+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src1142 started at 14:27:36 on 29-Aug-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src1142 in P-1 CELL 0.71073 9.6107 13.1064 13.7556 95.945 108.667 103.670 ZERR 2.00 0.0003 0.0003 0.0004 0.002 0.001 0.002 LATT 1 SFAC C H N O P CL UNIT 35 73 20 16 12 1 V = 1564.51 F(000) = 748.0 Mu = 0.44 mm-1 Cell Wt = 1437.22 Rho = 1.525 MERG 2 OMIT -3.00 55.00 OMIT 1 -1 1 OMIT 1 1 0 OMIT -1 0 3 EQIV $1 -x, -y+1, -z FREE C18 C18_$1 FMAP 2 PLAN 30 SIZE 0.01 0.03 0.10 ACTA BOND WGHT 0.09350 11.47110 L.S. 4 TEMP -153.00 FVAR 0.65755 C1 1 0.783637 0.443570 0.363672 11.00000 0.03377 0.05051 = 0.04221 0.01799 0.00616 0.00338 AFIX 23 H1A 2 0.888250 0.473572 0.416532 11.00000 -1.20000 H1B 2 0.710695 0.464101 0.393350 11.00000 -1.20000 AFIX 0 C2 1 0.774253 0.489101 0.264275 11.00000 0.05784 0.05860 = 0.05027 0.02407 0.01574 -0.00620 AFIX 23 H2A 2 0.795634 0.567821 0.281071 11.00000 -1.20000 H2B 2 0.853323 0.473484 0.238245 11.00000 -1.20000 AFIX 0 C3 1 0.618948 0.441946 0.180283 11.00000 0.05872 0.05884 = 0.04675 0.03100 0.01350 0.00585 AFIX 23 H3A 2 0.540530 0.462329 0.203986 11.00000 -1.20000 H3B 2 0.617486 0.470986 0.116443 11.00000 -1.20000 AFIX 0 C4 1 0.513661 -0.131228 0.198600 11.00000 0.20612 0.09241 = 0.23420 0.05679 0.12882 0.09629 AFIX 23 H4A 2 0.493837 -0.195038 0.230351 11.00000 -1.20000 H4B 2 0.625494 -0.106803 0.214002 11.00000 -1.20000 AFIX 0 C5 1 0.438758 -0.165691 0.085748 11.00000 0.11400 0.12264 = 0.15351 -0.05612 0.05274 0.03806 AFIX 23 H5A 2 0.377509 -0.241433 0.071533 11.00000 -1.20000 H5B 2 0.519727 -0.163743 0.055462 11.00000 -1.20000 AFIX 0 C6 1 0.337672 -0.106094 0.028474 11.00000 0.19246 0.07015 = 0.09512 -0.01564 0.06880 0.01420 AFIX 23 H6A 2 0.347688 -0.105839 -0.040931 11.00000 -1.20000 H6B 2 0.230559 -0.146226 0.016334 11.00000 -1.20000 AFIX 0 C7 1 0.021182 0.161190 0.263509 11.00000 0.02557 0.05558 = 0.03484 0.01175 0.01165 0.01025 AFIX 23 H7A 2 -0.015825 0.086583 0.223969 11.00000 -1.20000 H7B 2 -0.062168 0.195164 0.239095 11.00000 -1.20000 AFIX 0 C8 1 0.058932 0.160362 0.379457 11.00000 0.02672 0.04333 = 0.03557 0.01939 0.01527 0.01335 C9 1 0.195516 0.113738 0.419185 11.00000 0.03020 0.04755 = 0.04396 0.02164 0.01925 0.01664 AFIX 23 H9A 2 0.220518 0.112235 0.494559 11.00000 -1.20000 H9B 2 0.169090 0.039605 0.380642 11.00000 -1.20000 AFIX 0 C10 1 -0.083915 0.088933 0.392451 11.00000 0.03587 0.04456 = 0.04733 0.02215 0.02434 0.01401 AFIX 23 H10A 2 -0.173628 0.114916 0.360433 11.00000 -1.20000 H10B 2 -0.105981 0.014524 0.356027 11.00000 -1.20000 AFIX 0 C11 1 0.096668 0.272954 0.440592 11.00000 0.03252 0.04771 = 0.03638 0.01806 0.01807 0.01477 AFIX 23 H11A 2 0.189139 0.318799 0.433134 11.00000 -1.20000 H11B 2 0.010687 0.303319 0.411097 11.00000 -1.20000 AFIX 0 C12 1 -0.463894 0.341680 0.637166 11.00000 0.04974 0.19345 = 0.06842 0.00134 0.02346 0.06307 AFIX 23 H12A 2 -0.450940 0.336735 0.710718 11.00000 -1.20000 H12B 2 -0.575150 0.321189 0.596213 11.00000 -1.20000 AFIX 0 C13 1 -0.390925 0.457985 0.632097 11.00000 0.20642 0.17058 = 0.10720 0.07638 0.09988 0.15708 AFIX 23 H13A 2 -0.410263 0.463751 0.558013 11.00000 -1.20000 H13B 2 -0.440733 0.505368 0.660701 11.00000 -1.20000 AFIX 0 C14 1 -0.230040 0.493875 0.688803 11.00000 0.18140 0.08550 = 0.11038 0.05089 0.09050 0.07691 AFIX 23 H14A 2 -0.208258 0.487054 0.762835 11.00000 -1.20000 H14B 2 -0.188801 0.569981 0.686594 11.00000 -1.20000 AFIX 0 C15 1 0.097598 0.118721 0.923384 11.00000 0.06882 0.05946 = 0.06231 0.02764 0.01118 0.00218 AFIX 23 H15A 2 0.147188 0.083737 0.882229 11.00000 -1.20000 H15B 2 0.062886 0.068196 0.965302 11.00000 -1.20000 AFIX 0 C16 1 0.213478 0.220001 0.996399 11.00000 0.07101 0.07196 = 0.04623 0.02705 -0.00011 -0.01217 AFIX 23 H16A 2 0.167423 0.251485 1.042499 11.00000 -1.20000 H16B 2 0.304563 0.202185 1.041037 11.00000 -1.20000 AFIX 0 C17 1 0.261321 0.300394 0.932891 11.00000 0.05573 0.06431 = 0.06819 0.02665 -0.01365 -0.00859 AFIX 23 H17A 2 0.334580 0.366579 0.980983 11.00000 -1.20000 H17B 2 0.314174 0.270501 0.890902 11.00000 -1.20000 AFIX 0 N1 3 0.442093 0.283063 0.284860 11.00000 0.02998 0.03922 = 0.03902 0.01473 0.01760 0.01241 N2 3 0.569015 0.143821 0.212377 11.00000 0.04312 0.06657 = 0.05693 0.00451 0.02542 0.01837 N3 3 0.288468 0.071259 0.223824 11.00000 0.03162 0.04183 = 0.05122 0.00152 0.00958 0.00315 N4 3 0.746256 0.325515 0.338606 11.00000 0.02883 0.05976 = 0.04256 0.02224 0.01518 0.01186 N5 3 0.474766 -0.050201 0.250727 11.00000 0.09252 0.05878 = 0.09241 0.00521 0.01635 0.03527 AFIX 43 H5 2 0.477762 -0.050880 0.315264 11.00000 -1.20000 AFIX 0 N6 3 -0.154004 0.252086 0.546911 11.00000 0.04464 0.07685 = 0.03306 0.02169 0.01588 0.03850 N7 3 -0.144176 0.277431 0.746464 11.00000 0.05236 0.08600 = 0.03306 0.01757 0.01721 0.02529 N8 3 0.053091 0.187258 0.694352 11.00000 0.03488 0.10236 = 0.04329 0.04024 0.01630 0.03351 N9 3 -0.393368 0.264486 0.595037 11.00000 0.03148 0.13514 = 0.04614 0.00077 0.01052 0.02999 N10 3 -0.029718 0.142112 0.854935 11.00000 0.05128 0.05726 = 0.03461 0.01647 0.01125 -0.00573 O1 4 0.582192 0.325322 0.156020 11.00000 0.03905 0.07826 = 0.03300 0.01646 0.01510 0.00760 O2 4 0.360427 -0.005854 0.072416 11.00000 0.09962 0.10800 = 0.06044 -0.02739 0.00367 0.04995 O3 4 0.153869 0.218959 0.242372 11.00000 0.02829 0.05183 = 0.03383 0.01788 0.01253 0.01155 O4 4 0.326514 0.181247 0.402379 11.00000 0.02695 0.05236 = 0.03426 0.01973 0.01423 0.01457 O5 4 -0.058471 0.090958 0.502770 11.00000 0.03880 0.05882 = 0.05468 0.03272 0.02986 0.02387 O6 4 0.123524 0.273698 0.550385 11.00000 0.03636 0.05544 = 0.03967 0.01816 0.02049 0.01705 O7 4 -0.159178 0.427465 0.639924 11.00000 0.10951 0.07059 = 0.07783 0.01878 0.05697 0.02355 O8 4 0.136359 0.325369 0.866640 11.00000 0.05461 0.06463 = 0.05919 0.03249 0.00170 -0.00017 P1 5 0.309155 0.187162 0.284046 11.00000 0.02736 0.03923 = 0.03184 0.01014 0.01258 0.00887 P2 5 0.578578 0.263533 0.248483 11.00000 0.02834 0.04972 = 0.03368 0.01245 0.01563 0.01197 P3 5 0.423966 0.045403 0.192848 11.00000 0.04735 0.04766 = 0.05235 -0.00482 0.01213 0.01784 P4 5 -0.012892 0.203612 0.578261 11.00000 0.03332 0.06450 = 0.03959 0.02982 0.02046 0.02802 P5 5 -0.207782 0.301736 0.633594 11.00000 0.03339 0.06092 = 0.03292 0.01192 0.01299 0.01887 P6 5 -0.000957 0.232276 0.784192 11.00000 0.03409 0.06637 = 0.03100 0.02201 0.00741 0.00594 PART 1 C18 1 0.091646 0.540134 0.004895 10.33000 0.07135 0.06424 = 0.04998 -0.02831 0.04226 0.00675 AFIX 23 H18A 2 0.038412 0.465795 -0.034218 10.33000 -1.20000 H18B 2 0.048646 0.553708 0.059823 10.33000 -1.20000 AFIX 0 CL1 6 0.274118 0.553541 0.059369 10.33000 0.20336 0.10990 = 0.06924 0.01562 0.06018 0.06182 CL2 6 0.062050 0.622160 -0.073794 10.33000 0.21666 0.11609 = 0.10718 -0.03926 0.03952 0.02538 PART 0 H4N 2 0.759599 0.305629 0.386364 11.00000 0.06591 H9N 2 -0.431444 0.239870 0.532962 11.00000 0.07206 H10N 2 -0.139946 0.072668 0.804166 11.00000 0.13171 HKLF 4 Covalent radii and connectivity table for 2007src1142 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - N4 C2 C2 - C3 C1 C3 - O1 C2 C4 - N5 C5 C5 - C4 C6 C6 - O2 C5 C7 - O3 C8 C8 - C7 C11 C10 C9 C9 - O4 C8 C10 - O5 C8 C11 - O6 C8 C12 - N9 C13 C13 - C14 C12 C14 - C13 O7 C15 - N10 C16 C16 - C17 C15 C17 - O8 C16 N1 - P1 P2 N2 - P2 P3 N3 - P1 P3 N4 - C1 P2 N5 - C4 P3 N6 - P5 P4 N7 - P5 P6 N8 - P4 P6 N9 - C12 P5 N10 - C15 P6 O1 - C3 P2 O2 - C6 P3 O3 - C7 P1 O4 - C9 P1 O5 - C10 P4 O6 - C11 P4 O7 - C14 P5 O8 - C17 P6 P1 - N1 N3 O3 O4 P2 - N2 O1 N1 N4 P3 - O2 N2 N3 N5 P4 - N8 N6 O6 O5 P5 - N7 N6 O7 N9 P6 - N7 O8 N8 N10 C18_a - Cl2_a Cl1_a Cl1_a - C18_a Cl2_a - C18_a Operators for generating equivalent atoms: $1 -x, -y+1, -z 32823 Reflections read, of which 110 rejected -12 =< h =< 12, -17 =< k =< 16, -17 =< l =< 17, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -5 13 2 -0.13 0.07 7 1.19 7 4 3 -1.10 0.74 2 6.35 2 Inconsistent equivalents 7129 Unique reflections, of which 0 suppressed R(int) = 0.0519 R(sigma) = 0.0435 Friedel opposites merged Maximum memory for data reduction = 3716 / 71393 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. ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 35.00 34.66 H 73.00 73.32 N 20.00 20.00 O 16.00 16.00 P 12.00 12.00 CL 1.00 1.32 Least-squares cycle 1 Maximum vector length = 511 Memory required = 4872 / 527700 wR2 = 0.2806 before cycle 1 for 7129 data and 409 / 409 parameters GooF = S = 1.084; Restrained GooF = 1.084 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0935 * P )^2 + 11.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65776 0.00230 0.090 OSF Mean shift/esd = 0.027 Maximum = 0.142 for x H10N Max. shift = 0.020 A for H10N Max. dU =-0.005 for H10N Least-squares cycle 2 Maximum vector length = 511 Memory required = 4872 / 527700 wR2 = 0.2806 before cycle 2 for 7129 data and 409 / 409 parameters GooF = S = 1.084; Restrained GooF = 1.084 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0935 * P )^2 + 11.