+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2006src0701 started at 21:48:05 on 02-Jun-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2006src0701 in P-1 CELL 0.71073 8.0334 10.0791 11.1829 97.451 111.006 103.992 ZERR 2.00 0.0001 0.0002 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H N O P CL UNIT 14 28 6 4 6 8 V = 796.48 F(000) = 412.0 Mu = 1.04 mm-1 Cell Wt = 813.84 Rho = 1.697 MERG 2 OMIT -3.00 55.00 OMIT 1 0 0 OMIT -1 3 0 OMIT -1 -2 2 FMAP 2 PLAN 20 SIZE 0.05 0.20 0.38 ACTA BOND WGHT 0.03030 0.51810 L.S. 4 TEMP -153.00 FVAR 0.80149 MOLE 1 C1 1 0.067025 0.492872 0.663481 11.00000 0.01056 0.02041 = 0.01486 0.00620 0.00394 0.00253 AFIX 23 H1A 2 -0.031787 0.424161 0.582997 11.00000 -1.20000 H1B 2 0.026574 0.576974 0.676394 11.00000 -1.20000 AFIX 0 C2 1 0.089794 0.427707 0.782295 11.00000 0.01175 0.01164 = 0.01299 0.00350 0.00401 0.00299 C3 1 0.247238 0.534508 0.904653 11.00000 0.01422 0.01640 = 0.01447 0.00375 0.00552 0.00237 AFIX 23 H3A 2 0.207248 0.617396 0.923880 11.00000 -1.20000 H3B 2 0.269169 0.491371 0.981295 11.00000 -1.20000 AFIX 0 C4 1 -0.091966 0.406617 0.805691 11.00000 0.01578 0.01821 = 0.01939 0.00579 0.00853 0.00495 AFIX 23 H4A 2 -0.076690 0.366697 0.883901 11.00000 -1.20000 H4B 2 -0.107919 0.500007 0.826667 11.00000 -1.20000 AFIX 0 C5 1 -0.270824 0.311169 0.690484 11.00000 0.01485 0.03257 = 0.02523 0.00836 0.00663 0.00010 AFIX 137 H5A 2 -0.291483 0.351815 0.613398 11.00000 -1.50000 H5B 2 -0.377828 0.302678 0.714964 11.00000 -1.50000 H5C 2 -0.257922 0.217773 0.669170 11.00000 -1.50000 AFIX 0 C6 1 0.136034 0.289362 0.756694 11.00000 0.01901 0.01332 = 0.02617 0.00452 0.01119 0.00448 AFIX 23 H6A 2 0.044766 0.231511 0.668216 11.00000 -1.20000 H6B 2 0.262134 0.312727 0.755161 11.00000 -1.20000 AFIX 0 C7 1 0.132999 0.201004 0.857202 11.00000 0.02390 0.01651 = 0.03974 0.01412 0.01102 0.00690 AFIX 137 H7A 2 0.215302 0.259134 0.946185 11.00000 -1.50000 H7B 2 0.177147 0.121273 0.838953 11.00000 -1.50000 H7C 2 0.004599 0.165824 0.851054 11.00000 -1.50000 AFIX 0 N1 3 0.600495 0.644130 0.743508 11.00000 0.01552 0.01274 = 0.03151 0.00677 0.01239 0.00648 N2 3 0.655911 0.913785 0.712849 11.00000 0.01999 0.01595 = 0.03172 0.01144 0.01715 0.00912 N3 3 0.376725 0.791575 0.783919 11.00000 0.01671 0.01339 = 0.02846 0.00558 0.01377 0.00532 O1 4 0.243244 0.533538 0.645532 11.00000 0.01375 0.01644 = 0.01439 0.00373 0.00623 0.00160 O2 4 0.423376 0.581105 0.887492 11.00000 0.01241 0.01839 = 0.01638 0.00677 0.00254 0.00086 P1 5 0.415706 0.643712 0.764987 11.00000 0.01164 0.01132 = 0.01623 0.00385 0.00542 0.00324 P2 5 0.719717 0.776946 0.717220 11.00000 0.01335 0.01490 = 0.01911 0.00575 0.00882 0.00663 P3 5 0.483490 0.921747 0.747999 11.00000 0.01305 0.01167 = 0.01591 0.00355 0.00631 0.00532 CL1 6 0.985396 0.830159 0.849679 11.00000 0.01423 0.02004 = 0.02832 0.00690 0.00463 0.00406 CL2 6 0.748311 0.719301 0.549945 11.00000 0.03369 0.04194 = 0.02151 0.00977 0.01572 0.02426 CL3 6 0.569658 1.092626 0.894287 11.00000 0.02589 0.01556 = 0.01934 -0.00102 0.00817 0.00347 CL4 6 0.303862 0.975796 0.600111 11.00000 0.02427 0.02709 = 0.02099 0.00702 0.00203 0.01318 HKLF 4 Covalent radii and connectivity table for 2006src0701 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - O1 C2 C2 - C1 C3 C4 C6 C3 - O2 C2 C4 - C5 C2 C5 - C4 C6 - C7 C2 C7 - C6 N1 - P2 P1 N2 - P2 P3 N3 - P3 P1 O1 - C1 P1 O2 - C3 P1 P1 - O2 O1 N1 N3 P2 - N1 N2 Cl2 Cl1 P3 - N3 N2 Cl3 Cl4 Cl1 - P2 Cl2 - P2 Cl3 - P3 Cl4 - P3 16286 Reflections read, of which 16 rejected -10 =< h =< 10, -13 =< k =< 13, -14 =< l =< 14, Max. 2-theta = 54.98 0 Systematic absence violations 0 Inconsistent equivalents 3645 Unique reflections, of which 0 suppressed R(int) = 0.0254 R(sigma) = 0.0221 Friedel opposites merged Maximum memory for data reduction = 1701 / 36728 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 = 2178 / 218440 wR2 = 0.0677 before cycle 1 for 3645 data and 174 / 174 parameters GooF = S = 1.089; Restrained GooF = 1.089 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0303 * P )^2 + 0.52 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80146 0.00097 -0.026 OSF Mean shift/esd = 0.005 Maximum = -0.027 for U22 P3 Max. shift = 0.000 A for H5A Max. dU = 0.000 for C4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2178 / 218440 wR2 = 0.0678 before cycle 2 for 3645 data and 174 / 174 parameters GooF = S = 1.090; Restrained GooF = 1.090 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0303 * P )^2 + 0.52 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80145 0.00097 -0.011 OSF Mean shift/esd = 0.002 Maximum = -0.011 for OSF Max. shift = 0.000 A for H5A Max. dU = 0.000 for C4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2178 / 218440 wR2 = 0.0678 before cycle 3 for 3645 data and 174 / 174 parameters GooF = S = 1.089; Restrained GooF = 1.089 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0303 * P )^2 + 0.52 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80145 0.00097 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H7B Max. dU = 0.000 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2178 / 218440 wR2 = 0.0678 before cycle 4 for 3645 data and 174 / 174 parameters GooF = S = 1.090; Restrained GooF = 1.090 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0303 * P )^2 + 0.52 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80145 0.00097 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y Cl3 Max. shift = 0.000 A for N1 Max. dU = 0.000 for O1 Largest correlation matrix elements 0.561 U13 N2 / U33 N2 0.533 U13 P2 / U33 P2 0.505 U13 P1 / U33 P1 0.556 U13 Cl2 / U33 Cl2 0.521 U12 Cl2 / U11 Cl2 0.504 