+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0656 started at 20:19:58 on 14-Jun-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0656 in Pbca CELL 0.71073 11.4593 16.8538 19.0612 90.000 90.000 90.000 ZERR 8.00 0.0002 0.0002 0.0002 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O P CL UNIT 72 144 24 16 24 32 V = 3681.34 F(000) = 1776.0 Mu = 0.91 mm-1 Cell Wt = 3479.79 Rho = 1.570 MERG 2 OMIT -3.00 55.00 OMIT 0 4 0 OMIT 1 2 1 OMIT 2 2 0 OMIT 4 5 4 FMAP 2 PLAN 20 SIZE 0.02 0.10 0.12 ACTA BOND WGHT 0.03790 2.31020 L.S. 4 TEMP -153.00 FVAR 0.36477 C1 1 0.496596 0.055323 0.636844 11.00000 0.02514 0.04686 = 0.03072 0.01019 0.00047 0.00122 AFIX 23 H1A 2 0.515931 0.018046 0.598424 11.00000 -1.20000 H1B 2 0.535921 0.036241 0.679901 11.00000 -1.20000 AFIX 0 C2 1 0.543878 0.137748 0.618261 11.00000 0.02436 0.04223 = 0.02156 0.00092 0.00266 0.00046 C3 1 0.522931 0.159738 0.541274 11.00000 0.02505 0.03422 = 0.02323 0.00042 0.00323 -0.00292 AFIX 23 H3A 2 0.577048 0.203005 0.528026 11.00000 -1.20000 H3B 2 0.541174 0.113229 0.511506 11.00000 -1.20000 AFIX 0 C4 1 0.679522 0.129628 0.623045 11.00000 0.02392 0.04551 = 0.03050 -0.00410 0.00217 0.00174 AFIX 23 H4A 2 0.703549 0.084350 0.593277 11.00000 -1.20000 H4B 2 0.714767 0.178059 0.602677 11.00000 -1.20000 AFIX 0 C5 1 0.731294 0.117377 0.696199 11.00000 0.03010 0.08759 = 0.03774 -0.00280 -0.00613 0.00628 AFIX 137 H5A 2 0.714185 0.163763 0.725445 11.00000 -1.50000 H5B 2 0.815993 0.110556 0.692438 11.00000 -1.50000 H5C 2 0.696879 0.069961 0.717590 11.00000 -1.50000 AFIX 0 C6 1 0.494606 0.200990 0.668520 11.00000 0.02837 0.05330 = 0.02085 -0.00100 0.00262 0.00606 AFIX 23 H6A 2 0.409365 0.205020 0.660855 11.00000 -1.20000 H6B 2 0.506946 0.182756 0.717332 11.00000 -1.20000 AFIX 0 C7 1 0.547560 0.283119 0.660765 11.00000 0.04642 0.04921 = 0.03227 -0.01162 0.00716 0.00438 AFIX 23 H7A 2 0.632082 0.279646 0.671065 11.00000 -1.20000 H7B 2 0.539155 0.300127 0.611309 11.00000 -1.20000 AFIX 0 C8 1 0.494481 0.346205 0.707502 11.00000 0.06411 0.06348 = 0.02944 -0.00632 -0.00064 0.03015 AFIX 23 H8A 2 0.504649 0.330419 0.757155 11.00000 -1.20000 H8B 2 0.409692 0.349552 0.697989 11.00000 -1.20000 AFIX 0 C9 1 0.549236 0.427876 0.696390 11.00000 0.10396 0.04913 = 0.04843 -0.01845 -0.00997 0.03161 AFIX 137 H9A 2 0.629357 0.427682 0.714367 11.00000 -1.50000 H9B 2 0.503438 0.467948 0.721488 11.00000 -1.50000 H9C 2 0.550041 0.440398 0.646185 11.00000 -1.50000 AFIX 0 N1 3 0.334407 0.038030 0.513740 11.00000 0.02571 0.02644 = 0.02455 0.00154 0.00449 0.00148 N2 3 0.186092 0.163276 0.504039 11.00000 0.02775 0.03285 = 0.02731 0.00620 0.00334 0.00356 N3 3 