0.25735 0.53337 1.00000 0.01772 0.02233 0.02098 0.00337 0.00946 0.00641 0.01933 0.00330 0.00020 0.00017 0.00016 0.00000 0.00075 0.00084 0.00079 0.00064 0.00063 0.00062 0.00033 N2 0.63751 0.15327 0.90559 1.00000 0.01991 0.01651 0.01527 0.00191 0.00497 0.00101 0.01803 0.00313 0.00020 0.00016 0.00016 0.00000 0.00075 0.00080 0.00075 0.00061 0.00060 0.00060 0.00033 N3 0.71888 0.35464 0.78035 1.00000 0.02195 0.01871 0.02026 0.00140 0.00935 0.00260 0.02014 0.00327 0.00020 0.00017 0.00015 0.00000 0.00076 0.00082 0.00077 0.00062 0.00061 0.00061 0.00033 C1 -0.37868 0.38821 0.39996 1.00000 0.02511 0.02648 0.02700 0.00272 0.00629 0.01034 0.02601 0.00468 0.00027 0.00024 0.00022 0.00000 0.00101 0.00114 0.00106 0.00088 0.00085 0.00084 0.00043 C2 -0.20012 0.34513 0.42554 1.00000 0.02145 0.01703 0.01761 -0.00163 0.00377 0.00317 0.01960 0.00376 0.00024 0.00020 0.00018 0.00000 0.00090 0.00093 0.00087 0.00071 0.00071 0.00070 0.00038 C3 -0.00249 0.20379 0.58397 1.00000 0.01632 0.01236 0.01953 -0.00105 0.00523 0.00046 0.01676 0.00358 0.00023 0.00018 0.00017 0.00000 0.00084 0.00087 0.00087 0.00068 0.00067 0.00066 0.00037 C4 0.11166 0.19324 0.50475 1.00000 0.02299 0.01796 0.01547 0.00213 0.00763 0.00435 0.01861 0.00391 0.00024 0.00020 0.00019 0.00000 0.00092 0.00092 0.00087 0.00070 0.00070 0.00071 0.00037 C5 0.26591 0.13978 0.56191 1.00000 0.02022 0.01570 0.01919 -0.00042 0.01055 0.00196 0.01782 0.00376 0.00024 0.00019 0.00018 0.00000 0.00088 0.00091 0.00088 0.00069 0.00072 0.00069 0.00037 C6 0.30656 0.09707 0.69728 1.00000 0.01449 0.01269 0.01882 -0.00106 0.00522 0.00036 0.01591 0.00353 0.00022 0.00018 0.00017 0.00000 0.00083 0.00087 0.00085 0.00067 0.00066 0.00066 0.00036 C7 0.19101 0.10333 0.77621 1.00000 0.02089 0.02050 0.01553 0.00197 0.00692 0.00354 0.01902 0.00387 0.00024 0.00020 0.00018 0.00000 0.00089 0.00096 0.00087 0.00071 0.00069 0.00072 0.00038 C8 0.03685 0.15560 0.71883 1.00000 0.01748 0.01992 0.01937 -0.00047 0.00992 0.00272 0.01832 0.00380 0.00024 0.00020 0.00018 0.00000 0.00086 0.00095 0.00088 0.00071 0.00071 0.00070 0.00037 C9 0.69205 0.30641 0.89752 1.00000 0.01335 0.01788 0.01763 0.00135 0.00354 0.00369 0.01667 0.00367 0.00022 0.00019 0.00017 0.00000 0.00080 0.00091 0.00085 0.00069 0.00064 0.00066 0.00036 C10 0.72036 0.39728 1.01547 1.00000 0.03233 0.02547 0.01774 0.00153 0.01000 0.00369 0.02535 0.00424 0.00027 0.00022 0.00020 0.00000 0.00106 0.00106 0.00093 0.00078 0.00079 0.00082 0.00042 C11 0.77954 0.54650 1.01033 1.00000 0.03481 0.02223 0.02158 -0.00383 0.00852 0.00366 0.02697 0.00431 0.00028 0.00022 0.00020 0.00000 0.00109 0.00107 0.00096 0.00080 0.00080 0.00083 0.00043 C12 0.80772 0.59886 0.88901 1.00000 0.01695 0.01666 0.02541 0.00197 0.00460 0.00325 0.02038 0.00385 0.00023 0.00020 0.00019 0.00000 0.00086 0.00094 0.00095 0.00074 0.00071 0.00069 0.00039 C13 0.77795 0.50118 0.77739 1.00000 0.02402 0.01879 0.02115 0.00298 