+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0712r started at 12:04:05 on 16-Nov-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0712r in Pn CELL 0.71073 9.8278 9.4884 12.0388 90.000 94.740 90.000 ZERR 2.00 0.0004 0.0005 0.0005 0.000 0.003 0.000 LATT -1 SYMM 1/2 + X, - Y, 1/2 + Z SFAC C H B O P BR UNIT 50 46 2 4 2 2 V = 1118.78 F(000) = 488.0 Mu = 1.93 mm-1 Cell Wt = 954.25 Rho = 1.416 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 20 SIZE 0.01 0.17 0.40 TEMP -153 ACTA BOND $H WGHT 0.02350 L.S. 10 FVAR 0.21676 MOLE 1 BR1 6 0.889375 0.514801 0.677926 11.00000 0.03984 0.03003 = 0.02095 -0.00219 -0.00085 -0.00192 MOLE 2 C1 1 0.277344 0.781198 0.488855 11.00000 0.01684 0.02310 = 0.02263 0.00168 -0.00401 0.00045 C2 1 0.358834 0.664886 0.469069 11.00000 0.03295 0.02476 = 0.01966 -0.00306 -0.00017 -0.00113 AFIX 43 H2 2 0.359641 0.628502 0.397395 11.00000 -1.20000 AFIX 0 C3 1 0.437980 0.604141 0.555799 11.00000 0.03491 0.02597 = 0.02730 0.00137 0.00265 0.00101 AFIX 43 H3 2 0.493516 0.527725 0.542256 11.00000 -1.20000 AFIX 0 C4 1 0.435462 0.656550 0.664169 11.00000 0.03064 0.03130 = 0.02413 0.00927 -0.00414 -0.00121 AFIX 43 H4 2 0.488983 0.615608 0.722829 11.00000 -1.20000 AFIX 0 C5 1 0.351877 0.770610 0.682897 11.00000 0.03339 0.03922 = 0.01850 -0.00397 -0.00507 -0.00636 AFIX 43 H5 2 0.348923 0.805424 0.754870 11.00000 -1.20000 AFIX 0 C6 1 0.273441 0.832830 0.596645 11.00000 0.02697 0.03472 = 0.02124 -0.00299 0.00108 0.00215 AFIX 43 H6 2 0.217932 0.909218 0.610323 11.00000 -1.20000 AFIX 0 C7 1 0.020753 0.787357 0.338394 11.00000 0.02182 0.02162 = 0.02235 -0.00346 0.00103 0.00093 C8 1 -0.023855 0.673171 0.399228 11.00000 0.02687 0.01938 = 0.02694 -0.00178 -0.00109 0.00140 AFIX 43 H8 2 0.031009 0.638259 0.459658 11.00000 -1.20000 AFIX 0 C9 1 -0.149948 0.611803 0.369566 11.00000 0.03388 0.02398 = 0.02798 -0.00088 0.00261 -0.00353 AFIX 43 H9 2 -0.178771 0.534841 0.409316 11.00000 -1.20000 AFIX 0 C10 1 -0.232538 0.665111 0.281006 11.00000 0.02400 0.03470 = 0.02958 -0.00699 0.00248 -0.00916 AFIX 43 H10 2 -0.315899 0.622430 0.259999 11.00000 -1.20000 AFIX 0 C11 1 -0.191389 0.782362 0.223210 11.00000 0.02542 0.03673 = 0.02015 0.00224 -0.00392 -0.00078 AFIX 43 H11 2 -0.249127 0.820064 0.165666 11.00000 -1.20000 AFIX 0 C12 1 -0.064183 0.843949 0.250817 11.00000 0.02366 0.02722 = 0.02150 0.00148 0.00204 -0.00257 AFIX 43 H12 2 -0.036300 0.921653 0.211438 11.00000 -1.20000 AFIX 0 C13 1 0.150654 1.047388 0.415295 11.00000 0.02587 0.01671 = 0.01751 0.00216 -0.00104 -0.00002 C14 1 0.030079 1.088554 0.457085 11.00000 0.01828 0.03176 = 0.02613 -0.00161 0.00105 -0.00216 AFIX 43 H14 2 -0.040277 1.023710 0.461253 11.00000 -1.20000 AFIX 0 C15 1 0.013312 1.225187 0.492677 11.00000 0.01917 0.02918 = 0.03656 -0.00712 0.00333 0.00316 AFIX 43 H15 2 -0.067012 1.251078 0.523047 11.00000 -1.20000 AFIX 0 C16 1 0.115090 1.323622 0.483452 11.00000 0.03410 0.02622 = 0.02442 -0.00011 -0.00169 0.00581 AFIX 43 H16 2 0.102655 1.415759 0.506942 11.00000 -1.20000 AFIX 0 C17 1 0.235280 1.286025 0.439530 11.00000 0.03721 0.02962 = 0.03257 -0.00260 0.01077 -0.01223 AFIX 43 H17 2 0.302686 1.353225 0.431618 11.00000 -1.20000 AFIX 0 C18 1 0.255331 1.147133 0.407086 11.00000 0.02640 0.03037 = 0.03507 -0.01123 0.00851 -0.00738 AFIX 43 H18 2 0.337504 1.120455 0.380130 11.00000 -1.20000 AFIX 0 C19 1 0.288436 0.865037 0.257449 11.00000 0.02250 0.02573 = 0.02088 0.00202 0.00288 0.00014 AFIX 23 H19A 2 0.371266 0.917451 0.278672 11.00000 -1.20000 H19B 2 0.314829 0.767881 0.246289 11.00000 -1.20000 