0.157436 0.053041 0.608098 11.00000 0.02609 0.03200 = 0.03165 0.00589 0.01019 0.00116 O1 4 0.369367 0.054587 0.648254 11.00000 0.02709 0.04727 = 0.02590 0.00681 0.00518 -0.00308 O2 4 0.402218 0.185406 0.526961 11.00000 0.02788 0.02957 = 0.02499 0.00118 0.00026 0.00004 P1 5 0.285115 0.021265 0.590794 11.00000 0.02455 0.02846 = 0.02716 0.00585 0.00654 0.00113 P2 5 0.312951 0.127880 0.490863 11.00000 0.02367 0.02802 = 0.02094 0.00280 0.00304 0.00039 P3 5 0.110359 0.126820 0.565453 11.00000 0.02381 0.02961 = 0.02710 0.00158 0.00522 0.00267 CL1 6 0.285250 -0.096076 0.604130 11.00000 0.04182 0.03001 = 0.04682 0.01202 0.01484 0.00590 CL2 6 0.346945 0.134546 0.388367 11.00000 0.03326 0.03836 = 0.02126 0.00323 0.00440 0.00006 CL3 6 0.073482 0.214196 0.633443 11.00000 0.06388 0.03518 = 0.03201 -0.00033 0.01369 0.01056 CL4 6 -0.048356 0.102405 0.528334 11.00000 0.02379 0.05782 = 0.05575 0.00457 -0.00081 -0.00040 HKLF 4 Covalent radii and connectivity table for 2007src0656 in Pbca C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - O1 C2 C2 - C3 C1 C6 C4 C3 - O2 C2 C4 - C5 C2 C5 - C4 C6 - C7 C2 C7 - C8 C6 C8 - C7 C9 C9 - C8 N1 - P2 P1 N2 - P3 P2 N3 - P3 P1 O1 - C1 P1 O2 - C3 P2 P1 - O1 N3 N1 Cl1 P2 P2 - O2 N2 N1 Cl2 P1 P3 - N3 N2 Cl4 Cl3 Cl1 - P1 Cl2 - P2 Cl3 - P3 Cl4 - P3 h k l Fo^2 Sigma Why rejected 5 2 0 29.49 5.29 observed but should be systematically absent 5 2 0 20.43 5.07 observed but should be systematically absent 9 7 0 14.19 3.54 observed but should be systematically absent 61045 Reflections read, of which 3812 rejected -14 =< h =< 14, -21 =< k =< 21, -24 =< l =< 24, Max. 2-theta = 54.96 3 Systematic absence violations 0 Inconsistent equivalents 4213 Unique reflections, of which 0 suppressed R(int) = 0.0494 R(sigma) = 0.0258 Friedel opposites merged Maximum memory for data reduction = 1986 / 41701 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 = 2526 / 240175 wR2 = 0.0821 before cycle 1 for 4213 data and 192 / 192 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0379 * P )^2 + 2.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36407 0.00049 -1.430 OSF Mean shift/esd = 0.178 Maximum = -1.430 for OSF Max. shift = 0.004 A for H5A Max. dU = 0.000 for N2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2526 / 240175 wR2 = 0.0821 before cycle 2 for 4213 data and 192 / 192 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0379 * P )^2 + 2.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36379 0.00049 -0.563 OSF Mean shift/esd = 0.060 Maximum = -0.563 for OSF Max. shift = 0.002 A for H5A Max. dU = 0.000 for N2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2526 / 240175 wR2 = 0.0821 before cycle 3 for 4213 data and 192 / 192 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0379 * P )^2 + 2.