++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XS - CRYSTAL STRUCTURE SOLUTION - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker AXS All Rights Reserved + + shelxs started at 11:36:41 on 15-Jan-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL p21c in P2(1)/c CELL 0.71073 12.2837 9.4548 7.3046 90.000 99.932 90.000 ZERR 4.00 0.0004 0.0004 0.0003 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 36 44 4 4 V = 835.64 At vol = 19.0 F(000) = 320.0 mu = 0.08 mm-1 Max single Patterson vector = 35.7 cell wt = 596.75 rho = 1.186 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 TREF HKLF 4 h k l F*F Sigma Why Rejected -5.00 0.00 -1.00 4.21 1.05 Observed but should be systematically absent 10092 Reflections read, of which 368 rejected Maximum h, k, l and 2-Theta = 15. 12. 9. 55.14 1917 Unique reflections, of which 1653 observed R(int) = 0.0683 R(sigma) = 0.0442 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 0.90 0.80 N(observed) 4. 12. 35. 50. 71. 76. 58. 80. 100. 147. 209. 289. 374. N(measured) 4. 12. 35. 52. 71. 79. 61. 81. 102. 152. 221. 325. 503. N(theory) 6. 14. 35. 52. 71. 79. 61. 81. 102. 152. 221. 325. 504. Two-theta 0.0 8.2 11.7 16.3 20.5 24.1 27.4 29.4 31.7 34.5 37.7 41.6 46.5 52.7 Highest memory for sort/merge = 4156 / 9585 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 525 443 373 311 264 218 190 163 131 104 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.817 1.268 0.952 0.964 0.1 seconds elapsed time SUMMARY OF PARAMETERS FOR p21c in P2(1)/c 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 11 nf 16 s+ 0.800 s- 0.200 wr 0.200 PHAN steps 10 cool 0.900 Boltz 0.400 ns 131 mtpr 40 mnqr 10 TREF np 256. nE 202 kapscal 0.900 ntan 2 wn -0.950 FMAP code 8 PLAN npeaks -19 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 131 Reflections and 1101. unique TPR for phase annealing 202 Phases refined using 3267. unique TPR 229 Reflections and 4079. unique TPR for R(alpha) 0.0 seconds elapsed time 1963 Unique negative quartets found, 1349 used for phase refinement 0.0 seconds elapsed time Highest memory used to derive phase relations = 3265 / 24460 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 10 0 2 3.592 0.77 0 2 2 2.656 0.55 10 2 0 2.368 0.60 0 2 4 2.283 0.93 -6 4 6 2.491 0.50 2 8 0 1.993 0.50 2 4 4 2.217 0.49 -10 2 2 1.883 0.50 8 6 0 1.821 0.47 2 6 0 1.424 0.46 -2 0 6 1.749 0.99 6 2 2 1.508 0.46 4 2 4 1.535 0.46 4 2 0 1.333 0.45 2 6 2 1.297 0.49 -2 2 2 1.287 0.64 2 2 2 1.261 0.64 -8 2 2 1.502 0.45 10 0 0 1.366 0.40 -8 2 6 1.303 0.46 -2 6 4 1.243 0.54 Expected value of Sigma-1 = 0.670 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment 0 1 2 2.929 random phase 0 2 2 2.656 random phase 1 1 2 2.275 random phase 1 4 3 2.539 random phase 1 0 2 2.060 random phase 1 1 1 2.014 random phase 0 2 4 2.283 0 sigma-1 = 0.929 4 3 1 1.991 random phase 6 3 0 1.879 random phase -2 1 1 1.501 random phase -2 0 6 1.749 0 sigma-1 = 0.991 5 1 0 1.471 random phase 3 2 2 1.449 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 196 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 5427 / 58634 0.0 seconds elapsed time STRUCTURE SOLUTION for p21c in P2(1)/c Phase annealing cycle: 1 Beta = 0.07940 Ralpha 0.212 0.053 0.258 0.058 0.053 0.052 0.359 0.038 0.203 0.671 0.437 0.350 0.532 1.072 0.355 0.295 0.129 0.028 0.298 0.626 Nqual -0.218-0.142 0.339-0.554-0.591 0.020-0.402-0.566 0.269-0.122-0.137-0.549-0.021 0.253 0.030-0.212-0.153-0.749 0.246 0.292 Mabs 0.772 1.035 0.742 0.982 1.021 1.011 0.686 1.032 0.775 0.567 0.635 0.683 0.609 0.488 0.689 0.702 0.887 1.073 0.738 0.578 Phase annealing cycle: 2 Beta = 0.08823 Ralpha 0.075 0.057 0.255 0.054 0.052 0.058 0.289 0.042 0.206 0.290 0.350 0.233 0.283 0.532 0.066 0.164 0.040 0.032 0.074 0.607 Nqual -0.530 0.126 0.202-0.670-0.674 0.001-0.521-0.816 0.177-0.263-0.406-0.494 0.006 0.141-0.032-0.337-0.795-0.885 0.141 0.354 Mabs 1.024 1.153 0.749 