+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXS-97 - CRYSTAL STRUCTURE SOLUTION - MSDOS 32-BIT VERSION + + Copyright(C) George M. Sheldrick 1986-97 Release 97-1 + + M33015 started at 15:21:45 on 17-May-1998 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL Tetracycline Hydrochloride C22H25ClN2O8 P212121 Z=4 CELL 1.5406 10.980703 12.852671 15.733348 90.0 90.0 90.0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC CL C O N H UNIT 4 88 32 8 100 V = 2220.47 At vol = 16.8 F(000) = 1008.0 mu = 1.98 mm-1 Max single Patterson vector = 42.1 cell wt = 1923.56 rho = 1.438 TREF 500 HKLF 3 ** WARNING - IT WOULD BE BETTER TO INPUT F-SQUARED THAN F SO ** THAT ZERO AND NEGATIVE INTENSITIES ARE TREATED CORRECTLY 287 Reflections read, of which 0 rejected Maximum h, k, l and 2-Theta = 10. 12. 15. 95.08 287 Unique reflections, of which 213 observed R(int) = 0.0000 R(sigma) = 0.1551 Friedel opposites merged NUMBER OF UNIQUE DATA AS A FUNCTION OF RESOLUTION IN ANGSTROMS Resolution Inf 5.00 3.50 2.50 2.00 1.70 1.50 1.40 1.30 1.20 1.10 1.00 N(observed) 14. 21. 37. 41. 30. 25. 13. 13. 8. 6. 5. N(measured) 15. 21. 41. 45. 33. 34. 16. 23. 22. 23. 14. N(theory) 15. 26. 62. 88. 109. 130. 90. 121. 158. 232. 317. Two-theta 0.0 17.7 25.4 35.9 45.3 53.9 61.8 66.8 72.7 79.9 88.9 100.8 Highest memory for sort/merge = 2439 / 1435 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 71 53 34 24 19 13 7 4 3 3 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.665 0.672 1.052 0.583 0.2 seconds elapsed time SUMMARY OF PARAMETERS FOR Tetracycline Hydrochloride C22H25ClN2O8 P212121 Z=4 ESEL Emin 1.200 Emax 5.000 DelU 0.005 renorm 0.700 axis 0 OMIT s 4.00 2theta(lim) 180.0 INIT nn 12 nf 16 s+ 0.800 s- 0.200 wr 0.200 PHAN steps 10 cool 0.900 Boltz 0.300 ns 155 mtpr 40 mnqr 10 TREF np 500. nE 251 kapscal 0.850 ntan 3 wn -0.506 FMAP code 8 PLAN npeaks -43 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 69 Reflections and 275. unique TPR for phase annealing 69 Phases refined using 275. unique TPR 71 Reflections and 275. unique TPR for R(alpha) 0.2 seconds elapsed time 9 Unique negative quartets found, 9 used for phase refinement 0.1 seconds elapsed time Highest memory used to derive phase relations = 956 / 2311 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 0 0 2 1.483 0.66 2 2 0 1.219 0.60 2 0 4 1.358 0.53 10 0 2 1.929 0.54 0 4 8 1.241 0.46 0 4 10 1.224 0.46 2 0 12 1.642 0.46 Expected value of Sigma-1 = 0.191 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment 1 2 0 2.217 90 or 270 at random 2 2 3 1.796 random phase 3 2 1 1.705 random phase 2 1 3 1.770 random phase 1 1 5 1.702 random phase 2 2 1 1.347 random phase 2 0 4 1.358 0 or 180 at random 5 2 4 1.481 random phase 4 2 4 1.768 random phase 1 2 6 1.329 random phase 6 2 6 1.396 random phase 3 6 3 1.219 random phase All other phases random with initial weights of 0.200 replaced by 0.2*alpha (or 1 if less) during first 4 cycles - unit weights for all phases thereafter 9 Unique NQR employed in phase annealing 125 Parallel refinements, highest memory = 602 / 19124 0.0 seconds elapsed time STRUCTURE SOLUTION for Tetracycline Hydrochloride C22H25ClN2O8 P212121 Z=4 Phase annealing cycle: 1 Beta = 0.56984 Ralpha 1.463 1.387 0.689 0.994 0.463 1.470 1.218 1.125 1.078 1.211 0.953 1.459 0.828 0.680 0.720 0.654 0.878 1.131 0.556 1.675 Nqual -0.155-0.344-0.380-0.497 0.003-0.382 0.146-0.348-0.343-0.538-0.149 0.049-0.537-0.215 0.269-0.406-0.770-0.206-0.180 0.346 Mabs 0.463 0.476 0.583 0.516 0.642 0.467 0.511 0.518 0.515 0.492 0.543 0.479 0.556 0.591 0.602 0.610 0.563 0.517 0.626 0.462 Phase annealing cycle: 2 Beta = 0.63316 Ralpha 0.223 0.286 0.149 0.209 0.189 0.235 0.148 0.256 0.181 0.275 0.165 0.265 0.170 0.187 0.160 