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65785 0.00230 0.040 OSF Mean shift/esd = 0.015 Maximum = 0.168 for x H10N Max. shift = 0.023 A for H10N Max. dU =-0.003 for H10N Least-squares cycle 3 Maximum vector length = 511 Memory required = 4872 / 527700 wR2 = 0.2806 before cycle 3 for 7129 data and 409 / 409 parameters GooF = S = 1.084; Restrained GooF = 1.084 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0935 * P )^2 + 11.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65787 0.00230 0.009 OSF Mean shift/esd = 0.006 Maximum = 0.121 for x H10N Max. shift = 0.016 A for H10N Max. dU =-0.002 for H10N Least-squares cycle 4 Maximum vector length = 511 Memory required = 4872 / 527700 wR2 = 0.2806 before cycle 4 for 7129 data and 409 / 409 parameters GooF = S = 1.084; Restrained GooF = 1.084 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0935 * P )^2 + 11.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65787 0.00230 0.001 OSF Mean shift/esd = 0.004 Maximum = 0.084 for x H10N Max. shift = 0.011 A for H10N Max. dU =-0.001 for H10N Largest correlation matrix elements 0.812 U12 C13 / U22 C13 0.682 U13 C14 / U11 C14 0.629 U13 C4 / U11 C4 0.808 U12 C13 / U11 C13 0.669 U12 C13 / U23 C13 0.619 z C13 / x C13 0.793 U13 C13 / U23 C13 0.669 U13 C14 / U33 C14 0.615 U13 O7 / U33 O7 0.762 y C13 / x C13 0.659 U12 C14 / U23 C14 0.615 U12 C14 / U11 C14 0.703 U13 C13 / U33 C13 0.656 U13 C18_a / U11 C18_a 0.614 y C4 / x C4 0.696 U12 C4 / U11 C4 0.653 U13 C4 / U33 C4 0.613 U13 O7 / U11 O7 0.695 U12 C4 / U22 C4 0.643 U13 C4 / U23 C4 0.610 U12 C14 / U22 C14 0.691 U13 C13 / U11 C13 0.642 U13 C18_a / U33 C18_a 0.602 U12 C12 / U22 C12 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.8884 0.4735 0.4165 23 0.990 0.000 C1 N4 C2 H1B 0.7109 0.4641 0.3934 23 0.990 0.000 C1 N4 C2 H2A 0.7956 0.5678 0.2811 23 0.990 0.000 C2 C3 C1 H2B 0.8533 0.4735 0.2382 23 0.990 0.000 C2 C3 C1 H3A 0.5404 0.4623 0.2040 23 0.990 0.000 C3 O1 C2 H3B 0.6174 0.4710 0.1164 23 0.990 0.000 C3 O1 C2 H4A 0.4938 -0.1951 0.2305 23 0.990 0.000 C4 N5 C5 H4B 0.6256 -0.1069 0.2142 23 0.990 0.000 C4 N5 C5 H5A 0.3777 -0.2415 0.0715 23 0.990 0.000 C5 C4 C6 H5B 0.5199 -0.1636 0.0555 23 0.990 0.000 C5 C4 C6 H6A 0.3476 -0.1059 -0.0409 23 0.990 0.000 C6 O2 C5 H6B 0.2306 -0.1463 0.0165 23 0.990 0.000 C6 O2 C5 H7A -0.0158 0.0866 0.2240 23 0.990 0.000 C7 O3 C8 H7B -0.0622 0.1952 0.2391 23 0.990 0.000 C7 O3 C8 H9A 0.2205 0.1122 0.4946 23 0.990 0.000 C9 O4 C8 H9B 0.1691 0.0396 0.3806 23 0.990 0.000 C9 O4 C8 H10A -0.1736 0.1149 0.3605 23 0.990 0.000 C10 O5 C8 H10B -0.1059 0.0145 0.3561 23 0.990 0.000 C10 O5 C8 H11A 0.1891 0.3188 0.4331 23 0.990 0.000 C11 O6 C8 H11B 0.0107 0.3033 0.4111 23 0.990 0.000 C11 O6 C8 H12A -0.4507 0.3369 0.7109 23 0.990 0.000 C12 N9 C13 H12B -0.5752 0.3211 0.5964 23 0.990 0.000 C12 N9 C13 H13A -0.4109 0.4634 0.5578 23 0.990 0.000 C13 C14 C12 H13B -0.4413 0.5051 0.6606 23 0.990 0.000 C13 C14 C12 H14A -0.2086 0.4869 0.7627 23 0.990 0.000 C14 C13 O7 H14B -0.1892 0.5698 0.6865 23 0.990 0.000 C14 C13 O7 H15A 0.1470 0.0838 0.8823 23 0.990 0.000 C15 N10 C16 H15B 0.0626 0.0683 0.9653 23 0.990 0.000 C15 N10 C16 H16A 0.1671 0.2517 1.0424 23 0.990 0.000 C16 C17 C15 H16B 0.3043 0.2023 1.0412 23 0.990 0.000 C16 C17 C15 H17A 0.3346 0.3666 0.9809 23 0.990 0.000 C17 O8 C16 H17B 0.3141 0.2704 0.8910 23 0.990 0.000 C17 O8 C16 H5 0.4776 -0.0509 0.3152 43 0.880 0.000 N5 C4 P3 H18A 0.0382 0.4658 -0.0342 23 0.990 0.000 C18_a Cl2_a Cl1_a H18B 0.0485 0.5538 0.0599 23 0.990 0.000 C18_a Cl2_a Cl1_a 2007src1142 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.78370 0.44354 0.36364 1.00000 0.03381 0.05058 0.04215 0.01796 0.00625 0.00346 0.04490 0.01531 0.00075 0.00055 0.00053 0.00000 0.00319 0.00383 0.00346 0.00293 0.00272 0.00278 0.00154 H1A 0.88836 0.47349 0.41646 1.00000 0.05388 0.00000 0.00000 H1B 0.71086 0.46411 0.39340 1.00000 0.05388 0.00000 0.00000 C2 0.77425 0.48910 0.26429 1.00000 0.05780 0.05876 0.05025 0.02422 0.01571 -0.00598 0.05957 0.01785 0.00094 0.00066 0.00060 0.00000 0.00460 0.00461 0.00418 0.00357 0.00357 0.00361 0.00210 H2A 0.79560 0.56782 0.28112 1.00000 0.07148 0.00000 0.00000 H2B 0.85332 0.47353 0.23823 1.00000 0.07148 0.00000 0.00000 C3 0.61885 0.44192 0.18026 1.00000 0.05880 0.05904 0.04670 0.03112 0.01358 0.00601 0.05652 0.01788 0.00093 0.00063 0.00058 0.00000 0.00454 0.00454 0.00395 0.00350 0.00346 0.00358 0.00197 H3A 0.54042 0.46227 0.20398 1.00000 0.06782 0.00000 0.00000 H3B 0.61735 0.47098 0.11642 1.00000 0.06782 0.00000 0.00000 C4 0.51376 -0.13131 0.19874 1.00000 0.20618 0.09251 0.23258 0.05662 0.12876 0.09622 0.15261 0.05173 0.00240 0.00123 0.00171 0.00000 0.01901 0.00992 0.02204 0.01217 0.01756 0.01193 0.00737 H4A 0.49380 -0.19513 0.23045 1.00000 0.18314 0.00000 0.00000 H4B 0.62561 -0.10690 0.21423 1.00000 0.18314 0.00000 0.00000 C5 0.43888 -0.16569 0.08577 1.00000 0.11371 0.12339 0.15393 -0.05619 0.05257 0.03852 0.13476 0.03514 0.00181 0.00134 0.00142 0.00000 0.01100 0.01213 0.01448 0.01118 0.01037 0.00931 0.00667 H5A 0.37772 -0.24146 0.07146 1.00000 0.16171 0.00000 0.00000 H5B 0.51991 -0.16361 0.05551 1.00000 0.16171 0.00000 0.00000 C6 0.33771 -0.10612 0.02855 1.00000 0.19220 0.07001 0.09494 -0.01549 0.06828 0.01372 0.12151 0.03369 0.00219 0.00098 0.00107 0.00000 0.01653 0.00731 0.00908 0.00650 0.01027 0.00888 0.00549 H6A 0.34762 -0.10588 -0.04089 1.00000 0.14581 0.00000 0.00000 H6B 0.23063 -0.14627 0.01647 1.00000 0.14581 0.00000 0.00000 C7 0.02119 0.16119 0.26353 1.00000 0.02555 0.05551 0.03493 0.01181 0.01170 0.01023 0.03844 0.01464 0.00066 0.00056 0.00047 0.00000 0.00274 0.00377 0.00305 0.00269 0.00238 0.00257 0.00134 H7A -0.01582 0.08658 0.22399 1.00000 0.04613 0.00000 0.00000 H7B -0.06216 0.19516 0.23911 1.00000 0.04613 0.00000 0.00000 C8 0.05894 0.16036 0.37947 1.00000 0.02668 0.04340 0.03556 0.01938 0.01527 0.01337 0.03263 0.01411 0.00063 0.00049 0.00045 0.00000 0.00264 0.00319 0.00293 0.00246 0.00230 0.00235 0.00120 C9 0.19550 0.11371 0.41919 1.00000 0.03017 0.04758 0.04387 0.02163 0.01923 0.01663 0.03702 0.01542 0.00066 0.00052 0.00051 0.00000 0.00287 0.00346 0.00331 0.00274 0.00258 0.00256 0.00131 H9A 0.22050 0.11219 0.49456 1.00000 0.04442 0.00000 0.00000 H9B 0.16907 0.03959 0.38062 1.00000 0.04442 0.00000 0.00000 C10 -0.08382 0.08896 0.39251 1.00000 0.03569 0.04482 0.04724 0.02220 0.02421 0.01410 0.03869 0.01570 0.00070 0.00053 0.00051 0.00000 0.00310 0.00339 0.00351 0.00278 0.00278 0.00261 0.00135 H10A -0.17356 0.11491 0.36047 1.00000 0.04643 0.00000 0.00000 H10B -0.10585 0.01454 0.35611 1.00000 0.04643 0.00000 0.00000 C11 0.09665 0.27293 0.44059 1.00000 0.03260 0.04791 0.03638 0.01820 0.01816 0.01483 0.03610 0.01471 0.00069 0.00051 0.00046 0.00000 0.00292 0.00345 0.00305 0.00261 0.00249 0.00256 0.00128 H11A 0.18911 0.31878 0.43311 1.00000 0.04332 0.00000 0.00000 H11B 0.01066 0.30328 0.41110 1.00000 0.04332 0.00000 0.00000 C12 -0.46390 0.34170 0.63726 1.00000 0.04983 0.19321 0.06825 0.00185 0.02347 0.06314 0.09982 0.02806 0.00110 0.00127 0.00084 0.00000 0.00509 0.01419 0.00616 0.00738 0.00459 0.00716 0.00451 H12A -0.45067 0.33689 0.71087 1.00000 0.11978 0.00000 0.00000 H12B -0.57521 0.32106 0.59644 1.00000 0.11978 0.00000 0.00000 C13 -0.39147 0.45777 0.63194 1.00000 0.20763 0.17401 0.10761 0.07794 0.10044 0.15988 0.12877 0.04980 0.00231 0.00145 0.00115 0.00000 0.01742 0.01493 0.00993 0.01013 0.01155 0.01480 0.00657 H13A -0.41094 0.46343 0.55782 1.00000 0.15453 0.00000 0.00000 H13B -0.44129 0.50514 0.66055 1.00000 0.15453 0.00000 0.00000 C14 -0.23037 0.49368 0.68865 1.00000 0.18492 0.08517 0.11072 0.05123 0.09203 0.07805 0.10730 0.03920 0.00202 0.00100 0.00110 0.00000 0.01525 0.00773 0.00965 0.00716 0.01063 0.00940 0.00465 H14A -0.20859 0.48688 0.76269 1.00000 0.12876 0.00000 0.00000 H14B -0.18922 0.56980 0.68645 1.00000 0.12876 0.00000 0.00000 C15 0.09738 0.11877 0.92339 1.00000 0.06961 0.05995 0.06271 0.02799 0.01086 0.00153 0.06916 0.01986 0.00106 0.00071 0.00071 0.00000 0.00552 0.00499 0.00510 0.00409 0.00429 0.00413 0.00245 H15A 0.14704 0.08375 0.88231 1.00000 0.08299 0.00000 0.00000 H15B 0.06258 0.06828 0.96530 1.00000 0.08299 0.00000 0.00000 C16 0.21329 0.22014 0.99645 1.00000 0.07170 0.07192 0.04628 0.02726 -0.00046 -0.01246 0.07352 0.01884 0.00110 0.00074 0.00065 0.00000 0.00568 0.00553 0.00430 0.00398 0.00395 0.00443 0.00282 H16A 0.16714 0.25169 1.04244 1.00000 0.08822 0.00000 0.00000 H16B 0.30431 0.20233 1.04119 1.00000 0.08822 0.00000 0.00000 C17 0.26130 0.30043 0.93289 1.00000 0.05583 0.06488 0.06858 0.02682 -0.01368 -0.00878 0.07583 0.01919 0.00103 0.00074 0.00075 0.00000 0.00493 0.00536 0.00551 0.00439 0.00418 0.00404 0.00291 H17A 0.33457 0.36663 0.98094 1.00000 0.09100 0.00000 0.00000 H17B 0.31415 0.27045 0.89095 1.00000 0.09100 0.00000 0.00000 N1 0.44208 0.28304 0.28489 1.00000 0.03014 0.03932 0.03900 0.01472 0.01768 0.01256 0.03377 0.01182 0.00055 0.00040 0.00039 0.00000 0.00241 0.00266 0.00263 0.00211 0.00210 0.00204 0.00105 N2 0.56902 0.14382 0.21240 1.00000 0.04296 0.06675 0.05679 0.00442 0.02532 0.01813 0.05375 0.01487 0.00069 0.00054 0.00050 0.00000 0.00323 0.00404 0.00370 0.00305 0.00289 0.00291 0.00153 N3 0.28842 0.07127 0.22382 1.00000 0.03163 0.04202 0.05105 0.00164 0.00940 0.00320 0.04483 0.01233 0.00061 0.00045 0.00046 