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36379 0.00049 -0.002 OSF Mean shift/esd = 0.001 Maximum = 0.020 for U11 C8 Max. shift = 0.000 A for H5B Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2526 / 240175 wR2 = 0.0820 before cycle 4 for 4213 data and 192 / 192 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0379 * P )^2 + 2.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36379 0.00049 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.007 for U12 C9 Max. shift = 0.000 A for H5B Max. dU = 0.000 for C9 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.5159 0.0181 0.5984 23 0.990 0.000 C1 O1 C2 H1B 0.5359 0.0362 0.6799 23 0.990 0.000 C1 O1 C2 H3A 0.5770 0.2030 0.5280 23 0.990 0.000 C3 O2 C2 H3B 0.5412 0.1133 0.5115 23 0.990 0.000 C3 O2 C2 H4A 0.7035 0.0843 0.5933 23 0.990 0.000 C4 C5 C2 H4B 0.7148 0.1780 0.6027 23 0.990 0.000 C4 C5 C2 H5A 0.7138 0.1637 0.7255 137 0.980 0.000 C5 C4 H5A H5B 0.8160 0.1108 0.6925 137 0.980 0.000 C5 C4 H5A H5C 0.6971 0.0698 0.7175 137 0.980 0.000 C5 C4 H5A H6A 0.4094 0.2049 0.6609 23 0.990 0.000 C6 C7 C2 H6B 0.5070 0.1827 0.7173 23 0.990 0.000 C6 C7 C2 H7A 0.6321 0.2797 0.6711 23 0.990 0.000 C7 C8 C6 H7B 0.5391 0.3001 0.6113 23 0.990 0.000 C7 C8 C6 H8A 0.5045 0.3304 0.7572 23 0.990 0.000 C8 C7 C9 H8B 0.4096 0.3495 0.6980 23 0.990 0.000 C8 C7 C9 H9A 0.6292 0.4277 0.7145 137 0.980 0.000 C9 C8 H9A H9B 0.5032 0.4679 0.7214 137 0.980 0.000 C9 C8 H9A H9C 0.5502 0.4403 0.6462 137 0.980 0.000 C9 C8 H9A 2007src0656 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.49660 0.05532 0.63684 1.00000 0.02496 0.04636 0.03056 0.01026 0.00049 0.00124 0.03396 0.00368 0.00017 0.00013 0.00011 0.00000 0.00093 0.00114 0.00096 0.00085 0.00078 0.00082 0.00043 H1A 0.51593 0.01806 0.59841 1.00000 0.04075 0.00000 0.00000 H1B 0.53591 0.03622 0.67989 1.00000 0.04075 0.00000 0.00000 C2 0.54391 0.13774 0.61828 1.00000 0.02431 0.04176 0.02123 0.00106 0.00265 0.00046 0.02910 0.00334 0.00016 0.00012 0.00010 0.00000 0.00089 0.00104 0.00086 0.00075 0.00069 0.00077 0.00039 C3 0.52289 0.15976 0.54125 1.00000 0.02474 0.03389 0.02306 0.00038 0.00339 -0.00305 0.02723 0.00317 0.00015 0.00011 0.00009 0.00000 0.00088 0.00093 0.00085 0.00072 0.00071 0.00073 0.00037 H3A 0.57698 0.20305 0.52800 1.00000 0.03268 0.00000 0.00000 H3B 0.54116 0.11326 0.51147 1.00000 0.03268 0.00000 0.00000 C4 0.67950 0.12962 0.62304 1.00000 0.02387 0.04516 0.03018 -0.00414 0.00221 0.00171 0.03307 0.00346 0.00016 0.00013 0.00011 0.00000 0.00092 0.00115 