+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0457 started at 12:40:07 on 28-Apr-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0457 in P2(1)/n CELL 0.71073 9.5853 19.1332 12.3889 90.000 103.732 90.000 ZERR 4.00 0.0001 0.0003 0.0002 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O S PD UNIT 88 72 8 16 8 8 V = 2207.15 F(000) = 1280.0 Mu = 1.85 mm-1 Cell Wt = 2605.22 Rho = 1.960 MERG 2 OMIT -3.00 55.00 OMIT 2 4 1 OMIT 2 3 0 OMIT 1 2 0 SHEL 7 0.77 DELU C2 > S8 C72 > S78 DELU C22 > S28 C92 > S98 SIMU C2 > S8 C72 > S78 SIMU C22 > S28 C92 > S98 EADP C74 C81 N71 C97 N91 C76 FMAP 2 PLAN 10 SIZE 0.21 0.38 0.40 ACTA BOND $H WGHT 0.00000 4.03760 L.S. 8 TEMP -153.00 FVAR 0.37055 0.75426 0.81146 MOLE 1 PART 1 C2 1 0.719740 0.245648 0.921413 21.00000 0.02565 0.01661 = 0.02358 -0.00528 0.00126 0.00020 AFIX 43 H2 2 0.808684 0.267844 0.922381 21.00000 -1.20000 AFIX 0 C3 1 0.657898 0.254630 1.011577 21.00000 0.03761 0.02881 = 0.02101 -0.00634 0.00314 0.00431 AFIX 43 H3 2 0.702977 0.283356 1.072429 21.00000 -1.20000 AFIX 0 C4 1 0.529468 0.220976 1.011127 21.00000 0.03332 0.03318 = 0.01176 -0.00206 0.01094 0.00874 AFIX 43 H4 2 0.485914 0.225894 1.072053 21.00000 -1.20000 AFIX 0 C5 1 0.465822 0.180154 0.920607 21.00000 0.02490 0.02801 = 0.02259 0.00172 0.00918 0.00330 AFIX 43 H5 2 0.377207 0.157324 0.918516 21.00000 -1.20000 AFIX 0 C6 1 0.531930 0.172599 0.832560 21.00000 0.01580 0.02143 = 0.01635 0.00144 0.00203 0.00236 C7 1 0.483552 0.132841 0.732869 21.00000 0.01760 0.02251 = 0.01816 -0.00022 0.00552 -0.00101 C9 1 0.375985 0.060464 0.571003 21.00000 0.02688 0.03943 = 0.02777 -0.00996 0.00009 -0.00537 AFIX 43 H9 2 0.318940 0.031426 0.515462 21.00000 -1.20000 AFIX 0 C10 1 0.503837 0.089669 0.562344 21.00000 0.02986 0.03490 = 0.02161 -0.00449 0.00662 0.00071 AFIX 43 H10 2 0.545586 0.082385 0.500955 21.00000 -1.20000 AFIX 0 C11 1 0.566826 0.132112 0.655758 21.00000 0.01660 0.02598 = 0.01306 0.00065 0.00435 -0.00021 N1 3 0.657323 0.206619 0.833471 21.00000 0.01850 0.01810 = 0.01455 -0.00078 0.00136 0.00360 S8 5 0.329915 0.081963 0.692958 21.00000 0.02275 0.03356 = 0.03338 -0.00415 0.00655 -0.00761 MOLE 2 C22 1 0.751861 -0.029827 0.756729 31.00000 0.03776 0.02504 = 0.01707 -0.00113 0.00332 -0.00329 AFIX 43 H22 2 0.781499 -0.030888 0.688816 31.00000 -1.20000 AFIX 0 C23 1 0.643596 -0.074362 0.770285 31.00000 0.04663 0.03049 = 0.02827 -0.00327 0.00047 -0.01528 AFIX 43 H23 2 0.600296 -0.105918 0.712876 31.00000 -1.20000 AFIX 0 C24 1 0.599682 -0.072264 0.867948 31.00000 0.02997 0.03891 = 0.03783 0.00807 0.00518 -0.02075 AFIX 43 H24 2 0.523665 -0.101533 0.877917 31.00000 -1.20000 AFIX 0 C25 1 0.666646 -0.027337 0.951748 31.00000 0.02910 0.03599 = 0.02583 0.00531 0.00807 -0.00688 AFIX 43 H25 2 0.638235 -0.026229 1.020159 31.00000 -1.20000 AFIX 0 C26 1 0.776407 0.016431 0.935116 31.00000 0.01924 0.01974 = 0.01339 0.00309 -0.00207 0.00091 C27 1 0.858238 0.066872 1.009583 31.00000 0.02388 0.01708 = 0.01913 0.00028 0.00540 0.00237 C29 1 0.982146 0.149221 1.151933 31.00000 0.03460 0.02653 = 0.02735 -0.00829 0.00209 -0.00612 AFIX 43 H29 2 1.018072 0.177126 1.215922 31.00000 -1.20000 AFIX 0 C30 1 1.028571 0.154626 1.057132 31.00000 0.03118 0.02067 = 0.02895 -0.00210 0.00301 -0.00431 AFIX 43 H30 2 1.100150 0.186782 1.047485 31.00000 -1.20000 AFIX 0 C31 1 0.958500 0.106917 0.973573 31.00000 0.02139 0.01647 = 0.01901 0.00250 0.00254 0.00245 N21 3 0.816076 0.014692 0.836392 31.00000 0.02605 0.01690 = 0.01515 0.00317 0.00329 0.00092 S28 5 0.851177 0.086480 1.144392 31.00000 0.03532 0.03522 = 0.01870 -0.00346 0.00963 0.00107 MOLE 3 PART 2 SAME C22 > S28 C72 1 0.974162 0.127591 1.044176 -31.00000 0.05643 0.00996 = 0.01932 0.00529 0.01291 0.00910 AFIX 43 H72 2 1.046539 0.159079 1.033886 -31.00000 -1.20000 AFIX 0 C73 1 0.929626 0.126513 1.145770 -31.00000 0.04676 0.03207 = 0.01004 0.00404 0.01450 0.00715 AFIX 43 H73 2 0.969987 0.158082 1.204004 -31.00000 -1.20000 AFIX 0 C74 1 0.825440 0.078178 1.158356 -31.00000 0.02287 0.01988 = 0.01585 0.00119 0.00394 0.01370 AFIX 43 H74 2 0.797453 0.076316 1.226900 -31.00000 -1.20000 AFIX 0 C75 1 0.762300 0.033267 1.074468 -31.00000 0.03671 0.03843 = 0.02690 0.00066 0.01277 0.01654 AFIX 43 H75 2 0.688676 0.001762 1.082177 -31.00000 -1.20000 AFIX 0 C76 1 0.811992 0.036273 0.976914 -31.00000 0.02287 0.01988 = 0.01585 0.00119 0.00394 0.01370 C77 1 0.761657 -0.005458 0.880386 -31.00000 0.01933 0.03572 = 0.01663 0.01045 -0.00175 0.00454 C79 1 0.670024 -0.091276 0.729462 -31.00000 0.03948 0.03140 = 0.04772 0.00348 0.01142 -0.00818 AFIX 43 H79 2 0.623648 -0.127051 0.680788 -31.00000 -1.20000 AFIX 0 C80 1 0.769183 -0.045170 0.706091 -31.00000 0.03450 0.01749 = 0.02383 0.00583 0.00769 -0.00022 AFIX 43 H80 2 0.798271 -0.045982 0.637945 -31.00000 -1.20000 AFIX 0 C81 1 0.824036 0.003233 0.791047 -31.00000 0.02287 0.01988 = 0.01585 0.00119 0.00394 0.01370 N71 3 0.912158 0.083431 0.963518 -31.00000 0.02287 0.01988 = 0.01585 0.00119 0.00394 0.01370 S78 5 0.642177 -0.075091 0.858211 -31.00000 0.03039 0.03752 = 0.06168 0.01453 0.02044 -0.00803 MOLE 4 SAME C2 > S8 C92 1 0.512581 0.096468 0.606797 -21.00000 0.01935 0.04876 = 0.02596 -0.01063 0.00256 0.00068 AFIX 43 H92 2 0.557441 0.093704 0.546297 -21.00000 -1.20000 AFIX 0 C93 1 0.388862 0.058168 0.606277 -21.00000 0.03379 0.02818 = 0.04020 -0.01088 -0.01136 -0.00411 AFIX 43 H93 2 0.349728 0.027625 0.546270 -21.00000 -1.20000 AFIX 0 C94 1 0.324488 0.064936 0.692695 -21.00000 0.03336 0.02719 = 0.05846 -0.00282 0.00799 -0.01973 AFIX 43 H94 2 0.245466 0.035690 0.695862 -21.00000 -1.20000 AFIX 0 C95 1 0.371758 0.113294 0.775380 -21.00000 0.01567 0.02194 = 0.05236 0.00310 0.01050 0.00914 AFIX 43 H95 2 0.318532 0.122528 0.829451 -21.00000 -1.20000 AFIX 0 C96 1 0.498082 0.147921 0.777720 -21.00000 0.00618 0.02691 = 0.01576 0.00352 0.00053 0.00670 C97 1 0.576573 0.193283 0.859093 -21.00000 0.02287 0.01988 = 0.01585 0.00119 0.00394 0.01370 C99 1 0.685110 0.270746 1.016144 -21.00000 0.05719 0.03910 = 0.01945 -0.01093 0.00325 0.02087 AFIX 43 H99 2 0.713347 0.296623 1.083237 -21.00000 -1.20000 AFIX 0 C100 1 0.760802 0.268474 0.936217 -21.00000 0.03254 0.02045 = 0.02006 -0.00606 -0.00970 0.01221 AFIX 43 H100 2 0.845432 0.295045 0.939497 -21.00000 -1.20000 AFIX 0 C101 1 0.701541 0.223006 0.848437 -21.00000 0.01236 0.02757 = 0.01002 -0.00993 -0.00572 0.01138 N91 3 0.566620 0.137100 0.694146 -21.00000 0.02287 0.01988 = 0.01585 0.00119 0.00394 0.01370 S98 5 0.533900 0.221527 0.980871 -21.00000 0.05910 0.04227 = 0.02069 0.00646 0.02633 0.02342 MOLE 5 PART 0 C41 1 0.899826 0.104140 0.566457 11.00000 0.02410 0.02045 = 0.02057 -0.00001 0.00995 -0.00224 C42 1 0.933430 0.089160 0.455567 11.00000 0.04340 0.02913 = 0.02218 0.00166 0.01597 0.00664 AFIX 137 H42A 2 1.020672 0.060666 0.466960 11.00000 -1.50000 H42B 2 0.948359 0.133301 0.419785 11.00000 -1.50000 H42C 2 0.853052 0.063798 0.408039 11.00000 -1.50000 AFIX 0 C51 1 1.058738 0.230425 0.794727 11.00000 0.02420 0.02072 = 0.01804 0.00034 0.00753 -0.00258 C52 1 1.173429 0.285303 0.811069 11.00000 0.02711 0.02255 = 0.02956 0.00386 0.00451 -0.00536 AFIX 137 H52A 2 1.133783 0.328163 0.772355 11.00000 -1.50000 H52B 2 1.253144 0.268604 0.780960 11.00000 -1.50000 H52C 2 1.208351 0.295026 0.890579 11.00000 -1.50000 AFIX 0 O41 4 0.957286 0.066350 0.647704 11.00000 0.04506 0.02245 = 0.01947 0.00238 0.01114 0.00900 O42 4 0.815556 0.154715 0.568229 11.00000 0.02955 0.03335 = 0.01848 0.00315 0.01074 0.01086 O51 4 1.100434 0.168676 0.820171 11.00000 0.02363 0.01939 = 0.04030 0.00406 0.00322 -0.00077 O52 4 0.931646 0.249825 0.758669 11.00000 0.02404 0.02027 = 0.03590 0.00266 0.00319 -0.00055 PD1 6 0.959070 0.087565 0.816434 11.00000 0.02251 0.01739 = 0.02038 0.00541 0.00613 0.00220 PD2 6 0.748369 0.186027 0.706539 11.00000 0.02002 0.02017 = 0.01948 0.00291 0.00848 0.00458 HKLF 4 Covalent radii and connectivity table for 2009src0457 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 PD 1.380 C2_a - N1_a C3_a C3_a - C4_a C2_a C4_a - C5_a C3_a C5_a - C4_a C6_a C6_a - N1_a C5_a C7_a C7_a - C11_a C6_a S8_a C9_a - C10_a S8_a C10_a - C9_a C11_a C11_a - C7_a C10_a Pd2 N1_a - C2_a C6_a Pd2 S8_a - C9_a C7_a C22_a - N21_a C23_a C23_a - C24_a C22_a C24_a - C23_a C25_a C25_a - C24_a C26_a C26_a - N21_a C25_a C27_a C27_a - C31_a C26_a S28_a C29_a - C30_a S28_a C30_a - C29_a C31_a C31_a - C27_a C30_a Pd1 N21_a - C22_a C26_a Pd1 S28_a - C29_a C27_a C72_b - N71_b C73_b C73_b - C74_b C72_b C74_b - C75_b C73_b C75_b - C74_b C76_b C76_b - N71_b C75_b C77_b C77_b - C81_b C76_b S78_b C79_b - C80_b S78_b C80_b - C79_b C81_b C81_b - C77_b C80_b Pd1 N71_b - C72_b C76_b Pd1 S78_b - C79_b C77_b C92_b - N91_b C93_b C93_b - C94_b C92_b C94_b - C93_b C95_b C95_b - C96_b C94_b C96_b - N91_b C95_b C97_b C97_b - C101_b C96_b S98_b C99_b - C100_b S98_b C100_b - C99_b C101_b C101_b - C97_b C100_b Pd2 N91_b - C92_b C96_b Pd2 S98_b - C99_b C97_b C41 - O41 O42 C42 C42 - C41 C51 - O52 O51 C52 C52 - C51 O41 - C41 Pd1 O42 - C41 Pd2 O51 - C51 Pd1 O52 - C51 Pd2 Pd1 - N71_b C31_a N21_a C81_b O51 O41 Pd2 Pd2 - N91_b C11_a N1_a C101_b O42 O52 Pd1 h k l Fo^2 Sigma Why rejected 3 0 0 8.11 1.87 observed but should be systematically absent 3 0 0 9.01 2.05 observed but should be systematically absent 3 0 0 7.35 1.61 observed but should be systematically absent 7 0 0 26.71 4.86 observed but should be systematically absent 7 0 0 17.20 3.94 observed but should be systematically absent 7 0 0 15.82 3.19 observed but should be systematically absent 7 0 0 21.47 4.69 observed but should be systematically absent 7 0 0 18.28 3.59 observed but should be systematically absent 0 3 0 6.65 1.11 observed but should be systematically absent 0 3 0 8.68 1.53 observed but should be systematically absent 0 3 0 5.76 1.38 observed but should be systematically absent 0 13 0 24.74 4.36 observed but should be systematically absent 0 13 0 23.70 3.48 observed but should be systematically absent 0 13 0 23.44 4.50 observed but should be systematically absent 0 13 0 17.17 3.98 observed but should be systematically absent -8 0 1 13.17 3.08 observed but should be systematically absent 3 0 2 6.43 1.60 observed but should be systematically absent 7 0 2 20.35 4.60 observed but should be systematically absent 7 0 2 16.76 3.29 observed but should be systematically absent 2 0 3 23.58 3.90 observed but should be systematically absent 2 0 3 18.13 2.89 observed but should be systematically absent 2 0 3 25.14 3.54 observed but should be systematically absent 2 0 3 13.38 3.13 observed but should be systematically absent -3 0 4 5.36 1.17 observed but should be systematically absent -3 0 4 7.10 1.72 observed but should be systematically absent -6 0 7 10.62 2.32 observed but should be systematically absent -6 0 7 12.23 2.38 observed but should be systematically absent 27186 Reflections read, of which 542 rejected -12 =< h =< 12, -24 =< k =< 24, -16 =< l =< 16, Max. 2-theta = 54.97 27 Systematic absence violations 0 Inconsistent equivalents 5057 Unique reflections, of which 0 suppressed R(int) = 0.0375 R(sigma) = 0.0312 Friedel opposites merged Maximum memory for data reduction = 5183 / 50516 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 6463 / 603594 wR2 = 0.0611 before cycle 1 for 5057 data and 461 / 461 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 56. 