0.156 0.142 0.136 0.145 0.185 Nqual -0.550-0.512-0.537-0.391-0.563-0.467-0.452-0.626 0.239-0.729-0.509-0.210-0.864-0.529-0.634-0.664-0.620-0.408-0.426-0.749 Mabs 0.894 0.868 0.947 0.849 0.953 0.865 0.970 0.890 0.967 0.855 0.987 0.831 1.012 0.909 1.091 1.088 0.937 1.108 1.029 1.044 Phase annealing cycle: 3 Beta = 0.70351 Ralpha 0.156 0.263 0.246 0.239 0.213 0.281 0.160 0.223 0.142 0.171 0.169 0.196 0.207 0.196 0.218 0.163 0.215 0.161 0.189 0.247 Nqual -0.546-0.557-0.743-0.559-0.807-0.552-0.541-0.694-0.395-0.726-0.710-0.272-0.632-0.613-0.707-0.561-0.600-0.607-0.589-0.694 Mabs 0.951 0.841 0.858 0.857 0.889 0.812 0.983 0.893 1.037 1.012 0.955 0.942 0.895 0.908 1.010 0.942 0.973 0.997 0.898 0.925 Phase annealing cycle: 4 Beta = 0.78167 Ralpha 0.240 0.311 0.321 0.210 0.200 0.147 0.181 0.194 0.195 0.202 0.171 0.198 0.221 0.172 0.114 0.157 0.161 0.182 0.222 0.191 Nqual -0.759-0.622-0.060-0.701-0.889-0.675-0.529-0.385-0.621-0.683-0.510-0.506-0.539-0.773-0.662-0.633-0.811-0.628-0.714-0.552 Mabs 0.902 0.845 0.849 0.841 0.885 0.987 0.965 0.928 0.986 1.007 0.969 0.959 0.889 1.026 1.049 0.940 0.983 0.931 0.914 1.107 Phase annealing cycle: 5 Beta = 0.86853 Ralpha 0.182 0.198 0.297 0.130 0.192 0.115 0.161 0.164 0.162 0.236 0.211 0.114 0.192 0.142 0.218 0.184 0.187 0.167 0.177 0.195 Nqual -0.644-0.512-0.239-0.528-0.907-0.631-0.346-0.319-0.474-0.677-0.492-0.767-0.657-0.699-0.729-0.609-0.431-0.381-0.560-0.402 Mabs 0.887 0.904 0.801 0.986 0.970 1.016 0.963 0.971 1.041 0.936 1.018 1.060 0.886 1.020 1.034 1.007 0.927 0.995 1.039 1.003 Phase annealing cycle: 6 Beta = 0.96503 Ralpha 0.258 0.183 0.115 0.162 0.218 0.154 0.180 0.216 0.181 0.140 0.152 0.125 0.159 0.165 0.165 0.178 0.158 0.127 0.148 0.186 Nqual -0.569-0.346-0.652-0.783-0.769-0.721-0.490-0.471-0.412-0.742-0.399-0.700-0.711-0.635-0.537-0.618-0.681-0.541-0.738-0.611 Mabs 0.854 0.933 1.008 1.030 0.923 0.996 0.970 0.949 1.042 1.041 1.086 1.128 0.943 1.075 1.092 1.062 0.964 1.121 1.138 1.066 Phase annealing cycle: 7 Beta = 1.07225 Ralpha 0.276 0.216 0.166 0.191 0.193 0.189 0.144 0.163 0.222 0.188 0.148 0.144 0.219 0.171 0.157 0.132 0.163 0.164 0.175 0.196 Nqual -0.652-0.260-0.649-0.669-0.540-0.721-0.575-0.686-0.638-0.842-0.665-0.790-0.730-0.640-0.786-0.629-0.838-0.677-0.678-0.509 Mabs 0.835 0.995 1.018 0.964 0.945 1.052 0.967 0.904 0.915 1.020 1.111 1.077 0.918 1.001 1.170 1.092 0.987 1.055 1.043 1.001 Phase annealing cycle: 8 Beta = 1.19139 Ralpha 0.258 0.223 0.209 0.162 0.173 0.149 0.155 0.182 0.215 0.215 0.146 0.140 0.247 0.177 0.170 0.129 0.192 0.165 0.145 0.201 Nqual -0.540-0.391-0.614-0.644-0.666-0.799-0.701-0.505-0.744-0.722-0.502-0.818-0.774-0.443-0.603-0.741-0.935-0.636-0.523-0.611 Mabs 0.913 0.965 0.958 1.015 1.076 1.054 0.979 0.994 0.902 1.001 1.050 1.041 0.859 1.057 0.989 1.076 0.962 1.137 1.133 0.970 Phase annealing cycle: 9 Beta = 1.32377 Ralpha 0.143 0.203 0.235 0.174 0.117 0.219 0.178 0.219 0.227 0.200 0.147 0.135 0.205 0.129 0.152 0.161 0.158 0.149 0.170 0.153 Nqual -0.793-0.469-0.575-0.672-0.428-0.606-0.720-0.770-0.305-0.588-0.481-0.776-0.829-0.649-0.652-0.733-0.730-0.618-0.578-0.670 Mabs 0.942 0.982 0.992 1.042 1.105 1.006 0.948 0.936 0.911 1.022 1.094 1.076 0.947 1.121 1.092 1.031 0.929 1.122 1.061 1.013 Phase annealing cycle: 10 Beta = 1.47086 Ralpha 0.168 0.209 0.175 0.191 0.153 0.276 0.125 0.199 0.194 0.207 0.189 0.145 0.236 0.151 0.234 0.162 0.225 0.210 0.204 0.142 Nqual -0.627-0.466-0.734-0.775-0.642-0.694-0.649-0.738-0.785-0.601-0.475-0.662-0.695-0.769-0.365-0.548-0.649-0.707-0.865-0.565 Mabs 0.919 0.957 0.945 0.967 1.147 0.947 1.016 0.962 0.963 0.941 1.010 1.144 0.922 1.040 0.949 0.964 0.972 0.984 1.015 1.088 Phase refinement cycle: 1 Ralpha 0.223 0.221 0.166 0.189 0.160 0.191 0.163 0.190 