AFIX 0 C20 1 0.228374 0.921928 0.146933 11.00000 0.01597 0.02514 = 0.02221 -0.00015 0.00338 0.00104 C21 1 0.228025 1.066566 0.123142 11.00000 0.01975 0.02706 = 0.02799 -0.00271 0.00213 0.00202 AFIX 43 H21 2 0.259473 1.130319 0.178069 11.00000 -1.20000 AFIX 0 C22 1 0.181640 1.114721 0.019453 11.00000 0.02578 0.02607 = 0.03348 0.00865 0.00158 0.00187 AFIX 43 H22 2 0.179485 1.211010 0.004983 11.00000 -1.20000 AFIX 0 C23 1 0.137965 1.020318 -0.063836 11.00000 0.02097 0.03282 = 0.01919 0.00385 0.00103 0.00260 AFIX 43 H23 2 0.110156 1.054231 -0.134569 11.00000 -1.20000 AFIX 0 C24 1 0.134782 0.875319 -0.043905 11.00000 0.01537 0.03028 = 0.02169 0.00151 0.00220 0.00114 C25 1 0.180351 0.828639 0.064161 11.00000 0.01851 0.02455 = 0.02050 0.00221 0.00574 0.00218 AFIX 43 H25 2 0.178093 0.732838 0.080231 11.00000 -1.20000 AFIX 0 B1 3 0.081145 0.767731 -0.137974 11.00000 0.01771 0.03371 = 0.01887 0.00174 0.00054 0.00708 O2 4 0.027831 0.821540 -0.236935 11.00000 0.02840 0.03357 = 0.01877 -0.00077 -0.00120 0.00149 AFIX 147 H2A 2 -0.010298 0.758589 -0.274372 11.00000 -1.50000 AFIX 0 O3 4 0.086766 0.628254 -0.112496 11.00000 0.03155 0.03073 = 0.02406 -0.00232 -0.00444 0.00248 AFIX 147 H3A 2 0.041534 0.583628 -0.160804 11.00000 -1.50000 AFIX 0 P1 5 0.182081 0.869690 0.374173 11.00000 0.02125 0.02200 = 0.01682 -0.00124 -0.00072 -0.00059 HKLF 4 Covalent radii and connectivity table for 2009src0712r in Pn C 0.770 H 0.320 B 0.820 O 0.660 P 1.100 BR 1.140 Br1 - no bonds found C1 - C6 C2 P1 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - C6 C4 C6 - C5 C1 C7 - C12 C8 P1 C8 - C9 C7 C9 - C10 C8 C10 - C9 C11 C11 - C10 C12 C12 - C11 C7 C13 - C14 C18 P1 C14 - C15 C13 C15 - C14 C16 C16 - C15 C17 C17 - C16 C18 C18 - C17 C13 C19 - C20 P1 C20 - C25 C21 C19 C21 - C22 C20 C22 - C21 C23 C23 - C22 C24 C24 - C23 C25 B1 C25 - C20 C24 B1 - O3 O2 C24 O2 - B1 O3 - B1 P1 - C7 C13 C1 C19 Floating origin restraints generated 16100 Reflections read, of which 505 rejected -12 =< h =< 12, -12 =< k =< 12, -15 =< l =< 15, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 4 9 -4 9.26 1.32 4 9.38 1 7 -2 8.99 1.18 3 8.98 2 Inconsistent equivalents 4905 Unique reflections, of which 0 suppressed R(int) = 0.0613 R(sigma) = 0.0786 Friedel opposites not merged Maximum memory for data reduction = 2657 / 49078 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 3428 / 341992 wR2 = 0.0846 before cycle 1 for 4905 data and 273 / 273 parameters GooF = S = 1.044; Restrained GooF = 1.043 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.21688 0.00027 0.440 OSF Mean shift/su = 0.046 Maximum = 0.440 for OSF Max. shift = 0.004 A for H3A Max. dU = 0.000 for C22 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3428 / 341992 wR2 = 0.0846 before cycle 2 for 4905 data and 273 / 273 parameters GooF = S = 1.044; Restrained GooF = 1.044 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.21691 0.00027 0.090 OSF Mean shift/su = 0.016 Maximum = 0.090 for OSF Max. shift = 0.002 A for H3A Max. dU = 0.000 for C22 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3428 / 341992 wR2 = 0.0846 before cycle 3 for 4905 data and 273 / 273 parameters GooF = S = 1.044; Restrained GooF = 1.043 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.21690 0.00027 -0.001 OSF Mean shift/su = 0.001 Maximum = -0.017 for tors H2A Max. shift = 0.001 A for H2A Max. dU = 0.000 for O2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3428 / 341992 wR2 = 0.0846 before cycle 4 for 4905 data and 273 / 273 parameters GooF = S = 1.044; Restrained