0. 0. 0. 108. 246. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.025 0.000 0.000 0.000 0.005 0.009 0.000 0.000 GooF = S = 1.169; Restrained GooF = 1.129 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37055 0.00031 0.014 OSF 2 0.75449 0.00374 0.061 FVAR 2 3 0.81114 0.00338 -0.095 FVAR 3 Mean shift/su = 0.060 Maximum = 0.471 for x C4_a Max. shift = 0.012 A for C99_b Max. dU = 0.000 for C3_a Least-squares cycle 2 Maximum vector length = 511 Memory required = 6463 / 603594 wR2 = 0.0611 before cycle 2 for 5057 data and 461 / 461 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 56. 0. 0. 0. 108. 246. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.022 0.000 0.000 0.000 0.005 0.009 0.000 0.000 GooF = S = 1.170; Restrained GooF = 1.129 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37055 0.00031 -0.011 OSF 2 0.75466 0.00374 0.045 FVAR 2 3 0.81108 0.00338 -0.016 FVAR 3 Mean shift/su = 0.025 Maximum = -0.224 for U13 S98_b Max. shift = 0.003 A for C99_b Max. dU = 0.000 for C99_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 6463 / 603594 wR2 = 0.0611 before cycle 3 for 5057 data and 461 / 461 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 56. 0. 0. 0. 108. 246. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.022 0.000 0.000 0.000 0.005 0.009 0.000 0.000 GooF = S = 1.169; Restrained GooF = 1.128 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37055 0.00031 -0.001 OSF 2 0.75470 0.00374 0.013 FVAR 2 3 0.81110 0.00338 0.004 FVAR 3 Mean shift/su = 0.007 Maximum = -0.068 for U13 S98_b Max. shift = 0.001 A for C99_b Max. dU = 0.000 for C94_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 6463 / 603594 wR2 = 0.0611 before cycle 4 for 5057 data and 461 / 461 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 56. 0. 0. 0. 108. 246. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.022 0.000 0.000 0.000 0.005 0.009 0.000 0.000 GooF = S = 1.170; Restrained GooF = 1.129 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37055 0.00031 0.000 OSF 2 0.75472 0.00374 0.006 FVAR 2 3 0.81112 0.00338 0.008 FVAR 3 Mean shift/su = 0.003 Maximum = -0.026 for y S78_b Max. shift = 0.001 A for C99_b Max. dU = 0.000 for C99_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 6463 / 603594 wR2 = 0.0611 before cycle 5 for 5057 data and 461 / 461 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 56. 0. 0. 0. 108. 246. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.022 0.000 0.000 0.000 0.005 0.009 0.000 0.000 GooF = S = 1.169; Restrained GooF = 1.128 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37055 0.00031 -0.001 OSF 2 0.75473 0.00374 0.002 FVAR 2 3 0.81113 0.00338 0.002 FVAR 3 Mean shift/su = 0.001 Maximum = 0.012 for tors H42A Max. shift = 0.000 A for C99_b Max. dU = 0.000 for S78_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 6463 / 603594 wR2 = 0.0611 before cycle 6 for 5057 data and 461 / 461 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 56. 0. 0. 0. 108. 246. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.022 0.000 0.000 0.000 0.005 0.009 0.000 0.000 GooF = S = 1.169; Restrained GooF = 1.128 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37055 0.00031 -0.003 OSF 2 0.75474 0.00374 0.001 FVAR 2 3 0.81114 0.00338 0.002 FVAR 3 Mean shift/su = 0.001 Maximum = 0.012 for tors H42A Max. shift = 0.000 A for H42A Max. dU = 0.000 for C101_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 6463 / 603594 wR2 = 0.0611 before cycle 7 for 5057 data and 461 / 461 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 56. 0. 0. 0. 108. 246. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.022 0.000 0.000 0.000 0.005 0.009 0.000 0.000 GooF = S = 1.169; Restrained GooF = 1.128 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37055 0.00031 0.001 OSF 2 0.75474 0.00374 0.001 FVAR 2 3 0.81114 0.00338 0.001 FVAR 3 Mean shift/su = 0.000 Maximum = 0.011 for tors H42A Max. shift = 0.000 A for H42A Max. dU = 0.000 for C101_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 6463 / 603594 wR2 = 0.0611 before cycle 8 for 5057 data and 461 / 461 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 56. 0. 0. 0. 108. 246. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.022 0.000 0.000 0.000 0.005 0.009 0.000 0.000 GooF = S = 1.169; Restrained GooF = 1.128 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37055 0.00031 0.000 OSF 2 0.75474 0.00374 0.000 FVAR 2 3 0.81114 0.00338 0.000 FVAR 3 Mean shift/su = 0.000 Maximum = 0.010 for tors H42A Max. shift = 0.000 A for H42A Max. dU = 0.000 for C101_b Largest correlation matrix elements -0.917 y S98_b / y C4_a -0.873 x C94_b / x S8_a -0.834 y C93_b / U23 C9_a 0.907 U22 C99_b / y C3_a -0.864 y C99_b / y C3_a -0.831 x C99_b / x C3_a -0.898 x S98_b / x C4_a -0.861 U23 S98_b / y C4_a -0.818 z C94_b / z S8_a -0.896 y C99_b / U22 C3_a 0.852 y C94_b / U22 S8_a -0.815 y S78_b / U12 C24_a 0.893 y S98_b / U23 C4_a -0.850 y S78_b / y C24_a -0.814 U13 S98_b / x C4_a -0.880 z C99_b / z C3_a 0.840 x S98_b / U13 C4_a -0.811 U22 C99_b / y C99_b -0.879 U22 C94_b / y S8_a -0.836 U23 C4_a / y C4_a 0.809 z S98_b / U33 C4_a -0.873 y C93_b / y C9_a 0.835 U23 C93_b / y C9_a 0.804 U33 S98_b / U33 C4_a Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.8086 0.2679 0.9226 43 0.950 0.000 C2_a N1_a C3_a H3 0.7030 0.2833 1.0720 43 0.950 0.000 C3_a C4_a C2_a H4 0.4873 0.2262 1.0725 43 0.950 0.000 C4_a C5_a C3_a H5 0.3773 0.1575 0.9186 43 0.950 0.000 C5_a C4_a C6_a H9 0.3188 0.0316 