0.152 0.219 0.185 0.145 0.193 0.169 0.206 0.116 0.254 0.176 0.164 0.198 Nqual -0.586-0.724-0.613-0.614-0.795-0.352-0.772-0.803-0.735-0.757-0.645-0.714-0.537-0.476-0.558-0.625-0.621-0.707-0.499-0.804 Mabs 0.928 1.010 0.965 0.981 1.085 0.995 1.005 0.979 0.970 0.939 1.047 1.004 1.020 1.061 0.997 1.068 0.859 1.163 1.040 1.134 Phase refinement cycle: 2 Ralpha 0.155 0.211 0.108 0.168 0.170 0.188 0.160 0.132 0.123 0.152 0.180 0.188 0.146 0.149 0.175 0.188 0.153 0.158 0.130 0.161 Nqual -0.697-0.416-0.620-0.688-0.537-0.038-0.602-0.886-0.829-0.394-0.717-0.727-0.351-0.421-0.696-0.608-0.845-0.754-0.731-0.780 Mabs 1.009 1.035 1.040 0.981 1.099 1.072 1.062 1.072 1.042 1.096 1.131 1.044 1.104 1.058 1.006 1.078 1.004 1.118 1.142 1.086 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1913623. 0.136 -0.719 -0.652 1.011 0.136 ----- +- 1179507. 0.187 -0.605 -0.321 1.051 0.187 ---+- -- 1703231. 0.155 -0.615 -0.208 0.977 0.155 -+-+- ++ 127547. 0.145 -0.808 0.186 0.995 0.145 +-+-- -+ 637735. 0.178 -0.600 -0.021 1.158 0.178 -+-++ -- 1091523. 0.222 -0.522 0.197 0.999 0.222 +-+-- -+ 1263311. 0.144 -0.261 -0.824 1.111 0.204 ----+ +- 25099. 0.146 -0.748 0.535 1.008 0.146 ++-+- ++ 125495. 0.124 -0.738 -0.144 1.131 0.124 +-+-+ ++ 627475. 0.187 -0.392 0.723 1.056 0.200 ++--- -- 1040223. 0.186 -0.697 0.544 1.127 0.186 ++-++ -+ 1006811. 0.162 -0.567 0.195 1.035 0.162 +-+++ -+ 839751. 0.164 -0.721 0.360 0.999 0.164 +-++- -+ 4451. 0.138 -0.625 0.723 1.162 0.138 ++--- -- 22255. 0.199 -0.711 0.825 0.997 0.199 ++++- +- 111275. 0.171 -0.795 0.661 0.987 0.171 +++-- -+ 556375. 0.167 -0.770 0.374 0.959 0.167 +-+-- -- 684723. 0.136 -0.677 1.000 1.175 0.136 ++++- -- 1326463. 0.153 -0.689 -0.032 1.179 0.153 -+-+- -+ 340859. 0.154 -0.667 0.197 1.105 0.154 +-+-- -+ 1704295. 0.143 -0.700 -0.208 1.133 0.143 -+-+- ++ 132867. 0.174 -0.599 0.382 1.127 0.174 ++--+ -+ 664335. 0.162 -0.741 -0.371 1.051 0.162 --+++ -- 1224523. 0.132 -0.554 0.710 1.091 0.132 ++-+- -+ 1928311. 0.182 -0.530 0.196 1.047 0.182 +-+++ +- 1252947. 0.185 -0.729 0.197 0.984 0.185 +-+-- -+ 2070431. 0.145 -0.530 0.195 1.068 0.145 +-+++ +- 1963547. 0.143 -0.773 0.534 1.133 0.143 ++-+- ++ 1429127. 0.144 -0.576 -0.083 1.114 0.144 +---+ -+ 2062895. 0.127 -0.347 0.082 1.154 0.152 +---- +- 2090215. 0.166 -0.343 0.837 1.156 0.193 +++-- -- 1925867. 0.188 -0.559 0.197 1.020 0.188 +-+-- -+ 1998779. 0.141 -0.825 0.032 1.085 0.141 +-+-+ +- 1945883. 0.085 -0.593 0.723 1.157 0.085* ++--- -- 865719. 0.180 -0.768 1.000 1.059 0.180 ++++- -- 802155. 0.182 -0.135 1.000 0.969 0.320 ++++- -- 870947. 0.150 -0.571 0.885 1.044 0.150 ++-+- -- 1658047. 0.177 -0.671 0.083 1.081 0.177 -+++- +- 1605287. 0.183 -0.362 -0.258 1.062 0.204 +---+ ++ 1240727. 0.173 -0.857 0.660 1.038 0.173 +++-- -+ 160431. 0.192 -0.752 0.258 1.064 0.192 -+++- -- 1017959. 0.143 -0.401 -0.082 1.045 0.154 -++++ +- 2062467. 0.162 -0.734 0.093 1.069 0.162 -++++ -- 503039. 0.177 -0.672 -0.197 1.059 0.177 -+-++ +- 1955831. 0.139 -0.667 0.721 1.105 0.139 ++-++ -- 1072195. 0.156 -0.711 0.661 1.122 0.156 +++-- -+ 1589679. 0.177 -0.668 0.824 1.046 0.177 ++++- -+ 1711239. 0.170 -0.543 0.093 1.153 0.170 -++++ -- 1301179. 0.135 -0.578 -0.082 1.049 0.135 -++++ -+ 1952767. 0.137 -0.722 0.021 0.984 0.137 +-+-- ++ 1577587. 0.166 -0.265 0.885 1.090 0.224 ++-+- -- 1992967. 0.253 0.106 -0.371 0.961 0.628 --+++ -- 1573971. 0.149 -0.662 -0.660 1.127 0.149 ----- +- 1457631. 0.155 -0.392 0.484 1.110 0.168 +++++ ++ 66087. 0.149 -0.855 0.723 1.107 0.149 ++--- -- 1848803. 0.176 -0.868 0.660 1.088 0.176 +++++ +- 1903799. 0.192 -0.439 0.185 1.034 0.196 +-++- ++ 1690939. 0.147 -0.132 0.723 1.077 0.287 ++--- -- 413655. 0.191 0.112 -0.246 1.104 0.573 -++-+ -+ 2092523. 0.187 0.287 -0.672 0.994 0.817 ---+- ++ 1390407. 