0.00101 0.00083 0.00076 0.00081 0.00043 H4A 0.70352 0.08432 0.59329 1.00000 0.03968 0.00000 0.00000 H4B 0.71476 0.17803 0.60265 1.00000 0.03968 0.00000 0.00000 C5 0.73125 0.11740 0.69624 1.00000 0.02981 0.08718 0.03760 -0.00245 -0.00618 0.00629 0.05153 0.00435 0.00020 0.00017 0.00013 0.00000 0.00113 0.00192 0.00123 0.00118 0.00094 0.00115 0.00064 H5A 0.71377 0.16368 0.72554 1.00000 0.07729 0.00000 0.00000 H5B 0.81600 0.11085 0.69253 1.00000 0.07729 0.00000 0.00000 H5C 0.69712 0.06984 0.71755 1.00000 0.07729 0.00000 0.00000 C6 0.49462 0.20093 0.66853 1.00000 0.02807 0.05327 0.02064 -0.00101 0.00264 0.00613 0.03399 0.00352 0.00017 0.00013 0.00010 0.00000 0.00095 0.00121 0.00088 0.00081 0.00075 0.00086 0.00044 H6A 0.40937 0.20493 0.66087 1.00000 0.04079 0.00000 0.00000 H6B 0.50698 0.18270 0.71734 1.00000 0.04079 0.00000 0.00000 C7 0.54754 0.28311 0.66076 1.00000 0.04648 0.04866 0.03214 -0.01162 0.00715 0.00437 0.04243 0.00392 0.00020 0.00013 0.00011 0.00000 0.00123 0.00123 0.00111 0.00093 0.00093 0.00101 0.00051 H7A 0.63207 0.27967 0.67106 1.00000 0.05091 0.00000 0.00000 H7B 0.53913 0.30012 0.61130 1.00000 0.05091 0.00000 0.00000 C8 0.49439 0.34618 0.70751 1.00000 0.06413 0.06367 0.02918 -0.00635 -0.00059 0.03048 0.05233 0.00480 0.00024 0.00016 0.00012 0.00000 0.00158 0.00152 0.00108 0.00103 0.00107 0.00130 0.00064 H8A 0.50453 0.33039 0.75716 1.00000 0.06279 0.00000 0.00000 H8B 0.40961 0.34953 0.69797 1.00000 0.06279 0.00000 0.00000 C9 0.54914 0.42782 0.69641 1.00000 0.10428 0.04872 0.04811 -0.01842 -0.01004 0.03142 0.06704 0.00503 0.00029 0.00016 0.00014 0.00000 0.00241 0.00144 0.00148 0.00119 0.00151 0.00157 0.00086 H9A 0.62918 0.42766 0.71451 1.00000 0.10056 0.00000 0.00000 H9B 0.50322 0.46791 0.72140 1.00000 0.10056 0.00000 0.00000 H9C 0.55015 0.44029 0.64620 1.00000 0.10056 0.00000 0.00000 N1 0.33440 0.03804 0.51375 1.00000 0.02534 0.02638 0.02427 0.00165 0.00461 0.00140 0.02533 0.00267 0.00013 0.00009 0.00008 0.00000 0.00075 0.00074 0.00074 0.00058 0.00061 0.00059 0.00032 N2 0.18609 0.16327 0.50404 1.00000 0.02722 0.03259 0.02705 0.00622 0.00342 0.00366 0.02895 0.00287 0.00014 0.00010 0.00008 0.00000 0.00079 0.00082 0.00079 0.00065 0.00064 0.00064 0.00034 N3 0.15748 0.05307 0.60810 1.00000 0.02586 0.03163 0.03152 0.00605 0.01006 0.00126 0.02967 0.00296 0.00014 0.00009 0.00008 0.00000 0.00078 0.00081 0.00082 0.00065 0.00065 0.00063 0.00035 O1 0.36936 0.05458 0.64824 1.00000 0.02678 0.04712 0.02555 0.00674 0.00508 -0.00306 0.03315 0.00242 0.00012 0.00009 0.00007 0.00000 0.00068 0.00080 0.00066 0.00058 0.00054 0.00059 0.00031 O2 0.40224 0.18538 0.52696 1.00000 0.02794 0.02917 0.02458 