U13 C6 / U33 C6 0.552 U13 N2 / U11 N2 0.519 U13 N1 / U33 N1 0.503 U13 C4 / U33 C4 0.547 U13 N3 / U33 N3 0.517 U13 N3 / U11 N3 0.500 U13 N1 / U11 N1 0.544 U12 Cl2 / U22 Cl2 0.512 U13 P2 / U11 P2 0.533 U13 Cl2 / U11 Cl2 0.510 U13 P3 / U33 P3 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A -0.0318 0.4242 0.5830 23 0.990 0.000 C1 O1 C2 H1B 0.0266 0.5770 0.6764 23 0.990 0.000 C1 O1 C2 H3A 0.2072 0.6174 0.9239 23 0.990 0.000 C3 O2 C2 H3B 0.2692 0.4914 0.9813 23 0.990 0.000 C3 O2 C2 H4A -0.0767 0.3667 0.8839 23 0.990 0.000 C4 C5 C2 H4B -0.1079 0.5000 0.8267 23 0.990 0.000 C4 C5 C2 H5A -0.2915 0.3518 0.6134 137 0.980 0.000 C5 C4 H5A H5B -0.3778 0.3027 0.7150 137 0.980 0.000 C5 C4 H5A H5C -0.2579 0.2178 0.6692 137 0.980 0.000 C5 C4 H5A H6A 0.0448 0.2315 0.6682 23 0.990 0.000 C6 C7 C2 H6B 0.2621 0.3127 0.7552 23 0.990 0.000 C6 C7 C2 H7A 0.2153 0.2591 0.9462 137 0.980 0.000 C7 C6 H7A H7B 0.1771 0.1213 0.8390 137 0.980 0.000 C7 C6 H7A H7C 0.0046 0.1658 0.8511 137 0.980 0.000 C7 C6 H7A 2006src0701 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.06702 0.49287 0.66348 1.00000 0.01056 0.02041 0.01485 0.00620 0.00394 0.00253 0.01587 0.00388 0.00022 0.00018 0.00016 0.00000 0.00069 0.00083 0.00074 0.00063 0.00060 0.00061 0.00032 H1A -0.03179 0.42416 0.58300 1.00000 0.01905 0.00000 0.00000 H1B 0.02657 0.57697 0.67639 1.00000 0.01905 0.00000 0.00000 C2 0.08979 0.42771 0.78230 1.00000 0.01175 0.01164 0.01299 0.00350 0.00401 0.00299 0.01249 0.00364 0.00021 0.00016 0.00015 0.00000 0.00069 0.00073 0.00071 0.00057 0.00059 0.00057 0.00030 C3 0.24724 0.53451 0.90465 1.00000 0.01421 0.01640 0.01447 0.00374 0.00552 0.00237 0.01557 0.00379 0.00022 0.00017 0.00016 0.00000 0.00073 0.00080 0.00075 0.00061 0.00062 0.00061 0.00032 H3A 0.20725 0.61740 0.92388 1.00000 0.01869 0.00000 0.00000 H3B 0.26917 0.49137 0.98129 1.00000 0.01869 0.00000 0.00000 C4 -0.09197 0.40662 0.80569 1.00000 0.01577 0.01820 0.01938 0.00579 0.00853 0.00495 0.01730 0.00400 0.00022 0.00018 0.00017 0.00000 0.00076 0.00083 0.00080 0.00065 0.00066 0.00063 0.00033 H4A -0.07669 0.36670 0.88390 1.00000 0.02076 0.00000 0.00000 H4B -0.10792 0.50001 0.82667 1.00000 0.02076 0.00000 0.00000 C5 -0.27082 0.31117 0.69048 1.00000 0.01485 0.03257 0.02523 0.00836 0.00663 0.00010 0.02592 0.00438 0.00024 0.00021 0.00019 0.00000 0.00080 0.00104 0.00092 0.00078 0.00072 0.00072 0.00040 H5A -0.29148 0.35181 0.61340 1.00000 0.03887 0.00000 0.00000 H5B -0.37783 0.30268 0.71496 1.00000 0.03887 0.00000 0.00000 H5C -0.25792 0.21777 0.66917 1.00000 0.03887 0.00000 0.00000 C6 0.13603 0.28936 0.75669 1.00000 0.01900 0.01332 0.02617 0.00452 0.01118 0.00448 0.01902 0.00422 0.00024 0.00017 0.00018 0.00000 0.00079 0.00080 0.00088 0.00066 0.00070 0.00063 0.00034 H6A 0.04476 0.23151 0.66822 1.00000 0.02282 0.00000 0.00000 H6B 0.26213 