++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker Analytical X-ray Solutions All Rights Reserved + + 2007src1050 started at 16:39:46 on 15-Aug-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src1050 in Pc New: P21/c CELL 0.71073 7.7257 21.1223 11.5315 90.000 96.654 90.000 ZERR 4 0.0002 0.0007 0.0002 0.000 0.002 0.000 LATT 1 SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H N O S UNIT 80 116 4 8 4 V = 1869.09 F(000) = 752.0 Mu = 0.19 mm-1 Cell Wt = 1390.01 Rho = 1.235 SIZE 0.26x0.06x0.02 L.S. 6 FMAP 2 PLAN 20 ACTA BOND $H OMIT -3 55 SHEL 7 0.77 OMIT -2 1 4 OMIT -3 3 5 OMIT -3 2 6 WGHT 0.058100 4.344700 FVAR 0.65127 S1 5 0.34207 0.30956 0.37340 11.00000 0.02243 0.03703 = 0.02355 0.00073 -0.00101 -0.00329 O1 4 0.27610 0.33131 0.47738 11.00000 0.02607 0.03868 = 0.02953 -0.00239 0.00199 -0.00383 O2 4 0.26623 0.33121 0.26055 11.00000 0.02900 0.04511 = 0.02655 0.00374 -0.00624 -0.00196 N1 3 0.54681 0.32866 0.38437 11.00000 0.02383 0.04407 = 0.02287 0.00349 -0.00114 -0.00583 C1 1 0.65721 0.32435 0.49973 11.00000 0.02246 0.03776 = 0.02225 0.00534 -0.00156 -0.00442 AFIX 13 H1 2 0.60005 0.29568 0.55024 11.00000 -1.20000 AFIX 0 C2 1 0.82608 0.29201 0.46820 11.00000 0.02178 0.05090 = 0.03046 0.00374 -0.00066 -0.00342 AFIX 13 H2 2 0.92764 0.30861 0.51768 11.00000 -1.20000 AFIX 0 C3 1 0.83493 0.31084 0.34067 11.00000 0.02827 0.05749 = 0.03180 0.00327 0.00613 -0.00466 AFIX 23 H3A 2 0.88693 0.35241 0.33572 11.00000 -1.20000 H3B 2 0.90263 0.28039 0.30193 11.00000 -1.20000 AFIX 0 C4 1 0.64526 0.31115 0.28611 11.00000 0.02949 0.05112 = 0.02602 0.00258 0.00234 -0.00425 AFIX 23 H4A 2 0.62716 0.34200 0.22356 11.00000 -1.20000 H4B 2 0.61049 0.26971 0.25550 11.00000 -1.20000 AFIX 0 C5 1 0.81534 0.22172 0.48193 11.00000 0.02653 0.04474 = 0.03175 -0.00330 -0.00033 -0.00230 AFIX 43 H5 2 0.72287 0.20112 0.43877 11.00000 -1.20000 AFIX 0 C6 1 0.92479 0.18665 0.54944 11.00000 0.03319 0.04612 = 0.02788 -0.00238 0.00094 -0.00078 AFIX 43 H6 2 1.01820 0.20686 0.59232 11.00000 -1.20000 AFIX 0 C7 1 0.91039 0.11655 0.56250 11.00000 0.04481 0.05070 = 0.03686 -0.00184 0.00467 0.00473 AFIX 137 H7A 2 0.80193 0.10226 0.52188 11.00000 -1.50000 H7B 2 0.91473 0.10603 0.64377 11.00000 -1.50000 H7C 2 1.00526 0.09630 0.53024 11.00000 -1.50000 AFIX 0 C8 1 0.67576 0.38934 0.55860 11.00000 0.02537 0.03925 = 0.02654 0.00402 -0.00270 -0.00548 AFIX 13 H8 2 0.55761 0.40378 0.56789 11.00000 -1.20000 AFIX 0 C9 1 0.75814 0.44053 0.48899 11.00000 0.03132 0.04600 = 0.03221 0.01165 -0.00724 -0.01057 AFIX 23 H9A 2 0.87653 0.42836 0.47890 11.00000 -1.20000 H9B 2 0.69291 0.44414 0.41218 11.00000 -1.20000 AFIX 0 C10 1 0.76025 0.50425 0.55023 11.00000 0.03815 0.04069 = 0.04930 0.00918 -0.01095 -0.00913 AFIX 23 H10A 2 0.64151 0.51799 0.55511 11.00000 -1.20000 H10B 2 0.81598 0.53539 0.50510 11.00000 -1.20000 AFIX 0 C11 1 0.85795 0.50013 0.67278 11.00000 0.04253 0.04112 = 0.04876 -0.00138 -0.00983 -0.01085 AFIX 23 H11A 2 0.97982 0.49095 0.66755 11.00000 -1.20000 H11B 2 0.85119 0.54056 0.71192 11.00000 -1.20000 AFIX 0 C12 1 0.78082 0.44861 0.74374 11.00000 0.04893 0.05920 = 0.03481 -0.00581 -0.00691 -0.01627 AFIX 23 H12A 2 0.66382 0.46071 0.75750 11.00000 -1.20000 H12B 2 0.85056 0.44471 0.81895 11.00000 -1.20000 