0.00119 0.00019 -0.00003 0.02723 0.00218 0.00011 0.00007 0.00006 0.00000 0.00066 0.00064 0.00062 0.00050 0.00051 0.00051 0.00027 P1 0.28511 0.02127 0.59079 1.00000 0.02444 0.02826 0.02693 0.00585 0.00655 0.00114 0.02654 0.00086 0.00004 0.00003 0.00003 0.00000 0.00024 0.00024 0.00024 0.00018 0.00018 0.00018 0.00012 P2 0.31294 0.12788 0.49087 1.00000 0.02348 0.02779 0.02073 0.00278 0.00304 0.00037 0.02400 0.00081 0.00004 0.00003 0.00002 0.00000 0.00023 0.00024 0.00022 0.00017 0.00017 0.00017 0.00011 P3 0.11037 0.12683 0.56545 1.00000 0.02365 0.02944 0.02685 0.00166 0.00520 0.00270 0.02665 0.00085 0.00004 0.00003 0.00003 0.00000 0.00023 0.00024 0.00024 0.00018 0.00018 0.00018 0.00012 Cl1 0.28524 -0.09608 0.60412 1.00000 0.04167 0.02980 0.04651 0.01199 0.01483 0.00589 0.03933 0.00103 0.00005 0.00003 0.00003 0.00000 0.00028 0.00024 0.00030 0.00021 0.00022 0.00020 0.00014 Cl2 0.34694 0.13454 0.38836 1.00000 0.03312 0.03811 0.02107 0.00327 0.00441 0.00007 0.03077 0.00083 0.00004 0.00003 0.00002 0.00000 0.00024 0.00025 0.00021 0.00017 0.00017 0.00019 0.00011 Cl3 0.07347 0.21419 0.63344 1.00000 0.06377 0.03489 0.03179 -0.00030 0.01368 0.01057 0.04348 0.00105 0.00005 0.00003 0.00003 0.00000 0.00036 0.00026 0.00026 0.00020 0.00024 0.00024 0.00015 Cl4 -0.04836 0.10241 0.52834 1.00000 0.02362 0.05763 0.05551 0.00460 -0.00081 -0.00041 0.04559 0.00103 0.00004 0.00004 0.00003 0.00000 0.00023 0.00034 0.00034 0.00026 0.00022 0.00022 0.00015 Final Structure Factor Calculation for 2007src0656 in Pbca Total number of l.s. parameters = 192 Maximum vector length = 511 Memory required = 2334 / 25039 wR2 = 0.0821 before cycle 5 for 4213 data and 0 / 192 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0379 * P )^2 + 2.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0310 for 3673 Fo > 4sig(Fo) and 0.0383 for all 4213 data wR2 = 0.0821, GooF = S = 1.053, Restrained GooF = 1.053 for all data Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0515 0.0255 0.0249 C1 0.0418 0.0258 0.0197 C2 0.0349 0.0268 0.0201 C3 0.0463 0.0302 0.0228 C4 0.0881 0.0404 0.0261 C5 0.0547 0.0278 0.0195 C6 0.0547 0.0494 0.0232 C7 0.0947 0.0358 0.0264 C8 0.1223 0.0527 0.0261 C9 0.0306 0.0253 0.0202 N1 0.0387 0.0254 0.0227 N2 0.0422 0.0292 0.0177 N3 0.0492 0.0311 0.0192 O1 0.0295 0.0279 0.0243 O2 0.0361 0.0255 0.0180 P1 0.0291 0.0246 0.0183 P2 0.0331 0.0272 0.0196 P3 0.0641 0.0307 0.0233 Cl1 0.0389 0.0343 0.0191 Cl2 0.0715 0.0342 0.0248 Cl3 0.0613 0.0519 0.0236 Cl4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.030 0.045 0.061 0.077 0.098 0.125 0.163 0.232 1.000 Number in group 434. 420. 409. 445. 402. 433. 415. 413. 