1.064 1.063 1.151 0.726 1.192 0.779 0.725 0.688 0.764 0.720 0.614 1.025 0.827 1.176 1.139 1.013 0.581 Phase annealing cycle: 3 Beta = 0.09803 Ralpha 0.040 0.055 0.236 0.050 0.050 0.057 0.233 0.042 0.179 0.242 0.324 0.194 0.302 0.296 0.056 0.141 0.042 0.032 0.057 0.572 Nqual -0.817-0.063 0.003-0.627-0.656-0.001-0.146-0.816-0.133-0.206-0.679-0.609 0.185-0.085-0.095-0.151-0.816-0.885-0.001 0.269 Mabs 1.178 1.146 0.760 1.065 1.071 1.151 0.771 1.192 0.788 0.767 0.701 0.806 0.725 0.716 1.137 0.862 1.192 1.139 1.151 0.593 Phase annealing cycle: 4 Beta = 0.10892 Ralpha 0.042 0.055 0.214 0.050 0.051 0.058 0.217 0.042 0.161 0.223 0.317 0.160 0.301 0.240 0.058 0.144 0.042 0.032 0.059 0.515 Nqual -0.816-0.071 0.074-0.563-0.587 0.001-0.307-0.816-0.361-0.297-0.523-0.525-0.286-0.297 0.012 0.105-0.816-0.885 0.146 0.258 Mabs 1.192 1.140 0.783 1.086 1.082 1.152 0.782 1.192 0.823 0.779 0.705 0.838 0.717 0.749 1.151 0.865 1.192 1.139 1.153 0.608 Phase annealing cycle: 5 Beta = 0.12103 Ralpha 0.042 0.057 0.214 0.050 0.050 0.059 0.174 0.042 0.161 0.231 0.305 0.168 0.232 0.238 0.057 0.140 0.042 0.032 0.057 0.571 Nqual -0.816-0.056-0.015-0.563-0.595 0.146-0.144-0.816-0.362-0.434-0.690-0.716-0.490-0.169-0.001-0.011-0.816-0.885-0.001 0.258 Mabs 1.192 1.151 0.783 1.086 1.086 1.153 0.821 1.192 0.814 0.768 0.718 0.841 0.749 0.758 1.151 0.872 1.192 1.139 1.151 0.593 Phase annealing cycle: 6 Beta = 0.13447 Ralpha 0.042 0.058 0.214 0.051 0.051 0.057 0.161 0.042 0.154 0.222 0.300 0.164 0.184 0.236 0.058 0.146 0.042 0.032 0.058 0.599 Nqual -0.816 0.001 0.068-0.587-0.587-0.001-0.075-0.816-0.316-0.304-0.723-0.709-0.676-0.259 0.001-0.208-0.816-0.885 0.000 0.105 Mabs 1.192 1.151 0.785 1.082 1.082 1.151 0.839 1.192 0.830 0.777 0.725 0.843 0.785 0.759 1.151 0.863 1.192 1.139 1.151 0.587 Phase annealing cycle: 7 Beta = 0.14941 Ralpha 0.042 0.057 0.206 0.051 0.050 0.058 0.163 0.042 0.153 0.222 0.296 0.155 0.184 0.232 0.057 0.150 0.042 0.032 0.058 0.526 Nqual -0.816-0.001 0.100-0.619-0.595 0.001 0.019-0.816-0.325-0.338-0.805-0.601-0.683-0.120-0.001-0.178-0.816-0.885 0.001 0.041 Mabs 1.192 1.151 0.785 1.082 1.086 1.151 0.835 1.192 0.824 0.779 0.728 0.853 0.787 0.761 1.151 0.863 1.192 1.139 1.151 0.607 Phase annealing cycle: 8 Beta = 0.16602 Ralpha 0.042 0.058 0.205 0.051 0.051 0.057 0.166 0.042 0.140 0.224 0.280 0.156 0.191 0.230 0.058 0.153 0.042 0.032 0.057 0.465 Nqual -0.816 0.001 0.136-0.619-0.587-0.001-0.087-0.816-0.181-0.370-0.688-0.653-0.724-0.195 0.000-0.251-0.816-0.885-0.001 0.147 Mabs 1.192 1.151 0.792 1.082 1.082 1.150 0.836 1.192 0.836 0.776 0.733 0.852 0.780 0.759 1.151 0.868 1.192 1.139 1.150 0.628 Phase annealing cycle: 9 Beta = 0.18446 Ralpha 0.042 0.057 0.213 0.050 0.050 0.057 0.164 0.042 0.139 0.229 0.284 0.164 0.185 0.232 0.058 0.161 0.042 0.032 0.057 0.449 Nqual -0.816-0.001 0.148-0.595-0.595-0.001-0.136-0.816-0.120-0.330-0.763-0.651-0.693-0.267 0.000-0.304-0.816-0.885-0.001 0.040 Mabs 1.192 1.151 0.787 1.086 1.086 1.150 0.837 1.192 0.839 0.774 0.741 0.846 0.788 0.761 1.151 0.848 1.192 1.139 1.150 0.632 Phase annealing cycle: 10 Beta = 0.20496 Ralpha 0.042 0.058 0.203 0.051 0.051 0.057 0.169 0.042 0.139 0.220 0.291 0.161 0.192 0.243 0.058 0.162 0.042 0.032 0.057 0.433 Nqual -0.816 0.001 0.209-0.587-0.587-0.001-0.139-0.816-0.120-0.336-0.790-0.690-0.696-0.383 0.000-0.217-0.816-0.885-0.001 0.001 Mabs 1.192 1.151 0.794 1.082 1.082 1.151 0.826 1.192 0.839 0.779 0.727 0.847 0.789 0.756 1.151 0.849 1.192 1.139 1.150 0.638 Phase refinement cycle: 1 Ralpha 0.119 0.178 0.886 0.241 0.241 0.179 0.754 0.119 0.721 0.896 1.056 0.715 0.917 1.012 0.179 0.641 0.119 0.133 0.178 1.692 Nqual -0.764-0.018 0.126-0.646-0.646-0.010-0.130-0.764-0.221-0.447-0.493-0.481-0.532-0.125-0.010-0.258-0.764-0.909-0.018 0.030 Mabs 0.787 0.755 0.517 0.709 0.709 0.755 0.542 0.787 0.548 0.516 0.490 0.550 0.510 0.497 0.755 0.569 0.787 0.766 0.755 0.420 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1420309. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 810089. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 1953293. 0.281 -0.010 0.035 0.736 1.164 +---+ -+--+ ++++- --+++ + 1377857. 0.088 -0.825 0.557 0.969 0.103 -+-++ -+-++ ++--- +++-+ - 597829. 0.088 -0.825 0.557 0.969 0.103 -+-++ -+-++ ++--- +++-+ - 891993. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 265661. 0.296 -0.484 -0.001 0.719 0.514 -+--+ +++++ +-++- -+-+- - 1328305. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 350069. 0.235 -0.442 0.681 0.754 0.493 +--+- -++++ +---+ +-+-- - 1750345. 0.300 -0.644 -0.326 0.724 0.394 -+-+- +---- -++-+ ----+ + 363117. 0.420 -0.731 -0.501 0.658 0.468 +++-- ++-+- -++++ +-+-+ - 1815585. 0.254 -0.503 -0.293 0.740 0.454 --+++ ----+ -++-+ -+-++ + 689317. 0.342 -0.657 0.736 0.679 0.428 +++++ ++++- +---+ -+++- - 1349433. 0.351 -0.513 -0.326 0.681 0.542 -+-+- +---- -++-+ ----+ + 455709. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 181393. 0.193 -0.614 -0.609 0.804 0.306 --+-- +-+++ ---+- ++-+- - 906965. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 340521. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1702605. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 124417. 0.630 -0.064 0.456 0.572 1.414 --++- ++-++ +-+-- +-+++ + 622085. 0.332 -0.761 0.513 0.692 0.368 -+-+- +---- +++-+ +-+-+ + 1013273. 0.405 -0.748 -0.126 0.666 0.446 +++++ +-++- --+-+ --++- + 872061. 0.146 -0.547 -0.539 0.872 0.308 +---+ +-+-+ -+-+- -++-- - 166001. 0.312 -0.724 -0.241 0.706 0.363 +--+- --+++ -+-++ --+-- - 830005. 0.088 -0.825 0.557 0.969 0.103 -+-++ -+-++ ++--- +++-+ - 2052873. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 1875757. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 990177. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 756581. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1685753. 0.366 -0.511 0.359 0.673 0.559 +++-- ++--- ++++- -+--+ + 40157. 0.088 -0.825 0.557 0.969 0.103 -+-++ -+-++ ++--- +++-+ - 200785. 0.088 -0.801 0.557 0.973 0.110 -+-++ -+-++ ++--- +++-+ - 1035749. 0.280 -0.549 -0.327 0.725 0.441 --+++ ----+ -++-+ -++++ + 1135797. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 399017. 0.274 -0.429 -0.368 0.729 0.546 --+++ ----- ---++ ---++ - 984441. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 351505. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 1484681. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1904881. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1586817. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1065297. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 727901. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 252273. 0.088 -0.801 0.557 0.973 0.110 -+-++ -+-++ ++--- +++-+ - 851005. 0.088 -0.801 0.557 0.973 0.110 -+-++ -+-++ ++--- +++-+ - 1466601. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1995085. 0.088 -0.825 0.557 0.969 0.103 -+-++ -+-++ ++--- +++-+ - 384225. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1219837. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1229893. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 697705. 0.146 -0.547 -0.539 0.872 0.308 +---+ +-+-+ -+-+- -++-- - 1391373. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1874237. 0.088 -0.801 0.557 0.973 0.110 -+-++ -+-++ ++--- +++-+ - 2053325. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 410665. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 177441. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1878017. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 82133. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 866769. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 241721. 0.088 -0.801 0.557 0.973 0.110 -+-++ -+-++ ++--- +++-+ - 1316197. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1612985. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 971829. 