0.141 -0.878 -0.144 1.034 0.141 +-+-+ ++ 104503. 0.148 -0.649 0.824 1.061 0.148 ++++- -+ 930167. 0.184 -0.474 0.082 1.078 0.185 +---- -+ 515423. 0.166 -0.433 0.545 1.069 0.172 ++-++ +- 1275119. 0.147 -0.547 0.723 1.171 0.147 ++--- -- 1151915. 0.160 -0.528 -0.070 1.018 0.160 -++-+ -- 1534899. 0.171 -0.483 -0.661 1.017 0.172 ---++ +- 522515. 0.144 -0.692 0.824 1.143 0.144 ++++- -+ 275899. 0.165 -0.779 0.258 1.052 0.165 +---- -- 518555. 0.195 -0.675 0.421 1.025 0.195 +--+- -- 495623. 0.125 0.084 0.824 1.102 0.473 ++++- -+ 1854723. 0.196 -0.751 -0.195 0.976 0.196 -+--- +- 440331. 0.182 -0.445 0.245 0.986 0.186 +--+- -+ 456531. 0.163 -0.803 0.545 1.022 0.163 ++-++ +- 790375. 0.193 -0.730 0.421 1.088 0.193 +--+- -- 302663. 0.148 -0.616 0.535 1.050 0.148 +-++- -- 1274515. 0.173 -0.609 0.535 1.049 0.173 +-++- -- 1184719. 0.130 -0.671 0.081 1.084 0.130 +--++ +- 843435. 0.165 -0.609 1.000 1.153 0.165 ++++- -- 1323971. 0.167 -0.693 0.824 1.044 0.167 ++++- -+ 739547. 0.178 -0.362 0.382 1.107 0.199 ++--+ +- 1600583. 0.156 -0.821 0.535 1.077 0.156 +-++- -- 1495235. 0.141 -0.690 0.710 1.043 0.141 ++-+- -+ 1047015. 0.166 -0.733 -0.547 1.108 0.166 --+++ +- 863087. 0.220 -0.792 0.344 1.009 0.220 ++-++ ++ 364755. 0.164 -0.738 0.545 1.085 0.164 ++-++ +- 790295. 0.113 -0.772 -0.825 1.126 0.113 ----+ -+ 113335. 0.147 -0.727 0.535 1.029 0.147 +-++- -- 2023963. 0.196 -0.788 0.824 0.939 0.196 ++++- -+ 677411. 0.209 -0.693 1.000 1.053 0.209 ++++- -- 1479459. 0.172 -0.746 0.382 1.118 0.172 ++--+ -+ 183547. 0.197 -0.602 1.000 0.964 0.197 ++++- -- 1823775. 0.156 -0.656 0.661 1.084 0.156 +++-- -+ 1460055. 0.168 -0.695 -0.184 1.007 0.168 -+--+ -- 1532939. 0.163 -0.773 0.360 1.034 0.163 +-++- -+ 574739. 0.110 -0.502 -0.093 1.042 0.110 +---- ++ 1090031. 0.166 -0.750 0.383 1.018 0.166 ++--+ +- 853255. 0.176 -0.236 0.723 1.066 0.249 ++--- -- 1373239. 0.194 -0.827 0.825 1.166 0.194 ++++- +- 79679. 0.155 -0.574 -0.558 1.092 0.155 --++- ++ 1932567. 0.100 -0.725 0.360 1.115 0.100 +-++- -+ 1957203. 0.166 -0.712 -0.258 1.079 0.166 +---+ ++ 1717763. 0.150 0.113 0.421 1.103 0.534 +--+- -- 200207. 0.233 -0.310 -0.208 1.003 0.272 -+-+- ++ 178443. 0.164 -0.512 0.081 1.005 0.164 +--++ +- 1785563. 0.174 -0.737 0.824 1.122 0.174 ++++- -+ 269863. 0.187 0.185 0.421 1.049 0.664 +--+- -- 1255851. 0.121 -0.394 0.484 1.143 0.133 +++++ ++ 1274227. 0.171 -0.651 0.245 1.072 0.171 +--+- -+ 50003. 0.229 -0.093 -0.032 0.977 0.400 -+-+- +- 211167. 0.122 -0.492 0.195 1.063 0.122 +-+++ +- 537943. 0.152 -0.723 -0.672 1.192 0.152 ---+- ++ 1185255. 0.180 -0.633 0.558 1.104 0.180 ++--+ -- 1757215. 0.152 -0.766 0.019 1.017 0.152 +-+++ ++ 1562463. 0.192 -0.390 0.371 1.100 0.205 ++--- ++ 527019. 0.175 -0.692 0.083 1.115 0.175 -+++- +- 2037431. 0.220 -0.679 -0.547 1.011 0.220 --+++ +- 1745223. 0.160 -0.562 -0.083 1.181 0.160 +---+ -+ 489719. 0.185 -0.360 0.547 0.986 0.206 ++--- -+ 865663. 0.182 -0.594 0.382 1.106 0.182 ++--+ -+ 1264439. 0.126 -0.717 0.661 1.155 0.126 +++-- -+ 153695. 0.175 -0.828 0.547 1.044 0.175 ++--- -+ 134011. 0.176 -0.468 0.421 0.991 0.178 +--+- -- 1798547. 0.128 -0.417 0.545 1.065 0.136 ++-++ -+ 570391. 0.164 -0.584 -0.197 1.111 0.164 -+-++ -+ 2061759. 0.128 -0.729 -0.212 1.060 0.128 -+-+- ++ 1212327. 0.129 -0.642 -0.093 1.080 0.129 -+++- ++ 545931. 0.135 -0.504 0.197 1.147 0.135 +-+-- -+ 1468251. 0.117 -0.591 0.195 1.140 0.117 +-+++ +- 778895. 0.119 -0.652 0.824 1.105 0.119 ++++- -+ 1300763. 0.132 -0.704 0.824 1.068 0.132 ++++- -+ 388591. 0.125 -0.660 0.885 1.203 0.125 ++-+- -- 914175. 0.103 -0.804 0.360 1.021 0.103 +-++- -+ 712759. 0.133 -0.759 0.723 1.119 0.133 ++--- -- 1479707. 0.135 -0.798 0.535 1.127 0.135 +-++- -- 1553931. 0.132 -0.490 0.660 1.025 0.132 +++++ +- 1220391. 