AFIX 0 C13 1 0.77437 0.38484 0.68171 11.00000 0.03923 0.04521 = 0.02675 0.00557 -0.00652 -0.00894 AFIX 23 H13A 2 0.71731 0.35412 0.72695 11.00000 -1.20000 H13B 2 0.89222 0.37021 0.67647 11.00000 -1.20000 AFIX 0 C14 1 0.32913 0.22612 0.37153 11.00000 0.02196 0.03726 = 0.02554 -0.00008 0.00103 -0.00371 C15 1 0.35157 0.19288 0.47636 11.00000 0.02748 0.04257 = 0.02355 -0.00109 0.00057 -0.00557 AFIX 43 H15 2 0.36908 0.21450 0.54699 11.00000 -1.20000 AFIX 0 C16 1 0.34763 0.12741 0.47468 11.00000 0.03179 0.03958 = 0.03318 0.00415 0.00036 -0.00534 AFIX 43 H16 2 0.36281 0.10534 0.54491 11.00000 -1.20000 AFIX 0 C17 1 0.32134 0.09367 0.36984 11.00000 0.02662 0.03902 = 0.03828 -0.00159 -0.00085 -0.00483 C18 1 0.29982 0.12802 0.26651 11.00000 0.03522 0.04388 = 0.03059 -0.00609 0.00021 -0.00590 AFIX 43 H18 2 0.28215 0.10642 0.19586 11.00000 -1.20000 AFIX 0 C19 1 0.30392 0.19328 0.26576 11.00000 0.03046 0.04523 = 0.02231 -0.00052 -0.00236 -0.00646 AFIX 43 H19 2 0.29002 0.21525 0.19542 11.00000 -1.20000 AFIX 0 C20 1 0.30976 0.02282 0.36865 11.00000 0.05280 0.04046 = 0.05037 -0.00396 -0.00379 -0.00704 AFIX 3 H20A 2 0.19193 0.00875 0.34481 11.00000 -1.20000 H20B 2 0.34268 0.00879 0.45240 11.00000 -1.20000 H20C 2 0.39185 0.00451 0.32159 11.00000 -1.20000 AFIX 0 HKLF 4 1 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 Covalent radii and connectivity table for 2007src1050 in Pc New: P21/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 S1 - O1 O2 N1 C14 O1 - S1 O2 - S1 N1 - C4 C1 S1 C1 - N1 C8 C2 C2 - C5 C3 C1 C3 - C4 C2 C4 - N1 C3 C5 - C6 C2 C6 - C5 C7 C7 - C6 C8 - C9 C1 C13 C9 - C10 C8 C10 - C9 C11 C11 - C12 C10 C12 - C13 C11 C13 - C12 C8 C14 - C15 C19 S1 C15 - C16 C14 C16 - C15 C17 C17 - C18 C16 C20 C18 - C19 C17 C19 - C18 C14 C20 - C17 h k l Fo^2 Sigma Why rejected 0 7 0 26.97 5.61 observed but should be systematically absent 0 9 0 54.21 6.54 observed but should be systematically absent 0 9 0 55.58 5.78 observed but should be systematically absent 0 11 0 35.53 6.62 observed but should be systematically absent 0 11 0 35.58 7.06 observed but should be systematically absent 21359 Reflections read, of which 453 rejected -10 =< h =< 10, -27 =< k =< 27, -11 =< l =< 14, Max. 2-theta = 54.95 5 Systematic absence violations 0 Inconsistent equivalents 4239 Unique reflections, of which 0 suppressed R(int) = 0.0585 R(sigma) = 0.0478 Friedel opposites merged Maximum memory for data reduction = 2646 / 41943 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 = 3317 / 271120 wR2 = 0.1737 before cycle 1 for 4239 data and 218 / 218 parameters GooF = S = 0.965; Restrained GooF = 0.965 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0581 * P )^2 + 4.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65127 0.00171 0.002 OSF Mean shift/esd = 0.004 Maximum = -0.032 for y O1 Max. shift = 0.000 A for C20 Max. dU = 0.000 for C16 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3317 / 271120 wR2 = 0.1737 before cycle 2 for 4239 data and 218 / 218 parameters GooF = S = 0.965; Restrained GooF = 0.965 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0581 * P )^2 + 4.