GooF = 1.044 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.21690 0.00027 -0.001 OSF Mean shift/su = 0.000 Maximum = -0.006 for tors H2A Max. shift = 0.000 A for H2A Max. dU = 0.000 for C17 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3428 / 341992 wR2 = 0.0846 before cycle 5 for 4905 data and 273 / 273 parameters GooF = S = 1.044; Restrained GooF = 1.044 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.21690 0.00027 0.000 OSF Mean shift/su = 0.000 Maximum = -0.002 for tors H2A Max. shift = 0.000 A for H2A Max. dU = 0.000 for C18 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3428 / 341992 wR2 = 0.0846 before cycle 6 for 4905 data and 273 / 273 parameters GooF = S = 1.044; Restrained GooF = 1.044 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.21690 0.00027 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for U11 Br1 Max. shift = 0.000 A for H2A Max. dU = 0.000 for O3 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3428 / 341992 wR2 = 0.0846 before cycle 7 for 4905 data and 273 / 273 parameters GooF = S = 1.044; Restrained GooF = 1.044 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.21690 0.00027 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U11 P1 Max. shift = 0.000 A for H2A Max. dU = 0.000 for C9 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3428 / 341992 wR2 = 0.0846 before cycle 8 for 4905 data and 273 / 273 parameters GooF = S = 1.044; Restrained GooF = 1.044 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.21690 0.00027 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H2A Max. dU = 0.000 for C11 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3428 / 341992 wR2 = 0.0846 before cycle 9 for 4905 data and 273 / 273 parameters GooF = S = 1.044; Restrained GooF = 1.044 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.21690 0.00027 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H3A Max. dU = 0.000 for C12 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3428 / 341992 wR2 = 0.0846 before cycle 10 for 4905 data and 273 / 273 parameters GooF = S = 1.044; Restrained GooF = 1.044 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.21690 0.00027 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U11 Br1 Max. shift = 0.000 A for H2A Max. dU = 0.000 for C22 Largest correlation matrix elements -0.582 U33 C23 / z C23 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.3595 0.6277 0.3958 43 0.950 0.000 C2 C3 C1 H3 0.4948 0.5260 0.5419 43 0.950 0.000 C3 C2 C4 H4 0.4901 0.6147 0.7241 43 0.950 0.000 C4 C5 C3 H5 0.3489 0.8062 0.7565 43 0.950 0.000 C5 C6 C4 H6 0.2167 0.9109 0.6106 43 0.950 0.000 C6 C5 C1 H8 0.0323 0.6375 0.4610 43 0.950 0.000 C8 C9 C7 H9 -0.1795 0.5332 0.4102 43 0.950 0.000 C9 C10 C8 H10 -0.3177 0.6215 0.2595 43 0.950 0.000 C10 C9 C11 H11 -0.2504 0.8209 0.1644 43 0.950 0.000 C11 C10 C12 H12 -0.0357 0.9234 0.2106 43 0.950 0.000 C12 C11 C7 H14 -0.0419 1.0223 0.4612 43 0.950 0.000 C14 C15 C13 H15 -0.0688 1.2517 0.5237 43 0.950 0.000 C15 C14 C16 H16 0.1024 1.4178 0.5075 43 0.950 0.000 C16 C15 C17 H17 0.3042 1.3547 0.4314 43 0.950 0.000 C17 C16 C18 H18 0.3393 1.1199 0.3795 43 0.950 0.000 C18 C17 C13 H19A 0.3730 0.9185 0.2791 23 0.990 0.000 C19 C20 P1 H19B 0.3154 0.7658 0.2461 23 0.990 0.000 C19 C20 P1 H21 0.2602 1.1317 0.1793 43 0.950 0.000 C21 C22 C20 H22 0.1794 1.2131 0.0047 43 0.950 0.000 C22 C21 C23 H23 0.1095 1.0550 -0.1361 43 0.950 0.000 C23 C22 C24 H25 0.1781 0.7307 0.0806 43 0.950 0.000 C25 C20 C24 H2A -0.0107 0.7569 -0.2755 147 0.840 0.000 O2 B1 H2A H3A 