0.135 -0.645 0.245 1.067 0.135 +--+- -+ 1732031. 0.126 -0.549 0.885 1.174 0.126 ++-+- -- 1107999. 0.130 -0.655 0.321 1.058 0.130 +++-+ ++ 853031. 0.113 -0.593 0.258 1.058 0.113 +---- -- 467767. 0.131 -0.586 -0.245 1.061 0.131 -++-+ -+ 850247. 0.121 -0.740 0.661 1.087 0.121 +++-- -+ 824919. 0.131 -0.689 0.197 1.042 0.131 +-+-- -+ 1990727. 0.113 -0.608 0.360 1.087 0.113 +-++- -+ 2092895. 0.125 -0.716 -0.672 1.194 0.125 ---+- ++ 355919. 0.122 -0.476 0.998 1.066 0.123 ++++- -- 425783. 0.135 -0.734 -0.835 1.025 0.135 ----- ++ 494055. 0.121 -0.782 0.651 1.034 0.121 ++++- ++ 1050891. 0.128 -0.493 0.723 1.097 0.129 ++--- -- 1788127. 0.114 -0.538 0.723 1.182 0.114 ++--- -- 36987. 0.130 -0.756 0.661 1.240 0.130 +++-- -+ 1205075. 0.134 -0.743 0.371 1.065 0.134 ++--- ++ 766747. 0.130 -0.817 1.000 1.114 0.130 ++++- -- 2013019. 0.133 -0.774 0.885 1.161 0.133 ++-+- -- 1381695. 0.131 -0.732 -0.497 1.163 0.131 ---+- +- 52615. 0.128 -0.568 0.660 1.114 0.128 +++++ +- 1287535. 0.117 -0.740 0.372 1.149 0.117 +-+-- -- 291827. 0.117 -0.517 -0.486 1.086 0.117 ---++ -- 868887. 0.092 -0.495 -0.093 1.089 0.092 +---- ++ 765275. 0.125 -0.770 0.372 1.062 0.125 +-+-- -- 992651. 0.126 -0.481 0.837 1.083 0.127 +++-- -- 805739. 0.121 -0.700 0.032 1.061 0.121 +-+-+ -+ 961439. 0.135 -0.788 0.545 1.111 0.135 ++-++ +- 882895. 0.133 -0.683 0.837 1.126 0.133 +++-- -- CFOM Range Frequency 0.000 - 0.020 0 0.020 - 0.040 0 0.040 - 0.060 0 0.060 - 0.080 0 0.080 - 0.100 2 0.100 - 0.120 11 0.120 - 0.140 58 0.140 - 0.160 121 0.160 - 0.180 136 0.180 - 0.200 86 0.200 - 0.220 32 0.220 - 0.240 19 0.240 - 0.260 8 0.260 - 0.280 4 0.280 - 0.300 4 0.300 - 0.320 1 0.320 - 0.340 3 0.340 - 0.360 0 0.360 - 0.380 2 0.380 - 0.400 1 0.400 - 0.420 1 0.420 - 0.440 0 0.440 - 0.460 2 0.460 - 0.480 1 0.480 - 0.500 0 0.500 - 0.520 0 0.520 - 0.540 1 0.540 - 0.560 0 0.560 - 0.580 2 0.580 - 0.600 0 0.600 - 9.999 5 500. Phase sets refined - best is code 1945883. with CFOM = 0.0854 6.2 seconds elapsed time Tangent expanded to 69 out of 71 E greater than 1.200 Highest memory used = 435 / 673 0.0 seconds elapsed time FMAP and GRID set by program FMAP 8 1 11 GRID -3.125 -2 -2 3.125 2 2 E-Fourier for Tetracycline Hydrochloride C22H25ClN2O8 P212121 Z=4 Maximum = 301.33, minimum = -148.45 highest memory used = 8931 / 1726 0.1 seconds elapsed time Heavy-atom assignments: x y z s.o.f. Height CL1 0.0573 0.4185 0.9045 1.0000 301.3 CL2 0.1320 0.7633 0.8953 1.0000 201.3 CL3 0.0268 0.7590 0.0442 1.0000 198.2 CL4 0.0256 0.4720 0.3360 1.0000 194.6 CL5 0.1689 0.3245 0.4170 1.0000 183.3 CL6 0.1822 0.8509 0.4244 1.0000 177.7 Peak list optimization RE = 0.355 for 25 surviving atoms and 71 E-values Highest memory used = 1746 / 639 0.1 seconds elapsed time E-Fourier for Tetracycline Hydrochloride C22H25ClN2O8 P212121 Z=4 Maximum = 330.89, minimum = -178.28 highest memory used = 8979 / 1772 0.1 seconds elapsed time Peak list optimization RE = 0.325 for 28 surviving atoms and 71 E-values Highest memory used = 1794 / 639 0.1 seconds elapsed time E-Fourier for Tetracycline Hydrochloride C22H25ClN2O8 P212121 Z=4 Maximum = 303.37, minimum = -152.24 highest memory used = 8979 / 1772 0.1 seconds elapsed time Molecule 1 scale 0.403 inches = 1.023 cm per Angstrom 32 39 CL1 21 26 33 15 42 14 41 13 37 25 36 22 40 31 38 31 35 35 19 40 19 1 29 14 7 CL5 9 13 37 CL4 23 22 28 11 27 18 8 12 C** 3 23 29 43 4 39 26 1 22 20 6 24 11 17 41 19 12 34 25 2 43 13 CL5 9 12 35 5 28 40 42 10 14 CL3 31 33 3736 15 24 35 ** CL514 28 16 10 30 34 1*5 40 16 39 CL2 CL3 24 9 17 34 CL5 3135 Atom Peak x y z SOF Height Distances and Angles CL1 0. 0.0573 0.4185 0.9045 1.000 2.05 0 15 1.455 0 21 1.822 109.0 0 32 2.205 53.0 143.5 0 36 2.459 93.0 87.9 121.2 0 37 2.461 108.6 89.6 124.9 17.1 CL2 0. 