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65127 0.00171 0.001 OSF Mean shift/esd = 0.001 Maximum = -0.012 for y O1 Max. shift = 0.000 A for C20 Max. dU = 0.000 for C9 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3317 / 271120 wR2 = 0.1737 before cycle 3 for 4239 data and 218 / 218 parameters GooF = S = 0.965; Restrained GooF = 0.965 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0581 * P )^2 + 4.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65128 0.00171 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y O1 Max. shift = 0.000 A for H7A Max. dU = 0.000 for C12 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3317 / 271120 wR2 = 0.1737 before cycle 4 for 4239 data and 218 / 218 parameters GooF = S = 0.965; Restrained GooF = 0.965 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0581 * P )^2 + 4.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65127 0.00171 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C3 Max. shift = 0.000 A for H7C Max. dU = 0.000 for C2 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3317 / 271120 wR2 = 0.1737 before cycle 5 for 4239 data and 218 / 218 parameters GooF = S = 0.965; Restrained GooF = 0.965 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0581 * P )^2 + 4.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65127 0.00171 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z S1 Max. shift = 0.000 A for H16 Max. dU = 0.000 for C20 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3317 / 271120 wR2 = 0.1737 before cycle 6 for 4239 data and 218 / 218 parameters GooF = S = 0.965; Restrained GooF = 0.965 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0581 * P )^2 + 4.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65127 0.00171 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z S1 Max. shift = 0.000 A for H7B Max. dU = 0.000 for C4 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.6000 0.2957 0.5502 13 0.980 0.000 C1 N1 C8 C2 H2 0.9276 0.3086 0.5177 13 0.980 0.000 C2 C5 C3 C1 H3A 0.8869 0.3524 0.3357 23 0.970 0.000 C3 C4 C2 H3B 0.9026 0.2804 0.3019 23 0.970 0.000 C3 C4 C2 H4A 0.6272 0.3420 0.2236 23 0.970 0.000 C4 N1 C3 H4B 0.6105 0.2697 0.2555 23 0.970 0.000 C4 N1 C3 H5 0.7229 0.2011 0.4388 43 0.930 0.000 C5 C6 C2 H6 1.0182 0.2069 0.5923 43 0.930 0.000 C6 C5 C7 H7A 0.8019 0.1023 0.5219 137 0.960 0.000 C7 C6 H7A H7B 0.9147 0.1060 0.6438 137 0.960 0.000 C7 C6 H7A H7C 1.0053 0.0963 0.5302 137 0.960 0.000 C7 C6 H7A H8 0.5576 0.4038 0.5679 13 0.980 0.000 C8 C9 C1 C13 H9A 0.8765 0.4284 0.4789 23 0.970 0.000 C9 C10 C8 H9B 0.6929 0.4441 0.4122 23 0.970 0.000 C9 C10 C8 H10A 0.6415 0.5180 0.5551 23 0.970 0.000 C10 C9 C11 H10B 0.8160 0.5354 0.5051 23 0.970 0.000 C10 C9 C11 H11A 0.9798 0.4909 0.6675 23 0.970 0.000 C11 C12 C10 H11B 0.8512 0.5406 0.7119 23 0.970 0.000 C11 C12 C10 H12A 0.8506 0.4447 0.8189 23 0.970 0.000 C12 C13 C11 H12B 0.6638 0.4607 0.7575 23 0.970 0.000 C12 C13 C11 H13A 0.7173 0.3541 0.7270 23 0.970 0.000 C13 C12 C8 H13B 0.8922 0.3702 0.6765 23 0.970 0.000 C13 C12 C8 H15 0.3691 0.2145 0.5470 43 0.930 0.000 C15 C16 C14 H16 0.3628 0.1053 0.5449 43 0.930 0.000 C16 C15 C17 H18 0.2822 0.1064 0.1959 43 0.930 0.000 C18 C19 C17 H19 0.2900 0.2153 0.1954 43 0.930 0.000 C19 C18 C14 2007src1050 in Pc New: P21/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.34207 