418. 424. GooF 1.136 1.108 1.089 1.115 1.013 0.981 1.048 0.998 0.952 1.062 K 1.677 0.995 0.979 0.977 0.981 0.985 0.995 1.009 1.013 0.995 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 426. 416. 430. 417. 421. 417. 421. 421. 423. 421. GooF 0.988 0.932 0.974 0.878 0.926 0.879 0.995 0.962 1.016 1.713 K 0.983 1.003 1.010 0.998 1.012 1.022 1.025 1.021 1.014 0.976 R1 0.101 0.068 0.064 0.045 0.042 0.034 0.032 0.023 0.021 0.030 Recommended weighting scheme: WGHT 0.0343 2.5309 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 7 4 3 78.05 6.69 6.02 0.010 1.48 1 3 5 117.57 36.71 5.83 0.023 3.04 5 3 5 270.72 130.61 5.79 0.042 1.85 2 5 6 74.83 174.50 4.96 0.049 2.14 3 0 2 274.58 454.44 4.93 0.079 3.55 6 3 3 203.21 100.31 4.92 0.037 1.74 3 3 5 2111.86 1627.03 4.82 0.150 2.43 6 3 5 139.81 64.52 4.33 0.030 1.63 0 8 1 988.37 739.93 4.12 0.101 2.09 4 1 0 7714.65 9331.91 4.11 0.359 2.82 4 4 0 770.92 1028.44 4.03 0.119 2.37 3 3 1 906.33 1179.47 3.99 0.128 3.12 6 2 1 1753.24 2190.41 3.98 0.174 1.85 7 1 6 39.17 5.88 3.94 0.009 1.45 3 1 5 334.74 220.75 3.90 0.055 2.66 2 5 0 816.29 1070.25 3.90 0.122 2.91 5 0 2 624.57 843.40 3.86 0.108 2.23 6 0 4 168.01 278.39 3.86 0.062 1.77 1 5 8 337.27 226.37 3.85 0.056 1.92 2 1 0 4621.12 5556.25 3.76 0.277 5.42 6 3 1 202.18 119.75 3.72 0.041 1.80 0 0 4 58812.55 69853.62 3.46 0.982 4.77 4 3 6 289.58 201.53 3.31 0.053 1.99 6 0 0 7864.56 6680.55 3.25 0.304 1.91 5 3 3 1637.19 1362.04 3.22 0.137 2.01 1 1 8 1177.50 962.32 3.21 0.115 2.31 5 15 4 42.39 4.70 3.20 0.008 0.99 6 1 1 3521.48 4119.43 3.19 0.238 1.89 14 6 2 81.97 6.00 3.18 0.009 0.78 2 6 0 358.87 487.19 3.16 0.082 2.52 3 3 7 3161.49 3699.79 3.15 0.226 2.06 5 3 1 1457.99 1750.04 3.12 0.155 2.11 1 0 8 3742.85 4385.24 3.12 0.246 2.33 6 5 2 40.94 10.50 3.09 0.012 1.64 1 16 15 102.41 205.91 3.09 0.053 0.81 1 3 10 648.37 509.97 3.08 0.084 1.78 4 3 7 697.35 551.59 3.07 0.087 1.86 2 17 14 263.90 400.50 3.05 0.074 0.79 14 4 1 67.07 7.88 3.05 0.010 0.80 11 3 12 173.71 273.59 3.04 0.061 0.86 0 10 2 644.30 815.09 3.02 0.106 1.66 4 5 6 1955.90 1660.56 2.97 0.151 1.80 4 7 20 51.79 6.10 2.96 0.009 0.85 1 6 1 5466.69 4769.32 2.94 0.257 2.70 1 6 7 277.82 200.86 2.93 0.053 1.93 11 3 8 8.64 45.54 2.91 0.025 0.94 2 16 0 -3.02 36.46 2.89 0.022 1.04 8 6 16 74.18 161.10 2.87 0.047 0.87 3 6 9 418.51 320.27 2.87 0.066 1.55 2 1 9 1592.46 1347.71 2.87 0.136 1.97 Bond lengths and angles C1 - Distance Angles O1 1.4742 (0.0023) C2 1.5326 (0.0028) 113.06 (0.16) C1 - O1 C2 - Distance Angles C3 1.5336 (0.0025) C1 1.5326 (0.0028) 112.63 (0.16) C6 1.5396 (0.0026) 111.76 (0.16) 110.70 (0.16) C4 1.5624 (0.0025) 103.47 (0.14) 105.01 (0.16) 112.92 (0.16) C2 - C3 C1 C6 C3 - Distance Angles O2 1.4739 (0.0021) C2 1.5336 (0.0025) 113.28 (0.14) C3 - O2 C4 - Distance Angles C5 1.5300 (0.0030) C2 1.5624 (0.0025) 116.75 (0.17) C4 - C5 C5 - Distance Angles C4 1.5300 (0.0030) C5 - C6 - Distance Angles C7 1.5193 (0.0031) C2 1.5396 (0.0026) 115.05 (0.16) C6 - C7 C7 - Distance Angles C8 1.5149 (0.0029) C6 1.5193 (0.0031) 114.95 (0.20) C7 - C8 C8 - Distance Angles C7 1.5149 (0.0029) C9 1.5269 (0.0042) 112.68 (0.22) C8 - C7 C9 - Distance Angles C8 1.5269 (0.0042) C9 - N1 - Distance Angles P2 1.5947 (0.0015) P1 1.5986 (0.0015) 111.39 (0.09) N1 - P2 N2 - Distance Angles P3 1.5813 (0.0016) P2 1.5912 (0.0016) 118.20 (0.10) N2 - P3 N3 - Distance Angles P3 1.5803 (0.0016) P1 1.5922 (0.0016) 118.17 (0.10) N3 - P3 O1 - Distance Angles C1 1.4742 (0.0023) P1 1.5642 (0.0015) 120.68 (0.12) O1 - C1 O2 - Distance Angles C3 1.4739 (0.0022) P2 1.5682 (0.0013) 120.80 (0.11) O2 - C3 P1 - Distance Angles O1 1.5642 (0.0015) N3 1.5922 (0.0016) 107.52 (0.08) N1 1.5986 (0.0015) 111.20 (0.08) 117.08 (0.08) Cl1 1.9939 (0.0007) 105.45 (0.06) 107.95 (0.06) 106.99 (0.06) P2 2.6378 (0.0006) 100.74 (0.05) 91.79 (0.06) 34.26 (0.05) 140.14 (0.03) P1 - O1 N3 N1 Cl1 P2 - Distance Angles O2 1.5682 (0.0013) N2 1.5912 (0.0016) 107.18 (0.08) N1 1.5947 (0.0015) 111.48 (0.08) 116.97 (0.08) Cl2 1.9956 (0.0006) 105.50 (0.05) 108.16 (0.06) 106.92 (0.06) P1 2.6378 (0.0006) 100.55 (0.05) 91.77 (0.06) 34.36 (0.05) 140.26 (0.03) P2 - O2 N2 N1 Cl2 P3 - Distance Angles N3 1.5803 (0.0016) N2 1.5813 (0.0016) 119.92 (0.08) Cl4 1.9945 (0.0007) 109.37 (0.07) 108.54 (0.07) Cl3 2.0066 (0.0007) 108.48 (0.07) 107.98 (0.07) 100.85 (0.03) P3 - N3 N2 Cl4 Cl1 - Distance Angles P1 1.9939 (0.0007) Cl1 - Cl2 - Distance Angles P2 1.9956 (0.0006) Cl2 - Cl3 - Distance Angles P3 2.0066 (0.0007) Cl3 - Cl4 - Distance Angles P3 1.9945 (0.0007) Cl4 - FMAP and GRID set by program FMAP 2 2 21 GRID -1.389 24 -2 1.389 1 2 R1 = 0.0381 for 4213 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.36 at 0.9767 0.0906 0.2820 [ 0.98 A from C9 ] Deepest hole -0.38 at 0.2743 0.0072 0.6314 [ 0.82 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2719 / 32400 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4767 0.4094 0.7180 1.00000 0.05 0.36 0.98 C9 1.03 H9B 1.10 C8 1.33 H8B Q2 1 0.4351 0.3189 0.7147 1.00000 0.05 0.30 0.67 H8B 0.83 C8 1.15 H8A 1.76 C7 Q3 1 0.2359 0.1410 0.5010 1.00000 0.05 0.26 0.69 N2 0.93 P2 1.91 P3 2.08 N1 Q4 1 0.5143 0.1071 0.7296 1.00000 0.05 0.24 1.30 H6B 1.54 H1B 1.98 C6 1.98 C1 Q5 1 0.6147 0.1282 0.6203 1.00000 0.05 0.23 0.75 C4 0.83 C2 1.36 H4A 1.46 H4B Q6 1 0.4633 0.1719 0.5293 1.00000 