0.8680 1.2633 0.6047 1.000 1.46 0 10 2.035 0 16 1.457 55.9 0 24 2.456 157.5 105.5 CL3 0. 0.4732 1.2410 0.5442 1.000 1.52 0 CL5 2.387 0 2 1.685 107.1 0 40 2.342 164.9 81.1 0 43 2.312 100.7 50.8 74.4 27 24 1.448 60.8 113.0 128.5 153.2 CL4 0. 0.4744 0.5280 0.8360 1.000 2.36 0 7 1.570 0 12 1.996 89.3 0 19 2.365 118.7 147.9 0 38 1.819 52.3 127.8 69.5 CL5 0. 0.6689 1.1755 0.5830 1.000 1.69 0 CL3 2.387 0 10 1.919 133.6 0 34 1.886 83.9 131.0 0 35 1.873 91.3 131.5 57.0 27 24 2.102 37.0 170.0 53.5 58.3 46 36 2.226 134.6 75.9 100.3 56.8 113.1 54 40 2.243 114.9 107.6 32.6 50.4 80.1 71.4 CL6 0. 0.1822 0.8509 0.4244 1.000 3.12 0 1 2.189 0 3 1.167 36.5 0 20 1.907 72.3 106.9 0 22 2.453 142.1 105.8 144.3 1 164. 0.3535 0.8681 0.4942 1.000 2.86 0 CL6 2.189 0 3 1.431 29.0 0 11 1.784 100.4 123.4 0 20 2.428 48.4 76.3 53.7 22 19 2.284 158.5 170.4 66.0 112.9 2 162. 0.3688 1.1597 0.5859 1.000 1.50 0 CL3 1.685 0 11 2.273 116.6 0 17 2.444 106.5 103.1 0 39 2.446 141.7 72.8 38.2 0 41 2.125 104.0 138.8 56.8 71.3 0 43 1.807 82.9 155.3 84.0 101.8 30.8 3 158. 0.2492 0.8082 0.4702 1.000 3.08 0 CL6 1.167 0 1 1.431 114.5 0 18 1.784 131.7 113.8 4 157. 0.1399 0.9663 0.2948 1.000 3.35 0 6 1.401 0 20 2.372 41.9 5 156. 0.3121 1.1283 0.2625 1.000 3.13 0 6 2.271 0 28 2.099 91.2 0 30 2.053 145.0 56.7 0 33 2.343 113.6 130.2 99.1 6 150. 0.1703 1.0511 0.3465 1.000 2.86 0 4 1.401 0 5 2.271 99.5 0 20 1.625 103.0 118.3 7 146. 0.3999 0.4854 0.7582 1.000 2.82 0 CL4 1.570 0 8 2.445 117.0 0 25 2.316 144.6 96.7 0 38 1.512 72.3 164.5 72.4 8 145. 0.4380 0.5669 0.6203 1.000 3.26 0 7 2.445 0 14 2.344 90.8 0 23 1.752 135.9 104.4 0 27 1.589 94.2 52.9 65.8 9 144. 0.4576 1.0402 0.4539 1.000 2.59 0 11 1.682 0 31 1.831 136.2 0 35 2.425 125.8 21.3 22 19 2.010 74.7 63.5 64.8 27 24 2.231 117.2 65.7 49.2 105.4 10 137. 0.7625 1.1793 0.6860 1.000 1.25 0 CL2 2.035 0 CL5 1.919 77.8 0 16 1.714 44.7 118.3 32 28 1.204 113.0 110.6 111.0 11 126. 0.3465 1.0029 0.5209 1.000 2.29 0 1 1.784 0 2 2.273 164.2 0 9 1.682 95.6 87.2 0 20 1.987 80.0 115.3 96.1 22 19 2.255 67.7 101.0 59.3 135.4 12 125. 0.4933 0.6637 0.7757 1.000 2.24 0 CL4 1.996 31 28 2.438 105.3 57 43 1.921 111.9 120.8 13 123. 0.1320 0.6348 0.4920 1.000 3.44 0 14 2.424 0 18 1.434 71.5 0 22 2.315 163.0 114.9 21 19 1.459 95.0 164.2 75.8 36 31 2.352 37.1 108.6 134.3 58.8 47 37 2.238 46.0 82.9 117.7 81.7 54.3 14 123. 0.2505 0.5065 0.5689 1.000 3.56 0 8 2.344 0 13 2.424 114.7 0 18 2.394 80.2 34.6 0 27 1.878 42.4 80.7 51.4 36 31 1.522 172.5 68.8 103.4 135.4 43 35 1.746 150.5 82.5 112.9 163.2 34.0 47 37 1.829 110.7 61.6 71.3 116.6 76.8 54.7 52 40 2.261 101.6 127.2 139.7 144.1 80.1 50.9 70.6 15 120. 0.0081 0.4809 0.8353 1.000 2.15 0 CL1 1.455 0 32 1.766 85.8 0 42 1.504 145.0 128.0 39 33 2.418 116.8 127.2 38.4 16 117. 0.9143 1.2089 0.6793 1.000 1.31 0 CL2 1.457 0 10 1.714 79.4 32 28 2.422 86.1 27.6 34 30 2.446 121.2 71.8 47.8 17 117. 0.1705 1.2420 0.5645 1.000 1.19 0 2 2.444 0 39 1.600 71.0 0 40 2.025 72.6 141.3 0 41 2.192 54.3 88.4 80.6 26 24 1.734 163.0 116.3 95.8 137.6 40 34 0.925 86.4 143.4 21.1 101.6 79.2 44 35 2.460 118.1 165.7 45.6 105.8 51.8 35.8 18 110. 0.2460 0.6809 0.5155 1.000 3.26 0 3 1.784 0 13 1.434 107.0 0 14 2.394 176.2 73.8 0 23 2.463 95.0 158.0 84.2 0 27 1.912 131.2 113.9 50.2 47.1 19 110. 0.4635 0.4378 0.9668 1.000 2.00 0 CL4 2.365 0 38 2.428 44.6 5 1 2.284 112.4 136.2 6 9 2.010 101.4 137.3 73.2 9 11 2.255 81.1 124.8 46.3 46.0 12 13 1.459 125.9 81.3 108.0 124.0 151.5 23 22 2.415 87.7 67.4 76.5 149.6 108.6 68.3 35 31 2.027 105.6 104.0 119.4 54.0 99.1 83.2 151.0 42 35 2.402 83.4 82.4 138.5 66.0 104.0 89.4 144.4 23.7 20 109. 0.2155 0.9960 0.4340 1.000 2.64 0 CL6 1.907 0 1 2.428 59.2 0 4 2.372 72.7 118.0 0 6 1.625 107.5 144.7 35.1 0 11 1.987 103.7 46.3 153.6 141.7 21 107. 