0.30956 0.37340 1.00000 0.02243 0.03703 0.02355 0.00073 -0.00101 -0.00329 0.02796 0.00121 0.00009 0.00004 0.00006 0.00000 0.00034 0.00040 0.00033 0.00028 0.00024 0.00028 0.00019 O1 0.27610 0.33131 0.47738 1.00000 0.02607 0.03868 0.02953 -0.00239 0.00199 -0.00383 0.03152 0.00352 0.00025 0.00010 0.00017 0.00000 0.00102 0.00119 0.00102 0.00084 0.00078 0.00085 0.00046 O2 0.26623 0.33121 0.26055 1.00000 0.02900 0.04511 0.02655 0.00374 -0.00624 -0.00196 0.03429 0.00362 0.00026 0.00011 0.00017 0.00000 0.00107 0.00128 0.00101 0.00087 0.00080 0.00091 0.00049 N1 0.54681 0.32866 0.38437 1.00000 0.02383 0.04407 0.02287 0.00349 -0.00114 -0.00583 0.03056 0.00425 0.00030 0.00013 0.00020 0.00000 0.00118 0.00150 0.00112 0.00099 0.00088 0.00103 0.00055 C1 0.65721 0.32435 0.49973 1.00000 0.02246 0.03776 0.02225 0.00534 -0.00156 -0.00442 0.02782 0.00487 0.00035 0.00014 0.00023 0.00000 0.00132 0.00167 0.00126 0.00109 0.00099 0.00111 0.00060 H1 0.60005 0.29568 0.55024 1.00000 0.03338 0.00000 0.00000 C2 0.82608 0.29201 0.46820 1.00000 0.02178 0.05090 0.03046 0.00374 -0.00066 -0.00342 0.03467 0.00557 0.00037 0.00016 0.00026 0.00000 0.00139 0.00196 0.00150 0.00130 0.00110 0.00126 0.00069 H2 0.92764 0.30861 0.51768 1.00000 0.04161 0.00000 0.00000 C3 0.83493 0.31084 0.34067 1.00000 0.02827 0.05749 0.03180 0.00327 0.00613 -0.00466 0.03898 0.00595 0.00040 0.00018 0.00026 0.00000 0.00153 0.00215 0.00153 0.00141 0.00118 0.00142 0.00074 H3A 0.88693 0.35241 0.33572 1.00000 0.04678 0.00000 0.00000 H3B 0.90262 0.28039 0.30193 1.00000 0.04678 0.00000 0.00000 C4 0.64526 0.31115 0.28611 1.00000 0.02949 0.05112 0.02602 0.00258 0.00234 -0.00425 0.03561 0.00559 0.00038 0.00017 0.00025 0.00000 0.00151 0.00197 0.00139 0.00129 0.00111 0.00135 0.00069 H4A 0.62716 0.34200 0.22356 1.00000 0.04274 0.00000 0.00000 H4B 0.61049 0.26972 0.25549 1.00000 0.04274 0.00000 0.00000 C5 0.81534 0.22172 0.48193 1.00000 0.02653 0.04474 0.03175 -0.00330 -0.00033 -0.00230 0.03463 0.00548 0.00039 0.00016 0.00026 0.00000 0.00148 0.00190 0.00150 0.00127 0.00115 0.00127 0.00068 H5 0.72287 0.20112 0.43877 1.00000 0.04156 0.00000 0.00000 C6 0.92479 0.18665 0.54944 1.00000 0.03319 0.04612 0.02788 -0.00238 0.00094 -0.00078 0.03593 0.00561 0.00040 0.00016 0.00025 0.00000 0.00158 0.00189 0.00144 0.00129 0.00115 0.00136 0.00069 H6 1.01820 0.20686 0.59232 1.00000 0.04312 0.00000 0.00000 C7 0.91039 0.11655 0.56250 1.00000 0.04481 0.05070 0.03686 -0.00184 0.00467 0.00473 0.04413 0.00642 0.00047 0.00017 0.00029 0.00000 0.00193 0.00213 0.00171 0.00148 0.00140 0.00158 0.00080 H7A 0.80193 0.10226 0.52188 1.00000 0.06619 0.00000 0.00000 H7B 0.91473 0.10603 0.64377 1.00000 0.06619 0.00000 0.00000 H7C 1.00526 0.09630 0.53024 1.00000 0.06619 0.00000 0.00000 C8 0.67576 0.38934 0.55860 1.00000 0.02537 0.03925 0.02654 0.00402 -0.00270 -0.00548 0.03083 0.00503 0.00037 0.00015 0.00024 0.00000 0.00139 0.00172 0.00137 0.00117 0.00105 0.00119 0.00063 H8 0.55761 0.40378 0.56789 1.00000 0.03700 0.00000 0.00000 C9 0.75814 0.44053 0.48899 1.00000 0.03132 0.04600 0.03221 0.01165 -0.00724 -0.01057 0.03737 0.00545 0.00041 0.00016 0.00026 0.00000 0.00157 0.00193 0.00153 0.00132 0.00119 0.00136 0.00073 H9A 0.87653 0.42836 0.47890 1.00000 0.04484 0.00000 0.00000 H9B 