0.00000 0.00267 0.00298 0.00326 0.00245 0.00239 0.00224 0.00129 N4 0.74622 0.32553 0.33856 1.00000 0.02893 0.05992 0.04237 0.02223 0.01515 0.01192 0.04231 0.01402 0.00061 0.00051 0.00048 0.00000 0.00262 0.00364 0.00315 0.00279 0.00237 0.00241 0.00131 N5 0.47470 -0.05025 0.25073 1.00000 0.09246 0.05876 0.09258 0.00518 0.01684 0.03511 0.08364 0.01954 0.00102 0.00062 0.00073 0.00000 0.00610 0.00454 0.00607 0.00414 0.00487 0.00432 0.00250 H5 0.47756 -0.05094 0.31524 1.00000 0.10037 0.00000 0.00000 N6 -0.15397 0.25212 0.54693 1.00000 0.04465 0.07685 0.03309 0.02182 0.01593 0.03856 0.04628 0.01463 0.00065 0.00053 0.00041 0.00000 0.00307 0.00407 0.00268 0.00265 0.00237 0.00297 0.00139 N7 -0.14413 0.27750 0.74648 1.00000 0.05230 0.08601 0.03303 0.01759 0.01721 0.02530 0.05513 0.01549 0.00074 0.00059 0.00045 0.00000 0.00356 0.00471 0.00288 0.00292 0.00264 0.00333 0.00159 N8 0.05310 0.18727 0.69437 1.00000 0.03502 0.10206 0.04338 0.04034 0.01643 0.03359 0.05495 0.01598 0.00064 0.00061 0.00046 0.00000 0.00289 0.00517 0.00318 0.00335 0.00251 0.00321 0.00169 N9 -0.39332 0.26447 0.59510 1.00000 0.03155 0.13486 0.04614 0.00075 0.01061 0.02995 0.07186 0.01844 0.00074 0.00079 0.00059 0.00000 0.00316 0.00747 0.00388 0.00425 0.00291 0.00387 0.00240 N10 -0.02961 0.14212 0.85497 1.00000 0.05147 0.05707 0.03449 0.01635 0.01103 -0.00593 0.05209 0.01404 0.00074 0.00052 0.00045 0.00000 0.00350 0.00363 0.00286 0.00258 0.00260 0.00284 0.00155 O1 0.58219 0.32533 0.15599 1.00000 0.03900 0.07860 0.03292 0.01645 0.01504 0.00762 0.05085 0.01128 0.00054 0.00045 0.00035 0.00000 0.00248 0.00355 0.00231 0.00227 0.00197 0.00235 0.00123 O2 0.36044 -0.00589 0.07246 1.00000 0.09981 0.10826 0.06078 -0.02783 0.00371 0.05010 0.09567 0.01608 0.00090 0.00065 0.00052 0.00000 0.00538 0.00564 0.00392 0.00377 0.00364 0.00457 0.00252 O3 0.15389 0.21896 0.24239 1.00000 0.02834 0.05180 0.03389 0.01790 0.01264 0.01161 0.03685 0.00985 0.00045 0.00036 0.00032 0.00000 0.00200 0.00253 0.00212 0.00186 0.00169 0.00180 0.00093 O4 0.32651 0.18126 0.40238 1.00000 0.02693 0.05236 0.03431 0.01969 0.01422 0.01454 0.03557 0.00988 0.00044 0.00035 0.00031 0.00000 0.00195 0.00251 0.00210 0.00185 0.00167 0.00178 0.00091 O5 -0.05841 0.09100 0.50280 1.00000 0.03870 0.05889 0.05469 0.03277 0.02986 0.02388 0.04392 0.01180 0.00051 0.00039 0.00037 0.00000 0.00234 0.00284 0.00275 0.00230 0.00215 0.00211 0.00109 O6 0.12355 0.27368 0.55039 1.00000 0.03642 0.05549 0.03972 0.01829 0.02054 0.01708 0.04069 0.01076 0.00049 0.00038 0.00034 0.00000 0.00225 0.00270 0.00232 0.00201 0.00191 0.00200 0.00100 O7 -0.15916 0.42748 0.63996 1.00000 0.10898 0.07074 0.07786 0.01866 0.05669 0.02353 0.08001 0.01717 0.00089 0.00053 0.00054 0.00000 0.00544 0.00403 0.00428 0.00332 0.00410 0.00376 0.00192 O8 0.13637 0.32535 0.86660 1.00000 0.05475 0.06473 0.05946 0.03288 0.00174 0.00003 0.06584 0.01276 0.00065 0.00047 0.00044 0.00000 0.00318 0.00345 0.00332 0.00277 0.00261 0.00262 0.00162 P1 0.30916 0.18715 0.28406 1.00000 0.02738 0.03932 0.03186 0.01014 0.01259 0.00892 0.03220 0.00356 0.00017 0.00013 0.00012 0.00000 0.00070 0.00080 0.00074 0.00060 0.00058 0.00059 0.00035 P2 0.57857 0.26352 0.24849 1.00000 0.02836 0.04981 0.03370 0.01244 0.01563 0.01200 0.03565 0.00378 0.00017 0.00014 0.00012 0.00000 0.00073 0.00093 0.00078 0.00066 0.00062 0.00064 0.00037 P3 0.42397 0.04537 0.19287 1.00000 0.04738 0.04777 0.05238 -0.00484 0.01212 0.01788 0.05097 0.00443 0.00023 0.00016 0.00016 0.00000 0.00102 0.00102 0.00108 0.00081 0.00084 0.00082 0.00049 P4 -0.01288 0.20361 0.57826 1.00000 0.03333 0.06458 0.03965 0.02988 0.02049 0.02805 0.03986 0.00441 0.00018 0.00015 0.00013 0.00000 0.00079 0.00109 0.00085 0.00078 0.00068 0.00076 0.00041 P5 -0.20776 0.30175 0.63361 1.00000 0.03342 0.06099 0.03297 0.01196 0.01302 0.01892 0.04096 0.00413 0.00019 0.00015 0.00013 0.00000 0.00081 0.00108 0.00080 0.00072 0.00066 0.00074 0.00041 P6 -0.00093 0.23227 0.78420 1.00000 0.03416 0.06647 0.03100 0.02204 0.00742 0.00597 0.04549 0.00419 0.00020 0.00016 0.00013 0.00000 0.00084 0.00117 0.00080 0.00077 0.00066 0.00076 0.00046 C18_a 0.09147 0.54012 0.00492 0.33000 0.07077 0.06484 0.04883 -0.02828 0.04173 0.00678 0.06168 0.05272 0.00290 0.00203 0.00183 0.00000 0.01570 0.01473 0.01275 0.01117 0.01232 0.01189 0.00706 H18A_a 0.03819 0.46577 -0.03416 0.33000 0.07401 0.00000 0.00000 H18B_a 0.04852 0.55378 0.05985 0.33000 0.07401 0.00000 0.00000 Cl1_a 0.27389 0.55358 0.05928 0.33000 0.20553 0.10947 0.06949 0.01543 0.06100 0.06153 0.12228 0.02948 0.00173 0.00089 0.00074 0.00000 0.01317 0.00735 