0.0410 0.5825 -0.1623 147 0.840 0.000 O3 B1 H3A 2009src0712r in Pn ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Br1 0.88938 0.51480 0.67793 1.00000 0.03989 0.03009 0.02099 -0.00220 -0.00085 -0.00191 0.03051 0.00076 0.00005 0.00004 0.00004 0.00000 0.00019 0.00021 0.00016 0.00022 0.00013 0.00024 0.00011 C1 0.27737 0.78120 0.48886 1.00000 0.01678 0.02323 0.02266 0.00175 -0.00403 0.00035 0.02121 0.00624 0.00033 0.00037 0.00029 0.00000 0.00166 0.00195 0.00188 0.00146 0.00146 0.00140 0.00075 C2 0.35878 0.66489 0.46900 1.00000 0.03268 0.02484 0.01975 -0.00288 -0.00033 -0.00117 0.02590 0.00665 0.00039 0.00040 0.00031 0.00000 0.00206 0.00209 0.00191 0.00149 0.00166 0.00161 0.00083 H2 0.35955 0.62775 0.39577 1.00000 0.03108 0.00000 0.00000 C3 0.43803 0.60405 0.55578 1.00000 0.03500 0.02602 0.02737 0.00149 0.00260 0.00091 0.02946 0.00716 0.00041 0.00041 0.00031 0.00000 0.00210 0.00215 0.00215 0.00168 0.00175 0.00166 0.00086 H3 0.49475 0.52599 0.54195 1.00000 0.03535 0.00000 0.00000 C4 0.43548 0.65653 0.66422 1.00000 0.03070 0.03118 0.02416 0.00917 -0.00403 -0.00127 0.02903 0.00704 0.00037 0.00042 0.00031 0.00000 0.00210 0.00229 0.00211 0.00170 0.00176 0.00163 0.00091 H4 0.49015 0.61472 0.72415 1.00000 0.03483 0.00000 0.00000 C5 0.35190 0.77061 0.68294 1.00000 0.03319 0.03917 0.01877 -0.00392 -0.00496 -0.00640 0.03077 0.00673 0.00036 0.00043 0.00033 0.00000 0.00227 0.00235 0.00183 0.00176 0.00188 0.00163 0.00094 H5 0.34889 0.80618 0.75646 1.00000 0.03693 0.00000 0.00000 C6 0.27342 0.83285 0.59665 1.00000 0.02704 0.03480 0.02106 -0.00296 0.00105 0.00201 0.02769 0.00674 0.00038 0.00042 0.00030 0.00000 0.00196 0.00234 0.00189 0.00164 0.00166 0.00164 0.00085 H6 0.21670 0.91086 0.61061 1.00000 0.03323 0.00000 0.00000 C7 0.02074 0.78735 0.33839 1.00000 0.02183 0.02162 0.02247 -0.00355 0.00105 0.00091 0.02202 0.00623 0.00035 0.00037 0.00029 0.00000 0.00181 0.00198 0.00193 0.00149 0.00151 0.00145 0.00077 C8 -0.02379 0.67317 0.39929 1.00000 0.02682 0.01919 0.02720 -0.00184 -0.00087 0.00120 0.02458 0.00675 0.00037 0.00039 0.00032 0.00000 0.00194 0.00200 0.00200 0.00155 0.00161 0.00154 0.00081 H8 0.03227 0.63752 0.46101 1.00000 0.02949 0.00000 0.00000 C9 -0.14998 0.61179 0.36959 1.00000 0.03391 0.02409 0.02801 -0.00101 0.00252 -0.00339 0.02867 0.00676 0.00039 0.00040 0.00032 0.00000 0.00216 0.00207 0.00206 0.00159 0.00175 0.00160 0.00086 H9 -0.17945 0.53319 0.41021 1.00000 0.03441 0.00000 0.00000 C10 -0.23258 0.66511 0.28099 1.00000 0.02421 0.03456 0.02947 -0.00690 0.00259 -0.00904 0.02939 0.00701 0.00038 0.00044 0.00032 0.00000 0.00193 0.00228 0.00201 0.00167 0.00166 0.00163 0.00085 H10 -0.31772 0.62149 0.25951 1.00000 0.03527 0.00000 0.00000 C11 -0.19144 0.78240 0.22317 1.00000 0.02539 0.03677 0.02024 0.00216 -0.00369 -0.00082 0.02777 0.00671 0.00037 0.00042 0.00030 0.00000 0.00186 0.00236 0.00182 0.00164 0.00156 0.00163 0.00084 H11 -0.25044 0.82092 0.16441 1.00000 0.03333 0.00000 0.00000 C12 -0.06418 0.84401 0.25078 1.00000 0.02358 0.02720 0.02149 0.00128 0.00199 -0.00249 0.02408 0.00642 0.00035 0.00039 0.00029 0.00000 0.00186 0.00205 0.00182 0.00148 0.00153 0.00150 0.00078 H12 -0.03567 0.92338 0.21056 1.00000 0.02890 0.00000 0.00000 C13 0.15065 1.04739 0.41532 1.00000 0.02594 0.01669 0.01760 0.00219 -0.00109 0.00000 0.02023 0.00647 0.00039 0.00035 0.00028 0.00000 0.00179 0.00186 0.00179 0.00143 0.00141 0.00154 0.00073 C14 0.03002 1.08851 0.45706 1.00000 0.01845 0.03169 0.02598 -0.00157 0.00093 -0.00197 0.02542 0.00690 0.00037 0.00042 0.00031 0.00000 0.00182 0.00232 