+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0607 started at 22:50:50 on 14-May-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0607 in P2(1)2(1)2(1) CELL 0.71073 11.7560 15.6189 18.4464 90.000 90.000 90.000 ZERR 8.00 0.0004 0.0003 0.0006 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 F P UNIT 104 152 16 8 48 8 V = 3387.05 F(000) = 1504.0 Mu = 0.22 mm-1 Cell Wt = 2914.18 Rho = 1.429 MERG 2 OMIT -3.00 55.00 OMIT -1 2 1 OMIT 0 2 3 OMIT -1 3 1 OMIT 0 0 4 OMIT 1 2 1 OMIT 0 2 2 FMAP 2 PLAN 20 SIZE 0.02 0.14 0.20 ACTA BOND WGHT 0.07890 0.11620 L.S. 4 TEMP 20.00 FVAR 0.51002 C16 1 0.164746 0.709672 -0.386516 11.00000 0.08416 0.08073 = 0.10461 0.02082 0.05246 -0.00304 AFIX 137 H16A 2 0.136451 0.766515 -0.394689 11.00000 -1.50000 H16B 2 0.163039 0.678086 -0.431147 11.00000 -1.50000 H16C 2 0.241544 0.712686 -0.369010 11.00000 -1.50000 AFIX 0 C19 1 -0.085586 0.749049 -0.321673 11.00000 0.05460 0.06140 = 0.08164 0.00831 -0.00579 0.00890 AFIX 137 H19A 2 -0.062402 0.767127 -0.274177 11.00000 -1.50000 H19B 2 -0.166844 0.743145 -0.322960 11.00000 -1.50000 H19C 2 -0.062235 0.790928 -0.356739 11.00000 -1.50000 AFIX 0 H1N 2 0.382944 0.660452 -0.243042 11.00000 0.04928 H2N 2 0.465920 0.724071 -0.273557 11.00000 0.07128 H3N 2 -0.053243 0.540433 -0.299905 11.00000 0.06448 H4N 2 -0.130516 0.605248 -0.259153 11.00000 0.06904 MOLE 1 C1 1 0.539640 0.607200 -0.253816 11.00000 0.04458 0.05053 = 0.05926 0.00328 0.00247 0.00589 AFIX 13 H1 2 0.514639 0.553426 -0.231557 11.00000 -1.20000 AFIX 0 C2 1 0.638348 0.643500 -0.210461 11.00000 0.04175 0.06189 = 0.06667 0.01361 0.00167 0.00380 C3 1 0.670603 0.737832 -0.105960 11.00000 0.07388 0.10538 = 0.07977 -0.00595 -0.01936 -0.00921 AFIX 137 H3A 2 0.749039 0.725700 -0.116165 11.00000 -1.50000 H3B 2 0.651459 0.716185 -0.058805 11.00000 -1.50000 H3C 2 0.658489 0.798601 -0.107104 11.00000 -1.50000 AFIX 0 C4 1 0.474886 0.707203 -0.163264 11.00000 0.04099 0.07505 = 0.05301 -0.00131 0.00336 -0.00108 C5 1 0.437386 0.799518 -0.157061 11.00000 0.07303 0.07779 = 0.08448 -0.00600 0.01191 0.01797 AFIX 137 H5A 2 0.450854 0.819562 -0.108618 11.00000 -1.50000 H5B 2 0.357722 0.803690 -0.167940 11.00000 -1.50000 H5C 2 0.479774 0.833910 -0.190686 11.00000 -1.50000 AFIX 0 C6 1 0.416486 0.649745 -0.107720 11.00000 0.06262 0.10188 = 0.05986 0.00972 0.01205 -0.01168 AFIX 137 H6A 2 0.436034 0.591093 -0.117046 11.00000 -1.50000 H6B 2 0.335546 0.656723 -0.111284 11.00000 -1.50000 H6C 2 0.441121 0.665255 -0.059872 11.00000 -1.50000 AFIX 0 C7 1 0.564269 0.591912 -0.333586 11.00000 0.06329 0.06327 = 0.07016 -0.00459 0.01008 0.00599 AFIX 23 H7A 2 0.595014 0.644117 -0.354258 11.00000 -1.20000 H7B 2 0.622264 0.547996 -0.337635 11.00000 -1.20000 AFIX 0 C8 1 0.461542 0.564727 -0.377886 11.00000 0.07033 0.06163 = 0.06968 -0.00951 0.00320 0.01585 C9 1 0.448054 0.596616 -0.447203 11.00000 0.09020 0.09278 = 0.06591 -0.00685 0.00384 0.01131 AFIX 43 H9 2 0.501476 0.634980 -0.465300 11.00000 -1.20000 AFIX 0 C10 1 0.357861 0.573152 -0.490054 11.00000 0.10504 0.14573 = 0.07554 -0.00751 -0.00576 0.02646 AFIX 43 H10 2 0.350069 0.595522 -0.536512 11.00000 -1.20000 AFIX 0 C11 1 0.280839 0.517350 -0.463970 11.00000 0.10564 0.10151 = 0.10041 -0.03061 -0.04116 0.02446 AFIX 43 H11 2 0.220494 0.500610 -0.493327 11.00000 -1.20000 AFIX 0 C12 1 0.289078 0.484414 -0.394961 11.00000 0.08206 0.07030 = 0.14555 -0.01734 -0.01547 0.00186 AFIX 43 H12 2 0.233906 0.447139 -0.377372 11.00000 -1.20000 AFIX 0 C13 1 0.381974 0.507927 -0.351548 11.00000 0.08553 0.06127 = 0.09871 -0.00433 -0.01800 0.00356 AFIX 43 H13 2 0.389801 0.485265 -0.305194 11.00000 -1.20000 AFIX 0 C14 1 0.033071 0.611499 -0.221997 11.00000 0.03222 0.06398 = 0.04787 -0.00360 0.00116 0.00196 AFIX 13 H14 2 0.009869 0.658793 -0.190370 11.00000 -1.20000 AFIX 0 C15 1 0.131597 0.641374 -0.268030 11.00000 0.03782 0.05717 = 0.07355 -0.00577 0.01153 0.00112 C17 1 -0.030856 0.663849 -0.339237 11.00000 0.04929 0.05590 = 0.05258 0.00231 0.00425 0.00094 C18 1 -0.068963 0.627754 -0.411325 11.00000 0.10773 0.07916 = 0.05698 0.00084 -0.01386 -0.00596 AFIX 137 H18A 2 -0.053446 0.668501 -0.449012 11.00000 -1.50000 H18B 2 -0.149137 0.616236 -0.409705 11.00000 -1.50000 H18C 2 -0.028498 0.575609 -0.421022 11.00000 -1.50000 AFIX 0 C20 1 0.052029 0.532688 -0.175429 11.00000 0.04686 0.07381 = 0.06187 0.00520 0.00427 0.01015 AFIX 23 H20A 2 0.066551 0.483701 -0.206397 11.00000 -1.20000 H20B 2 0.118339 0.541355 -0.145008 11.00000 -1.20000 AFIX 0 C21 1 -0.049520 0.514786 -0.128580 11.00000 0.05762 0.06041 = 0.05141 0.01103 0.00564 0.01095 C22 1 -0.129993 0.454989 -0.148338 11.00000 0.07300 0.06132 = 0.08571 0.00169 0.01695 0.00161 AFIX 43 H22 2 -0.118440 0.420827 -0.188969 11.00000 -1.20000 AFIX 0 C23 1 -0.229966 0.445774 -0.106714 11.00000 0.07742 0.07661 = 0.13660 0.01834 0.02964 -0.01043 AFIX 43 H23 2 -0.284492 0.405689 -0.120215 11.00000 -1.20000 AFIX 0 C24 1 -0.247051 0.495141 -0.046999 11.00000 0.09332 0.10064 = 0.10453 0.03209 0.04648 0.01522 AFIX 43 H24 2 -0.313697 0.489368 -0.020281 11.00000 -1.20000 AFIX 0 C25 1 -0.165823 0.553726 -0.025965 11.00000 0.11564 0.11403 = 0.06590 0.00903 0.03301 0.01751 AFIX 43 H25 2 -0.176157 0.586240 0.015754 11.00000 -1.20000 AFIX 0 C26 1 -0.069658 0.563591 -0.067147 11.00000 0.07963 0.09582 = 0.05762 0.00279 0.00428 0.01097 AFIX 43 H26 2 -0.016177 0.604362 -0.053421 11.00000 -1.20000 AFIX 0 N1 3 0.453020 0.674858 -0.239508 11.00000 0.02946 0.06318 = 0.05857 0.00516 0.00568 -0.00001 N2 3 0.598612 0.696646 -0.160601 11.00000 0.03927 0.06927 = 0.05815 0.00333 -0.00435 -0.00153 N3 3 -0.056731 0.599697 -0.279337 11.00000 0.03769 0.05313 = 0.05365 -0.00166 -0.00059 -0.00120 N4 3 0.093137 0.666410 -0.332499 11.00000 0.04797 0.05651 = 0.06276 0.00136 0.01774 -0.00227 O1 4 0.739240 0.624505 -0.219840 11.00000 0.03808 0.11787 = 0.09325 0.02267 0.00607 0.02187 O2 4 0.229838 0.642183 -0.245202 11.00000 0.03026 0.09855 = 0.11513 -0.00950 0.00099 -0.00562 F1 5 0.470302 0.705643 0.118472 11.00000 0.11794 0.09004 = 0.16959 -0.00269 -0.03580 0.04302 F2 5 0.492512 0.576303 0.170934 11.00000 0.10635 0.09770 = 0.11704 0.02860 0.01717 -0.02172 F3 5 0.610990 0.683899 0.198585 11.00000 0.12485 0.08634 = 0.08145 -0.02366 -0.01073 0.00728 F4 5 0.669998 0.571730 0.135495 11.00000 0.10030 0.11100 = 0.11509 -0.02447 -0.00985 0.03780 F5 5 0.653664 0.699613 0.082537 11.00000 0.15704 0.15172 = 0.11631 0.03392 0.02698 -0.05571 F6 5 0.532797 0.594144 0.053779 11.00000 0.17042 0.10518 = 0.07339 -0.01655 -0.03378 0.00496 F7 5 -0.472211 0.298752 -0.133263 11.00000 0.07788 0.07607 = 0.12877 0.00036 -0.00469 0.01251 F8 5 -0.532801 0.412989 -0.069504 11.00000 0.15102 0.10976 = 0.07670 -0.02960 -0.03211 -0.00065 F9 5 -0.647088 0.298676 -0.082416 11.00000 0.12762 0.11161 = 0.08938 0.01502 0.03666 -0.01730 F10 5 -0.688391 0.420243 -0.140567 11.00000 0.11379 0.11858 = 0.11602 -0.02058 -0.01099 0.05027 F11 5 -0.625218 0.305404 -0.201898 11.00000 0.08892 0.10086 = 0.08013 -0.03544 0.00258 -0.01339 F12 5 -0.513419 0.420540 -0.189213 11.00000 0.13587 0.07784 = 0.09063 0.01449 0.00910 -0.02187 P1 6 0.570143 0.640096 0.125370 11.00000 0.07826 0.05621 = 0.05738 0.00269 0.00578 -0.00075 P2 6 -0.580893 0.360435 -0.134905 11.00000 0.07576 0.05665 = 0.05630 -0.00435 0.00097 0.00184 HKLF 4 Covalent radii and connectivity table for 2007src0607 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 P 1.100 C16 - N4 C19 - C17 C1 - N1 C7 C2 C2 - O1 N2 C1 C3 - N2 C4 - N2 C5 N1 C6 C5 - C4 C6 - C4 C7 - C1 C8 C8 - C13 C9 C7 C9 - C10 C8 C10 - C11 C9 C11 - C10 C12 C12 - C11 C13 C13 - C8 C12 C14 - N3 C15 C20 C15 - O2 N4 C14 C17 - N4 C18 C19 N3 C18 - C17 C20 - C21 C14 C21 - C22 C26 C20 C22 - C21 C23 C23 - C24 C22 C24 - C23 C25 C25 - C26 C24 C26 - C25 C21 N1 - C1 C4 N2 - C2 C4 C3 N3 - C14 C17 N4 - C15 C17 C16 O1 - C2 O2 - C15 F1 - P1 F2 - P1 F3 - P1 F4 - P1 F5 - P1 F6 - P1 F7 - P2 F8 - P2 F9 - P2 F10 - P2 F11 - P2 F12 - P2 P1 - F1 F6 F5 F3 F2 F4 P2 - F8 F9 F10 F12 F11 F7 44953 Reflections read, of which 82 rejected -15 =< h =< 14, -18 =< k =< 19, -20 =< l =< 23, Max. 2-theta = 54.24 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -11 6 7 -8.06 3.61 3 18.31 7 2 16 7.31 4.30 4 39.41 6 2 17 41.03 4.53 5 37.03 3 Inconsistent equivalents 7443 Unique reflections, of which 0 suppressed R(int) = 0.0883 R(sigma) = 0.0713 Friedel opposites not merged Maximum memory for data reduction = 3781 / 73945 Default effective X-H distances for T = 20.