0.1431 0.3101 0.8601 1.000 2.68 0 CL1 1.822 0 26 2.112 148.2 22 106. 0.0264 0.7222 0.3865 1.000 3.59 0 CL6 2.453 0 13 2.315 78.7 0 29 1.021 152.1 124.5 21 19 2.415 114.5 35.8 89.8 25 23 1.458 80.3 114.0 76.0 118.3 23 105. 0.4485 0.6945 0.5820 1.000 3.05 0 8 1.752 0 18 2.463 91.2 0 27 1.820 52.8 50.3 24 22 1.458 127.6 136.6 135.9 33 29 1.564 127.6 103.9 100.9 39.3 24 102. 1.0484 1.3079 0.5200 1.000 1.88 0 CL2 2.456 1 CL3 1.448 79.5 3 CL5 2.102 161.7 82.3 7 9 2.231 75.1 104.7 109.6 19 17 1.734 106.9 120.7 82.8 134.3 37 31 2.229 114.0 138.0 79.8 48.5 94.3 41 34 1.806 136.0 124.2 57.1 123.1 30.2 74.9 45 35 1.945 140.0 128.8 55.0 70.6 83.7 26.0 57.0 25 100. 0.2279 0.3933 0.7182 1.000 3.17 0 7 2.316 0 26 2.429 126.5 0 38 2.353 37.8 100.7 39 33 2.393 144.7 83.2 129.0 55 41 2.015 108.2 42.7 109.6 106.9 26 96. 0.1807 0.2141 0.7543 1.000 3.53 0 21 2.112 0 25 2.429 70.8 55 41 1.663 121.0 55.2 27 96. 0.3122 0.6280 0.6192 1.000 2.98 0 8 1.589 0 14 1.878 84.6 0 18 1.912 121.0 78.4 0 23 1.820 61.4 123.5 82.6 28 95. 0.2127 1.2678 0.2614 1.000 2.62 0 5 2.099 0 30 1.971 60.5 8 10 1.204 103.9 101.8 10 12 2.438 142.2 142.2 98.8 18 16 2.422 68.1 66.7 41.3 140.2 29 93. -0.0585 0.7022 0.3656 1.000 3.69 0 22 1.021 25 23 1.564 64.7 30 93. 0.3440 1.2467 0.1778 1.000 3.20 0 5 2.053 0 28 1.971 62.8 18 16 2.446 68.3 65.5 31 92. 0.6243 1.0349 0.4523 1.000 2.74 0 9 1.831 0 34 2.476 110.3 0 35 0.979 115.9 37.0 13 13 2.352 93.8 142.5 106.8 16 14 1.522 157.8 89.8 85.7 74.0 22 19 2.027 62.6 132.4 100.2 38.0 110.9 27 24 2.229 65.8 44.8 60.6 141.4 134.4 104.9 49 37 2.096 131.5 82.5 49.9 60.1 58.2 74.3 108.2 32 90. -0.1205 0.4982 0.9011 1.000 1.68 0 CL1 2.205 0 15 1.766 41.2 50 39 1.630 128.7 112.1 33 89. 0.5129 1.0957 0.3051 1.000 3.18 0 5 2.343 17 15 2.418 77.9 29 25 2.393 151.0 84.6 56 42 1.552 94.3 37.0 85.1 34 89. 0.7107 1.2114 0.4705 1.000 2.16 0 CL5 1.886 0 31 2.476 77.9 0 35 1.794 61.1 19.2 20 17 0.925 126.8 110.0 126.6 27 24 1.806 69.4 60.4 65.4 70.6 51 39 2.406 118.6 132.6 146.9 23.4 83.2 54 40 1.209 90.1 76.9 69.8 142.9 135.2 140.2 35 84. 0.6660 1.0801 0.4931 1.000 2.43 0 CL5 1.873 0 9 2.425 110.3 0 31 0.979 153.0 42.8 0 34 1.794 61.9 114.0 123.8 16 14 1.746 146.1 103.0 60.3 110.1 20 17 2.460 70.6 97.0 108.7 17.6 112.1 22 19 2.402 108.1 49.2 56.1 158.6 88.6 144.7 27 24 1.945 66.8 60.2 93.4 57.6 140.0 44.5 101.4 46 36 1.975 70.6 124.0 119.5 114.1 85.7 131.0 76.4 134.2 49 37 1.645 91.0 122.1 103.0 123.4 65.2 140.8 73.2 154.8 20.9 54 40 1.783 75.6 148.1 127.0 39.5 79.7 54.2 161.0 97.1 87.8 88.3 36 82. 0.2488 0.5176 0.9088 1.000 1.86 0 CL1 2.459 0 37 0.734 81.5 0 38 1.781 101.2 113.7 2 CL5 2.226 145.2 104.8 106.9 42 35 1.975 129.6 53.3 115.7 52.5 37 81. 0.2491 0.4981 0.9527 1.000 1.71 0 CL1 2.461 0 36 0.734 81.3 0 38 2.182 90.6 48.3 12 13 2.238 105.5 121.5 73.3 15 14 1.829 107.2 161.9 144.4 72.4 35 31 2.096 151.8 126.6 110.6 65.6 45.0 42 35 1.645 155.6 105.7 111.7 90.8 60.1 27.1 53 40 2.389 108.0 99.2 140.5 130.2 63.2 67.3 48.2 38 76. 0.3414 0.4436 0.8382 1.000 2.51 0 CL4 1.819 0 7 1.512 55.3 0 19 2.428 65.9 118.0 0 25 2.353 125.0 69.8 162.3 0 36 1.781 98.8 124.9 79.2 110.2 0 37 2.182 101.4 140.4 65.1 120.3 17.9 39 75. 0.1507 1.1208 0.5828 1.000 1.47 0 2 2.446 0 17 1.600 70.8 38 32 1.630 113.2 175.8 40 34 2.406 63.6 13.3 167.5 40 74. 0.2994 1.3441 0.5255 1.000 1.15 0 CL3 2.342 0 17 2.025 99.5 4 CL5 2.243 123.6 73.2 14 14 2.261 132.7 109.9 100.5 40 34 1.209 108.4 16.0 57.3 109.7 44 35 1.783 177.6 80.2 54.0 49.4 70.7 48 37 2.389 136.2 122.7 65.7 46.2 110.3 43.5 41 70. 0.2804 1.2504 0.6806 1.000 0.68 0 2 2.125 0 17 2.192 68.9 0 43 1.088 58.2 119.2 28 25 2.015 146.8 97.6 110.1 30 26 1.663 129.5 101.9 134.0 82.1 42 69. 0.0218 0.5094 0.7431 1.000 2.52 0 15 1.504 39 33 1.552 104.6 43 68. 