0.31273 0.75516 1.00000 0.02282 0.00000 0.00000 C7 0.13300 0.20100 0.85720 1.00000 0.02389 0.01651 0.03974 0.01412 0.01102 0.00690 0.02641 0.00476 0.00026 0.00019 0.00021 0.00000 0.00090 0.00088 0.00109 0.00078 0.00083 0.00071 0.00041 H7A 0.21531 0.25913 0.94618 1.00000 0.03961 0.00000 0.00000 H7B 0.17715 0.12127 0.83895 1.00000 0.03961 0.00000 0.00000 H7C 0.00460 0.16583 0.85106 1.00000 0.03961 0.00000 0.00000 N1 0.60049 0.64413 0.74351 1.00000 0.01551 0.01273 0.03151 0.00676 0.01239 0.00648 0.01852 0.00352 0.00019 0.00015 0.00015 0.00000 0.00066 0.00068 0.00080 0.00058 0.00061 0.00054 0.00030 N2 0.65591 0.91379 0.71285 1.00000 0.01999 0.01594 0.03171 0.01144 0.01715 0.00912 0.01931 0.00363 0.00020 0.00015 0.00015 0.00000 0.00071 0.00073 0.00082 0.00061 0.00065 0.00058 0.00031 N3 0.37672 0.79158 0.78392 1.00000 0.01671 0.01338 0.02846 0.00558 0.01376 0.00532 0.01796 0.00346 0.00019 0.00015 0.00015 0.00000 0.00066 0.00069 0.00078 0.00058 0.00061 0.00054 0.00030 O1 0.24324 0.53354 0.64553 1.00000 0.01374 0.01644 0.01439 0.00372 0.00623 0.00160 0.01529 0.00263 0.00015 0.00012 0.00011 0.00000 0.00053 0.00058 0.00054 0.00044 0.00045 0.00044 0.00024 O2 0.42337 0.58111 0.88749 1.00000 0.01240 0.01839 0.01637 0.00677 0.00254 0.00086 0.01719 0.00268 0.00015 0.00012 0.00011 0.00000 0.00053 0.00060 0.00057 0.00046 0.00045 0.00045 0.00025 P1 0.41571 0.64371 0.76499 1.00000 0.01164 0.01131 0.01622 0.00385 0.00542 0.00324 0.01313 0.00095 0.00005 0.00004 0.00004 0.00000 0.00019 0.00020 0.00020 0.00015 0.00016 0.00015 0.00010 P2 0.71972 0.77695 0.71722 1.00000 0.01335 0.01490 0.01911 0.00575 0.00881 0.00663 0.01452 0.00101 0.00006 0.00004 0.00004 0.00000 0.00019 0.00021 0.00021 0.00016 0.00016 0.00016 0.00010 P3 0.48349 0.92175 0.74800 1.00000 0.01305 0.01166 0.01591 0.00355 0.00631 0.00532 0.01310 0.00097 0.00006 0.00004 0.00004 0.00000 0.00019 0.00020 0.00020 0.00015 0.00016 0.00015 0.00010 Cl1 0.98540 0.83016 0.84968 1.00000 0.01423 0.02003 0.02831 0.00690 0.00463 0.00406 0.02218 0.00099 0.00005 0.00004 0.00004 0.00000 0.00019 0.00021 0.00023 0.00017 0.00016 0.00015 0.00010 Cl2 0.74831 0.71930 0.54994 1.00000 0.03369 0.04194 0.02151 0.00977 0.01571 0.02426 0.02840 0.00123 0.00007 0.00005 0.00004 0.00000 0.00024 0.00028 0.00022 0.00019 0.00019 0.00021 0.00012 Cl3 0.56966 1.09263 0.89429 1.00000 0.02589 0.01556 0.01934 -0.00102 0.00817 0.00347 0.02166 0.00098 0.00006 0.00004 0.00004 0.00000 0.00021 0.00020 0.00020 0.00015 0.00017 0.00016 0.00010 Cl4 0.30386 0.97580 0.60011 1.00000 0.02426 0.02708 0.02099 0.00702 0.00203 0.01318 0.02510 0.00106 0.00006 0.00005 0.00004 0.00000 0.00022 0.00024 0.00021 0.00017 0.00017 0.00018 0.00011 Final Structure Factor Calculation for 2006src0701 in P-1 Total number of l.s. parameters = 174 Maximum vector length = 511 Memory required = 