0.05 0.23 0.74 O2 0.75 C3 1.37 H3B 1.40 H3A Q7 1 0.3188 0.0668 0.4977 1.00000 0.05 0.23 0.60 N1 1.04 P2 1.97 P1 2.23 N2 Q8 1 0.2061 0.0480 0.5950 1.00000 0.05 0.22 0.62 N3 1.01 P1 1.81 P3 2.13 O1 Q9 1 0.1989 0.0630 0.6083 1.00000 0.05 0.22 0.50 N3 1.26 P1 1.69 P3 2.10 O1 Q10 1 0.1631 0.1421 0.4871 1.00000 0.05 0.21 0.55 N2 1.63 P3 1.74 P2 2.55 H7B Q11 1 0.1150 0.0613 0.5811 1.00000 0.05 0.20 0.72 N3 1.14 P3 2.07 P1 2.23 CL4 Q12 1 0.3585 0.0508 0.5209 1.00000 0.05 0.20 0.38 N1 1.51 P2 1.65 P1 2.33 O2 Q13 1 0.5413 0.2042 0.5280 1.00000 0.05 0.20 0.41 H3A 0.82 C3 1.56 H3B 1.62 O2 Q14 1 0.5243 0.1694 0.6404 1.00000 0.05 0.19 0.72 C2 0.83 C6 1.50 H6B 1.50 H6A Q15 1 0.3236 0.0088 0.5015 1.00000 0.05 0.19 0.56 N1 1.77 P1 2.02 P2 2.41 H4A Q16 1 0.1643 0.0789 0.5942 1.00000 0.05 0.19 0.52 N3 1.15 P3 1.69 P1 2.24 N2 Q17 1 0.5532 0.1977 0.5427 1.00000 0.05 0.19 0.40 H3A 0.73 C3 1.55 H3B 1.76 C2 Q18 1 0.4299 0.0548 0.6419 1.00000 0.05 0.19 0.70 O1 0.77 C1 1.43 H1A 1.45 H1B Q19 1 0.7399 0.0990 0.5378 1.00000 0.05 0.18 1.16 H4A 1.84 C4 1.84 H4B 2.34 H3B Q20 1 0.3769 0.1631 0.5386 1.00000 0.05 0.17 0.52 O2 1.31 P2 1.67 C3 2.13 H3B Shortest distances between peaks (including symmetry equivalents) 13 17 0.33 8 9 0.37 9 16 0.55 11 16 0.68 7 12 0.69 8 16 0.71 3 10 0.88 12 15 0.89 7 15 0.98 6 20 1.02 6 13 1.05 9 11 1.09 8 11 1.10 6 17 1.15 5 14 1.30 3 7 1.57 1 2 1.60 3 20 1.81 7 20 1.92 12 20 1.93 14 17 1.95 4 14 2.00 5 17 2.01 13 20 2.02 15 19 2.10 17 20 2.10 3 12 2.10 4 18 2.12 5 19 2.19 7 10 2.20 14 18 2.21 3 16 2.22 13 14 2.23 6 14 2.23 8 12 2.25 7 8 2.28 10 16 2.30 10 11 2.32 8 15 2.33 5 13 2.33 6 12 2.37 4 5 2.40 3 8 2.41 3 15 2.44 12 18 2.45 3 11 2.46 3 9 2.47 9 12 2.48 5 18 2.49 6 7 2.50 7 9 2.52 7 16 2.56 5 6 2.56 14 20 2.57 8 10 2.64 9 15 2.65 10 20 2.66 12 16 2.67 9 10 2.70 3 6 2.71 17 19 2.71 8 18 2.72 9 18 2.73 18 20 2.75 15 20 2.76 10 12 2.79 15 16 2.80 7 11 2.83 13 19 2.89 10 15 2.92 6 18 2.94 7 19 2.95 10 13 2.96 8 20 2.96 9 20 2.96 11 15 2.97 12 19 2.98 Time profile in seconds ----------------------- 0.04: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.01: 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 0.01: Analyse other restraints etc. 15.20: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.64: Structure factors and derivatives 1.95: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.40: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.07: Merge reflections for Fourier and .fcf 0.12: Fourier summations 0.08: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0656 finished at 20:20:28 Total CPU time: 20.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++