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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 = 4980 / 568230 wR2 = 0.1542 before cycle 1 for 7443 data and 437 / 437 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0789 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50968 0.00112 -0.301 OSF Mean shift/esd = 0.046 Maximum = -0.301 for OSF Max. shift = 0.004 A for H1N Max. dU =-0.001 for H3N Least-squares cycle 2 Maximum vector length = 511 Memory required = 4980 / 568230 wR2 = 0.1542 before cycle 2 for 7443 data and 437 / 437 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0789 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50953 0.00112 -0.138 OSF Mean shift/esd = 0.016 Maximum = -0.138 for OSF Max. shift = 0.002 A for H3N Max. dU = 0.000 for H3N Least-squares cycle 3 Maximum vector length = 511 Memory required = 4980 / 568230 wR2 = 0.1542 before cycle 3 for 7443 data and 437 / 437 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0789 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50952 0.00112 -0.004 OSF Mean shift/esd = 0.002 Maximum = -0.015 for tors H3A Max. shift = 0.001 A for H4N Max. dU = 0.000 for H3N Least-squares cycle 4 Maximum vector length = 511 Memory required = 4980 / 568230 wR2 = 0.1542 before cycle 4 for 7443 data and 437 / 437 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0789 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50952 0.00112 -0.002 OSF Mean shift/esd = 0.001 Maximum = -0.008 for tors H3A Max. shift = 0.000 A for H3B Max. dU = 0.000 for H4N 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 H16A 0.1365 0.7666 -0.3946 137 0.960 0.000 C16 N4 H16A H16B 0.1630 0.6782 -0.4312 137 0.960 0.000 C16 N4 H16A H16C 0.2416 0.7127 -0.3690 137 0.960 0.000 C16 N4 H16A H19A -0.0626 0.7670 -0.2741 137 0.960 0.000 C19 C17 H19A H19B -0.1668 0.7432 -0.3231 137 0.960 0.000 C19 C17 H19A H19C -0.0619 0.7910 -0.3566 137 0.960 0.000 C19 C17 H19A H1 0.5147 0.5535 -0.2316 13 0.980 0.000 C1 N1 C7 C2 H3A 0.7490 0.7256 -0.1161 137 0.960 0.000 C3 N2 H3A H3B 0.6513 0.7163 -0.0588 137 0.960 0.000 C3 N2 H3A H3C 0.6586 0.7986 -0.1072 137 0.960 0.000 C3 N2 H3A H5A 0.4508 0.8196 -0.1086 137 0.960 0.000 C5 C4 H5A H5B 0.3578 0.8038 -0.1680 137 0.960 0.000 C5 C4 H5A H5C 0.4799 0.8339 -0.1907 137 0.960 0.000 C5 C4 H5A H6A 0.4361 0.5911 -0.1170 137 0.960 0.000 C6 C4 H6A H6B 0.3355 0.6567 -0.1113 137 0.960 0.000 C6 C4 H6A H6C 0.4411 0.6653 -0.0599 137 0.960 0.000 C6 C4 H6A H7A 0.6222 0.5480 -0.3376 23 0.970 0.000 C7 C1 C8 H7B 0.5951 0.6441 -0.3542 23 0.970 0.000 C7 C1 C8 H9 0.5015 0.6350 -0.4653 43 0.930 0.000 C9 C10 C8 H10 0.3500 0.5955 -0.5365 43 0.930 0.000 C10 C11 C9 H11 0.2204 0.5006 -0.4933 43 0.930 0.000 C11 C10 C12 H12 0.2340 0.4470 -0.3774 43 0.930 0.000 C12 C11 C13 H13 0.3898 0.4853 -0.3052 43 0.930 0.000 C13 C8 C12 H14 0.0099 0.6588 -0.1904 13 0.980 0.000 C14 N3 C15 C20 H18A -0.0535 0.6686 -0.4490 137 0.960 0.000 C18 C17 H18A H18B -0.1491 0.6162 -0.4097 137 0.960 0.000 C18 C17 H18A H18C -0.0284 0.5757 -0.4211 137 0.960 0.000 C18 C17 H18A H20A 0.0666 0.4837 -0.2064 23 0.970 0.000 C20 C21 C14 H20B 0.1183 0.5414 -0.1450 23 0.970 0.000 C20 C21 C14 H22 -0.1184 0.4209 -0.1890 43 0.930 0.000 C22 C21 C23 H23 -0.2845 0.4057 -0.1203 43 0.930 0.000 C23 C24 C22 H24 -0.3137 0.4894 -0.0203 43 0.930 0.000 C24 C23 C25 H25 -0.1762 0.5862 0.0158 43 0.930 0.000 C25 C26 C24 H26 -0.0162 0.6044 -0.0534 43 0.930 0.000 C26 C25 C21 2007src0607 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C16 0.16477 0.70971 -0.38649 1.00000 0.08423 0.08031 0.10439 0.02074 0.05230 -0.00326 0.08964 0.00897 0.00038 0.00027 0.00026 0.00000 0.00314 0.00276 0.00353 0.00248 0.00295 0.00227 0.00148 H16A 0.13651 0.76657 -0.39462 1.00000 0.13446 0.00000 0.00000 H16B 0.16302 0.67818 -0.43115 1.00000 0.13446 0.00000 0.00000 H16C 0.24157 0.71267 -0.36900 1.00000 0.13446 0.00000 0.00000 C19 -0.08555 0.74905 -0.32167 1.00000 0.05450 0.06135 0.08146 0.00836 -0.00573 0.00894 0.06577 0.00660 0.00031 0.00021 0.00023 0.00000 0.00224 0.00214 0.00257 0.00192 0.00204 0.00165 0.00099 H19A -0.06258 0.76703 -0.27410 1.00000 0.09866 0.00000 0.00000 H19B -0.16681 0.74322 -0.32314 1.00000 0.09866 0.00000 0.00000 H19C -0.06195 0.79098 -0.35663 1.00000 0.09866 0.00000 0.00000 H1N 0.38338 0.66062 -0.24298 1.00000 0.04883 0.05781 0.00298 0.00208 0.00169 0.00000 0.00939 H2N 0.46587 0.72410 -0.27373 1.00000 0.07115 0.06101 0.00312 0.00238 0.00199 0.00000 0.01076 H3N -0.05326 0.54069 -0.29975 1.00000 0.06350 0.06136 0.00299 0.00233 0.00187 0.00000 0.01000 H4N -0.13030 0.60514 -0.25915 1.00000 0.06872 0.06306 0.00336 0.00230 0.00207 0.00000 0.01114 C1 0.53967 0.60722 -0.25382 1.00000 0.04446 0.05023 0.05919 0.00330 