0.00522 0.00488 0.00688 0.00801 0.00408 Cl2_a 0.06217 0.62206 -0.07372 0.33000 0.21833 0.11611 0.10753 -0.03974 0.03958 0.02577 0.16081 0.03050 0.00207 0.00112 0.00105 0.00000 0.01583 0.00915 0.00867 0.00733 0.00926 0.00952 0.00584 H4N 0.75885 0.30607 0.38591 1.00000 0.06330 0.21257 0.01057 0.00745 0.00709 0.00000 0.02890 H9N -0.43048 0.24027 0.53403 1.00000 0.07165 0.22311 0.01082 0.00765 0.00761 0.00000 0.03016 H10N -0.13234 0.07566 0.80548 1.00000 0.11969 0.29343 0.01438 0.01009 0.00949 0.00000 0.04169 Final Structure Factor Calculation for 2007src1142 in P-1 Total number of l.s. parameters = 409 Maximum vector length = 511 Memory required = 4463 / 25039 wR2 = 0.2806 before cycle 5 for 7129 data and 0 / 409 parameters GooF = S = 1.084; Restrained GooF = 1.084 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0935 * P )^2 + 11.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1088 for 5654 Fo > 4sig(Fo) and 0.1308 for all 7129 data wR2 = 0.2806, GooF = S = 1.084, Restrained GooF = 1.084 for all data Occupancy sum of asymmetric unit = 41.99 for non-hydrogen and 36.66 for hydrogen atoms Principal mean square atomic displacements U 0.0683 0.0349 0.0315 C1 0.0989 0.0506 0.0292 C2 0.0907 0.0534 0.0254 C3 0.2597 0.1498 0.0483 C4 0.2437 0.1157 0.0449 C5 0.2091 0.1071 0.0483 C6 0.0570 0.0337 0.0247 C7 0.0501 0.0256 0.0222 C8 0.0565 0.0301 0.0244 C9 0.0572 0.0358 0.0231 C10 0.0521 0.0319 0.0243 C11 0.2062 0.0676 0.0257 C12 may be split into -0.4562 0.3541 0.6329 and -0.4716 0.3293 0.6416 0.2754 0.0703 0.0406 C13 may be split into -0.3678 0.4675 0.6334 and -0.4151 0.4480 0.6305 0.1964 0.0724 0.0531 C14 0.1100 0.0572 0.0402 C15 0.1394 0.0462 0.0350 C16 0.1426 0.0499 0.0349 C17 0.0451 0.0316 0.0246 N1 0.0729 0.0561 0.0323 N2 0.0575 0.0477 0.0292 N3 0.0666 0.0337 0.0267 N4 0.1222 0.0806 0.0481 N5 0.0827 0.0325 0.0236 N6 0.0860 0.0493 0.0300 N7 0.1081 0.0343 0.0225 N8 0.1424 0.0464 0.0267 N9 0.0893 0.0389 0.0281 N10 0.0853 0.0391 0.0281 O1 0.1697 0.0774 0.0398 O2 0.0558 0.0283 0.0264 O3 0.0564 0.0266 0.0238 O4 0.0754 0.0330 0.0234 O5 0.0581 0.0371 0.0269 O6 0.1174 0.0707 0.0519 O7 0.1157 0.0459 0.0360 O8 0.0407 0.0306 0.0253 P1 0.0506 0.0332 0.0232 P2 0.0723 0.0454 0.0352 P3 0.0727 0.0248 0.0221 P4 0.0611 0.0319 0.0299 P5 0.0781 0.0345 0.0239 P6 0.1180 0.0607 0.0064 C18_a 0.2069 0.1032 0.0567 Cl1_a 0.2361 0.1883 0.0581 Cl2_a Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.018 0.028 0.038 0.051 0.066 0.084 0.113 0.171 1.000 Number in group 716. 734. 722. 684. 741. 708. 703. 697. 709. 715. GooF 1.299 1.090 1.201 1.026 1.056 1.007 0.991 0.924 1.069 1.116 K 13.172 2.434 1.585 1.217 1.169 1.079 1.043 0.999 1.017 1.010 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 732. 705. 715. 697. 728. 716. 695. 710. 715. 716. GooF 0.988 0.974 0.932 0.899 0.845 0.927 0.973 1.073 1.209 1.733 K 1.185 1.124 1.096 1.059 1.027 1.004 0.988 0.998 1.013 1.034 R1 0.266 0.237 0.192 0.175 0.154 0.137 0.105 0.082 0.087 0.096 Recommended weighting scheme: WGHT 0.0902 11.6045 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) -3 3 3 397.82 42.52 6.42 0.041 2.60 -2 1 1 359.66 48.78 6.37 0.044 4.75 1 -1 2 1039.48 364.76 6.34 0.120 4.63 -6 8 0 295.06 16.52 6.24 0.025 1.26 5 -9 2 325.20 23.62 6.24 0.030 1.23 1 -5 3 1738.30 679.28 5.82 0.164 2.33 -7 8 0 169.53 0.24 5.73 0.003 1.15 -4 -8 7 208.57 0.50 5.72 0.004 1.14 -1 0 2 196.77 17.65 5.44 0.026 6.35 -2 -4 8 223.74 20.95 5.35 0.029 1.56 -1 -2 1 2325.92 1117.81 5.31 0.210 4.76 2 -7 4 192.63 13.90 5.29 0.023 1.64 0 -7 6 221.51 25.71 5.23 0.032 1.52 2 -4 8 499.83 160.39 5.15 0.079 1.37 3 -9 5 585.03 204.85 5.00 0.090 1.26 1 -12 7 218.07 10.33 4.98 0.020 0.99 1 3 1 378.61 36.80 4.90 0.038 3.07 -1 2 2 886.80 377.44 4.87 0.122 4.48 -1 0 5 1351.25 657.03 4.87 0.161 2.73 0 -7 5 359.40 98.20 4.86 0.062 1.62 2 -3 1 318.48 876.83 4.82 0.186 3.33 5 0 1 332.39 77.55 4.78 0.055 1.65 7 -10 3 119.68 1.87 4.75 0.009 0.98 -1 -5 7 111.07 0.13 4.74 0.002 1.65 0 0 4 631.64 252.84 4.73 0.100 3.20 2 -8 4 107.68 0.62 4.69 0.005 1.49 -5 7 1 246.56 40.47 4.55 0.040 1.49 1 -4 4 315.55 93.21 4.50 0.061 2.36 1 -6 1 147.33 16.00 4.50 0.025 2.18 -4 4 1 171.16 24.44 4.47 0.031 2.14 -3 3 2 467.86 168.67 4.43 0.081 2.78 -5 3 1 128.26 9.85 4.34 0.020 1.86 -2 3 1 203.38 589.70 4.33 0.152 3.55 -3 1 0 710.89 325.63 4.30 0.113 3.03 -2 1 8 251.43 50.77 4.27 0.045 1.67 0 -11 8 139.43 10.13 4.25 0.020 1.02 -3 3 0 10129.74 6587.15 4.14 0.509 2.79 3 -8 2 247.73 58.86 4.14 0.048 1.53 -3 -3 11 182.34 35.74 4.13 0.038 1.22 -4 -8 9 153.80 16.72 4.13 0.026 1.07 0 -3 7 706.87 