0.5155 43 0.950 0.000 C9_a C10_a S8_a H10 0.5457 0.0823 0.5010 43 0.950 0.000 C10_a C9_a C11_a H22 0.7816 -0.0308 0.6888 43 0.950 0.000 C22_a N21_a C23_a H23 0.6002 -0.1060 0.7128 43 0.950 0.000 C23_a C24_a C22_a H24 0.5238 -0.1015 0.8786 43 0.950 0.000 C24_a C23_a C25_a H25 0.6382 -0.0262 1.0202 43 0.950 0.000 C25_a C24_a C26_a H29 1.0181 0.1772 1.2160 43 0.950 0.000 C29_a C30_a S28_a H30 1.1002 0.1868 1.0475 43 0.950 0.000 C30_a C29_a C31_a H72 1.0462 0.1591 1.0340 43 0.950 0.000 C72_b N71_b C73_b H73 0.9701 0.1581 1.2039 43 0.950 0.000 C73_b C74_b C72_b H74 0.7981 0.0766 1.2265 43 0.950 0.000 C74_b C75_b C73_b H75 0.6888 0.0019 1.0829 43 0.950 0.000 C75_b C74_b C76_b H79 0.6248 -0.1269 0.6802 43 0.950 0.000 C79_b C80_b S78_b H80 0.7979 -0.0461 0.6379 43 0.950 0.000 C80_b C79_b C81_b H92 0.5573 0.0939 0.5462 43 0.950 0.000 C92_b N91_b C93_b H93 0.3502 0.0271 0.5465 43 0.950 0.000 C93_b C94_b C92_b H94 0.2445 0.0357 0.6960 43 0.950 0.000 C94_b C93_b C95_b H95 0.3189 0.1228 0.8297 43 0.950 0.000 C95_b C96_b C94_b H99 0.7121 0.2962 1.0844 43 0.950 0.000 C99_b C100_b S98_b H100 0.8454 0.2952 0.9393 43 0.950 0.000 C100_b C99_b C101_b H42A 1.0206 0.0606 0.4670 137 0.980 0.000 C42 C41 H42A H42B 0.9486 0.1333 0.4199 137 0.980 0.000 C42 C41 H42A H42C 0.8530 0.0639 0.4080 137 0.980 0.000 C42 C41 H42A H52A 1.1338 0.3282 0.7724 137 0.980 0.000 C52 C51 H52A H52B 1.2531 0.2686 0.7810 137 0.980 0.000 C52 C51 H52A H52C 1.2083 0.2950 0.8906 137 0.980 0.000 C52 C51 H52A 2009src0457 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2_a 0.71968 0.24565 0.92151 0.75474 0.02562 0.01674 0.02376 -0.00510 0.00141 0.00025 0.02279 0.01014 0.00057 0.00027 0.00049 0.00374 0.00257 0.00273 0.00268 0.00195 0.00212 0.00170 0.00101 H2_a 0.80864 0.26787 0.92258 0.75474 0.02734 0.00374 0.00000 C3_a 0.65788 0.25452 1.01120 0.75474 0.03883 0.02886 0.02099 -0.00698 0.00265 0.00470 0.03030 0.01300 0.00115 0.00067 0.00088 0.00374 0.00353 0.00488 0.00288 0.00222 0.00258 0.00236 0.00152 H3_a 0.70301 0.28330 1.07197 0.75474 0.03636 0.00374 0.00000 C4_a 0.53044 0.22118 1.01129 0.75474 0.03444 0.03307 0.01069 -0.00289 0.00911 0.00915 0.02544 0.02018 0.00127 0.00069 0.00067 0.00374 0.00296 0.00289 0.00400 0.00351 0.00309 0.00216 0.00167 H4_a 0.48735 0.22616 1.07246 0.75474 0.03053 0.00374 0.00000 C5_a 0.46594 0.18018 0.92055 0.75474 0.02493 0.02820 0.02238 0.00173 0.00911 0.00337 0.02459 0.00821 0.00042 0.00021 0.00033 0.00374 0.00189 0.00203 0.00202 0.00169 0.00161 0.00161 0.00086 H5_a 0.37727 0.15746 0.91865 0.75474 0.02950 0.00374 0.00000 C6_a 0.53175 0.17255 0.83253 0.75474 0.01582 0.02153 0.01660 0.00158 0.00218 0.00231 0.01827 0.00891 0.00043 0.00023 0.00037 0.00374 0.00207 0.00237 0.00221 0.00164 0.00176 0.00150 0.00082 C7_a 0.48370 0.13288 0.73289 0.75474 0.01776 0.02253 0.01802 -0.00016 0.00565 -0.00089 0.01920 0.00860 0.00051 0.00027 0.00039 0.00374 0.00201 0.00226 0.00245 0.00184 0.00206 0.00154 0.00089 C9_a 0.37599 0.06056 0.57108 0.75474 0.02683 0.03916 0.02784 -0.00957 0.00009 -0.00516 0.03235 0.01353 0.00093 0.00058 0.00057 0.00374 0.00288 0.00327 0.00365 0.00334 0.00298 0.00251 0.00181 H9_a 0.31885 0.03158 0.51551 0.75474 0.03882 0.00374 0.00000 C10_a 0.50386 0.08967 0.56235 0.75474 0.02988 0.03492 0.02149 -0.00461 0.00663 0.00069 0.02867 0.01082 0.00069 0.00034 0.00043 0.00374 0.00252 0.00266 0.00287 0.00237 0.00261 0.00194 0.00117 H10_a 0.54565 0.08234 0.50100 0.75474 0.03440 0.00374 0.00000 C11_a 0.56669 0.13209 0.65578 0.75474 0.01663 0.02596 0.01303 0.00055 0.00410 -0.00033 0.01844 0.00909 0.00050 0.00026 0.00037 0.00374 0.00181 0.00211 0.00213 0.00196 0.00191 0.00156 0.00093 N1_a 0.65734 0.20664 0.83350 0.75474 0.01844 0.01830 0.01481 -0.00062 0.00152 0.00366 0.01759 0.00831 0.00051 0.00028 0.00041 0.00374 0.00258 0.00228 0.00204 0.00149 0.00201 0.00165 0.00091 S8_a 0.32995 0.08197 0.69295 0.75474 0.02272 0.03348 0.03344 -0.00412 0.00657 -0.00772 0.02990 0.00353 0.00026 0.00015 0.00019 0.00374 0.00077 0.00132 0.00084 0.00069 0.00057 0.00063 0.00049 C22_a 0.75194 -0.02981 0.75669 0.81114 0.03777 0.02496 0.01696 -0.00128 0.00314 -0.00340 0.02712 0.00786 0.00045 0.00021 0.00036 0.00338 0.00222 0.00202 0.00196 0.00158 0.00173 0.00173 0.00084 H22_a 0.78158 -0.03082 0.68878 0.81114 0.03255 0.00338 0.00000 C23_a 0.64355 -0.07447 0.77021 0.81114 0.04599 0.03074 0.02796 -0.00295 0.00098 -0.01534 0.03620 0.00855 0.00055 0.00025 0.00042 0.00338 0.00295 0.00245 0.00261 0.00189 0.00210 0.00215 0.00113 H23_a 0.60022 -0.10605 0.71284 0.81114 0.04344 0.00338 0.00000 C24_a 0.59970 -0.07225 0.86846 0.81114 0.03067 0.03929 0.03715 0.00789 0.00683 -0.02068 0.03591 0.01648 0.00083 0.00052 0.00077 0.00338 0.00443 0.00315 0.00323 0.00226 0.00292 0.00344 0.00189 H24_a 0.52378 -0.10151 0.87863 0.81114 0.04309 0.00338 0.00000 C25_a 0.66654 -0.02737 0.95180 0.81114 0.02896 0.03596 0.02588 0.00536 0.00806 -0.00690 0.03001 0.00724 0.00040 0.00020 0.00032 0.00338 0.00192 0.00209 0.00191 0.00158 0.00157 0.00160 0.00086 H25_a 0.63821 -0.02617 1.02024 0.81114 0.03601 0.00338 0.00000 C26_a 0.77643 0.01641 0.93497 0.81114 0.01903 0.01969 0.01345 0.00312 -0.00223 0.00080 0.01841 0.00730 0.00037 0.00019 0.00031 0.00338 0.00174 0.00189 0.00183 0.00145 0.00156 0.00136 0.00072 C27_a 0.85818 0.06685 1.00966 0.81114 0.02383 0.01715 0.01898 0.00036 0.00550 0.00240 0.01991 0.00727 0.00039 0.00019 0.00029 0.00338 0.00177 0.00163 0.00168 0.00139 0.00148 0.00140 0.00071 C29_a 0.98219 0.14925 1.15201 0.81114 0.03457 0.02646 0.02740 -0.00845 0.00196 -0.00613 0.03038 0.00849 0.00053 0.00026 0.00041 0.00338 0.00275 0.00252 0.00209 0.00181 