0.00220 0.00593 0.05129 0.00581 0.00027 0.00020 0.00018 0.00000 0.00185 0.00168 0.00203 0.00153 0.00177 0.00150 0.00080 H1 0.51465 0.55346 -0.23156 1.00000 0.06155 0.00000 0.00000 C2 0.63833 0.64350 -0.21045 1.00000 0.04156 0.06182 0.06651 0.01373 0.00168 0.00373 0.05663 0.00651 0.00028 0.00024 0.00020 0.00000 0.00196 0.00198 0.00229 0.00199 0.00169 0.00165 0.00085 C3 0.67059 0.73783 -0.10596 1.00000 0.07387 0.10566 0.07958 -0.00593 -0.01919 -0.00934 0.08637 0.00706 0.00039 0.00030 0.00024 0.00000 0.00299 0.00327 0.00297 0.00260 0.00254 0.00238 0.00132 H3A 0.74901 0.72555 -0.11607 1.00000 0.12956 0.00000 0.00000 H3B 0.65127 0.71632 -0.05878 1.00000 0.12956 0.00000 0.00000 H3C 0.65864 0.79862 -0.10721 1.00000 0.12956 0.00000 0.00000 C4 0.47486 0.70721 -0.16327 1.00000 0.04098 0.07485 0.05277 -0.00121 0.00333 -0.00107 0.05620 0.00600 0.00027 0.00023 0.00019 0.00000 0.00194 0.00225 0.00207 0.00174 0.00171 0.00161 0.00086 C5 0.43743 0.79954 -0.15707 1.00000 0.07298 0.07786 0.08419 -0.00618 0.01179 0.01815 0.07834 0.00746 0.00037 0.00024 0.00023 0.00000 0.00259 0.00244 0.00286 0.00216 0.00238 0.00203 0.00113 H5A 0.45083 0.81956 -0.10862 1.00000 0.11751 0.00000 0.00000 H5B 0.35779 0.80375 -0.16801 1.00000 0.11751 0.00000 0.00000 H5C 0.47991 0.83392 -0.19066 1.00000 0.11751 0.00000 0.00000 C6 0.41649 0.64975 -0.10772 1.00000 0.06239 0.10181 0.05983 0.00975 0.01213 -0.01149 0.07468 0.00706 0.00032 0.00027 0.00020 0.00000 0.00233 0.00278 0.00227 0.00217 0.00189 0.00228 0.00107 H6A 0.43610 0.59110 -0.11702 1.00000 0.11202 0.00000 0.00000 H6B 0.33554 0.65668 -0.11130 1.00000 0.11202 0.00000 0.00000 H6C 0.44108 0.66530 -0.05987 1.00000 0.11202 0.00000 0.00000 C7 0.56428 0.59189 -0.33356 1.00000 0.06304 0.06296 0.07015 -0.00462 0.00999 0.00591 0.06539 0.00658 0.00032 0.00024 0.00020 0.00000 0.00229 0.00205 0.00247 0.00180 0.00208 0.00177 0.00095 H7A 0.62224 0.54795 -0.33758 1.00000 0.07846 0.00000 0.00000 H7B 0.59508 0.64408 -0.35424 1.00000 0.07846 0.00000 0.00000 C8 0.46154 0.56473 -0.37790 1.00000 0.07024 0.06148 0.06956 -0.00962 0.00315 0.01597 0.06709 0.00683 0.00034 0.00023 0.00022 0.00000 0.00257 0.00205 0.00264 0.00190 0.00215 0.00193 0.00100 C9 0.44805 0.59661 -0.44718 1.00000 0.08990 0.09310 0.06562 -0.00706 0.00400 0.01144 0.08287 0.00823 0.00041 0.00028 0.00024 0.00000 0.00332 0.00284 0.00267 0.00235 0.00261 0.00260 0.00123 H9 0.50148 0.63498 -0.46528 1.00000 0.09945 0.00000 0.00000 C10 0.35785 0.57316 -0.49004 1.00000 0.10488 0.14552 0.07562 -0.00782 -0.00578 0.02665 0.10867 0.01154 0.00052 0.00046 0.00030 0.00000 0.00429 0.00512 0.00348 0.00348 0.00336 0.00405 0.00176 H10 0.35004 0.59554 -0.53650 1.00000 0.13041 0.00000 0.00000 C11 0.28080 0.51731 -0.46392 1.00000 0.10519 0.10136 0.10063 -0.03103 -0.04100 0.02468 0.10239 0.00930 0.00052 0.00037 0.00036 0.00000 0.00443 0.00368 0.00453 0.00336 0.00364 0.00343 0.00178 H11 0.22042 0.50058 -0.49325 1.00000 0.12287 0.00000 0.00000 C12 0.28912 0.48437 -0.39496 1.00000 0.08189 0.07009 0.14507 -0.01701 -0.01572 0.00202 0.09902 0.00899 0.00042 0.00029 0.00038 0.00000 0.00338 0.00273 0.00542 0.00311 0.00348 0.00240 0.00166 H12 0.23401 0.44705 -0.37737 1.00000 0.11882 0.00000 0.00000 C13 0.38196 0.50793 -0.35156 1.00000 0.08520 0.06112 0.09856 -0.00422 -0.01789 0.00346 0.08163 0.00754 0.00038 0.00025 0.00028 0.00000 0.00308 0.00229 0.00351 0.00230 0.00278 0.00215 0.00129 H13 0.38977 0.48530 -0.30519 1.00000 0.09795 0.00000 0.00000 C14 0.03306 0.61149 -0.22198 1.00000 0.03196 0.06374 0.04771 -0.00374 0.00105 0.00194 0.04781 0.00542 0.00026 0.00021 0.00017 0.00000 0.00163 0.00189 0.00183 0.00153 0.00146 0.00140 0.00077 H14 0.00986 0.65878 -0.19036 1.00000 0.05737 0.00000 0.00000 C15 0.13158 0.64138 -0.26805 1.00000 0.03781 0.05710 0.07348 -0.00604 0.01154 0.00116 0.05613 0.00617 0.00027 0.00023 0.00021 0.00000 0.00187 0.00190 0.00247 0.00193 0.00171 0.00155 0.00086 C17 -0.03086 0.66385 -0.33923 1.00000 0.04923 0.05576 0.05234 0.00213 0.00426 0.00093 0.05244 0.00581 0.00028 0.00020 0.00018 0.00000 0.00193 0.00183 0.00200 0.00150 0.00170 0.00144 0.00081 C18 -0.06895 0.62778 -0.41135 1.00000 0.10729 0.07926 0.05685 0.00064 -0.01393 -0.00596 0.08113 0.00678 0.00041 0.00026 0.00020 0.00000 0.00335 0.00259 0.00225 0.00198 0.00231 0.00252 0.00120 H18A -0.05353 0.66858 -0.44901 1.00000 0.12170 0.00000 0.00000 H18B -0.14909 0.61617 -0.40972 1.00000 