0.00917 0.00285 0.02132 0.00403 0.00025 0.00020 0.00020 0.00000 0.00093 0.00097 0.00094 0.00075 0.00074 0.00073 0.00039 H1A -0.22660 0.24516 0.58601 1.00000 0.03007 0.04864 0.00312 0.00245 0.00232 0.00000 0.00590 H1B -0.42768 0.37527 0.47782 1.00000 0.04350 0.05439 0.00336 0.00275 0.00268 0.00000 0.00663 H1C -0.46751 0.33357 0.31844 1.00000 0.04962 0.06224 0.00361 0.00296 0.00283 0.00000 0.00721 H1D -0.36400 0.48533 0.37543 1.00000 0.05689 0.06245 0.00376 0.00340 0.00288 0.00000 0.00793 H2A 0.61361 0.12964 0.98174 1.00000 0.03200 0.05008 0.00305 0.00252 0.00250 0.00000 0.00603 H4 0.08452 0.22207 0.41398 1.00000 0.02699 0.04654 0.00281 0.00233 0.00230 0.00000 0.00543 H5 0.33675 0.13130 0.50603 1.00000 0.01851 0.04290 0.00267 0.00218 0.00206 0.00000 0.00474 H7 0.21865 0.07524 0.87009 1.00000 0.02805 0.04760 0.00285 0.00235 0.00232 0.00000 0.00543 H8 -0.04061 0.15873 0.76973 1.00000 0.02220 0.04341 0.00277 0.00222 0.00207 0.00000 0.00503 H10 0.70139 0.35749 1.09624 1.00000 0.02771 0.04636 0.00284 0.00240 0.00228 0.00000 0.00547 H11 0.80003 0.61261 1.09043 1.00000 0.04355 0.05693 0.00332 0.00284 0.00265 0.00000 0.00657 H13 0.79611 0.53347 0.69333 1.00000 0.02358 0.04452 0.00272 0.00233 0.00222 0.00000 0.00512 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 238 Maximum vector length = 511 Memory required = 2032 / 25039 wR2 = 0.0806 before cycle 5 for 2415 data and 0 / 238 parameters GooF = S = 1.111; Restrained GooF = 1.111 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0275 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0313 for 2240 Fo > 4sig(Fo) and 0.0340 for all 2415 data wR2 = 0.0806, GooF = S = 1.111, Restrained GooF = 1.111 for all data Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0381 0.0338 0.0161 Cl1 0.0187 0.0148 0.0142 S1 0.0246 0.0224 0.0141 O1 0.0280 0.0214 0.0137 O2 0.0390 0.0261 0.0198 O3 0.0236 0.0204 0.0140 N1 0.0241 0.0156 0.0144 N2 0.0248 0.0192 0.0165 N3 0.0303 0.0273 0.0204 C1 0.0240 0.0204 0.0144 C2 0.0205 0.0187 0.0111 C3 0.0234 0.0181 0.0143 C4 0.0249 0.0151 0.0135 C5 0.0199 0.0168 0.0110 C6 0.0229 0.0195 0.0146 C7 0.0243 0.0183 0.0123 C8 0.0189 0.0179 0.0132 C9 0.0351 0.0247 0.0163 C10 0.0370 0.0274 0.0165 C11 0.0273 0.0178 0.0160 C12 0.0259 0.0215 0.0165 C13 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.026 0.051 0.076 0.106 0.139 0.173 0.216 0.270 0.370 1.000 Number in group 243. 248. 238. 239. 241. 243. 241. 239. 241. 242. GooF 1.105 1.125 1.317 1.114 1.172 0.890 0.997 0.950 1.070 1.295 K 1.098 0.945 0.931 0.951 0.961 0.993 1.005 1.020 1.013 1.009 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.44 1.80 inf Number in group 244. 249. 233. 246. 239. 238. 243. 241. 240. 