0.00190 0.00180 0.00096 H29_a 1.01813 0.17716 1.21599 0.81114 0.03646 0.00338 0.00000 C30_a 1.02858 0.15462 1.05711 0.81114 0.03109 0.02070 0.02890 -0.00198 0.00308 -0.00426 0.02758 0.00817 0.00047 0.00022 0.00035 0.00338 0.00221 0.00220 0.00210 0.00163 0.00169 0.00165 0.00087 H30_a 1.10016 0.18677 1.04746 0.81114 0.03309 0.00338 0.00000 C31_a 0.95856 0.10693 0.97351 0.81114 0.02129 0.01652 0.01907 0.00263 0.00265 0.00241 0.01932 0.00796 0.00041 0.00020 0.00033 0.00338 0.00190 0.00179 0.00185 0.00154 0.00151 0.00136 0.00075 N21_a 0.81611 0.01471 0.83640 0.81114 0.02610 0.01673 0.01517 0.00309 0.00314 0.00084 0.01963 0.00580 0.00033 0.00015 0.00027 0.00338 0.00157 0.00142 0.00153 0.00120 0.00132 0.00120 0.00064 S28_a 0.85118 0.08648 1.14440 0.81114 0.03540 0.03526 0.01875 -0.00353 0.00958 0.00108 0.02927 0.00257 0.00016 0.00008 0.00011 0.00338 0.00079 0.00069 0.00056 0.00046 0.00043 0.00051 0.00035 C72_b 0.97387 0.12755 1.04436 0.18886 0.05642 0.01008 0.01992 0.00567 0.01298 0.00898 0.02815 0.03425 0.00209 0.00080 0.00127 0.00338 0.01168 0.00777 0.00781 0.00545 0.00697 0.00588 0.00338 H72_b 1.04617 0.15907 1.03401 0.18886 0.03378 0.00338 0.00000 C73_b 0.92969 0.12652 1.14560 0.18886 0.04686 0.03153 0.00975 0.00329 0.01354 0.00706 0.02824 0.03754 0.00230 0.00103 0.00132 0.00338 0.01249 0.01104 0.00637 0.00634 0.00788 0.00648 0.00368 H73_b 0.97009 0.15805 1.20387 0.18886 0.03388 0.00338 0.00000 C74_b 0.82593 0.07836 1.15793 0.18886 0.02282 0.01983 0.01556 0.00112 0.00357 0.01390 0.01957 0.04004 0.00262 0.00127 0.00179 0.00338 0.00328 0.00313 0.00314 0.00242 0.00259 0.00214 0.00138 H74_b 0.79811 0.07661 1.22655 0.18886 0.02348 0.00338 0.00000 C75_b 0.76235 0.03335 1.07477 0.18886 0.03656 0.03838 0.02711 0.00053 0.01259 0.01615 0.03317 0.03035 0.00172 0.00085 0.00116 0.00338 0.00833 0.00833 0.00677 0.00571 0.00604 0.00588 0.00329 H75_b 0.68877 0.00194 1.08289 0.18886 0.03980 0.00338 0.00000 C76_b 0.81187 0.03617 0.97670 0.18886 0.02282 0.01983 0.01556 0.00112 0.00357 0.01390 0.01957 0.02841 0.00166 0.00082 0.00110 0.00338 0.00328 0.00313 0.00314 0.00242 0.00259 0.00214 0.00138 C77_b 0.76119 -0.00575 0.88014 0.18886 0.01982 0.03582 0.01651 0.01004 -0.00223 0.00400 0.02515 0.02490 0.00157 0.00077 0.00118 0.00338 0.00717 0.00832 0.00649 0.00555 0.00605 0.00560 0.00295 C79_b 0.67074 -0.09105 0.72903 0.18886 0.03916 0.03355 0.04607 0.00319 0.01296 -0.00793 0.03912 0.03364 0.00221 0.00102 0.00158 0.00338 0.01043 0.01019 0.01078 0.00756 0.00914 0.00747 0.00437 H79_b 0.62479 -0.12686 0.68023 0.18886 0.04694 0.00338 0.00000 C80_b 0.76885 -0.04531 0.70609 0.18886 0.03487 0.01734 0.02342 0.00575 0.00794 -0.00024 0.02504 0.02942 0.00175 0.00077 0.00133 0.00338 0.00843 0.00717 0.00751 0.00552 0.00670 0.00596 0.00318 H80_b 0.79792 -0.04608 0.63794 0.18886 0.03004 0.00338 0.00000 C81_b 0.82377 0.00309 0.79089 0.18886 0.02282 0.01983 0.01556 0.00112 0.00357 0.01390 0.01957 0.03030 0.00173 0.00080 0.00124 0.00338 0.00328 0.00313 0.00314 0.00242 0.00259 0.00214 0.00138 N71_b 0.91200 0.08341 0.96377 0.18886 0.02282 0.01983 0.01556 0.00112 0.00357 0.01390 0.01957 0.02548 0.00154 0.00071 0.00115 0.00338 0.00328 0.00313 0.00314 0.00242 0.00259 0.00214 0.00138 S78_b 0.64184 -0.07511 0.85759 0.18886 0.03104 0.03703 0.06054 0.01410 0.02185 -0.00813 0.04103 0.02265 0.00100 0.00061 0.00109 0.00338 0.00461 0.00305 0.00465 0.00270 0.00351 0.00314 0.00216 C92_b 0.51266 0.09652 0.60683 0.24526 0.01935 0.04868 0.02542 -0.01096 0.00272 0.00065 0.03158 0.03189 0.00200 0.00108 0.00142 0.00374 0.00654 0.00945 0.00922 0.00781 0.00763 0.00571 0.00369 H92_b 0.55728 0.09392 0.54618 0.24526 0.03790 0.00374 0.00000 C93_b 0.38888 0.05789 0.60636 0.24526 0.03366 0.02835 0.04057 -0.00951 -0.01118 -0.00401 0.03755 0.03740 0.00296 0.00171 0.00182 0.00374 0.00847 0.00856 0.01293 0.01049 0.00889 0.00617 0.00526 H93_b 0.35025 0.02713 0.54655 0.24526 0.04506 0.00374 0.00000 C94_b 0.32378 0.06476 0.69284 0.24526 0.03358 0.02646 0.05836 -0.00213 0.00800 -0.02025 0.03995 0.04617 0.00382 0.00176 0.00272 0.00374 0.01009 0.01464 0.01228 0.00830 0.00772 0.00848 0.00719 H94_b 0.24448 0.03570 0.69600 0.24526 0.04794 0.00374 0.00000 C95_b 0.37193 0.11339 0.77548 0.24526 0.01572 0.02166 0.05257 0.00320 0.01037 0.00915 0.02960 0.02355 0.00110 0.00059 0.00117 0.00374 0.00492 0.00557 0.00801 0.00528 0.00504 0.00400 0.00276 H95_b 0.31894 0.12277 0.82966 0.24526 0.03552 0.00374 0.00000 C96_b 0.49787 0.14784 0.77771 0.24526 0.00676 0.02715 0.01507 0.00301 0.00106 0.00703 0.01658 0.02325 0.00124 0.00072 0.00108 0.00374 0.00512 0.00813 0.00741 0.00523 0.00573 0.00402 0.00249 C97_b 0.57653 0.19320 0.85873 0.24526 0.02282 0.01983 0.01556 0.00112 0.00357 0.01390 0.01957 0.02347 0.00149 0.00068 0.00099 0.00374 0.00328 0.00313 0.00314 0.00242 0.00259 0.00214 0.00138 C99_b 0.68408 0.27056 1.01707 0.24526 0.05662 0.03792 0.01780 -0.01256 0.00197 0.02137 0.03860 0.03632 0.00349 0.00217 0.00261 0.00374 0.01344 0.01730 0.00753 0.00809 0.00826 0.00734 0.00507 H99_b 0.71209 0.29620 1.08443 0.24526 0.04632 0.00374 0.00000 C100_b 0.76089 0.26848 0.93606 0.24526 0.03238 0.02053 0.02044 -0.00531 -0.00953 0.01215 0.02710 0.02769 0.00170 0.00085 0.00140 0.00374 0.00771 0.00883 0.00681 0.00583 0.00567 0.00497 0.00309 H100_b 0.84537 0.29516 0.93931 0.24526 0.03252 0.00374 0.00000 C101_b 0.70156 0.22293 0.84828 0.24526 0.01259 0.02820 0.01003 -0.00958 -0.00555 0.01182 0.01832 0.02659 0.00168 0.00107 0.00148 0.00374 0.00738 0.00999 0.00615 0.00555 0.00571 0.00493 0.00312 N91_b 0.56694 0.13716 0.69421 0.24526 0.02282 0.01983 0.01556 0.00112 0.00357 0.01390 