0.12170 0.00000 0.00000 H18C -0.02838 0.57569 -0.42109 1.00000 0.12170 0.00000 0.00000 C20 0.05203 0.53269 -0.17543 1.00000 0.04684 0.07357 0.06161 0.00510 0.00426 0.01007 0.06067 0.00696 0.00030 0.00023 0.00021 0.00000 0.00201 0.00216 0.00221 0.00180 0.00182 0.00167 0.00090 H20A 0.06656 0.48370 -0.20640 1.00000 0.07281 0.00000 0.00000 H20B 0.11833 0.54136 -0.14500 1.00000 0.07281 0.00000 0.00000 C21 -0.04956 0.51478 -0.12859 1.00000 0.05719 0.06026 0.05132 0.01106 0.00558 0.01085 0.05625 0.00650 0.00031 0.00021 0.00019 0.00000 0.00218 0.00188 0.00204 0.00166 0.00184 0.00166 0.00085 C22 -0.13000 0.45502 -0.14835 1.00000 0.07288 0.06119 0.08563 0.00164 0.01680 0.00158 0.07323 0.00758 0.00035 0.00024 0.00024 0.00000 0.00267 0.00219 0.00305 0.00205 0.00238 0.00186 0.00113 H22 -0.11841 0.42087 -0.18898 1.00000 0.08788 0.00000 0.00000 C23 -0.23001 0.44575 -0.10676 1.00000 0.07714 0.07643 0.13690 0.01830 0.02981 -0.01016 0.09682 0.01033 0.00041 0.00030 0.00034 0.00000 0.00309 0.00285 0.00492 0.00305 0.00327 0.00237 0.00162 H23 -0.28453 0.40567 -0.12028 1.00000 0.11619 0.00000 0.00000 C24 -0.24707 0.49511 -0.04704 1.00000 0.09327 0.09998 0.10503 0.03207 0.04656 0.01521 0.09943 0.01225 0.00047 0.00034 0.00034 0.00000 0.00372 0.00354 0.00429 0.00325 0.00323 0.00306 0.00169 H24 -0.31373 0.48935 -0.02033 1.00000 0.11931 0.00000 0.00000 C25 -0.16582 0.55369 -0.02598 1.00000 0.11534 0.11399 0.06615 0.00899 0.03273 0.01747 0.09849 0.01135 0.00050 0.00037 0.00027 0.00000 0.00417 0.00390 0.00305 0.00275 0.00310 0.00339 0.00161 H25 -0.17615 0.58616 0.01576 1.00000 0.11819 0.00000 0.00000 C26 -0.06964 0.56359 -0.06716 1.00000 0.07940 0.09587 0.05745 0.00287 0.00431 0.01078 0.07757 0.00813 0.00039 0.00029 0.00022 0.00000 0.00292 0.00285 0.00243 0.00216 0.00230 0.00237 0.00114 H26 -0.01615 0.60436 -0.05343 1.00000 0.09309 0.00000 0.00000 N1 0.45305 0.67488 -0.23949 1.00000 0.02936 0.06312 0.05858 0.00514 0.00565 0.00003 0.05035 0.00525 0.00024 0.00019 0.00016 0.00000 0.00148 0.00174 0.00181 0.00137 0.00135 0.00125 0.00069 N2 0.59861 0.69663 -0.16060 1.00000 0.03906 0.06922 0.05783 0.00332 -0.00436 -0.00149 0.05537 0.00487 0.00022 0.00019 0.00016 0.00000 0.00156 0.00178 0.00182 0.00148 0.00146 0.00128 0.00073 N3 -0.05672 0.59971 -0.27935 1.00000 0.03756 0.05291 0.05353 -0.00167 -0.00056 -0.00111 0.04800 0.00466 0.00023 0.00018 0.00016 0.00000 0.00164 0.00157 0.00163 0.00128 0.00135 0.00120 0.00065 N4 0.09315 0.66641 -0.33251 1.00000 0.04788 0.05646 0.06250 0.00142 0.01762 -0.00229 0.05561 0.00509 0.00022 0.00017 0.00017 0.00000 0.00167 0.00160 0.00190 0.00137 0.00154 0.00123 0.00072 O1 0.73923 0.62450 -0.21983 1.00000 0.03804 0.11773 0.09299 0.02254 0.00610 0.02190 0.08292 0.00548 0.00020 0.00020 0.00017 0.00000 0.00138 0.00225 0.00215 0.00177 0.00129 0.00142 0.00089 O2 0.22986 0.64213 -0.24520 1.00000 0.03017 0.09851 0.11472 -0.00931 0.00102 -0.00558 0.08113 0.00485 0.00019 0.00020 0.00017 0.00000 0.00125 0.00180 0.00238 0.00190 0.00138 0.00130 0.00082 F1 0.47030 0.70564 0.11849 1.00000 0.11781 0.08973 0.16962 -0.00280 -0.03586 0.04306 0.12572 0.00550 0.00027 0.00016 0.00020 0.00000 0.00239 0.00177 0.00301 0.00192 0.00234 0.00166 0.00114 F2 0.49250 0.57631 0.17093 1.00000 0.10626 0.09774 0.11680 0.02877 0.01714 -0.02194 0.10693 0.00535 0.00025 0.00017 0.00017 0.00000 0.00203 0.00169 0.00226 0.00158 0.00177 0.00156 0.00091 F3 0.61094 0.68389 0.19859 1.00000 0.12492 0.08633 0.08114 -0.02375 -0.01078 0.00718 0.09747 0.00442 0.00025 0.00017 0.00013 0.00000 0.00222 0.00155 0.00171 0.00134 0.00155 0.00150 0.00084 F4 0.66997 0.57173 0.13547 1.00000 0.10017 0.11085 0.11503 -0.02444 -0.00992 0.03795 0.10868 0.00500 0.00023 0.00018 0.00017 0.00000 0.00200 0.00186 0.00220 0.00179 0.00175 0.00155 0.00091 F5 0.65361 0.69962 0.08253 1.00000 0.15706 0.15255 0.11622 0.03432 0.02698 -0.05627 0.14194 0.00645 0.00034 0.00024 0.00018 0.00000 0.00312 0.00288 0.00246 0.00219 0.00233 0.00248 0.00134 F6 0.53279 0.59414 0.05378 1.00000 0.17049 0.10507 0.07306 -0.01654 -0.03375 0.00497 0.11621 0.00489 0.00031 0.00017 0.00015 0.00000 0.00286 0.00177 0.00159 0.00148 0.00189 0.00200 0.00100 F7 -0.47220 0.29874 -0.13329 1.00000 0.07776 0.07596 0.12859 0.00045 -0.00468 0.01253 0.09410 0.00436 0.00021 0.00014 0.00016 0.00000 0.00163 0.00138 0.00219 0.00152 0.00158 0.00118 0.00078 F8 -0.53282 0.41296 -0.06950 1.00000 0.15093 