242. GooF 1.090 1.001 0.870 0.936 1.023 0.908 0.862 0.840 1.393 1.804 K 0.983 0.993 1.004 1.008 1.018 1.027 1.021 1.013 1.020 0.988 R1 0.063 0.050 0.036 0.038 0.035 0.028 0.023 0.020 0.031 0.036 Recommended weighting scheme: WGHT 0.0275 0.4581 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 -1 2 2233.24 2855.10 6.24 0.777 4.07 0 -3 4 36.26 18.28 4.83 0.062 1.95 -2 -1 6 9.84 25.05 4.59 0.073 1.63 1 -1 4 13.00 29.57 4.57 0.079 2.09 0 -2 6 21.31 8.89 4.46 0.043 1.54 -4 -1 4 4.73 0.23 4.46 0.007 1.65 -2 0 2 165.62 217.66 4.19 0.215 3.47 -3 1 4 29.16 16.12 3.68 0.058 2.08 1 -2 2 1503.41 1743.44 3.61 0.607 3.05 -2 -2 5 205.09 254.03 3.59 0.232 1.77 -1 0 4 45.41 66.89 3.58 0.119 2.52 -3 3 1 7.70 2.38 3.54 0.022 2.23 0 -4 1 1376.66 1157.35 3.42 0.495 2.25 1 -9 2 1.35 8.22 3.29 0.042 1.02 -3 1 2 679.41 789.08 3.29 0.409 2.56 -1 -10 3 6.84 19.49 3.22 0.064 0.87 -1 5 0 1627.55 1391.56 3.20 0.543 1.88 -2 4 4 7.09 15.53 3.18 0.057 1.72 -1 -3 11 56.28 81.06 3.15 0.131 0.87 -1 -4 2 84.73 63.02 3.15 0.115 1.99 -1 -5 9 65.04 89.76 3.12 0.138 0.96 0 -1 2 744.30 851.57 3.08 0.424 4.37 0 4 0 399.84 334.20 3.08 0.266 2.27 -2 1 2 1014.93 1146.95 3.03 0.493 3.46 -2 -4 2 647.89 553.48 3.02 0.342 1.76 -2 -1 2 7.65 15.52 3.01 0.057 3.07 8 -2 1 7.09 15.17 2.99 0.057 0.90 0 -1 1 521.09 601.12 2.97 0.357 6.87 0 5 7 27.29 42.99 2.97 0.095 1.05 0 -2 4 408.91 474.17 2.95 0.317 2.19 -3 0 2 425.40 508.16 2.92 0.328 2.50 -1 5 10 10.26 20.65 2.89 0.066 0.85 2 -4 1 171.76 210.61 2.89 0.211 2.08 -4 1 6 13.16 22.42 2.82 0.069 1.46 -2 3 2 9.69 17.69 2.78 0.061 2.52 1 0 5 51.18 68.04 2.77 0.120 1.72 -1 1 4 17.72 27.80 2.75 0.077 2.43 -1 -2 4 36.21 24.79 2.75 0.072 2.20 -6 2 8 8.21 3.37 2.74 0.027 1.04 0 -2 2 3.99 0.37 2.70 0.009 3.43 -2 -1 3 354.34 407.70 2.70 0.294 2.67 6 -5 2 52.52 69.71 2.70 0.121 1.06 -4 1 4 142.19 116.39 2.69 0.157 1.77 2 4 1 46.65 30.81 2.68 0.081 1.65 1 2 4 236.39 200.21 2.67 0.206 1.79 3 -2 1 401.51 344.72 2.66 0.270 2.19 -8 7 3 58.30 84.08 2.61 0.133 0.88 -6 5 9 29.00 41.43 2.59 0.094 0.90 0 -4 4 6.60 12.90 2.59 0.052 1.72 2 -3 3 44.31 58.94 2.58 0.112 1.90 Bond lengths and angles Cl1 - Distance Angles C12 1.7357 (0.0019) Cl1 - S1 - Distance Angles O1 1.4256 (0.0013) O2 1.4425 (0.0013) 118.97 (0.08) N2 1.6434 (0.0017) 110.06 (0.08) 102.71 (0.08) C6 1.7526 (0.0017) 108.81 (0.08) 109.07 (0.08) 106.48 (0.08) S1 - O1 O2 N2 O1 - Distance Angles S1 1.4256 (0.0013) O1 - O2 - Distance Angles S1 1.4425 (0.0013) O2 - O3 - Distance Angles C2 1.2186 (0.0022) O3 - N1 - Distance Angles C2 1.3675 (0.0024) C3 1.4019 (0.0023) 127.46 (0.15) N1 - C2 N2 - Distance Angles C9 1.4100 (0.0023) S1 1.6434 (0.0017) 124.98 (0.12) N2 - C9 N3 - Distance Angles C9 1.3256 (0.0023) C13 1.3476 (0.0025) 117.04 (0.16) N3 - C9 C1 - Distance Angles C2 1.5012 (0.0026) C1 - C2 - Distance Angles O3 1.2186 (0.0022) N1 1.3675 (0.0024) 123.62 (0.16) C1 1.5012 (0.0026) 121.77 (0.17) 114.60 (0.16) C2 - O3 N1 C3 - Distance Angles C4 1.3961 (0.0024) C8 1.3978 (0.0025) 119.61 (0.16) N1 1.4019 (0.0023) 123.04 (0.16) 117.32 (0.15) C3 - C4 C8 C4 - Distance Angles