2004 / 25039 wR2 = 0.0678 before cycle 5 for 3645 data and 0 / 174 parameters GooF = S = 1.090; Restrained GooF = 1.090 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0303 * P )^2 + 0.52 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0262 for 3233 Fo > 4sig(Fo) and 0.0318 for all 3645 data wR2 = 0.0678, GooF = S = 1.090, Restrained GooF = 1.090 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0233 0.0138 0.0105 C1 0.0148 0.0116 0.0111 C2 0.0192 0.0144 0.0131 C3 0.0200 0.0178 0.0141 C4 0.0398 0.0245 0.0135 C5 0.0266 0.0173 0.0132 C6 0.0434 0.0239 0.0119 C7 0.0315 0.0134 0.0106 N1 0.0333 0.0124 0.0122 N2 0.0290 0.0130 0.0118 N3 0.0199 0.0145 0.0115 O1 0.0265 0.0138 0.0113 O2 0.0166 0.0120 0.0108 P1 0.0195 0.0140 0.0100 P2 0.0159 0.0133 0.0100 P3 0.0327 0.0197 0.0141 Cl1 0.0484 0.0224 0.0144 Cl2 0.0281 0.0240 0.0128 Cl3 0.0360 0.0261 0.0132 Cl4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.021 0.040 0.061 0.083 0.106 0.135 0.173 0.223 0.300 1.000 Number in group 374. 365. 356. 374. 362. 365. 358. 363. 364. 364. GooF 1.052 1.041 1.176 1.058 1.132 1.135 0.960 0.959 0.974 1.350 K 1.054 0.954 0.948 0.954 0.979 0.983 1.006 1.017 1.017 0.976 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.64 inf Number in group 367. 375. 351. 369. 365. 366. 360. 363. 362. 367. GooF 0.958 0.910 0.888 0.816 0.850 0.965 0.925 0.899 1.005 2.078 K 0.974 0.990 1.001 1.000 1.017 1.025 1.017 1.009 0.998 0.953 R1 0.070 0.049 0.039 0.030 0.030 0.029 0.023 0.019 0.018 0.035 Recommended weighting scheme: WGHT 0.0303 0.5175 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) 0 0 2 11364.89 14468.13 6.43 1.000 5.07 -1 2 1 8719.75 11325.72 6.40 0.885 4.30 -2 5 0 66.64 34.62 5.72 0.049 1.95 -1 0 2 120.11 199.70 5.72 0.117 5.26 1 -2 1 6510.75 8030.89 5.65 0.745 4.20 -4 0 4 253.15 185.73 5.04 0.113 1.85 1 1 0 4574.60 5977.68 4.94 0.643 5.00 -2 1 2 10039.63 11928.23 4.94 0.908 3.64 -3 -1 3 12.19 1.85 4.75 0.011 2.31 -1 -2 3 215.21 159.43 4.57 0.105 3.06 -1 4 2 507.34 406.86 4.50 0.168 2.15 -2 -3 3 26.58 11.18 4.40 0.028 2.19 -1 4 1 88.76 129.08 4.38 0.094 2.37 -2 -4 2 236.75 180.50 4.28 0.112 1.88 1 -1 1 6412.45 7758.35 4.25 0.732 5.16 2 -3 2 199.76 261.48 4.24 0.134 2.37 -2 1 4 651.11 538.64 4.19 0.193 2.52 1 -4 1 17.85 35.94 4.11 0.050 2.49 -1 1 3 8304.38 9572.04 4.05 0.813 3.33 -5 2 2 33.03 17.44 4.03 0.035 1.60 -4 0 2 1175.69 1001.97 4.00 0.263 1.95 -3 4 1 45.16 27.00 3.90 0.043 2.04 -3 0 4 42.59 66.71 3.83 0.068 2.25 0 -3 3 134.84 177.78 3.79 0.111 2.65 -2 0 1 4681.88 5352.54 3.73 0.608 3.89 0 3 1 3740.48 4286.43 3.73 0.544 2.84 0 -2 6 12.20 26.71 3.72 0.043 1.73 0 1 0 11.74 25.19 3.68 0.042 9.50 -4 1 1 323.29 393.45 3.65 0.165 1.96 -3 1 2 14.54 5.36 3.59 0.019 2.65 -1 -2 5 5.60 0.38 3.53 0.005 2.13 0 0 1 -0.99 4.03 3.48 0.017 10.14 -1 -1 2 3693.59 4313.68 3.47 