0.088 -0.801 0.557 0.973 0.110 -+-++ -+-++ ++--- +++-+ - 1415041. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 905613. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 27421. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 1705801. 0.088 -0.801 0.557 0.973 0.110 -+-++ -+-++ ++--- +++-+ - 844345. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 360909. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 1681421. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1412773. 0.088 -0.825 0.557 0.969 0.103 -+-++ -+-++ ++--- +++-+ - 1038949. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 1308801. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1305297. 0.088 -0.825 0.557 0.969 0.103 -+-++ -+-++ ++--- +++-+ - 1379909. 0.088 -0.825 0.557 0.969 0.103 -+-++ -+-++ ++--- +++-+ - 1621645. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 22269. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 513653. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1923045. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 18497. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1073433. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1268097. 0.364 -0.459 0.582 0.677 0.604 +--+- -++++ +---+ --+-- - 1954897. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 1708153. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1978385. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 991073. 0.088 -0.825 0.557 0.969 0.103 -+-++ -+-++ ++--- +++-+ - 1931341. 0.088 -0.801 0.557 0.973 0.110 -+-++ -+-++ ++--- +++-+ - 1541353. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 1233725. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1832437. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 49349. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 865945. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 637929. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1252601. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 568021. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1349797. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 752045. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1338341. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 800217. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 500389. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1617617. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1052501. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1068201. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1620313. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1371917. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 390421. 0.088 -0.825 0.557 0.969 0.103 -+-++ -+-++ ++--- +++-+ - 1948605. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 480629. 0.088 -0.825 0.557 0.969 0.103 -+-++ -+-++ ++--- +++-+ - 731289. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1738413. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 852005. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1629133. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1229737. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1961865. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 417449. 0.088 -0.825 0.557 0.969 0.103 -+-++ -+-++ ++--- +++-+ - 1785369. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 219517. 0.095 -0.285 0.871 1.021 0.536 ++++- -++-+ +---- ++-+- - 349205. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 2038433. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1097585. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 742597. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1047881. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 221921. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 13773. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1124981. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1109605. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 422541. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 484045. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 746585. 0.030 -0.976 0.838 1.082 0.030* +--++ +-+-- +-+-- +++-- + 1611701. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 680165. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1303673. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1134545. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1308941. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 39769. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 198845. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 994225. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 776821. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 394261. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1503481. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1106961. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 793581. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 241177. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1902925. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 843181. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1765229. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 267325. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 178949. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 279421. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 391669. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 602973. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 917713. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1692945. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 338589. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 2057173. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1342605. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1094277. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1977397. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 52613. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1411785. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1960677. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 147469. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1411545. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1188253. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1788025. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1205013. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1698309. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 2088137. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 300401. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1312233. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 966085. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 104893. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1346373. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1864081. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 463277. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1077413. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1815125. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 2084081. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1338385. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1627069. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1459173. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 2002345. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 1276581. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 532521. 0.056 -0.874 0.590 1.082 0.062 --++- +--+- +++-- ++-++ + 1559345. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 419669. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 400469. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 238037. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 164845. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + 264133. 0.030 -0.976 0.838 1.082 0.030 +--++ +-+-- +-+-- +++-- + CFOM Range Frequency 0.000 - 0.020 0 0.020 - 0.040 75 0.040 - 0.060 0 0.060 - 0.080 57 0.080 - 0.100 1 0.100 - 0.120 58 0.120 - 0.140 0 0.140 - 0.160 0 0.160 - 0.180 0 0.180 - 0.200 0 0.200 - 0.220 0 0.220 - 0.240 0 0.240 - 0.260 0 0.260 - 0.280 0 0.280 - 0.300 0 0.300 - 0.320 3 0.320 - 0.340 1 0.340 - 0.360 0 0.360 - 0.380 2 0.380 - 0.400 1 0.400 - 0.420 2 0.420 - 0.440 3 0.440 - 0.460 5 0.460 - 0.480 1 0.480 - 0.500 3 0.500 - 0.520 1 0.520 - 0.540 31 0.540 - 0.560 4 0.560 - 0.580 1 0.580 - 0.600 0 0.600 - 9.999 7 256. Phase sets refined - best is code 746585. with CFOM = 0.0301 0.3 seconds elapsed time Tangent expanded to 525 out of 525 E greater than 1.200 Highest memory used = 2226 / 2956 0.0 seconds elapsed time FMAP and GRID set by program FMAP 8 3 11 GRID -3.125 -2 -2 3.125 2 2 E-Fourier for p21c in P2(1)/c Maximum = 293.87, minimum = -74.43 highest memory used = 8714 / 6602 0.0 seconds elapsed time Peak list optimization RE = 0.162 for 11 surviving atoms and 525 E-values Highest memory used = 1529 / 4725 0.0 seconds elapsed time E-Fourier for p21c in P2(1)/c Maximum = 306.63, minimum = -85.49 highest memory used = 8714 / 6602 0.0 seconds elapsed time Peak list optimization RE = 0.154 for 11 surviving atoms and 525 E-values Highest memory used = 1529 / 4725 0.0 seconds elapsed time E-Fourier for p21c in P2(1)/c Maximum = 313.12, minimum = -63.23 highest memory used = 8714 / 6602 0.0 seconds elapsed time Molecule 1 scale 1.000 inches = 2.540 cm per Angstrom 11 15 6 8 12 5 19 7 16 17 14 13 3 4 2 9 18 1 10 14 12 Atom Peak x y z SOF Height Distances and Angles 1 313. 0.9754 0.7606 0.1501 1.000 0.73 0 9 1.191 0 14 1.175 125.4 0 18 1.972 151.4 83.1 2 278. 1.0511 0.5451 0.2299 1.000 1.12 0 3 1.427 0 9 1.385 127.6 0 17 1.996 28.8 131.2 3 257. 1.1597 0.5612 0.1880 1.000 1.06 0 2 1.427 0 4 1.411 123.1 0 5 1.378 117.7 119.1 0 17 1.013 108.6 102.3 53.7 4 253. 1.1907 0.6754 0.0838 1.000 1.06 0 3 1.411 0 7 1.364 120.6 0 13 1.076 126.8 43.5 0 17 1.904 31.3 101.9 95.6 5 245. 1.2383 0.4630 0.2602 1.000 0.93 0 3 1.378 0 6 1.395 120.0 0 12 1.142 124.3 115.1 0 17 1.129 46.4 107.6 109.5 6 241. 1.3459 0.4744 0.2246 1.000 0.85 0 5 1.395 0 8 1.384 122.1 0 11 1.553 118.2 119.7 7 238. 1.2952 0.6842 0.0451 1.000 1.02 0 4 1.364 0 8 1.429 121.0 0 13 0.943 51.8 122.7 0 16 0.980 129.4 109.6 100.7 0 19 1.278 125.4 81.0 73.9 59.9 8 238. 1.3776 0.5826 0.1174 1.000 0.90 0 6 1.384 0 7 1.429 117.1 0 15 1.142 128.3 114.2 0 16 1.985 144.8 27.7 86.7 0 19 1.761 134.7 45.8 80.2 35.3 9 225. 0.9658 0.6428 0.2029 1.000 1.00 0 1 1.191 0 2 1.385 123.7 0 10 1.523 122.3 113.8 10 192. 0.8598 0.5899 0.2613 1.000 1.14 0 9 1.523 11 169. 1.4319 0.3615 0.3095 1.000 0.70 0 6 1.553 12 56. 1.2258 0.3787 0.3666 1.000 0.73 0 5 1.142 0 17 1.854 35.0 2 14 1.653 116.8 100.5 13 54. 1.2610 0.7437 0.1219 1.000 0.36 0 4 1.076 0 7 0.943 84.7 0 16 1.481 111.5 40.6 0 19 1.362 148.5 64.4 47.8 14 52. 0.9031 0.8425 0.1123 1.000 0.72 0 1 1.175 1 12 1.653 144.3 15 51. 1.4644 0.6101 0.0924 1.000 0.73 0 8 1.142 0 19 1.929 64.1 16 47. 1.3270 0.7543 -0.0292 1.000 1.06 0 7 0.980 0 8 1.985 42.7 0 13 1.481 38.7 72.7 0 19 1.156 73.0 61.7 60.7 17 47. 1.2138 0.5697 0.3090 1.000 0.19 0 2 1.996 0 3 1.013 42.7 0 4 1.904 79.5 46.4 0 5 1.129 96.5 79.9 101.8 0 12 1.854 89.3 97.8 134.6 35.5 18 45. 1.0649 0.9150 0.0713 1.000 0.27 0 1 1.972 19 44. 1.3704 0.7686 0.1232 1.000 0.00 0 7 1.278 0 8 1.761 53.2 0 13 1.362 41.7 83.2 0 15 1.929 82.2 35.7 118.3 0 16 1.156 47.1 83.0 71.5 89.0 Atom Code x y z Height Symmetry transformation 12 1 0.7742 0.8787 0.1334 0.70 2.0000-X 0.5000+Y 0.5000-Z 14 2 1.0969 0.3425 0.3877 1.06 2.0000-X -0.5000+Y 0.5000-Z 0.0 seconds elapsed time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxs finished at 11:36:41 Total elapsed time: 0.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++