0.01957 0.02600 0.00152 0.00071 0.00098 0.00374 0.00328 0.00313 0.00314 0.00242 0.00259 0.00214 0.00138 S98_b 0.53295 0.22131 0.98063 0.24526 0.05836 0.04229 0.01944 0.00536 0.02398 0.02302 0.03756 0.02135 0.00127 0.00063 0.00062 0.00374 0.00323 0.00280 0.00384 0.00312 0.00329 0.00229 0.00194 C41 0.89983 0.10414 0.56646 1.00000 0.02408 0.02043 0.02062 0.00000 0.00992 -0.00223 0.02094 0.00530 0.00029 0.00014 0.00023 0.00000 0.00138 0.00132 0.00137 0.00109 0.00114 0.00111 0.00056 C42 0.93344 0.08916 0.45557 1.00000 0.04336 0.02913 0.02224 0.00165 0.01602 0.00661 0.03020 0.00647 0.00037 0.00016 0.00025 0.00000 0.00183 0.00157 0.00150 0.00121 0.00139 0.00137 0.00068 H42A 1.02058 0.06059 0.46696 1.00000 0.04529 0.00000 0.00000 H42B 0.94856 0.13330 0.41986 1.00000 0.04529 0.00000 0.00000 H42C 0.85298 0.06388 0.40799 1.00000 0.04529 0.00000 0.00000 C51 1.05875 0.23043 0.79472 1.00000 0.02420 0.02072 0.01807 0.00034 0.00750 -0.00257 0.02058 0.00523 0.00030 0.00014 0.00022 0.00000 0.00139 0.00131 0.00131 0.00106 0.00111 0.00111 0.00055 C52 1.17343 0.28530 0.81107 1.00000 0.02711 0.02254 0.02957 0.00387 0.00453 -0.00534 0.02677 0.00560 0.00031 0.00015 0.00026 0.00000 0.00148 0.00141 0.00157 0.00121 0.00125 0.00120 0.00062 H52A 1.13378 0.32816 0.77236 1.00000 0.04016 0.00000 0.00000 H52B 1.25315 0.26860 0.78097 1.00000 0.04016 0.00000 0.00000 H52C 1.20834 0.29502 0.89058 1.00000 0.04016 0.00000 0.00000 O41 0.95728 0.06635 0.64771 1.00000 0.04508 0.02243 0.01947 0.00237 0.01112 0.00898 0.02841 0.00416 0.00024 0.00010 0.00016 0.00000 0.00128 0.00101 0.00102 0.00083 0.00094 0.00093 0.00046 O42 0.81555 0.15472 0.56823 1.00000 0.02953 0.03336 0.01848 0.00314 0.01074 0.01085 0.02628 0.00404 0.00021 0.00011 0.00016 0.00000 0.00108 0.00113 0.00099 0.00084 0.00085 0.00090 0.00045 O51 1.10043 0.16868 0.82017 1.00000 0.02363 0.01939 0.04030 0.00405 0.00321 -0.00078 0.02851 0.00396 0.00021 0.00010 0.00019 0.00000 0.00102 0.00098 0.00127 0.00091 0.00093 0.00083 0.00046 O52 0.93165 0.24982 0.75867 1.00000 0.02403 0.02027 0.03592 0.00267 0.00320 -0.00056 0.02740 0.00389 0.00021 0.00010 0.00018 0.00000 0.00104 0.00098 0.00122 0.00087 0.00091 0.00082 0.00045 Pd1 0.95907 0.08757 0.81643 1.00000 0.02251 0.01739 0.02038 0.00541 0.00613 0.00220 0.01992 0.00041 0.00002 0.00001 0.00002 0.00000 0.00012 0.00011 0.00011 0.00008 0.00009 0.00008 0.00006 Pd2 0.74837 0.18603 0.70654 1.00000 0.02002 0.02017 0.01948 0.00291 0.00848 0.00458 0.01925 0.00041 0.00002 0.00001 0.00002 0.00000 0.00011 0.00011 0.00011 0.00008 0.00008 0.00008 0.00006 Final Structure Factor Calculation for 2009src0457 in P2(1)/n Total number of l.s. parameters = 461 Maximum vector length = 511 Memory required = 6002 / 25039 wR2 = 0.0611 before cycle 9 for 5057 data and 0 / 461 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 56. 0. 0. 0. 108. 246. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.022 0.000 0.000 0.000 0.005 0.009 0.000 0.000 GooF = S = 1.169; Restrained GooF = 1.128 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0282 for 4711 Fo > 4sig(Fo) and 0.0314 for all 5057 data wR2 = 0.0611, GooF = S = 1.169, Restrained GooF = 1.128 for all data Occupancy sum of asymmetric unit = 32.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0318 0.0226 0.0140 C2_a 0.0450 0.0291 0.0168 C3_a 0.0432 0.0257 0.0074 C4_a 0.0310 0.0240 0.0188 C5_a 0.0224 0.0184 0.0140 C6_a 0.0227 0.0189 0.0160 C7_a 0.0447 0.0344 0.0180 C9_a 0.0366 0.0298 0.0196 C10_a 0.0260 0.0166 0.0127 C11_a 0.0234 0.0156 0.0138 N1_a 0.0388 0.0322 0.0187 S8_a 0.0401 0.0246 0.0167 C22_a 0.0586 0.0309 0.0191 C23_a 0.0611 0.0354 0.0112 C24_a 0.0421 0.0286 0.0193 C25_a 0.0252 0.0202 0.0099 C26_a 0.0246 0.0188 0.0164 C27_a 0.0393 0.0353 0.0165 C29_a 0.0358 0.0282 0.0187 C30_a 0.0233 0.0206 0.0141 C31_a 0.0270 0.0191 0.0127 N21_a 0.0366 0.0349 0.0163 S28_a 0.0581 0.0192 0.0072 C72_b 0.0498 0.0288 0.0061 C73_b 0.0357 0.0156 0.0073 C74_b 0.0536 0.0284 0.0174 C75_b 0.0357 0.0156 0.0073 C76_b 0.0402 0.0261 0.0092 C77_b 0.0468 0.0448 0.0257 C79_b 0.0349 0.0267 0.0135 C80_b 0.0357 0.0156 0.0073 C81_b 0.0357 0.0156 0.0073 N71_b 0.0672 0.0421 0.0138 S78_b 0.0536 0.0226 0.0186 C92_b 0.0644 0.0330 0.0153 C93_b 0.0602 0.0503 0.0094 C94_b 0.0529 0.0274 0.0085 C95_b 0.0294 0.0158 0.0045 C96_b 0.0357 0.0156 0.0073 C97_b 0.0777 0.0285 0.0095 C99_b 0.0546 0.0152 0.0115 C100_b 0.0428 0.0076 0.0045 C101_b 0.0357 0.0156 0.0073 N91_b 0.0758 0.0281 0.0088 S98_b 0.0269 0.0205 0.0155 C41 0.0470 0.0269 0.0166 C42 0.0257 0.0202 0.0158 C51 0.0356 0.0268 0.0180 C52 0.0482 0.0193 0.0177 O41 0.0428 0.0215 0.0145 O42 0.0436 0.0233 0.0186 O51 0.0388 0.0236 0.0198 O52 0.0253 0.0212 0.0133 Pd1 0.0265 0.0169 0.0143 Pd2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.024 0.048 0.070 0.095 0.122 0.154 0.193 0.242 0.330 1.000 Number in group 530. 502. 492. 509. 496. 508. 512. 502. 503. 503. GooF 1.778 1.219 1.136 1.108 1.039 1.090 0.898 0.933 0.956 1.252 K 2.416 1.118 0.995 0.974 0.980 0.984 0.999 1.001 1.010 1.000 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.64 inf Number in group 523. 508. 496. 501. 507. 504. 505. 510. 497. 