0.546 4.64 5 -1 5 5.94 1.23 3.47 0.009 1.02 2 -4 2 1.66 9.61 3.46 0.026 2.10 -5 1 3 49.34 31.84 3.40 0.047 1.60 -3 -3 3 319.94 385.00 3.37 0.163 1.82 -2 4 3 9985.86 11212.05 3.33 0.880 1.95 -1 -4 4 176.26 219.80 3.29 0.123 1.94 -2 0 2 2160.61 2445.66 3.29 0.411 3.71 -1 3 2 65.63 90.40 3.29 0.079 2.69 -4 8 10 14.86 56.80 3.22 0.063 0.78 1 2 4 1002.15 877.13 3.21 0.246 1.76 1 1 1 3669.85 4130.91 3.19 0.534 3.90 -1 3 4 175.79 136.17 3.18 0.097 1.95 -3 1 0 1023.42 1166.96 3.18 0.284 2.49 -4 9 2 347.63 289.01 3.17 0.141 1.04 0 -3 6 1052.18 920.80 3.17 0.252 1.66 4 2 4 61.85 43.20 3.10 0.055 1.11 -2 3 2 0.74 6.05 3.09 0.020 2.61 Bond lengths and angles C1 - Distance Angles O1 1.4686 (0.0019) C2 1.5299 (0.0022) 111.38 (0.12) C1 - O1 C2 - Distance Angles C1 1.5299 (0.0022) C3 1.5328 (0.0021) 108.25 (0.13) C4 1.5440 (0.0022) 108.13 (0.13) 106.54 (0.13) C6 1.5451 (0.0022) 109.31 (0.13) 111.24 (0.13) 113.19 (0.13) C2 - C1 C3 C4 C3 - Distance Angles O2 1.4684 (0.0019) C2 1.5328 (0.0021) 112.38 (0.13) C3 - O2 C4 - Distance Angles C5 1.5274 (0.0024) C2 1.5440 (0.0022) 115.34 (0.14) C4 - C5 C5 - Distance Angles C4 1.5274 (0.0024) C5 - C6 - Distance Angles C7 1.5251 (0.0025) C2 1.5451 (0.0022) 115.13 (0.15) C6 - C7 C7 - Distance Angles C6 1.5251 (0.0025) C7 - N1 - Distance Angles P2 1.5747 (0.0015) P1 1.5856 (0.0014) 121.30 (0.09) N1 - P2 N2 - Distance Angles P2 1.5839 (0.0014) P3 1.5860 (0.0014) 119.88 (0.09) N2 - P2 N3 - Distance Angles P3 1.5678 (0.0014) P1 1.5985 (0.0014) 121.87 (0.09) N3 - P3 O1 - Distance Angles C1 1.4686 (0.0019) P1 1.5753 (0.0011) 115.90 (0.10) O1 - C1 O2 - Distance Angles C3 1.4684 (0.0019) P1 1.5688 (0.0012) 117.20 (0.10) O2 - C3 P1 - Distance Angles O2 1.5688 (0.0012) O1 1.5753 (0.0012) 104.33 (0.06) N1 1.5856 (0.0014) 107.74 (0.07) 108.26 (0.07) N3 1.5985 (0.0014) 109.52 (0.07) 109.60 (0.07) 116.66 (0.08) P1 - O2 O1 N1 P2 - Distance Angles N1 1.5747 (0.0015) N2 1.5839 (0.0014) 119.81 (0.08) Cl2 1.9951 (0.0006) 108.97 (0.06) 108.16 (0.06) Cl1 2.0027 (0.0006) 108.32 (0.06) 108.83 (0.06) 101.13 (0.03) P2 - N1 N2 Cl2 P3 - Distance Angles N3 1.5678 (0.0015) N2 1.5860 (0.0014) 118.88 (0.07) Cl3 2.0007 (0.0006) 109.12 (0.06) 108.29 (0.06) Cl4 2.0043 (0.0006) 110.43 (0.06) 107.85 (0.06) 100.72 (0.02) P3 - N3 N2 Cl3 Cl1 - Distance Angles P2 2.0027 (0.0006) Cl1 - Cl2 - Distance Angles P2 1.9951 (0.0006) Cl2 - Cl3 - Distance Angles P3 2.0007 (0.0006) Cl3 - Cl4 - Distance Angles P3 2.0043 (0.0006) Cl4 - FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.0317 for 3645 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.0235 0.7661 0.7639 [ 1.26 A from CL1 ] Deepest hole -0.49 at 0.4315 0.5735 0.7587 [ 0.75 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 2118 / 22234 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.0235 0.7661 0.7639 