0.00200 0.00167 0.00158 0.00158 0.00083 H14 -0.04188 1.02229 0.46125 1.00000 0.03051 0.00000 0.00000 C15 0.01329 1.22521 0.49270 1.00000 0.01935 0.02913 0.03641 -0.00692 0.00323 0.00306 0.02825 0.00653 0.00035 0.00040 0.00032 0.00000 0.00181 0.00223 0.00221 0.00168 0.00166 0.00153 0.00085 H15 -0.06876 1.25166 0.52374 1.00000 0.03390 0.00000 0.00000 C16 0.11509 1.32370 0.48350 1.00000 0.03408 0.02652 0.02430 -0.00007 -0.00191 0.00583 0.02854 0.00699 0.00039 0.00041 0.00031 0.00000 0.00208 0.00214 0.00195 0.00160 0.00163 0.00165 0.00084 H16 0.10241 1.41780 0.50753 1.00000 0.03425 0.00000 0.00000 C17 0.23531 1.28606 0.43952 1.00000 0.03710 0.02975 0.03253 -0.00266 0.01088 -0.01208 0.03268 0.00739 0.00042 0.00043 0.00034 0.00000 0.00222 0.00236 0.00223 0.00178 0.00191 0.00179 0.00096 H17 0.30415 1.35471 0.43141 1.00000 0.03922 0.00000 0.00000 C18 0.25538 1.14718 0.40707 1.00000 0.02651 0.03034 0.03501 -0.01112 0.00842 -0.00742 0.03029 0.00703 0.00040 0.00041 0.00034 0.00000 0.00204 0.00228 0.00229 0.00173 0.00182 0.00166 0.00091 H18 0.33931 1.11993 0.37952 1.00000 0.03635 0.00000 0.00000 C19 0.28848 0.86499 0.25746 1.00000 0.02248 0.02587 0.02074 0.00212 0.00290 0.00024 0.02297 0.00662 0.00036 0.00038 0.00029 0.00000 0.00174 0.00205 0.00182 0.00143 0.00146 0.00146 0.00077 H19A 0.37304 0.91846 0.27911 1.00000 0.02756 0.00000 0.00000 H19B 0.31539 0.76582 0.24606 1.00000 0.02756 0.00000 0.00000 C20 0.22838 0.92192 0.14695 1.00000 0.01597 0.02518 0.02237 -0.00016 0.00343 0.00104 0.02107 0.00621 0.00033 0.00039 0.00028 0.00000 0.00164 0.00200 0.00181 0.00150 0.00147 0.00140 0.00075 C21 0.22804 1.06663 0.12315 1.00000 0.01971 0.02695 0.02807 -0.00252 0.00213 0.00208 0.02490 0.00690 0.00036 0.00041 0.00031 0.00000 0.00174 0.00216 0.00197 0.00160 0.00154 0.00149 0.00080 H21 0.26018 1.13175 0.17926 1.00000 0.02988 0.00000 0.00000 C22 0.18163 1.11479 0.01944 1.00000 0.02583 0.02620 0.03359 0.00861 0.00175 0.00187 0.02858 0.00698 0.00036 0.00041 0.00032 0.00000 0.00195 0.00217 0.00221 0.00172 0.00171 0.00161 0.00087 H22 0.17944 1.21315 0.00467 1.00000 0.03430 0.00000 0.00000 C23 0.13792 1.02037 -0.06388 1.00000 0.02084 0.03269 0.01943 0.00377 0.00112 0.00260 0.02435 0.00954 0.00057 0.00041 0.00051 0.00000 0.00144 0.00272 0.00195 0.00187 0.00132 0.00181 0.00088 H23 0.10950 1.05500 -0.13614 1.00000 0.02922 0.00000 0.00000 C24 0.13475 0.87531 -0.04391 1.00000 0.01537 0.03044 0.02169 0.00148 0.00220 0.00112 0.02246 0.00652 0.00035 0.00039 0.00028 0.00000 0.00159 0.00218 0.00202 0.00152 0.00155 0.00147 0.00080 C25 0.18038 0.82858 0.06416 1.00000 0.01849 0.02464 0.02039 0.00215 0.00572 0.00218 0.02094 0.00644 0.00033 0.00039 0.00028 0.00000 0.00170 0.00193 0.00178 0.00146 0.00147 0.00143 0.00074 H25 0.17814 0.73071 0.08056 1.00000 0.02513 0.00000 0.00000 B1 0.08115 0.76780 -0.13797 1.00000 0.01781 0.03386 0.01882 0.00168 0.00049 0.00714 0.02355 0.00780 0.00040 0.00047 0.00033 0.00000 0.00187 0.00261 0.00205 0.00175 0.00161 0.00173 0.00090 O2 0.02782 0.82152 -0.23696 1.00000 0.02841 0.03359 0.01880 -0.00078 -0.00112 0.00152 0.02710 0.00455 0.00025 0.00028 0.00019 0.00000 0.00141 0.00160 0.00131 0.00114 0.00112 0.00117 0.00058 H2A -0.01068 0.75687 -0.27549 1.00000 0.04065 0.00000 0.00000 O3 0.08674 0.62824 -0.11251 1.00000 0.03159 0.03074 0.02408 -0.00232 -0.00444 0.00255 0.02918 0.00460 0.00026 0.00027 0.00021 0.00000 0.00146 0.00160 0.00138 0.00113 0.00113 0.00116 0.00060 H3A 0.04101 0.58248 -0.16232 1.00000 0.04376 0.00000 0.00000 P1 0.18209 0.86970 0.37418 1.00000 0.02130 0.02202 