506. GooF 1.088 0.996 0.932 0.979 1.027 1.095 1.171 1.189 1.318 1.704 K 0.954 0.985 0.998 1.015 1.006 1.014 1.021 1.019 1.009 0.985 R1 0.068 0.054 0.041 0.037 0.036 0.031 0.026 0.022 0.019 0.022 Recommended weighting scheme: WGHT 0.0000 4.0501 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 3 1 96.60 5.38 6.20 0.009 1.83 2 5 7 124.61 7.50 5.99 0.010 1.40 3 4 4 402.87 180.42 5.73 0.050 1.80 2 12 4 170.89 27.41 5.50 0.020 1.31 2 11 1 104.46 16.57 4.90 0.015 1.60 -2 0 2 1999.94 1514.61 4.71 0.146 4.20 1 0 1 14798.74 24887.12 4.46 0.593 6.64 4 4 3 59.35 0.12 4.34 0.001 1.71 0 1 4 71.67 10.85 4.25 0.012 2.97 1 17 1 106.46 17.74 4.17 0.016 1.11 2 1 10 179.31 62.23 3.97 0.030 1.10 -3 6 4 66.87 8.45 3.95 0.011 1.95 -3 3 4 8194.80 9404.81 3.90 0.364 2.31 4 7 3 70.24 1.52 3.88 0.005 1.52 6 9 1 312.42 161.68 3.84 0.048 1.22 -5 5 1 103.09 31.87 3.76 0.021 1.71 5 2 4 154.88 62.13 3.71 0.030 1.42 -3 11 5 73.80 10.10 3.71 0.012 1.36 0 3 2 7364.92 6503.64 3.62 0.303 4.38 -1 17 2 55.70 1.27 3.62 0.004 1.10 -8 10 3 47.78 2.22 3.61 0.006 1.01 1 15 7 60.43 3.49 3.60 0.007 1.00 -3 23 1 28.56 219.48 3.55 0.056 0.81 3 1 1 4096.78 4698.45 3.55 0.258 2.82 -1 8 7 61.65 8.37 3.52 0.011 1.42 -7 5 3 37.18 0.34 3.51 0.002 1.28 -7 7 3 119.36 41.75 3.51 0.024 1.22 -4 10 2 50.73 6.29 3.46 0.009 1.49 1 5 10 70.00 3.22 3.42 0.007 1.11 -1 6 4 146.47 68.06 3.42 0.031 2.22 1 14 7 88.47 9.40 3.42 0.012 1.05 2 6 2 10142.78 11147.62 3.41 0.397 2.30 7 3 1 35.55 0.08 3.37 0.001 1.26 -5 4 13 132.21 18.19 3.35 0.016 0.90 4 15 0 93.85 18.60 3.34 0.016 1.12 2 13 5 83.74 17.59 3.33 0.016 1.18 -5 22 5 124.02 290.41 3.31 0.064 0.77 1 5 2 2685.83 3119.18 3.30 0.210 2.94 3 3 0 56.69 14.73 3.30 0.014 2.79 3 8 7 78.59 16.08 3.27 0.015 1.19 -5 2 2 17643.93 18969.74 3.26 0.517 1.87 -3 2 1 10837.94 11834.70 3.25 0.409 3.03 -5 15 1 360.71 208.74 3.25 0.054 1.06 7 10 3 90.80 0.26 3.23 0.002 1.01 5 4 0 450.79 305.57 3.22 0.066 1.74 -3 4 5 87.29 30.04 3.20 0.021 1.97 -4 4 8 44.23 0.49 3.20 0.003 1.37 0 2 8 42.00 2.10 3.17 0.005 1.49 -4 8 4 707.53 510.80 3.16 0.085 1.58 2 3 5 3634.36 4140.35 3.15 0.242 1.87 Bond lengths and angles C2_a - Distance Angles N1_a 1.3392 (0.0057) C3_a 1.3882 (0.0081) 121.81 (0.46) H2_a 0.9500 119.10 119.10 C2_a - N1_a C3_a C3_a - Distance Angles C4_a 1.3783 (0.0125) C2_a 1.3882 (0.0081) 119.39 (0.62) H3_a 0.9500 120.30 120.30 C3_a - C4_a C2_a C4_a - Distance Angles C5_a 1.3898 (0.0100) C3_a 1.3783 (0.0124) 119.00 (0.65) H4_a 0.9500 120.50 120.50 C4_a - C5_a C3_a C5_a - Distance Angles C4_a 1.3898 (0.0100) C6_a 1.3911 (0.0053) 119.73 (0.53) H5_a 0.9500 120.13 120.13 C5_a - C4_a C6_a C6_a - Distance Angles N1_a 1.3667 (0.0053) C5_a 1.3911 (0.0053) 120.35 (0.41) C7_a 1.4291 (0.0061) 111.33 (0.37) 128.30 (0.41) C6_a - N1_a C5_a C7_a - Distance Angles C11_a 1.3807 (0.0057) C6_a 1.4291 (0.0061) 118.88 (0.39) S8_a 1.7376 (0.0048) 112.70 (0.34) 128.42 (0.35) C7_a - C11_a C6_a C9_a - Distance Angles C10_a 1.3737 (0.0083) S8_a 1.7200 (0.0064) 113.09 (0.49) H9_a 0.9500 123.46 123.46 C9_a - C10_a S8_a C10_a - Distance Angles C9_a 1.3737 (0.0083) C11_a 1.4249 (0.0060) 112.34 (0.47) H10_a 0.9500 123.83 123.83 C10_a - C9_a C11_a C11_a - Distance Angles C7_a 1.3807 (0.0057) C10_a 1.4249 (0.0060) 111.49 (0.39) Pd2 1.9932 (0.0047) 112.32 (0.31) 136.09 (0.35) C11_a - C7_a C10_a N1_a - Distance Angles C2_a 1.3392 (0.0057) C6_a 1.3667 (0.0053) 119.67 (0.39) Pd2 2.0107 (0.0046) 123.61 (0.32) 116.38 (0.30) N1_a - C2_a C6_a S8_a - Distance Angles C9_a 1.7200 (0.0065) C7_a 1.7376 (0.0049) 90.37 (0.30) S8_a - C9_a C22_a - Distance Angles N21_a 1.3381 (0.0050) C23_a 1.3857 (0.0059) 122.00 (0.40) H22_a 0.9500 119.00 119.00 C22_a - N21_a C23_a C23_a - Distance Angles C24_a 1.3795 (0.0088) C22_a 1.3857 (0.0059) 118.81 (0.52) H23_a 0.9500 120.60 120.60 C23_a - C24_a C22_a C24_a - Distance Angles C23_a 1.3795 (0.0088) C25_a 1.3783 (0.0097) 119.69 (0.59) H24_a 0.9500 120.15 120.15 C24_a - C23_a C25_a C25_a - Distance Angles C24_a 1.3783 (0.0097) C26_a 1.3996 (0.0048) 119.58 (0.44) H25_a 0.9500 120.21 120.21 C25_a - C24_a C26_a C26_a - Distance Angles N21_a 1.3629 (0.0046) C25_a 1.3996 (0.0048) 119.94 (0.35) C27_a 1.4344 (0.0051) 111.61 (0.30) 128.44 (0.36) C26_a - N21_a C25_a C27_a - Distance Angles C31_a 1.3852 (0.0049) C26_a 1.4344 (0.0051) 118.61 (0.34) S28_a 1.7277 (0.0037) 112.42 (0.28) 128.97 (0.29) C27_a - C31_a C26_a C29_a - Distance Angles C30_a 1.3559 (0.0061) S28_a 1.7240 (0.0046) 112.94 (0.33) H29_a 0.9500 123.53 123.53 C29_a - C30_a S28_a C30_a - Distance Angles C29_a 1.3559 (0.0061) C31_a 1.4233 (0.0054) 112.79 (0.37) H30_a 0.9500 123.60 123.60 C30_a - C29_a C31_a C31_a - Distance Angles C27_a 1.3852 (0.0049) C30_a 1.4233 (0.0054) 111.30 (0.34) Pd1 1.9821 (0.0040) 112.20 (0.28) 136.36 (0.28) C31_a - C27_a C30_a N21_a - Distance Angles C22_a 1.3381 (0.0050) C26_a 1.3629 (0.0046) 119.95 (0.33) Pd1 2.0108 (0.0031) 123.90 (0.27) 115.91 (0.23) N21_a - C22_a C26_a S28_a - Distance Angles C29_a 1.7240 (0.0047) C27_a 1.7277 (0.0037) 90.54 (0.21) S28_a - C29_a C72_b - Distance Angles N71_b 1.3344 (0.0153) C73_b 1.4160 (0.0154) 118.72 (1.49) H72_b 0.9500 120.64 120.64 C72_b - N71_b C73_b C73_b - Distance Angles C74_b 1.3906 (0.0173) C72_b 1.4160 (0.0154) 118.60 (1.60) H73_b 0.9500 120.70 120.70 C73_b - C74_b C72_b C74_b - Distance Angles C75_b 1.3698 (0.0184) C73_b 1.3906 (0.0173) 122.42 (1.70) H74_b 0.9500 118.79 118.79 C74_b - C75_b C73_b C75_b - Distance Angles C74_b 1.3698 (0.0185) C76_b 1.4065 (0.0141) 116.39 (1.45) H75_b 0.9500 121.80 121.80 C75_b - C74_b C76_b C76_b - Distance Angles N71_b 1.3553 (0.0148) C75_b 1.4065 (0.0141) 121.42 (1.29) C77_b 1.4263 (0.0147) 112.68 (1.14) 125.83 (1.37) C76_b - N71_b C75_b C77_b - Distance Angles C81_b 1.3878 (0.0145) C76_b 1.4263 (0.0147) 118.31 (1.23) S78_b 1.7310 (0.0139) 111.03 (1.03) 130.31 (1.18) C77_b - C81_b C76_b C79_b - Distance Angles C80_b 1.3631 (0.0159) S78_b 1.7076 (0.0157) 110.64 (1.20) H79_b 0.9500 124.68 124.68 C79_b - C80_b S78_b C80_b - Distance Angles C79_b 1.3631 (0.0159) C81_b 1.4056 (0.0152) 114.94 (1.37) H80_b 0.9500 