0.10982 0.07653 -0.02980 -0.03221 -0.00051 0.11243 0.00447 0.00029 0.00018 0.00014 0.00000 0.00264 0.00185 0.00172 0.00145 0.00180 0.00194 0.00097 F9 -0.64705 0.29868 -0.08242 1.00000 0.12749 0.11170 0.08955 0.01523 0.03695 -0.01736 0.10958 0.00558 0.00028 0.00019 0.00015 0.00000 0.00239 0.00205 0.00185 0.00156 0.00175 0.00176 0.00096 F10 -0.68837 0.42026 -0.14057 1.00000 0.11362 0.11851 0.11617 -0.02060 -0.01108 0.05035 0.11610 0.00549 0.00025 0.00019 0.00017 0.00000 0.00224 0.00203 0.00234 0.00192 0.00187 0.00171 0.00100 F11 -0.62519 0.30541 -0.20191 1.00000 0.08885 0.10080 0.08014 -0.03547 0.00250 -0.01339 0.08993 0.00393 0.00022 0.00017 0.00013 0.00000 0.00169 0.00166 0.00165 0.00139 0.00133 0.00138 0.00076 F12 -0.51343 0.42055 -0.18920 1.00000 0.13607 0.07772 0.09051 0.01462 0.00917 -0.02208 0.10143 0.00493 0.00027 0.00016 0.00015 0.00000 0.00239 0.00144 0.00180 0.00130 0.00164 0.00155 0.00088 P1 0.57013 0.64009 0.12537 1.00000 0.07819 0.05609 0.05735 0.00273 0.00580 -0.00076 0.06388 0.00175 0.00009 0.00006 0.00005 0.00000 0.00068 0.00048 0.00055 0.00046 0.00049 0.00048 0.00028 P2 -0.58089 0.36044 -0.13490 1.00000 0.07563 0.05657 0.05627 -0.00435 0.00094 0.00183 0.06282 0.00171 0.00009 0.00006 0.00005 0.00000 0.00066 0.00049 0.00054 0.00047 0.00047 0.00047 0.00027 Final Structure Factor Calculation for 2007src0607 in P2(1)2(1)2(1) Total number of l.s. parameters = 437 Maximum vector length = 511 Memory required = 4545 / 27090 wR2 = 0.1542 before cycle 5 for 7443 data and 2 / 437 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0789 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0549 for 4178 Fo > 4sig(Fo) and 0.1229 for all 7443 data wR2 = 0.1542, GooF = S = 1.011, Restrained GooF = 1.011 for all data Flack x parameter = -0.1210 with esd 0.1316 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 46.00 for non-hydrogen and 38.00 for hydrogen atoms Principal mean square atomic displacements U 0.1504 0.0832 0.0353 C16 0.0847 0.0668 0.0458 C19 0.0613 0.0518 0.0407 C1 0.0785 0.0506 0.0409 C2 0.1082 0.0959 0.0550 C3 0.0750 0.0536 0.0401 C4 0.0952 0.0879 0.0519 C5 0.1059 0.0732 0.0450 C6 0.0772 0.0677 0.0512 C7 0.0834 0.0724 0.0455 C8 0.1033 0.0832 0.0622 C9 0.1598 0.0919 0.0744 C10 0.1674 0.0793 0.0605 C11 0.1523 0.0785 0.0663 C12 0.1116 0.0728 0.0605 C13 0.0647 0.0470 0.0317 C14 0.0783 0.0560 0.0340 C15 0.0578 0.0533 0.0462 C17 0.1120 0.0782 0.0532 C18 0.0791 0.0597 0.0431 C20 0.0757 0.0495 0.0436 C21 0.0974 0.0616 0.0608 C22 0.1516 0.0863 0.0526 C23 0.1644 0.0842 0.0497 C24 0.1444 0.1013 0.0498 C25 0.1017 0.0744 0.0566 C26 0.0667 0.0560 0.0283 N1 0.0703 0.0577 0.0381 N2 0.0549 0.0516 0.0375 N3 0.0743 0.0568 0.0358 N4 0.1360 0.0803 0.0324 O1 0.1191 0.0946 0.0297 O2 0.1934 0.1286 0.0551 F1 0.1376 0.1230 0.0602 F2 0.1316 0.1011 0.0597 F3 0.1584 0.1022 0.0654 F4 0.2114 0.1515 0.0630 F5 0.1823 0.1083 0.0581 F6 0.1290 0.0892 0.0641 F7 0.1650 0.1214 0.0509 F8 0.1514 0.1194 0.0579 F9 0.1751 0.1083 0.0648 F10 0.1310 0.0863 0.0525 F11 0.1438 0.0997 0.0608 F12 0.0797 0.0588 0.0531 P1 0.0758 0.0607 0.0519 P2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.014 0.018 0.023 0.029 0.039 0.054 0.078 0.127 1.000 Number in group 804. 790. 659. 735. 780. 722. 737. 732. 739. 745. GooF 0.904 0.904 0.898 1.002 1.048 1.076 1.183 1.084 1.005 0.970 K 0.299 1.099 0.841 1.079 0.949 0.944 0.993 1.004 1.025 0.968 Resolution(A) 0.78 0.81 0.84 0.88 0.93 0.98 1.06 1.16 1.33 1.66 inf Number in group 768. 726. 740. 762. 751. 730. 734. 747. 739. 746. GooF 0.853 0.912 0.905 0.996 1.012 1.107 1.054 1.040 0.998 1.191 K 0.493 0.930 1.053 1.013 0.990 0.998 1.025 1.043 1.018 0.951 R1 0.514 0.420 0.348 0.280 0.193 0.113 0.065 0.052 0.036 0.039 ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** Recommended weighting scheme: WGHT 0.0769 0.1688 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) 1 1 2 6359.64 11412.26 5.40 0.530 6.58 -1 1 2 7305.44 11414.23 4.65 0.530 6.58 3 0 22 127.59 30.69 4.52 0.027 0.82 5 0 6 606.88 417.55 4.50 0.101 1.87 12 0 6 9.02 62.55 4.45 0.039 0.93 -6 10 14 -22.30 37.60 4.05 0.030 0.90 2 6 7 81.83 123.63 3.89 0.055 1.77 0 2 9 104.21 65.10 3.86 0.040 1.98 0 9 1 119.81 77.17 3.86 0.044 1.73 -2 2 1 147.06 104.64 3.77 0.051 4.55 -1 15 9 -17.17 25.10 3.71 0.025 0.93 7 0 8 9.20 47.10 3.71 0.034 1.36 -4 7 13 225.44 153.17 3.67 0.061 1.11 -6 16 6 70.60 4.12 3.59 0.010 0.84 8 15 