0.3792 1.2469 0.6757 1.000 0.79 0 CL3 2.312 0 2 1.807 46.3 0 41 1.088 120.6 91.0 11 12 1.921 90.7 90.7 136.1 Atom Code x y z Height Symmetry transformation CL3 1 0.9732 1.2590 0.4558 2.29 0.5000+X 2.5000-Y 1.0000-Z CL5 2 0.3311 0.6755 0.9170 1.39 1.0000-X -0.5000+Y 1.5000-Z CL5 3 1.1689 1.3245 0.4170 2.42 0.5000+X 2.5000-Y 1.0000-Z CL5 4 0.1689 1.3245 0.4170 1.64 -0.5000+X 2.5000-Y 1.0000-Z 1 5 0.6465 0.3681 1.0058 2.17 1.0000-X -0.5000+Y 1.5000-Z 9 6 0.5424 0.5402 1.0461 1.35 1.0000-X -0.5000+Y 1.5000-Z 9 7 0.9576 1.4598 0.5461 1.20 0.5000+X 2.5000-Y 1.0000-Z 10 8 0.2625 1.3207 0.3140 2.23 -0.5000+X 2.5000-Y 1.0000-Z 11 9 0.6535 0.5029 0.9791 1.88 1.0000-X -0.5000+Y 1.5000-Z 12 10 0.0067 1.3363 0.2757 2.17 0.5000-X 2.0000-Y -0.5000+Z 12 11 0.5067 1.1637 0.7243 0.92 1.0000-X 0.5000+Y 1.5000-Z 13 12 0.3680 0.3652 0.9920 2.03 0.5000-X 1.0000-Y 0.5000+Z 13 13 0.6320 0.8652 0.5080 3.02 0.5000+X 1.5000-Y 1.0000-Z 14 14 0.2505 1.5065 0.5689 0.39 0.0000+X 1.0000+Y 0.0000+Z 14 15 0.2495 0.4935 1.0689 1.16 0.5000-X 1.0000-Y 0.5000+Z 14 16 0.7505 0.9935 0.4311 3.08 0.5000+X 1.5000-Y 1.0000-Z 15 17 0.5081 1.0191 0.1647 4.11 0.5000+X 1.5000-Y 1.0000-Z 16 18 0.4143 1.2911 0.3207 2.41 -0.5000+X 2.5000-Y 1.0000-Z 17 19 1.1705 1.2420 0.5645 1.96 1.0000+X 0.0000+Y 0.0000+Z 17 20 0.6705 1.2580 0.4355 2.15 0.5000+X 2.5000-Y 1.0000-Z 19 21 0.0365 0.5622 0.4668 3.72 0.5000-X 1.0000-Y -0.5000+Z 19 22 0.5365 0.9378 0.5332 2.59 1.0000-X 0.5000+Y 1.5000-Z 22 23 0.4736 0.2778 0.8865 2.91 0.5000-X 1.0000-Y 0.5000+Z 22 24 0.5264 0.7778 0.6135 2.70 0.5000+X 1.5000-Y 1.0000-Z 23 25 -0.0515 0.8055 0.4180 3.11 -0.5000+X 1.5000-Y 1.0000-Z 24 26 0.0484 1.3079 0.5200 1.10 -1.0000+X 0.0000+Y 0.0000+Z 24 27 0.5484 1.1921 0.4800 2.05 -0.5000+X 2.5000-Y 1.0000-Z 25 28 0.2279 1.3933 0.7182 0.00 0.0000+X 1.0000+Y 0.0000+Z 25 29 0.7279 1.1067 0.2818 3.43 0.5000+X 1.5000-Y 1.0000-Z 26 30 0.1807 1.2141 0.7543 0.36 0.0000+X 1.0000+Y 0.0000+Z 28 31 0.2873 0.7322 0.7614 1.93 0.5000-X 2.0000-Y 0.5000+Z 28 32 0.7127 1.2322 0.7386 0.79 0.5000+X 2.5000-Y 1.0000-Z 29 33 0.4415 0.7978 0.6344 2.46 0.5000+X 1.5000-Y 1.0000-Z 30 34 0.8440 1.2533 0.8222 0.41 0.5000+X 2.5000-Y 1.0000-Z 31 35 0.3757 0.5349 1.0477 1.23 1.0000-X -0.5000+Y 1.5000-Z 31 36 0.1243 0.4651 0.5477 3.70 -0.5000+X 1.5000-Y 1.0000-Z 31 37 1.1243 1.4651 0.5477 1.30 0.5000+X 2.5000-Y 1.0000-Z 32 38 0.1205 0.9982 0.5989 1.75 0.0000-X 0.5000+Y 1.5000-Z 33 39 0.0129 0.4043 0.6949 3.08 -0.5000+X 1.5000-Y 1.0000-Z 34 40 0.2107 1.2886 0.5295 1.24 -0.5000+X 2.5000-Y 1.0000-Z 34 41 1.2107 1.2886 0.5295 2.02 0.5000+X 2.5000-Y 1.0000-Z 35 42 0.3340 0.5801 1.0069 1.25 1.0000-X -0.5000+Y 1.5000-Z 35 43 0.1660 0.4199 0.5069 4.07 -0.5000+X 1.5000-Y 1.0000-Z 35 44 0.1660 1.4199 0.5069 0.90 -0.5000+X 2.5000-Y 1.0000-Z 35 45 1.1660 1.4199 0.5069 1.68 0.5000+X 2.5000-Y 1.0000-Z 36 46 0.7512 1.0176 0.5912 2.22 1.0000-X 0.5000+Y 1.5000-Z 37 47 0.2509 0.5019 0.4527 4.14 0.5000-X 1.0000-Y -0.5000+Z 37 48 0.2509 1.5019 0.4527 0.97 0.5000-X 2.0000-Y -0.5000+Z 37 49 0.7509 0.9981 0.5473 2.49 1.0000-X 0.5000+Y 1.5000-Z 39 50 -0.1507 0.6208 0.9172 1.18 0.0000-X -0.5000+Y 1.5000-Z 39 51 0.6507 1.3792 0.4172 1.84 0.5000+X 2.5000-Y 1.0000-Z 40 52 0.2994 0.3441 0.5255 4.33 0.0000+X -1.0000+Y 0.0000+Z 40 53 0.2006 0.6559 1.0255 0.82 0.5000-X 2.0000-Y 0.5000+Z 40 54 0.7994 1.1559 0.4745 2.39 0.5000+X 2.5000-Y 1.0000-Z 41 55 0.2804 0.2504 0.6806 3.85 0.0000+X -1.0000+Y 0.0000+Z 42 56 0.5218 0.9906 0.2569 3.76 0.5000+X 1.5000-Y 1.0000-Z 43 57 0.6208 0.7469 0.8243 1.84 1.0000-X -0.5000+Y 1.5000-Z 0.1 seconds elapsed time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + M33015 finished at 15:21:52 Total elapsed time: 7.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++