122.53 122.53 C80_b - C79_b C81_b C81_b - Distance Angles C77_b 1.3878 (0.0145) C80_b 1.4056 (0.0152) 111.05 (1.28) Pd1 2.0493 (0.0159) 110.51 (0.96) 138.25 (1.05) C81_b - C77_b C80_b N71_b - Distance Angles C72_b 1.3344 (0.0154) C76_b 1.3553 (0.0148) 122.35 (1.34) Pd1 1.9831 (0.0145) 120.36 (1.11) 117.24 (0.90) N71_b - C72_b C76_b S78_b - Distance Angles C79_b 1.7076 (0.0157) C77_b 1.7310 (0.0140) 92.30 (0.76) S78_b - C79_b C92_b - Distance Angles N91_b 1.3341 (0.0140) C93_b 1.3967 (0.0187) 118.62 (1.40) H92_b 0.9500 120.69 120.69 C92_b - N91_b C93_b C93_b - Distance Angles C94_b 1.3682 (0.0208) C92_b 1.3967 (0.0187) 119.40 (1.72) H93_b 0.9500 120.30 120.30 C93_b - C94_b C92_b C94_b - Distance Angles C93_b 1.3682 (0.0208) C95_b 1.3793 (0.0183) 120.77 (1.89) H94_b 0.9500 119.62 119.62 C94_b - C93_b C95_b C95_b - Distance Angles C96_b 1.3700 (0.0128) C94_b 1.3793 (0.0183) 118.53 (1.44) H95_b 0.9500 120.74 120.74 C95_b - C96_b C94_b C96_b - Distance Angles N91_b 1.3695 (0.0127) C95_b 1.3700 (0.0128) 119.65 (1.16) C97_b 1.4034 (0.0139) 111.01 (1.05) 129.29 (1.19) C96_b - N91_b C95_b C97_b - Distance Angles C101_b 1.3603 (0.0143) C96_b 1.4034 (0.0139) 121.77 (1.12) S98_b 1.7448 (0.0123) 110.54 (0.96) 127.68 (1.13) C97_b - C101_b C96_b C99_b - Distance Angles C100_b 1.3790 (0.0187) S98_b 1.6970 (0.0167) 111.09 (1.28) H99_b 0.9500 124.45 124.45 C99_b - C100_b S98_b C100_b - Distance Angles C99_b 1.3790 (0.0187) C101_b 1.4043 (0.0138) 113.18 (1.33) H100_b 0.9500 123.41 123.41 C100_b - C99_b C101_b C101_b - Distance Angles C97_b 1.3603 (0.0142) C100_b 1.4043 (0.0138) 112.94 (1.19) Pd2 2.0390 (0.0160) 108.42 (0.90) 138.63 (1.10) C101_b - C97_b C100_b N91_b - Distance Angles C92_b 1.3341 (0.0140) C96_b 1.3695 (0.0127) 122.31 (1.28) Pd2 1.9482 (0.0147) 120.81 (1.03) 116.86 (0.87) N91_b - C92_b C96_b S98_b - Distance Angles C99_b 1.6970 (0.0169) C97_b 1.7448 (0.0123) 92.11 (0.88) S98_b - C99_b C41 - Distance Angles O41 1.2554 (0.0034) O42 1.2641 (0.0033) 125.98 (0.25) C42 1.5110 (0.0037) 118.17 (0.24) 115.85 (0.25) C41 - O41 O42 C42 - Distance Angles C41 1.5110 (0.0037) H42A 0.9800 109.47 H42B 0.9800 109.47 109.47 H42C 0.9800 109.47 109.47 109.47 C42 - C41 H42A H42B C51 - Distance Angles O52 1.2502 (0.0033) O51 1.2629 (0.0033) 126.20 (0.25) C52 1.4987 (0.0038) 117.49 (0.24) 116.31 (0.25) C51 - O52 O51 C52 - Distance Angles C51 1.4987 (0.0038) H52A 0.9800 109.47 H52B 0.9800 109.47 109.47 H52C 0.9800 109.47 109.47 109.47 C52 - C51 H52A H52B O41 - Distance Angles C41 1.2554 (0.0034) Pd1 2.1255 (0.0020) 125.32 (0.18) O41 - C41 O42 - Distance Angles C41 1.2641 (0.0033) Pd2 2.0576 (0.0019) 124.40 (0.18) O42 - C41 O51 - Distance Angles C51 1.2629 (0.0033) Pd1 2.0535 (0.0020) 122.23 (0.18) O51 - C51 O52 - Distance Angles C51 1.2502 (0.0034) Pd2 2.1107 (0.0020) 127.40 (0.18) O52 - C51 Pd1 - Distance Angles N71_b 1.9831 (0.0145) C31_a 1.9821 (0.0040) 18.14 (0.36) N21_a 2.0108 (0.0031) 63.15 (0.42) 81.27 (0.15) C81_b 2.0493 (0.0160) 80.60 (0.56) 98.63 (0.42) 17.72 (0.35) O51 2.0535 (0.0020) 107.62 (0.41) 89.54 (0.13) 170.57 (0.11) 171.71 (0.40) O41 2.1255 (0.0020) 161.28 (0.41) 179.37 (0.13) 98.16 (0.11) 80.82 (0.40) 91.02 (0.09) Pd2 2.8594 (0.0003) 100.10 (0.39) 100.27 (0.10) 95.19 (0.08) 95.54 (0.44) 84.29 (0.06) 79.49 (0.05) Pd1 - N71_b C31_a N21_a C81_b O51 O41 Pd2 - Distance Angles N91_b 1.9482 (0.0147) C11_a 1.9932 (0.0048) 14.09 (0.30) N1_a 2.0107 (0.0046) 67.07 (0.36) 80.77 (0.17) C101_b 2.0390 (0.0160) 81.89 (0.52) 95.55 (0.42) 14.82 (0.36) O42 2.0576 (0.0019) 104.18 (0.34) 90.53 (0.14) 171.25 (0.13) 173.92 (0.41) O52 2.1107 (0.0020) 164.62 (0.34) 175.83 (0.15) 97.55 (0.13) 82.73 (0.41) 91.20 (0.08) Pd1 2.8594 (0.0003) 103.75 (0.39) 105.94 (0.14) 98.36 (0.17) 95.34 (0.61) 83.07 (0.05) 78.04 (0.05) Pd2 - N91_b C11_a N1_a C101_b O42 O52 FMAP and GRID set by program FMAP 2 2 25 GRID -1.136 -2 -2 1.136 2 2 R1 = 0.0309 for 5057 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.62 at 0.7929 0.2044 0.7524 [ 0.72 A from PD2 ] Deepest hole -0.90 at 0.6956 0.1600 0.6774 [ 0.74 A from PD2 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 5621 / 24029 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7929 0.2044 0.7524 1.00000 0.05 0.62 0.72 PD2 1.58 O52 1.67 C101 1.82 N1 Q2 1 1.1223 0.2593 0.8008 1.00000 0.05 0.47 0.69 C52 0.81 C51 1.35 H52B 1.37 H52A Q3 1 0.9348 0.0303 0.4299 1.00000 0.05 0.41 1.00 H42C 1.02 H42A 1.17 C42 1.98 H42B Q4 1 1.1044 0.0967 0.7990 1.00000 0.05 0.37 1.40 O51 1.47 PD1 2.06 H95 2.14 O41 Q5 1 0.7476 0.1370 0.7861 1.00000 0.05 0.37 1.36 PD2 1.76 N1 1.83 N91 1.91 C101 Q6 1 0.7277 0.1904 0.8141 1.00000 0.05 0.36 0.82 C101 0.83 N1 1.40 PD2 1.67 C97 Q7 1 0.9186 0.0644 0.7808 1.00000 0.05 0.36 0.68 PD1 1.51 C81 1.63 N21 1.77 O41 Q8 1 0.6187 0.1541 0.6600 1.00000 0.05 0.36 0.65 C11 0.79 N91 1.38 PD2 1.54 C92 Q9 1 0.7762 0.0479 1.1454 1.00000 0.05 0.35 0.75 C74 0.90 C75 1.03 S28 1.12 H74 Q10 1 0.7475 -0.0076 0.7029 1.00000 0.05 0.34 0.60 H22 0.75 C80 0.78 C22 1.18 C81 Shortest distances between peaks (including symmetry equivalents) 5 6 1.11 1 6 1.13 1 5 1.45 5 8 1.78 4 7 1.85 1 8 2.03 6 8 2.07 5 7 2.16 7 10 2.18 3 3 2.21 1 7 2.92 5 10 2.95 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 1.30: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.06: Set up l.s. refinement 0.00: Generate idealized H-atoms 4.30: Structure factors and derivatives 13.50: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 1.59: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0457 finished at 12:40:29 Total CPU time: 21.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++