0.69291 0.44414 0.41218 1.00000 0.04484 0.00000 0.00000 C10 0.76025 0.50425 0.55023 1.00000 0.03815 0.04069 0.04930 0.00918 -0.01095 -0.00913 0.04397 0.00582 0.00046 0.00017 0.00030 0.00000 0.00180 0.00193 0.00193 0.00151 0.00146 0.00146 0.00082 H10A 0.64151 0.51799 0.55511 1.00000 0.05276 0.00000 0.00000 H10B 0.81598 0.53539 0.50509 1.00000 0.05276 0.00000 0.00000 C11 0.85795 0.50013 0.67278 1.00000 0.04253 0.04112 0.04876 -0.00138 -0.00983 -0.01085 0.04532 0.00584 0.00047 0.00017 0.00030 0.00000 0.00191 0.00195 0.00195 0.00151 0.00148 0.00151 0.00083 H11A 0.97982 0.49095 0.66755 1.00000 0.05438 0.00000 0.00000 H11B 0.85119 0.54055 0.71192 1.00000 0.05438 0.00000 0.00000 C12 0.78082 0.44861 0.74374 1.00000 0.04893 0.05920 0.03481 -0.00581 -0.00691 -0.01627 0.04857 0.00580 0.00050 0.00018 0.00029 0.00000 0.00209 0.00238 0.00170 0.00154 0.00145 0.00173 0.00090 H12A 0.85056 0.44471 0.81895 1.00000 0.05828 0.00000 0.00000 H12B 0.66382 0.46071 0.75750 1.00000 0.05828 0.00000 0.00000 C13 0.77437 0.38484 0.68171 1.00000 0.03923 0.04521 0.02675 0.00557 -0.00652 -0.00894 0.03787 0.00535 0.00043 0.00016 0.00025 0.00000 0.00173 0.00191 0.00145 0.00129 0.00121 0.00143 0.00073 H13A 0.71731 0.35412 0.72695 1.00000 0.04545 0.00000 0.00000 H13B 0.89222 0.37021 0.67647 1.00000 0.04545 0.00000 0.00000 C14 0.32913 0.22612 0.37153 1.00000 0.02196 0.03726 0.02554 -0.00008 0.00103 -0.00371 0.02839 0.00493 0.00035 0.00014 0.00024 0.00000 0.00132 0.00161 0.00131 0.00114 0.00101 0.00113 0.00059 C15 0.35157 0.19288 0.47636 1.00000 0.02748 0.04257 0.02355 -0.00109 0.00057 -0.00557 0.03138 0.00513 0.00036 0.00015 0.00024 0.00000 0.00142 0.00176 0.00133 0.00117 0.00104 0.00125 0.00063 H15 0.36908 0.21450 0.54699 1.00000 0.03766 0.00000 0.00000 C16 0.34763 0.12741 0.47468 1.00000 0.03179 0.03958 0.03318 0.00415 0.00036 -0.00534 0.03511 0.00546 0.00039 0.00015 0.00027 0.00000 0.00156 0.00180 0.00152 0.00126 0.00118 0.00128 0.00068 H16 0.36281 0.10534 0.54490 1.00000 0.04214 0.00000 0.00000 C17 0.32134 0.09367 0.36984 1.00000 0.02662 0.03902 0.03828 -0.00159 -0.00085 -0.00483 0.03500 0.00534 0.00038 0.00016 0.00027 0.00000 0.00148 0.00174 0.00160 0.00132 0.00118 0.00125 0.00067 C18 0.29982 0.12802 0.26651 1.00000 0.03522 0.04388 0.03059 -0.00609 0.00021 -0.00590 0.03685 0.00544 0.00041 0.00016 0.00026 0.00000 0.00166 0.00192 0.00151 0.00129 0.00120 0.00137 0.00071 H18 0.28215 0.10642 0.19585 1.00000 0.04421 0.00000 0.00000 C19 0.30392 0.19328 0.26576 1.00000 0.03046 0.04523 0.02231 -0.00052 -0.00236 -0.00646 0.03309 0.00507 0.00038 0.00016 0.00024 0.00000 0.00149 0.00184 0.00133 0.00120 0.00107 0.00131 0.00066 H19 0.29002 0.21525 0.19541 1.00000 0.03971 0.00000 0.00000 C20 0.30976 0.02282 0.36865 1.00000 0.05280 0.04046 0.05037 -0.00396 -0.00379 -0.00704 0.04864 0.00628 0.00051 0.00017 0.00032 0.00000 0.00221 0.00199 0.00203 0.00157 0.00164 0.00161 0.00088 H20A 0.19193 0.00875 0.34481 1.00000 0.05837 0.00000 0.00000 H20B 0.34268 0.00879 0.45240 1.00000 0.05837 0.00000 0.00000 H20C 0.39185 0.00451 0.32159 1.00000 0.05837 0.00000 0.00000 Final Structure Factor Calculation for 2007src1050 in Pc New: P21/c Total number of l.s. parameters = 218 Maximum vector length = 511 Memory required = 3099 / 24017 wR2 = 0.1737 before cycle 7 for 4239 data and 0 / 218 parameters GooF = S = 0.965; Restrained GooF = 0.965 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0581 * P )^2 + 4.