0.01684 -0.00125 -0.00074 -0.00057 0.02019 0.00165 0.00009 0.00010 0.00007 0.00000 0.00044 0.00052 0.00044 0.00037 0.00036 0.00039 0.00020 Final Structure Factor Calculation for 2009src0712r in Pn Total number of l.s. parameters = 273 Maximum vector length = 511 Memory required = 3157 / 27090 wR2 = 0.0846 before cycle 11 for 4905 data and 2 / 273 parameters GooF = S = 1.044; Restrained GooF = 1.044 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0428 for 4183 Fo > 4sig(Fo) and 0.0565 for all 4905 data wR2 = 0.0846, GooF = S = 1.044, Restrained GooF = 1.044 for all data Flack x parameter = 0.0401 with su 0.0077 Expected values are 0 (within 3 su'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 = 30.00 for non-hydrogen and 23.00 for hydrogen atoms Principal mean square atomic displacements U 0.0410 0.0305 0.0201 Br1 0.0271 0.0229 0.0136 C1 0.0334 0.0261 0.0181 C2 0.0351 0.0283 0.0250 C3 0.0406 0.0297 0.0168 C4 0.0433 0.0340 0.0150 C5 0.0360 0.0266 0.0204 C6 0.0261 0.0215 0.0184 C7 0.0308 0.0242 0.0187 C8 0.0350 0.0281 0.0229 C9 0.0423 0.0276 0.0183 C10 0.0373 0.0290 0.0170 C11 0.0287 0.0227 0.0209 C12 0.0272 0.0188 0.0147 C13 0.0323 0.0259 0.0181 C14 0.0407 0.0264 0.0176 C15 0.0387 0.0251 0.0218 C16 0.0491 0.0293 0.0196 C17 0.0473 0.0233 0.0202 C18 0.0267 0.0227 0.0195 C19 0.0253 0.0227 0.0152 C20 0.0303 0.0254 0.0190 C21 0.0393 0.0263 0.0201 C22 0.0340 0.0210 0.0180 C23 0.0308 0.0215 0.0152 C24 0.0270 0.0210 0.0148 C25 0.0366 0.0194 0.0147 B1 0.0342 0.0289 0.0181 O2 0.0379 0.0291 0.0206 O3 0.0225 0.0223 0.0158 P1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.041 0.055 0.071 0.086 0.102 0.120 0.143 0.176 0.231 1.000 Number in group 511. 479. 500. 487. 496. 491. 479. 487. 481. 494. GooF 0.952 0.965 1.055 1.127 1.041 1.042 1.042 0.950 1.187 1.058 K 1.403 1.070 1.046 1.002 1.004 0.999 1.003 1.008 1.010 0.989 Resolution(A) 0.77 0.80 0.83 0.88 0.92 0.98 1.05 1.16 1.33 1.66 inf Number in group 491. 496. 499. 488. 482. 486. 500. 481. 489. 493. GooF 0.972 0.970 1.009 1.002 1.060 1.006 0.962 0.936 0.962 1.456 K 1.040 1.060 1.022 1.007 1.010 0.997 1.016 1.014 1.013 0.977 R1 0.174 0.131 0.109 0.082 0.064 0.048 0.035 0.027 0.022 0.025 Recommended weighting scheme: WGHT 0.0238 0.0000 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)/su Fc/Fc(max) Resolution(A) 0 0 2 171.32 752.70 13.31 0.184 6.00 10 3 -7 51.65 97.71 5.61 0.066 0.85 0 4 0 368.39 261.26 5.40 0.108 2.37 -2 0 0 1093.69 2063.45 5.39 0.304 4.90 2 2 4 35.85 89.94 5.05 0.064 2.19 1 0 5 1558.50 1903.25 3.65 0.292 2.29 0 3 -4 153.79 204.95 3.64 0.096 2.18 -2 1 1 4920.12 6439.47 3.58 0.538 4.19 -9 3 -9 220.63 444.46 3.46 0.141 0.79 -1 1 -1 835.98 979.85 3.35 0.210 5.78 -3 0 5 667.37 572.82 3.30 0.160 2.01 -4 4 6 202.45 154.68 3.21 0.083 1.34 -2 3 10 223.11 313.07 3.20 0.119 1.11 -1 8 6 142.23 216.63 3.18 0.099 1.02 9 5 6 119.98 196.10 3.17 0.094 0.83 6 6 -11 101.33 175.39 3.17 0.089 0.81 4 3 0 349.88 434.14 3.16 0.140 1.94 0 9 5 250.80 386.92 3.13 0.132 0.97 1 5 0 1267.13 1098.88 3.11 0.222 1.86 10 7 -3 47.47 115.09 3.08 0.072 0.79 -3 3 2 207.84 163.46 3.04 0.086 2.17 1 3 -4 371.73 320.60 3.00 0.120 2.15 1 9 -10 23.38 137.10 2.91 0.078 0.79 1 5 -1 1296.16 1129.98 2.88 0.225 1.85 1 1 -6 447.52 393.86 2.87 0.133 1.95 1 0 -5 1723.25 1967.03 2.87 0.297 2.38 -3 2 4 168.98 140.98 2.86 0.080 2.07 7 6 -6 78.78 112.74 2.86 0.071 0.95 0 4 -11 138.71 182.03 2.85 0.090 0.99 -1 9 3 317.29 432.87 2.85 0.139 1.02 0 2 0 326.03 265.72 2.84 0.109 4.74 -1 5 0 1509.91 1331.84 2.83 0.245 1.86 0 9 -6 10.68 52.42 