0 65.43 18.87 3.58 0.022 0.85 0 10 3 769.61 571.61 3.56 0.119 1.51 1 15 5 45.08 91.80 3.54 0.047 1.00 0 14 0 1502.93 1081.33 3.49 0.163 1.12 0 8 2 13.35 0.35 3.43 0.003 1.91 -4 2 5 788.86 601.23 3.38 0.122 2.21 8 12 2 47.03 18.70 3.35 0.021 0.97 -9 4 3 225.05 315.39 3.33 0.088 1.21 3 3 9 215.96 158.18 3.29 0.062 1.71 -7 4 10 216.68 147.16 3.28 0.060 1.18 2 2 1 126.94 93.03 3.28 0.048 4.55 -7 3 14 167.22 99.77 3.26 0.050 1.02 8 6 14 67.43 22.82 3.23 0.024 0.92 2 0 1 120.26 166.84 3.22 0.064 5.60 -6 9 11 11.56 44.77 3.20 0.033 1.03 -9 7 3 64.51 34.88 3.17 0.029 1.11 -1 14 2 128.62 83.76 3.17 0.045 1.10 -3 3 9 217.30 157.98 3.17 0.062 1.71 -3 10 16 -8.38 28.21 3.16 0.026 0.90 3 12 10 -9.09 20.48 3.15 0.022 1.03 9 4 1 156.53 219.37 3.14 0.073 1.24 9 12 5 27.76 65.04 3.13 0.040 0.89 -5 2 2 328.73 248.87 3.10 0.078 2.19 7 0 2 971.53 755.66 3.07 0.136 1.65 -7 11 8 57.59 95.10 3.07 0.048 0.98 4 0 8 42.15 15.91 3.07 0.020 1.81 2 18 0 86.95 34.10 3.05 0.029 0.86 6 1 6 396.86 297.80 3.05 0.086 1.64 6 4 15 57.32 22.25 3.05 0.023 1.01 2 13 12 49.20 95.00 3.04 0.048 0.93 6 0 17 -6.05 21.92 3.03 0.023 0.95 11 0 7 19.46 68.24 2.93 0.041 0.99 7 1 4 37.85 18.09 2.93 0.021 1.57 8 9 13 69.19 29.88 2.92 0.027 0.88 4 2 5 752.34 595.68 2.90 0.121 2.21 5 6 0 17.93 0.64 2.87 0.004 1.74 Bond lengths and angles C16 - Distance Angles N4 1.4690 (0.0044) C16 - C19 - Distance Angles C17 1.5130 (0.0045) C19 - C1 - Distance Angles N1 1.4912 (0.0039) C7 1.5180 (0.0049) 114.44 (0.27) C2 1.5187 (0.0049) 99.42 (0.26) 115.07 (0.29) C1 - N1 C7 C2 - Distance Angles O1 1.2349 (0.0038) N2 1.3237 (0.0045) 125.93 (0.35) C1 1.5187 (0.0049) 124.75 (0.35) 109.30 (0.27) C2 - O1 N2 C3 - Distance Angles N2 1.4650 (0.0047) C3 - C4 - Distance Angles N2 1.4650 (0.0042) C5 1.5120 (0.0052) 113.20 (0.31) N1 1.5158 (0.0046) 99.30 (0.27) 109.79 (0.31) C6 1.5251 (0.0047) 110.97 (0.31) 112.30 (0.31) 110.56 (0.29) C4 - N2 C5 N1 C5 - Distance Angles C4 1.5120 (0.0052) C5 - C6 - Distance Angles C4 1.5251 (0.0047) C6 - C7 - Distance Angles C1 1.5180 (0.0049) C8 1.5191 (0.0053) 114.47 (0.31) C7 - C1 C8 - Distance Angles C13 1.3778 (0.0058) C9 1.3807 (0.0055) 118.73 (0.41) C7 1.5191 (0.0053) 121.99 (0.38) 119.27 (0.39) C8 - C13 C9 C9 - Distance Angles C10 1.3725 (0.0069) C8 1.3807 (0.0055) 121.72 (0.49) C9 - C10 C10 - Distance Angles C11 1.3468 (0.0076) C9 1.3725 (0.0069) 119.10 (0.52) C10 - C11 C11 - Distance Angles C10 1.3468 (0.0076) C12 1.3756 (0.0075) 121.69 (0.52) C11 - C10 C12 - Distance Angles C11 1.3756 (0.0075) C13 1.4026 (0.0065) 119.01 (0.54) C12 - C11 C13 - Distance Angles C8 1.3778 (0.0058) C12 1.4026 (0.0065) 119.73 (0.48) C13 - C8 C14 - Distance Angles N3 1.5059 (0.0039) C15 1.5105 (0.0045) 100.37 (0.25) C20 1.5172 (0.0047) 113.68 (0.27) 117.16 (0.28) C14 - N3 C15 C15 - Distance Angles O2 1.2299 (0.0041) N4 1.3307 (0.0045) 128.49 (0.33) C14 1.5105 (0.0045) 122.04 (0.35) 109.46 (0.28) C15 - O2 N4 C17 - Distance Angles N4 1.4636 (0.0042) C18 1.5125 (0.0051) 112.30 (0.32) C19 1.5130 (0.0045) 112.40 (0.28) 112.96 (0.31) N3 1.5219 (0.0042) 98.94 (0.26) 109.51 (0.27) 109.80 (0.27) C17 - N4 C18 C19 C18 - Distance Angles C17 1.5125 (0.0051) C18 - C20 - Distance Angles C21 1.5004 (0.0048) C14 1.5172 (0.0047) 111.11 (0.28) C20 - C21 C21 - Distance Angles C22 1.3777 (0.0052) C26 1.3861 (0.0053) 118.17 (0.36) C20 1.5004 (0.0048) 121.35 (0.35) 120.25 (0.37) C21 - C22 C26 C22 - Distance Angles C21 1.3777 (0.0052) C23 1.4114 (0.0061) 119.84 (0.42) C22 - C21 C23 - Distance Angles C24 1.3594 (0.0073) C22 1.4114 (0.0061) 120.34 (0.48) C23 - C24 C24 - Distance Angles C23 1.3594 (0.0073) C25 1.3785 (0.0075) 120.17 (0.47) C24 - C23 C25 - Distance Angles C26 1.3710 (0.0063) C24 1.3785 (0.0075) 119.35 (0.49) C25 - C26 C26 - Distance Angles C25 1.3710 (0.0063) C21 1.3861 (0.0053) 122.10 (0.47) C26 - C25 N1 - Distance Angles C1 1.4912 (0.0039) C4 1.5158 (0.0046) 106.56 (0.25) N1 - C1 N2 - Distance Angles C2 1.3237 (0.0045) C4 1.4650 (0.0042) 113.43 (0.29) C3 1.4650 (0.0047) 123.34 (0.30) 123.17 (0.32) N2 - C2 C4 N3 - Distance Angles C14 1.5059 (0.0039) C17 1.5219 (0.0042) 106.83 (0.23) N3 - C14 N4 - Distance Angles C15 1.3307 (0.0045) C17 1.4636 (0.0042) 113.95 (0.28) C16 1.4690 (0.0044) 123.12 (0.32) 121.74 (0.33) N4 - C15 C17 O1 - Distance Angles C2 1.2349 (0.0038) O1 - O2 - Distance Angles C15 1.2299 (0.0041) O2 - F1 - Distance Angles P1 1.5626 (0.0027) F1 - F2 - Distance Angles P1 1.5911 (0.0027) F2 - F3 - Distance Angles P1 1.5881 (0.0026) F3 - F4 - Distance Angles P1 1.5976 (0.0026) F4 - F5 - Distance Angles P1 1.5658 (0.0030) F5 - F6 - Distance Angles P1 1.5659 (0.0027) F6 - F7 - Distance Angles P2 1.6007 (0.0025) F7 - F8 - Distance Angles P2 1.5644 (0.0026) F8 - F9 - Distance Angles P2 1.5726 (0.0027) F9 - F10 - Distance Angles P2 1.5749 (0.0027) F10 - F11 - Distance Angles P2 1.5930 (0.0024) F11 - F12 - Distance Angles P2 1.5853 (0.0026) F12 - P1 - Distance Angles F1 1.5626 (0.0027) F6 1.5659 (0.0027) 91.21 (0.17) F5 1.5658 (0.0030) 92.33 (0.21) 91.27 (0.19) F3 1.5881 (0.0026) 90.79 (0.16) 177.95 (0.17) 89.09 (0.18) F2 1.5911 (0.0027) 91.28 (0.17) 89.87 (0.17) 176.19 (0.20) 89.64 (0.16) F4 1.5976 (0.0026) 177.64 (0.19) 89.89 (0.16) 89.73 (0.20) 88.09 (0.15) 86.64 (0.16) P1 - F1 F6 F5 F3 F2 P2 - Distance Angles F8 1.5644 (0.0025) F9 1.5726 (0.0027) 91.46 (0.17) F10 1.5749 (0.0027) 91.72 (0.17) 90.45 (0.18) F12 1.5853 (0.0026) 89.77 (0.16) 178.44 (0.17) 90.47 (0.18) F11 1.5930 (0.0024) 177.83 (0.17) 89.14 (0.15) 90.36 (0.16) 89.59 (0.15) F7 1.6007 (0.0025) 90.74 (0.16) 90.80 (0.16) 177.21 (0.17) 88.22 (0.15) 87.17 (0.14) P2 - F8 F9 F10 F12 F11 FMAP and GRID set by program FMAP 2 3 22 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.1038 for 4146 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.4519 0.6395 0.1807 [ 1.11 A from F2 ] Deepest hole -0.31 at 0.6339 0.6550 0.1402 [ 0.83 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 4402 / 29403 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4519 0.6395 0.1807 1.00000 0.05 0.24 1.11 F2 1.56 F1 1.72 P1 2.02 F3 Q2 1 0.6041 0.5648 0.1690 1.00000 0.05 0.17 1.00 F4 1.33 F2 1.48 P1 1.84 H3N Q3 1 0.0543 0.7035 -0.4628 1.00000 0.05 0.16 1.40 H18A 1.46 H16B 1.87 H16A 1.92 C16 Q4 1 -0.5479 0.2996 -0.0345 1.00000 0.05 0.16 1.46 F9 1.89 F8 2.03 F7 2.04 H18A Q5 1 0.4207 0.9228 -0.1328 1.00000 0.05 0.15 1.71 H5A 1.88 H5C 1.99 C5 2.09 H7A Q6 1 0.4739 0.6770 -0.0524 1.00000 0.05 0.15 0.45 H6C 1.30 C6 1.85 H6A 1.98 H6B Q7 1 0.4590 0.8576 -0.1229 1.00000 0.05 0.15 0.66 H5A 1.13 C5 1.33 H5C 1.68 H5B Q8 1 0.4563 0.6999 -0.1458 1.00000 0.05 0.14 0.41 C4 1.15 C6 1.59 C5 1.68 H6C Q9 1 -0.0803 0.7041 -0.4236 1.00000 0.05 0.14 0.79 H18A 1.22 C18 1.61 H18B 1.78 C17 Q10 1 0.6867 0.6333 0.0997 1.00000 0.05 0.14 1.15 F5 1.18 F4 1.45 P1 2.09 F6 Q11 1 0.0937 0.7744 -0.3194 1.00000 0.05 0.14 1.48 H16A 1.70 N4 1.80 C16 1.97 H19C Q12 1 0.7361 0.7829 -0.1613 1.00000 0.05 0.14 1.23 H3A 1.37 H3C 1.46 C3 2.10 N2 Q13 1 0.5740 0.6979 0.0487 1.00000 0.05 0.13 1.12 F5 1.68 P1 1.69 F6 1.78 F1 Q14 1 -0.0487 0.5646 -0.2949 1.00000 0.05 0.13 0.39 H3N 0.63 N3 1.32 H4N 1.77 C17 Q15 1 -0.0201 0.8336 -0.4233 1.00000 0.05 0.13 1.48 H19C 2.03 H10 2.13 H9 2.18 H16A Q16 1 0.4450 0.6943 -0.0641 1.00000 0.05 0.13 0.46 H6C 1.11 C6 1.66 H6B 1.87 C4 Q17 1 0.0550 0.4362 -0.1540 1.00000 0.05 0.13 1.23 H20A 1.56 C20 1.80 C21 1.81 H20B Q18 1 -0.0868 0.6770 -0.4443 1.00000 0.05 0.12 0.42 H18A 1.00 C18 1.36 H18B 1.78 H18C Q19 1 0.5471 0.5799 -0.0801 1.00000 0.05 0.12 1.48 H6A 1.86 H6C 1.95 C6 2.43 H24 Q20 1 -0.0424 0.5535 -0.4787 1.00000 0.05 0.12 1.13 H18C 1.73 C18 1.88 H18A 1.97 F8 Shortest distances between peaks (including symmetry equivalents) 6 16 0.48 9 18 0.57 5 7 1.13 3 4 1.33 8 16 1.51 3 9 1.74 3 18 1.74 6 8 1.77 6 19 1.82 10 13 1.91 2 10 1.93 18 20 2.10 9 15 2.14 1 2 2.15 16 19 2.17 15 17 2.18 2 14 2.22 6 13 2.23 4 18 2.33 3 15 2.33 8 19 2.47 7 8 2.50 11 15 2.51 4 9 2.54 13 16 2.58 15 18 2.60 9 20 2.60 3 20 2.62 4 20 2.73 7 16 2.78 19 20 2.80 1 12 2.83 3 11 2.90 5 10 2.95 1 13 2.97 Time profile in seconds ----------------------- 0.13: 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 0.00: 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 0.01: Analyse other restraints etc. 7.12: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.01: Generate idealized H-atoms 8.95: Structure factors and derivatives 13.02: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 1.31: Solve l.s. equations 0.00: Generate HTAB table 0.01: Other dependent quantities, CIF, tables 0.18: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.15: Fourier summations 0.03: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0607 finished at 22:51:24 Total CPU time: 31.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++