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0678 for 3244 Fo > 4sig(Fo) and 0.0950 for all 4239 data wR2 = 0.1737, GooF = S = 0.965, Restrained GooF = 0.965 for all data Occupancy sum of asymmetric unit = 24.00 for non-hydrogen and 29.00 for hydrogen atoms Principal mean square atomic displacements U 0.0380 0.0264 0.0194 S1 0.0400 0.0300 0.0245 O1 0.0472 0.0365 0.0191 O2 0.0468 0.0251 0.0198 N1 0.0415 0.0234 0.0186 C1 0.0523 0.0311 0.0207 C2 0.0586 0.0329 0.0254 C3 0.0523 0.0288 0.0257 C4 0.0456 0.0339 0.0244 C5 0.0464 0.0346 0.0268 C6 0.0537 0.0423 0.0365 C7 0.0438 0.0280 0.0207 C8 0.0618 0.0283 0.0220 C9 0.0693 0.0349 0.0278 C10 0.0649 0.0449 0.0261 C11 0.0718 0.0494 0.0245 C12 0.0570 0.0347 0.0220 C13 0.0381 0.0263 0.0207 C14 0.0444 0.0276 0.0221 C15 0.0453 0.0312 0.0288 C16 0.0409 0.0402 0.0239 C17 0.0476 0.0373 0.0256 C18 0.0479 0.0316 0.0198 C19 0.0631 0.0487 0.0342 C20 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 0.050 0.064 0.081 0.108 0.162 1.000 Number in group 430. 419. 443. 417. 412. 430. 426. 422. 415. 425. GooF 1.186 1.101 1.064 1.020 0.956 0.954 0.860 0.874 0.778 0.753 K 7.712 1.814 1.259 1.083 1.034 1.009 1.003 1.014 1.000 0.998 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.65 inf Number in group 431. 419. 426. 420. 429. 423. 418. 423. 423. 427. GooF 1.081 1.030 1.001 1.012 0.916 0.840 0.855 0.890 0.872 1.103 K 1.084 1.076 1.034 1.077 1.018 0.998 0.997 0.995 1.003 0.998 R1 0.213 0.205 0.162 0.164 0.123 0.088 0.067 0.058 0.051 0.043 Recommended weighting scheme: WGHT 0.0180 3.4183 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 15 4 55.39 1.78 4.72 0.009 1.11 -5 2 4 35.25 0.23 4.56 0.003 1.41 0 4 2 35.04 1.34 4.53 0.008 3.88 1 0 6 288.34 154.60 4.38 0.081 1.80 -7 12 8 55.86 0.68 4.21 0.005 0.82 0 7 1 280.48 159.04 3.94 0.082 2.92 4 3 1 464.47 304.83 3.70 0.114 1.80 -6 0 2 31.32 1.65 3.67 0.008 1.28 6 13 0 36.88 2.51 3.65 0.010 1.00 -1 27 1 140.50 61.54 3.51 0.051 0.78 1 26 3 73.55 0.32 3.49 0.004 0.79 0 26 1 64.20 3.92 3.49 0.013 0.81 -4 2 4 96.13 44.36 3.21 0.044 1.67 6 3 0 62.61 20.20 3.20 0.029 1.26 7 18 1 71.96 12.14 3.10 0.023 0.79 5 23 2 65.83 0.02 3.09 0.001 0.77 -8 16 1 8.09 63.15 3.08 0.052 0.78 2 4 6 290.66 191.23 3.06 0.090 1.56 -4 18 9 31.39 0.32 3.06 0.004 0.81 5 22 1 161.07 59.76 3.05 0.051 0.81 0 3 6 186.28 109.94 3.04 0.069 1.84 -8 11 1 54.60 2.06 2.99 0.009 0.86 4 20 2 35.37 1.47 2.96 0.008 0.91 -3 8 14 18.72 70.53 2.94 0.055 0.77 1 23 3 209.20 120.33 2.93 0.072 0.88 -4 23 6 49.31 8.76 2.93 0.019 0.77 -7 1 9 36.81 3.39 2.92 0.012 0.88 1 15 6 63.69 24.79 2.92 0.033 1.11 6 10 2 18.24 0.57 2.91 0.005 1.06 -1 18 9 67.09 17.24 2.88 0.027 0.86 6 6 5 39.46 7.24 2.87 0.018 1.02 0 24 7 88.53 25.59 2.87 0.033 0.78 -2 14 8 27.76 5.55 2.84 0.015 1.02 1 8 2 312.33 214.50 2.83 0.096 2.26 -3 17 6 -8.55 14.24 2.82 0.025 0.99 -3 1 3 803.89 623.63 2.79 0.163 2.24 2 23 3 84.14 32.58 2.79 0.037 0.86 -5 11 9 21.79 0.22 2.76 0.003 0.91 -3 10 7 8.40 40.96 2.76 0.042 1.20 -4 4 5 94.43 48.65 2.75 0.046 1.50 -9 2 2 -7.75 25.82 2.74 0.033 0.86 6 