2.81 0.049 0.93 3 9 -7 61.40 116.50 2.72 0.072 0.88 -1 3 4 330.83 277.95 2.71 0.112 2.15 -9 1 7 301.27 216.30 2.71 0.099 0.95 3 5 2 411.02 344.23 2.70 0.124 1.57 0 1 -4 1305.49 1437.96 2.68 0.254 2.86 0 1 -11 2.83 43.01 2.67 0.044 1.08 -7 5 8 73.21 124.95 2.66 0.075 0.93 6 7 -1 66.25 27.46 2.66 0.035 1.04 -6 9 -2 46.17 123.48 2.64 0.074 0.87 3 3 -2 155.18 123.12 2.63 0.074 2.17 -5 7 9 22.08 86.08 2.62 0.062 0.88 -3 8 -2 479.78 566.81 2.62 0.160 1.09 -4 5 -6 517.39 608.32 2.61 0.165 1.17 -3 8 5 189.32 247.14 2.61 0.105 1.02 0 10 2 255.91 99.98 2.60 0.067 0.94 7 6 5 240.39 303.57 2.60 0.117 0.94 5 4 -5 359.48 306.50 2.59 0.117 1.32 Bond lengths and angles C1 - Distance Angles C6 1.3906 (0.0050) C2 1.3953 (0.0050) 119.95 (0.33) P1 1.8096 (0.0036) 119.73 (0.27) 120.27 (0.27) C1 - C6 C2 C2 - Distance Angles C3 1.3773 (0.0055) C1 1.3953 (0.0050) 119.85 (0.34) H2 0.9500 120.07 120.07 C2 - C3 C1 C3 - Distance Angles C2 1.3773 (0.0054) C4 1.3993 (0.0054) 120.40 (0.37) H3 0.9500 119.80 119.80 C3 - C2 C4 C4 - Distance Angles C5 1.3884 (0.0052) C3 1.3993 (0.0054) 119.03 (0.37) H4 0.9500 120.48 120.48 C4 - C5 C3 C5 - Distance Angles C6 1.3749 (0.0054) C4 1.3884 (0.0052) 120.97 (0.36) H5 0.9500 119.51 119.51 C5 - C6 C4 C6 - Distance Angles C5 1.3749 (0.0054) C1 1.3906 (0.0050) 119.77 (0.35) H6 0.9500 120.12 120.12 C6 - C5 C1 C7 - Distance Angles C12 1.3973 (0.0050) C8 1.3984 (0.0050) 120.04 (0.33) P1 1.7882 (0.0036) 118.43 (0.27) 121.46 (0.29) C7 - C12 C8 C8 - Distance Angles C9 1.3899 (0.0052) C7 1.3984 (0.0050) 120.07 (0.37) H8 0.9500 119.97 119.97 C8 - C9 C7 C9 - Distance Angles C10 1.3819 (0.0057) C8 1.3899 (0.0053) 119.99 (0.35) H9 0.9500 120.00 120.00 C9 - C10 C8 C10 - Distance Angles C9 1.3819 (0.0057) C11 1.3903 (0.0053) 120.19 (0.35) H10 0.9500 119.90 119.90 C10 - C9 C11 C11 - Distance Angles C10 1.3903 (0.0053) C12 1.3956 (0.0051) 120.53 (0.36) H11 0.9500 119.74 119.74 C11 - C10 C12 C12 - Distance Angles C11 1.3956 (0.0051) C7 1.3973 (0.0050) 119.09 (0.34) H12 0.9500 120.45 120.45 C12 - C11 C7 C13 - Distance Angles C14 1.3815 (0.0050) C18 1.4080 (0.0050) 119.34 (0.33) P1 1.7913 (0.0034) 122.63 (0.27) 118.01 (0.27) C13 - C14 C18 C14 - Distance Angles C15 1.3803 (0.0054) C13 1.3815 (0.0051) 120.42 (0.34) H14 0.9500 119.79 119.79 C14 - C15 C13 C15 - Distance Angles C14 1.3803 (0.0054) C16 1.3801 (0.0053) 120.37 (0.34) H15 0.9500 119.82 119.82 C15 - C14 C16 C16 - Distance Angles C15 1.3801 (0.0053) C17 1.3810 (0.0055) 120.30 (0.36) H16 0.9500 119.85 119.85 C16 - C15 C17 C17 - Distance Angles C16 1.3810 (0.0055) C18 1.3931 (0.0056) 119.84 (0.37) H17 0.9500 120.08 120.08 C17 - C16 C18 C18 - Distance Angles C17 1.3931 (0.0056) C13 1.4080 (0.0050) 119.67 (0.34) H18 0.9500 120.16 120.16 C18 - C17 C13 C19 - Distance Angles C20 1.5102 (0.0048) P1 1.8201 (0.0034) 117.61 (0.24) H19A 0.9900 107.90 107.90 H19B 0.9900 107.90 107.90 107.19 C19 - C20 P1 H19A C20 - Distance Angles C25 1.3865 (0.0049) C21 1.4026 (0.0054) 118.92 (0.32) C19 1.5102 (0.0048) 119.33 (0.32) 121.61 (0.32) C20 - C25 C21 C21 - Distance Angles C22 1.3717 (0.0051) C20 1.4026 (0.0054) 120.46 (0.35) H21 0.9500 119.77 119.77 C21 - C22 C20 C22 - Distance Angles C21 1.3717 (0.0052) C23 1.3865 (0.0064) 120.21 (0.39) H22 0.9500 119.90 119.90 C22 - C21 C23 C23 - Distance Angles C22 1.3865 (0.0064) C24 1.3980 (0.0054) 121.45 (0.50) H23 0.9500 119.28 119.28 C23 - C22 C24 C24 - Distance Angles C23 1.3980 (0.0054) C25 1.4121 (0.0048) 117.24 (0.38) B1 1.5817 (0.0055) 121.51 (0.38) 121.25 (0.33) C24 - C23 C25 C25 - Distance