1.00000 0.05 0.29 1.26 CL1 2.04 H1B 2.34 P2 2.50 CL2 Q2 1 0.3373 0.8852 0.5170 1.00000 0.05 0.28 1.36 CL4 2.00 H5C 2.36 P3 2.50 H5A Q3 1 -0.3775 0.1942 0.4980 1.00000 0.05 0.24 1.72 H5A 1.76 H5C 2.07 C5 2.23 CL4 Q4 1 0.2493 0.8338 0.5435 1.00000 0.05 0.24 1.38 CL4 2.27 P3 2.40 H5C 2.54 H6A Q5 1 -0.1032 0.0375 0.9327 1.00000 0.05 0.24 1.89 H7C 2.34 CL1 2.44 N2 2.54 CL1 Q6 1 -0.4085 0.4080 0.7067 1.00000 0.05 0.24 1.15 H5B 1.68 C5 1.76 H5A 2.18 H4B Q7 1 0.3660 0.2681 1.0359 1.00000 0.05 0.23 1.24 H7A 1.81 O2 2.08 C7 2.18 P1 Q8 1 0.5795 0.6394 1.0145 1.00000 0.05 0.23 1.44 O2 1.58 H7A 1.99 H3B 2.28 C7 Q9 1 0.3403 0.3420 0.9194 1.00000 0.05 0.23 1.29 H7A 1.67 H6B 1.74 C7 1.86 C6 Q10 1 -0.4471 0.2610 0.4674 1.00000 0.05 0.23 1.63 H5A 2.28 N2 2.30 C5 2.31 P2 Q11 1 0.3049 0.2991 1.0719 1.00000 0.05 0.22 1.28 H7A 1.88 N1 2.07 O2 2.21 P1 Q12 1 0.2939 0.4406 0.9653 1.00000 0.05 0.22 0.62 H3B 1.28 C3 1.74 H7A 2.02 O2 Q13 1 0.2368 0.2020 0.9729 1.00000 0.05 0.21 0.71 H7A 1.26 C7 1.45 H7B 1.79 H7C Q14 1 -0.3335 0.4164 0.6323 1.00000 0.05 0.21 0.84 H5A 1.42 C5 1.62 H5B 2.16 H4B Q15 1 0.4195 0.8953 0.6007 1.00000 0.05 0.21 1.37 CL4 1.50 P3 1.81 N2 2.51 N3 Q16 1 -0.1813 0.1232 0.5995 1.00000 0.05 0.21 1.53 H5C 1.70 H6A 2.08 CL4 2.41 C5 Q17 1 -0.4995 0.2281 0.5203 1.00000 0.05 0.21 1.69 H5A 1.99 H5B 2.01 C5 2.09 H5C Q18 1 -0.0031 0.4180 0.7859 1.00000 0.05 0.21 0.75 C2 0.81 C4 1.45 H4B 1.51 H4A Q19 1 0.6792 1.1263 1.0547 1.00000 0.05 0.20 1.64 CL3 2.13 N3 2.42 CL1 2.47 H3A Q20 1 0.0045 0.7371 0.6222 1.00000 0.05 0.20 1.82 H1B 1.87 CL2 2.67 CL1 2.69 C1 Shortest distances between peaks (including symmetry equivalents) 8 9 0.75 7 11 0.83 10 17 0.89 2 15 0.91 2 4 0.93 2 3 0.95 3 10 0.99 7 13 1.02 6 14 1.19 3 17 1.21 3 15 1.21 7 8 1.22 11 13 1.23 4 15 1.23 9 12 1.25 3 4 1.34 8 12 1.42 2 16 1.42 1 20 1.52 7 9 1.56 8 11 1.64 4 16 1.65 9 13 1.75 10 15 1.76 8 13 1.85 2 10 1.89 9 11 1.91 3 16 1.94 11 12 1.97 14 17 1.98 10 14 2.01 2 17 2.04 4 10 2.07 15 17 2.09 7 12 2.12 5 5 2.17 15 16 2.31 6 17 2.34 12 13 2.36 1 19 2.39 3 14 2.40 12 18 2.44 4 20 2.47 8 12 2.48 4 17 2.54 14 18 2.59 5 13 2.67 8 8 2.71 6 10 2.76 5 19 2.80 5 13 2.88 16 17 2.89 10 16 2.89 9 12 2.92 8 9 2.95 9 18 2.96 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 0.00: 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. 3.05: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.91: Structure factors and derivatives 1.32: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.27: Solve l.s. equations 0.00: Generate HTAB table 0.01: Other dependent quantities, CIF, tables 0.10: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.07: Fourier summations 0.02: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2006src0701 finished at 21:48:14 Total CPU time: 5.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++