11 0 38.86 10.90 2.74 0.022 1.06 8 1 2 50.56 13.50 2.72 0.024 0.93 -4 22 3 89.21 9.48 2.70 0.020 0.85 9 3 4 30.52 0.24 2.69 0.003 0.79 -2 6 3 119.32 67.68 2.68 0.054 2.23 -4 9 12 -9.31 19.26 2.68 0.029 0.84 0 8 1 1119.60 895.96 2.68 0.196 2.57 3 3 1 185.64 119.05 2.66 0.071 2.30 -1 7 3 441.75 326.23 2.66 0.118 2.31 Bond lengths and angles S1 - Distance Angles O1 1.4318 (0.0021) O2 1.4385 (0.0020) 120.56 (0.13) N1 1.6231 (0.0024) 107.05 (0.12) 106.42 (0.12) C14 1.7653 (0.0031) 107.78 (0.13) 106.85 (0.13) 107.60 (0.14) S1 - O1 O2 N1 O1 - Distance Angles S1 1.4318 (0.0021) O1 - O2 - Distance Angles S1 1.4385 (0.0020) O2 - N1 - Distance Angles C4 1.4828 (0.0038) C1 1.4975 (0.0033) 111.96 (0.22) S1 1.6231 (0.0024) 117.38 (0.19) 120.24 (0.18) N1 - C4 C1 C1 - Distance Angles N1 1.4975 (0.0033) C8 1.5308 (0.0042) 110.72 (0.23) C2 1.5527 (0.0041) 103.08 (0.22) 117.41 (0.24) H1 0.9800 108.42 108.42 108.42 C1 - N1 C8 C2 C2 - Distance Angles C5 1.4964 (0.0047) C3 1.5326 (0.0040) 111.60 (0.27) C1 1.5527 (0.0041) 110.69 (0.24) 104.04 (0.24) H2 0.9800 110.12 110.12 110.12 C2 - C5 C3 C1 C3 - Distance Angles C4 1.5263 (0.0041) C2 1.5326 (0.0040) 104.43 (0.23) H3A 0.9700 110.87 110.87 H3B 0.9700 110.87 110.87 108.91 C3 - C4 C2 H3A C4 - Distance Angles N1 1.4828 (0.0038) C3 1.5263 (0.0041) 103.83 (0.23) H4A 0.9700 110.99 110.99 H4B 0.9700 110.99 110.99 108.99 C4 - N1 C3 H4A C5 - Distance Angles C6 1.3105 (0.0043) C2 1.4964 (0.0047) 125.72 (0.29) H5 0.9300 117.14 117.14 C5 - C6 C2 C6 - Distance Angles C5 1.3105 (0.0043) C7 1.4938 (0.0048) 124.73 (0.30) H6 0.9300 117.63 117.63 C6 - C5 C7 C7 - Distance Angles C6 1.4938 (0.0048) H7A 0.9600 109.47 H7B 0.9600 109.47 109.47 H7C 0.9600 109.47 109.47 109.47 C7 - C6 H7A H7B C8 - Distance Angles C9 1.5287 (0.0040) C1 1.5308 (0.0042) 115.14 (0.24) C13 1.5343 (0.0037) 109.71 (0.24) 111.46 (0.24) H8 0.9800 106.68 106.68 106.68 C8 - C9 C1 C13 C9 - Distance Angles C10 1.5191 (0.0049) C8 1.5287 (0.0040) 111.43 (0.27) H9A 0.9700 109.34 109.34 H9B 0.9700 109.34 109.34 107.98 C9 - C10 C8 H9A C10 - Distance Angles C9 1.5191 (0.0049) C11 1.5256 (0.0044) 110.95 (0.28) H10A 0.9700 109.45 109.45 H10B 0.9700 109.45 109.45 108.04 C10 - C9 C11 H10A C11 - Distance Angles C12 1.5238 (0.0049) C10 1.5256 (0.0044) 110.85 (0.27) H11A 0.9700 109.47 109.47 H11B 0.9700 109.47 109.47 108.06 C11 - C12 C10 H11A C12 - Distance Angles C13 1.5231 (0.0048) C11 1.5238 (0.0049) 111.90 (0.29) H12A 0.9700 109.24 109.24 H12B 0.9700 109.24 109.24 107.92 C12 - C13 C11 H12A C13 - Distance Angles C12 1.5231 (0.0048) C8 1.5343 (0.0037) 111.44 (0.27) H13A 0.9700 109.34 109.34 H13B 0.9700 109.34 109.34 107.98 C13 - C12 C8 H13A C14 - Distance Angles C15 1.3912 (0.0039) C19 1.3970 (0.0039) 119.92 (0.28) S1 1.7653 (0.0031) 119.47 (0.22) 120.55 (0.23) C14 - C15 C19 C15 - Distance Angles C16 1.3832 (0.0045) C14 1.3912 (0.0039) 119.47 (0.27) H15 0.9300 120.26 120.26 C15 - C16 C14 C16 - Distance Angles C15 1.3832 (0.0045) C17 1.3978 (0.0043) 121.51 (0.28) H16 0.9300 119.25 119.25 C16 - C15 C17 C17 - Distance Angles C18 1.3885 (0.0043) C16 1.3978 (0.0043) 117.82 (0.30) C20 1.4990 (0.0047) 120.85 (0.29) 121.29 (0.29) C17 - C18 C16 C18 - Distance Angles C19 1.3787 (0.0046) C17 1.3885 (0.0043) 