Angles C20 1.3865 (0.0049) C24 1.4121 (0.0048) 121.67 (0.33) H25 0.9500 119.17 119.17 C25 - C20 C24 B1 - Distance Angles O3 1.3593 (0.0050) O2 1.3606 (0.0046) 124.61 (0.36) C24 1.5817 (0.0055) 117.51 (0.32) 117.82 (0.34) B1 - O3 O2 O2 - Distance Angles B1 1.3606 (0.0046) H2A 0.8400 109.47 O2 - B1 O3 - Distance Angles B1 1.3593 (0.0050) H3A 0.8400 109.47 O3 - B1 P1 - Distance Angles C7 1.7882 (0.0036) C13 1.7913 (0.0034) 107.95 (0.17) C1 1.8096 (0.0036) 111.95 (0.16) 108.42 (0.17) C19 1.8201 (0.0034) 110.97 (0.17) 111.09 (0.16) 106.47 (0.16) P1 - C7 C13 C1 FMAP and GRID set by program FMAP 2 2 23 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.0465 for 2561 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.8983 0.3273 0.6457 [ 1.69 A from H15 ] Deepest hole -0.48 at 0.9197 0.4014 0.6982 [ 1.14 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 3079 / 22938 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.1017 1.3273 0.6457 1.00000 0.05 0.29 1.69 H15 1.75 H19B 1.82 BR1 2.31 H25 Q2 1 -0.0063 1.5025 0.5459 1.00000 0.05 0.29 1.44 H16 1.70 H8 1.97 BR1 2.24 C16 Q3 1 0.0686 0.8776 0.1541 1.00000 0.05 0.28 1.35 H12 1.63 C20 1.67 C25 1.85 C12 Q4 1 0.8062 0.5057 0.6248 1.00000 0.05 0.28 1.00 BR1 2.61 H25 2.61 H9 2.96 H19B Q5 1 0.5727 0.5746 0.7247 1.00000 0.05 0.27 0.90 H4 1.67 C4 2.32 H3 2.35 C3 Q6 1 0.4446 0.8791 0.1857 1.00000 0.05 0.27 1.42 H19A 1.83 C19 1.86 H19B 2.18 C20 Q7 1 0.0414 1.4050 0.5608 1.00000 0.05 0.26 0.92 H16 1.45 C16 1.85 H15 1.90 C15 Q8 1 0.2150 1.2969 0.2271 1.00000 0.05 0.26 1.74 H21 2.36 H4 2.53 C21 2.55 C17 Q9 1 0.4399 0.7285 0.2946 1.00000 0.05 0.25 1.36 H19B 1.78 H2 1.92 H19A 2.00 C19 Q10 1 -0.0236 0.6646 -0.4013 1.00000 0.05 0.25 1.74 H2A 1.81 H8 1.95 BR1 2.40 C8 Q11 1 0.8558 0.4281 0.5953 1.00000 0.05 0.25 1.31 BR1 2.05 H15 2.30 H25 2.44 H9 Q12 1 -0.0182 1.2631 0.6071 1.00000 0.05 0.24 1.09 H15 1.48 C15 2.14 C16 2.29 H16 Q13 1 0.1034 1.2274 0.0751 1.00000 0.05 0.24 1.18 H22 1.51 C22 2.01 C21 2.11 H21 Q14 1 0.3795 1.0411 0.1790 1.00000 0.05 0.24 1.45 H21 1.60 C21 1.68 H19A 1.88 C20 Q15 1 0.1762 1.3137 0.0239 1.00000 0.05 0.24 0.98 H22 1.89 C22 2.37 H3 2.51 H9 Q16 1 0.4255 0.6630 0.2407 1.00000 0.05 0.24 1.46 H19B 1.87 BR1 2.05 H2 2.36 C19 Q17 1 0.1159 0.9023 0.6026 1.00000 0.05 0.24 0.99 H6 1.69 C6 2.31 O2 2.43 H2A Q18 1 0.0148 1.0410 0.0822 1.00000 0.05 0.24 1.99 C22 2.00 H12 2.13 C21 2.22 C23 Q19 1 0.1721 0.8324 0.6212 1.00000 0.05 0.24 0.88 H6 1.06 C6 1.95 C5 2.03 C1 Q20 1 0.1949 0.6510 0.5583 1.00000 0.05 0.24 1.73 C1 1.91 H8 1.93 C6 2.01 C2 Shortest distances between peaks (including symmetry equivalents) 17 19 0.88 9 16 0.90 4 11 0.97 2 7 1.05 1 12 1.15 1 16 1.16 1 11 1.19 13 15 1.28 7 12 1.59 6 14 1.66 2 10 1.68 2 11 1.68 6 12 1.70 3 18 1.83 5 8 1.85 12 16 1.88 1 9 1.88 19 20 1.90 7 11 1.92 1 4 1.93 6 9 1.94 1 7 1.95 13 18 1.98 11 12 1.99 11 16 2.02 1 6 2.06 2 4 2.14 8 13 2.16 6 16 2.17 10 20 2.24 4 10 2.29 1 2 2.30 9 12 2.33 4 16 2.37 2 12 2.39 4 15 2.41 2 20 2.42 8 15 2.45 4 8 2.45 10 19 2.49 10 11 2.54 17 20 2.58 7 10 2.59 7 16 2.61 14 17 2.62 5 13 2.64 10 17 2.64 4 7 2.67 4 5 2.76 7 20 2.78 9 11 2.88 4 12 2.89 5 15 2.90 6 17 2.90 2 16 2.95 8 14 3.00 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. 0.61: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.97: Structure factors and derivatives 3.69: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.39: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0712r finished at 12:04:13 Total CPU time: 6.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++