C5 1.3834 (0.0026) C3 1.3961 (0.0024) 119.81 (0.16) C4 - C5 C5 - Distance Angles C4 1.3834 (0.0026) C6 1.3838 (0.0025) 119.93 (0.16) C5 - C4 C6 - Distance Angles C5 1.3838 (0.0025) C7 1.3946 (0.0024) 120.84 (0.16) S1 1.7526 (0.0017) 120.60 (0.13) 118.56 (0.13) C6 - C5 C7 C7 - Distance Angles C8 1.3767 (0.0026) C6 1.3946 (0.0024) 119.15 (0.16) C7 - C8 C8 - Distance Angles C7 1.3767 (0.0026) C3 1.3978 (0.0025) 120.61 (0.16) C8 - C7 C9 - Distance Angles N3 1.3256 (0.0023) C10 1.3915 (0.0026) 124.13 (0.17) N2 1.4100 (0.0023) 118.25 (0.16) 117.58 (0.16) C9 - N3 C10 C10 - Distance Angles C11 1.3743 (0.0028) C9 1.3915 (0.0026) 118.05 (0.18) C10 - C11 C11 - Distance Angles C10 1.3743 (0.0028) C12 1.3808 (0.0027) 118.66 (0.18) C11 - C10 C12 - Distance Angles C13 1.3769 (0.0026) C11 1.3808 (0.0027) 119.57 (0.17) Cl1 1.7357 (0.0019) 119.58 (0.14) 120.84 (0.15) C12 - C13 C11 C13 - Distance Angles N3 1.3476 (0.0024) C12 1.3769 (0.0026) 122.53 (0.17) C13 - N3 FMAP and GRID set by program FMAP 2 1 20 GRID -2.941 -2 -2 2.941 2 2 R1 = 0.0338 for 2415 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.1438 0.1980 0.2480 [ 1.22 A from CL1 ] Deepest hole -0.39 at 0.4601 0.0474 0.8192 [ 0.69 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2007 / 17046 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8562 0.8020 0.7520 1.00000 0.05 0.24 1.22 CL1 1.90 H4 2.38 C12 2.49 H13 Q2 1 0.3921 0.0613 0.7308 1.00000 0.05 0.22 0.80 C6 0.95 S1 1.90 C7 1.93 C5 Q3 1 0.8302 0.5648 0.9518 1.00000 0.05 0.21 0.70 C12 0.81 C11 1.57 H11 1.75 C13 Q4 1 0.7448 0.5707 0.9232 1.00000 0.05 0.21 0.69 C12 0.88 C11 1.63 H11 1.73 C13 Q5 1 0.5833 0.1013 0.8499 1.00000 0.05 0.19 0.70 N2 0.95 S1 1.29 H2A 1.88 O2 Q6 1 0.2676 0.1223 0.7433 1.00000 0.05 0.18 0.70 C6 0.76 C7 1.49 H7 1.83 C5 Q7 1 0.0121 0.1610 0.6303 1.00000 0.05 0.18 0.62 C3 0.86 C8 1.58 H8 1.68 C4 Q8 1 0.0535 0.2280 0.5559 1.00000 0.05 0.18 0.60 C3 0.90 C4 1.53 H4 1.72 N1 Q9 1 0.7501 0.5451 0.8234 1.00000 0.05 0.18 0.74 C13 0.78 C12 1.48 H13 1.78 N3 Q10 1 0.7237 0.3549 0.9635 1.00000 0.05 0.18 0.67 C10 0.74 C9 1.40 H10 1.77 C11 Shortest distances between peaks (including symmetry equivalents) 3 4 0.66 4 9 1.05 7 8 1.06 3 9 1.24 2 6 1.28 2 5 1.57 3 10 1.97 4 10 2.04 6 7 2.10 9 10 2.29 5 6 2.44 5 10 2.48 6 8 2.49 1 9 2.54 1 4 2.92 Time profile in seconds ----------------------- 0.11: 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. 0.66: 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 2.63: Structure factors and derivatives 8.23: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.93: Solve l.s. equations 0.00: Generate HTAB table 0.19: Other dependent quantities, CIF, tables 0.33: Analysis of variance 0.16: Merge reflections for Fourier and .fcf 0.23: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 10:54:23 Total elapsed time: 13.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++