121.82 (0.28) H18 0.9300 119.09 119.09 C18 - C19 C17 C19 - Distance Angles C18 1.3787 (0.0046) C14 1.3970 (0.0039) 119.46 (0.27) H19 0.9300 120.27 120.27 C19 - C18 C14 C20 - Distance Angles C17 1.4990 (0.0047) H20A 0.9667 111.26 H20B 1.0140 105.96 107.76 H20C 0.9623 111.33 112.12 108.10 C20 - C17 H20A H20B FMAP and GRID set by program FMAP 2 1 20 GRID -2.941 24 -2 2.941 1 2 R1 = 0.0943 for 4239 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.68 at 0.0378 0.7185 0.1772 [ 1.40 A from H3B ] Deepest hole -0.37 at 0.4006 0.2910 0.4173 [ 0.75 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3469 / 33946 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9622 0.2185 0.3228 1.00000 0.05 0.68 1.40 H3B 2.20 C3 2.27 C5 2.43 H5 Q2 1 0.3401 0.2632 0.3756 1.00000 0.05 0.37 0.79 C14 0.98 S1 1.88 C15 1.94 C19 Q3 1 0.4189 0.0076 0.4013 1.00000 0.05 0.30 0.88 H20B 0.92 H20C 0.94 C20 1.80 H20A Q4 1 0.3042 0.0077 0.2889 1.00000 0.05 0.29 0.74 H20C 0.97 C20 1.14 H20A 1.87 H20B Q5 1 0.6798 0.3602 0.5181 1.00000 0.05 0.28 0.78 C8 0.80 C1 1.48 H8 1.56 H1 Q6 1 0.7892 0.3600 0.3198 1.00000 0.05 0.26 0.77 H3A 1.11 C3 1.53 C4 1.62 H4A Q7 1 0.4669 0.3363 0.3859 1.00000 0.05 0.25 0.64 N1 1.11 S1 1.87 C1 1.91 O1 Q8 1 0.5898 0.3289 0.4382 1.00000 0.05 0.23 0.67 N1 0.84 C1 1.46 H1 1.89 C4 Q9 1 0.8476 0.4985 0.4583 1.00000 0.05 0.22 1.00 H10B 1.33 C10 1.47 C9 1.51 H9A Q10 1 0.7054 0.4104 0.5223 1.00000 0.05 0.22 0.67 C8 0.87 C9 1.32 H8 1.45 H9B Q11 1 0.3477 0.2107 0.3214 1.00000 0.05 0.22 0.69 C14 0.78 C19 1.47 H19 1.82 C15 Q12 1 0.3378 0.1170 0.4148 1.00000 0.05 0.21 0.72 C17 0.72 C16 1.51 H16 1.72 C18 Q13 1 0.8013 0.2576 0.4413 1.00000 0.05 0.21 0.80 C2 0.89 C5 1.34 H5 1.64 H2 Q14 1 0.2053 0.3676 0.3069 1.00000 0.05 0.21 1.08 O2 1.74 S1 1.99 H11B 2.12 O1 Q15 1 0.6158 0.2532 0.6377 1.00000 0.05 0.20 1.34 H1 1.45 H4B 2.18 C4 2.22 H15 Q16 1 0.2296 0.1905 0.6086 1.00000 0.05 0.20 1.45 H15 1.66 H6 1.80 O2 1.88 C15 Q17 1 0.2666 0.1603 0.2619 1.00000 0.05 0.19 0.73 C18 0.75 C19 1.38 H18 1.41 H19 Q18 1 0.7527 0.4699 0.5403 1.00000 0.05 0.19 0.74 C10 0.86 C9 1.35 H10A 1.53 H9A Q19 1 0.3320 0.2288 0.5911 1.00000 0.05 0.19 0.68 H15 1.55 C15 1.74 H19 2.43 O2 Q20 1 0.6138 0.3502 0.2514 1.00000 0.05 0.19 0.39 H4A 0.94 C4 1.70 H4B 1.73 N1 Shortest distances between peaks (including symmetry equivalents) 7 8 1.08 5 10 1.08 16 19 1.16 5 8 1.27 2 11 1.28 10 18 1.32 11 17 1.38 9 18 1.40 3 4 1.48 6 20 1.50 2 7 1.82 12 17 2.01 7 20 2.05 1 13 2.12 8 10 2.12 5 7 2.17 7 14 2.22 8 13 2.22 8 20 2.23 15 19 2.26 11 12 2.26 6 8 2.27 9 10 2.32 5 18 2.39 3 12 2.40 2 8 2.42 9 9 2.44 3 3 2.49 2 14 2.53 5 6 2.53 15 20 2.55 5 13 2.56 2 17 2.57 6 13 2.57 2 19 2.60 14 16 2.62 6 10 2.71 5 15 2.72 4 12 2.72 6 7 2.73 7 10 2.77 8 15 2.79 1 17 2.81 13 15 2.82 7 11 2.88 12 16 2.92 11 19 2.94 4 9 2.96 1 11 2.98 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: 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. 0.16: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.00: Structure factors and derivatives 1.31: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.08: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src1050 finished at 16:39:49 Total CPU time: 2.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++