332.80 4.12 0.114 1.81 3 -7 5 102.74 7.38 4.10 0.017 1.44 2 -7 3 137.53 16.95 4.06 0.026 1.73 0 1 3 1116.95 2033.79 4.04 0.283 3.81 2 0 0 3968.35 2482.42 4.02 0.313 4.36 1 -6 5 395.91 158.40 3.91 0.079 1.76 6 -4 2 94.82 7.60 3.85 0.017 1.37 -2 3 3 428.11 892.56 3.83 0.187 2.92 4 -6 2 1674.24 998.10 3.82 0.198 1.66 -1 -2 9 72.05 1.24 3.80 0.007 1.50 Bond lengths and angles C1 - Distance Angles N4 1.4790 (0.0094) C2 1.5323 (0.0092) 109.78 (0.61) C1 - N4 C2 - Distance Angles C3 1.5031 (0.0105) C1 1.5323 (0.0092) 111.41 (0.57) C2 - C3 C3 - Distance Angles O1 1.4613 (0.0096) C2 1.5031 (0.0105) 110.57 (0.64) C3 - O1 C4 - Distance Angles N5 1.4085 (0.0156) C5 1.4566 (0.0225) 119.07 (1.40) C4 - N5 C5 - Distance Angles C4 1.4566 (0.0225) C6 1.4734 (0.0210) 118.51 (1.09) C5 - C4 C6 - Distance Angles O2 1.3242 (0.0131) C5 1.4734 (0.0210) 117.49 (1.27) C6 - O2 C7 - Distance Angles O3 1.4530 (0.0069) C8 1.5200 (0.0079) 111.62 (0.46) C7 - O3 C8 - Distance Angles C7 1.5200 (0.0079) C11 1.5198 (0.0089) 110.40 (0.49) C10 1.5413 (0.0076) 107.63 (0.49) 109.09 (0.48) C9 1.5441 (0.0077) 109.36 (0.48) 110.42 (0.50) 109.89 (0.47) C8 - C7 C11 C10 C9 - Distance Angles O4 1.4575 (0.0067) C8 1.5441 (0.0077) 108.25 (0.45) C9 - O4 C10 - Distance Angles O5 1.4537 (0.0074) C8 1.5413 (0.0077) 110.19 (0.51) C10 - O5 C11 - Distance Angles O6 1.4471 (0.0069) C8 1.5198 (0.0089) 111.63 (0.47) C11 - O6 C12 - Distance Angles N9 1.5085 (0.0128) C13 1.5360 (0.0205) 112.15 (0.88) C12 - N9 C13 - Distance Angles C14 1.4261 (0.0212) C12 1.5360 (0.0204) 112.71 (0.95) C13 - C14 C14 - Distance Angles C13 1.4261 (0.0213) O7 1.4572 (0.0130) 107.76 (1.12) C14 - C13 C15 - Distance Angles N10 1.4035 (0.0107) C16 1.5242 (0.0119) 111.11 (0.78) C15 - N10 C16 - Distance Angles C17 1.5179 (0.0114) C15 1.5242 (0.0119) 109.85 (0.70) C16 - C17 C17 - Distance Angles O8 1.3878 (0.0099) C16 1.5179 (0.0113) 111.66 (0.78) C17 - O8 N1 - Distance Angles P1 1.5622 (0.0050) P2 1.6091 (0.0048) 121.18 (0.33) N1 - P1 N2 - Distance Angles P2 1.5676 (0.0068) P3 1.5871 (0.0068) 124.28 (0.38) N2 - P2 N3 - Distance Angles P1 1.5885 (0.0058) P3 1.5898 (0.0060) 120.52 (0.34) N3 - P1 N4 - Distance Angles C1 1.4790 (0.0094) P2 1.6390 (0.0059) 115.89 (0.45) N4 - C1 N5 - Distance Angles C4 1.4085 (0.0156) P3 1.6399 (0.0084) 121.00 (1.02) N5 - C4 N6 - Distance Angles P5 1.5826 (0.0056) P4 1.5871 (0.0052) 120.73 (0.33) N6 - P5 N7 - Distance Angles P5 1.5723 (0.0059) P6 1.5833 (0.0067) 122.88 (0.39) N7 - P5 N8 - Distance Angles P4 1.5765 (0.0055) P6 1.5965 (0.0066) 122.37 (0.38) N8 - P4 N9 - Distance Angles C12 1.5085 (0.0128) P5 1.6216 (0.0066) 115.60 (0.72) N9 - C12 N10 - Distance Angles C15 1.4035 (0.0108) P6 1.6359 (0.0058) 118.94 (0.54) N10 - C15 O1 - Distance Angles C3 1.4613 (0.0096) P2 1.5827 (0.0048) 117.24 (0.43) O1 - C3 O2 - Distance Angles C6 1.3242 (0.0131) P3 1.5798 (0.0064) 128.11 (0.92) O2 - C6 O3 - Distance Angles C7 1.4530 (0.0069) P1 1.5891 (0.0043) 119.21 (0.37) O3 - C7 O4 - Distance Angles C9 1.4575 (0.0067) P1 1.5942 (0.0041) 116.62 (0.37) O4 - C9 O5 - Distance Angles C10 1.4537 (0.0074) P4 1.5918 (0.0054) 118.52 (0.39) O5 - C10 O6 - Distance Angles C11 1.4471 (0.0069) P4 1.5923 (0.0045) 116.71 (0.38) O6 - C11 O7 - Distance Angles C14 1.4572 (0.0130) P5 1.5880 (0.0069) 119.41 (0.69) O7 - C14 O8 - Distance Angles C17 1.3878 (0.0099) P6 1.5841 (0.0058) 119.35 (0.57) O8 - C17 P1 - Distance Angles N1 1.5622 (0.0050) N3 1.5885 (0.0058) 119.07 (0.29) O3 1.5891 (0.0043) 107.77 (0.25) 110.01 (0.27) O4 1.5942 (0.0041) 108.00 (0.25) 108.68 (0.29) 101.95 (0.22) P1 - N1 N3 O3 P2 - Distance Angles N2 1.5676 (0.0068) O1 1.5827 (0.0048) 109.03 (0.32) N1 1.6091 (0.0048) 116.10 (0.30) 107.71 (0.27) N4 1.6390 (0.0059) 110.20 (0.33) 101.83 (0.28) 110.96 (0.29) P2 - N2 O1 N1 P3 - Distance Angles O2 1.5798 (0.0064) N2 1.5871 (0.0068) 106.78 (0.43) N3 1.5898 (0.0060) 108.94 (0.36) 116.42 (0.31) N5 1.6399 (0.0084) 103.91 (0.44) 110.89 (0.41) 109.12 (0.43) P3 - O2 N2 N3 P4 - Distance Angles N8 1.5765 (0.0055) N6 1.5871 (0.0052) 118.20 (0.30) O6 1.5923 (0.0045) 108.62 (0.29) 109.67 (0.29) O5 1.5918 (0.0055) 107.74 (0.34) 108.78 (0.30) 102.69 (0.24) P4 - N8 N6 O6 P5 - Distance Angles N7 1.5723 (0.0059) N6 1.5826 (0.0056) 117.62 (0.32) O7 1.5880 (0.0069) 109.10 (0.39) 105.96 (0.34) N9 1.6216 (0.0066) 107.58 (0.39) 109.96 (0.36) 106.05 (0.46) P5 - N7 N6 O7 P6 - Distance Angles N7 1.5833 (0.0067) O8 1.5841 (0.0059) 107.52 (0.37) N8 1.5965 (0.0066) 115.84 (0.30) 109.44 (0.36) N10 1.6359 (0.0058) 110.62 (0.36) 102.24 (0.30) 110.27 (0.37) P6 - N7 O8 N8 C18_a - Distance Angles Cl2_a 1.6098 (0.0325) Cl1_a 1.6282 (0.0284) 110.91 (1.63) C18_a - Cl2_a Cl1_a - Distance Angles C18_a 1.6282 (0.0285) Cl1_a - Cl2_a - Distance Angles C18_a 1.6098 (0.0324) Cl2_a - FMAP and GRID set by program FMAP 2 3 35 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.1303 for 7129 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.51 at 0.5414 0.0203 0.4979 [ 2.41 A from H5 ] Deepest hole -0.74 at 0.0208 0.7269 0.1910 [ 0.70 A from P6 ] Mean = 0.00, Rms deviation from mean = 0.13 e/A^3, Highest memory used = 4179 / 31493 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5414 0.0203 0.4979 1.00000 0.05 1.51 2.41 H5 2.63 H5 2.81 H9N 3.08 H9B Q2 1 0.0261 0.1746 0.9644 1.00000 0.05 1.43 1.31 C15 1.41 N10 1.49 H16A 1.52 H15B Q3 1 0.3954 -0.0215 0.1892 1.00000 0.05 1.10 0.84 P3 1.11 N5 1.58 O2 1.79 H5 Q4 1 0.2621 0.1183 0.2638 1.00000 0.05 1.02 0.88 P1 0.92 N3 1.84 O4 1.85 O3 Q5 1 0.1845 0.2805 0.8299 1.00000 0.05 1.00 1.02 O8 1.31 H17B 1.34 C17 1.62 P6 Q6 1 0.0470 0.1944 0.7591 1.00000 0.05 1.00 0.87 P6 0.91 N8 1.82 N10 1.96 O8 Q7 1 -0.1527 0.3586 0.6822 1.00000 0.05 0.91 0.88 P5 1.13 O7 1.45 N7 2.08 C14 Q8 1 0.5406 0.1973 0.2303 1.00000 0.05 0.86 0.83 P2 0.85 N2 1.87 N1 1.96 P3 Q9 1 0.1769 0.3492 0.9517 1.00000 0.05 0.75 1.09 O8 1.22 C17 1.39 H17A 1.88 H16A Q10 1 0.0584 0.6442 -0.0815 1.00000 0.05 0.73 0.32 CL2 1.92 C18 2.39 H18B 2.47 H18A Q11 1 0.1745 0.5998 -0.0488 1.00000 0.05 0.72 1.14 CL2 1.41 C18 1.74 CL1 2.00 H18A Q12 1 -0.0077 0.5242 -0.0416 1.00000 0.05 0.68 0.92 C18 0.97 H18A 0.98 H18B 1.17 H18A Q13 1 0.0549 0.2896 0.8187 1.00000 0.05 0.67 0.81 P6 0.84 O8 1.81 N7 2.05 N8 Q14 1 0.1861 0.2902 1.0326 1.00000 0.05 0.66 0.54 H16A 1.12 C16 1.75 C17 1.79 H16B Q15 1 -0.4883 0.3837 0.5965 1.00000 0.05 0.61 0.84 C12 1.02 H12B 1.11 C13 1.39 H13A Q16 1 0.0868 0.5008 0.0308 1.00000 0.05 0.59 0.66 C18 0.88 H18A 0.97 H18B 1.38 H18A Q17 1 0.0291 0.1122 0.8396 1.00000 0.05 0.58 0.83 N10 1.11 C15 1.26 H15A 1.41 H10N Q18 1 0.0753 0.5953 0.0006 1.00000 0.05 0.56 0.78 C18 1.09 H18B 1.09 CL2 1.42 H18A Q19 1 0.2117 0.4084 0.9940 1.00000 0.05 0.53 1.46 H17A 1.79 O8 1.81 C17 1.88 CL1 Q20 1 0.5545 -0.0986 0.1764 1.00000 0.05 0.51 0.68 C4 0.75 H4B 1.41 C5 1.62 H4A Q21 1 -0.4986 0.2822 0.6343 1.00000 0.05 0.50 0.76 C12 1.03 H12B 1.10 H12A 1.34 N9 Q22 1 0.3574 -0.0609 0.0982 1.00000 0.05 0.48 0.83 O2 1.01 C6 1.49 H6B 1.65 P3 Q23 1 0.4653 -0.0799 0.0641 1.00000 0.05 0.47 1.12 C6 1.18 C5 1.33 H5B 1.47 H6A Q24 1 0.2379 0.0025 0.2069 1.00000 0.05 0.45 0.88 N3 1.21 H10N 1.82 P3 2.26 N10 Q25 1 0.5329 0.2499 0.1277 1.00000 0.05 0.45 0.97 O1 1.56 P2 1.93 N2 2.04 H16B Q26 1 -0.0237 0.1475 0.5356 1.00000 0.05 0.43 0.76 O5 0.86 P4 1.85 O6 1.88 C10 Q27 1 0.2349 0.2417 0.2813 1.00000 0.05 0.42 0.76 O3 1.12 P1 1.92 N1 1.96 O4 Q28 1 0.1981 0.4712 0.0856 1.00000 0.05 0.42 1.31 CL1 1.74 C18 1.84 H18A 1.96 H18B Q29 1 0.7284 0.3872 0.3317 1.00000 0.05 0.42 0.79 C1 0.87 N4 1.33 H1B 1.39 H4N Q30 1 0.8385 0.4194 0.3798 1.00000 0.05 0.41 0.67 C1 0.77 H1A 1.28 N4 1.53 H4N Shortest distances between peaks (including symmetry equivalents) 12 16 0.82 9 19 0.84 1 1 0.87 29 30 1.01 12 18 1.04 3 22 1.20 12 16 1.24 5 13 1.24 16 28 1.27 22 23 1.33 11 18 1.33 10 18 1.34 10 11 1.35 12 12 1.35 16 18 1.36 6 13 1.39 9 14 1.41 15 21 1.47 5 6 1.49 19 28 1.49 4 24 1.56 20 23 1.58 16 16 1.60 8 25 1.62 6 17 1.64 16 18 1.65 14 19 1.68 3 24 1.70 4 27 1.70 12 28 1.75 10 12 1.76 12 18 1.77 2 14 1.79 9 13 1.80 11 12 1.84 2 17 1.84 5 9 1.85 11 16 1.99 16 19 2.03 20 22 2.06 3 20 2.06 3 23 2.17 9 28 2.23 13 17 2.34 22 24 2.35 14 28 2.37 10 16 2.38 5 17 2.40 18 28 2.40 18 28 2.41 2 9 2.46 12 28 2.48 17 24 2.48 13 19 2.51 10 28 2.55 10 16 2.56 12 19 2.56 18 18 2.57 5 19 2.57 9 16 2.62 11 28 2.62 8 29 2.64 11 16 2.65 7 13 2.67 2 13 2.67 11 12 2.69 11 19 2.71 3 4 2.76 18 19 2.77 5 14 2.77 3 8 2.78 13 14 2.80 16 28 2.83 12 19 2.83 4 8 2.83 6 9 2.87 6 26 2.89 10 14 2.93 2 6 2.93 9 18 2.93 25 29 2.94 10 12 2.96 23 23 2.97 Time profile in seconds ----------------------- 0.06: 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. 4.47: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.78: Structure factors and derivatives 11.22: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.98: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.33: Analysis of variance 0.07: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.00: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src1142 finished at 14:28:08 Total CPU time: 21.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++