++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker Analytical X-ray Solutions All Rights Reserved + + co110 started at 15:29:06 on 13-Oct-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL Co110 in P-1 #2 CELL 0.71073 7.9999 9.3718 14.7362 82.625 81.527 81.726 ZERR 2 0.0002 0.0003 0.0005 0.001 0.001 0.001 LATT 1 SFAC C H N O F S Co UNIT 32 32 8 8 12 4 2 V = 1074.89 F(000) = 570.0 Mu = 1.08 mm-1 Cell Wt = 1130.76 Rho = 1.747 L.S. 4 PLAN 5 BOND FMAP 2.0 REM C:\Users\Richard\AppData\Roaming\Olex2Data\78dc9a30f39bbafe4282dfce00 REM 1f449b\samples\Co110\Co110.hkl WGHT 0.0376 0.5799 FVAR 0.4345 CO 7 0.09892 0.20544 0.24465 11.00000 0.01565 0.01883 0.01150 = -0.00482 -0.00034 0.00174 S21 6 0.46587 0.03684 0.19103 11.00000 0.01587 0.02008 0.01634 = -0.00578 -0.00118 0.00194 F21 5 0.41241 -0.19766 0.12419 11.00000 0.05055 0.03570 0.03668 = -0.01720 0.00121 -0.01614 F22 5 0.59649 -0.23719 0.22085 11.00000 0.02130 0.02328 0.06944 = -0.00392 -0.00140 0.00584 F23 5 0.32913 -0.19334 0.26977 11.00000 0.02547 0.03061 0.03583 = 0.00409 0.00633 -0.00371 O21 4 0.60667 0.05366 0.11929 11.00000 0.01780 0.02650 0.02576 = -0.00463 0.00153 -0.00085 O22 4 0.48136 0.06055 0.28342 11.00000 0.02593 0.03060 0.01992 = -0.00880 -0.00718 0.00603 N21 3 0.29065 0.11210 0.16349 11.00000 0.01909 0.02866 0.01263 = -0.00661 -0.00083 0.00631 N22 3 0.00158 0.26831 0.12327 11.00000 0.01740 0.01995 0.01528 = -0.00295 -0.00301 0.00009 C21 1 0.45036 -0.15836 0.20231 11.00000 0.01886 0.02419 0.02820 = -0.00469 0.00131 0.00010 C22 1 0.27198 0.13279 0.06430 11.00000 0.02964 0.05802 0.01293 = -0.00942 -0.00398 0.01603 AFIX 23 H22a 2 0.27779 0.03910 0.04185 11.00000 -1.20000 H22b 2 0.36457 0.18160 0.03003 11.00000 -1.20000 AFIX 0 C23 1 0.10403 0.22182 0.04888 11.00000 0.02218 0.02735 0.01608 = -0.00405 -0.00299 -0.00056 C24 1 0.05878 0.25248 -0.03938 11.00000 0.03326 0.03947 0.01553 = -0.00417 -0.00321 -0.00216 AFIX 43 H24 2 0.13092 0.21803 -0.08950 11.00000 -1.20000 AFIX 0 C25 1 -0.09569 0.33529 -0.05168 11.00000 0.03585 0.03792 0.02178 = 0.00550 -0.01383 -0.00792 AFIX 43 H25 2 -0.12830 0.35820 -0.11037 11.00000 -1.20000 AFIX 0 C26 1 -0.20097 0.38356 0.02446 11.00000 0.02579 0.02935 0.03409 = 0.00335 -0.01398 0.00059 AFIX 43 H26 2 -0.30508 0.43929 0.01714 11.00000 -1.20000 AFIX 0 C27 1 -0.15120 0.34881 0.11168 11.00000 0.02004 0.02133 0.02575 = 0.00018 -0.00465 -0.00141 C28 1 -0.26034 0.39422 0.19727 11.00000 0.02440 0.03901 0.03275 = -0.00597 -0.00295 0.01344 AFIX 137 H28a 2 -0.28605 0.30968 0.23821 11.00000 -1.50000 H28b 2 -0.36437 0.44973 0.18114 11.00000 -1.50000 H28c 2 -0.20060 0.45238 0.22736 11.00000 -1.50000 AFIX 0 S11 6 0.19328 0.47445 0.32335 11.00000 0.02126 0.01818 0.01539 = -0.00333 -0.00392 0.00042 F11 5 0.30005 0.41636 0.48616 11.00000 0.03642 0.03642 0.01787 = -0.00649 -0.00792 0.00375 F12 5 0.45741 0.54592 0.38626 11.00000 0.04690 0.03497 0.04594 = 0.00499 -0.02557 -0.01880 F13 5 0.46956 0.31706 0.37815 11.00000 0.02592 0.03402 0.03060 = -0.00814 -0.00683 0.00787 O11 4 0.09088 0.59904 0.35914 11.00000 0.03060 0.01855 0.02634 = -0.00472 -0.00469 0.00351 O12 4 0.28304 0.48773 0.23125 11.00000 0.02559 0.02644 0.01698 = -0.00050 -0.00240 -0.00307 N11 3 0.10194 0.33481 0.33928 11.00000 0.01936 0.02094 0.01364 = -0.00557 0.00047 -0.00120 N12 3 -0.05977 0.10746 0.34684 11.00000 0.01627 0.02013 0.01575 = -0.00192 -0.00323 0.00081 C11 1 0.36513 0.43619 0.39719 11.00000 0.02624 0.02240 0.02062 = -0.00313 -0.00619 -0.00196 C12 1 -0.02822 0.31833 0.42093 11.00000 0.02295 0.02550 0.01734 = -0.00852 0.00372 0.00019 AFIX 23 H12a 2 -0.11899 0.39877 0.41797 11.00000 -1.20000 H12b 2 0.02258 0.31887 0.47671 11.00000 -1.20000 AFIX 0 C13 1 -0.09943 0.17788 0.42322 11.00000 0.01597 0.02506 0.01693 = -0.00326 -0.00237 0.00209 C14 1 -0.20402 0.12508 0.50026 11.00000 0.02032 0.03529 0.01541 = -0.00068 -0.00113 0.00244 AFIX 43 H14 2 -0.22942 0.17497 0.55222 11.00000 -1.20000 AFIX 0 C15 1 -0.26961 -0.00279 0.49834 11.00000 0.01943 0.04173 0.02267 = 0.00921 -0.00258 -0.00540 AFIX 43 H15 2 -0.33987 -0.04031 0.54913 11.00000 -1.20000 AFIX 0 C16 1 -0.22947 -0.07480 0.41966 11.00000 0.02369 0.03048 0.02952 = 0.00696 -0.01075 -0.00797 AFIX 43 H16 2 -0.27291 -0.16102 0.41760 11.00000 -1.20000 AFIX 0 C17 1 -0.12489 -0.01823 0.34442 11.00000 0.01703 0.02382 0.02392 = 0.00126 -0.00938 -0.00067 C18 1 -0.07969 -0.08750 0.25616 11.00000 0.02460 0.02336 0.02958 = -0.00524 -0.00988 -0.00240 AFIX 137 H18a 2 -0.14265 -0.03283 0.20973 11.00000 -1.50000 H18c 2 -0.10769 -0.18501 0.26640 11.00000 -1.50000 H18b 2 0.04017 -0.08894 0.23593 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for Co110 in P-1 #2 C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 S 1.030 CO 1.250 Co - N11 N21 N12 N22 S21 - O22 O21 N21 C21 F21 - C21 F22 - C21 F23 - C21 O21 - S21 O22 - S21 N21 - C22 S21 Co N22 - C23 C27 Co C21 - F23 F22 F21 S21 C22 - N21 C23 C23 - N22 C24 C22 C24 - C25 C23 C25 - C26 C24 C26 - C25 C27 C27 - N22 C26 C28 C28 - C27 S11 - O11 O12 N11 C11 F11 - C11 F12 - C11 F13 - C11 O11 - S11 O12 - S11 N11 - C12 S11 Co N12 - C13 C17 Co C11 - F13 F12 F11 S11 C12 - N11 C13 C13 - N12 C14 C12 C14 - C15 C13 C15 - C14 C16 C16 - C17 C15 C17 - N12 C16 C18 C18 - C17 11963 Reflections read, of which 0 rejected -9 =< h =< 10, -12 =< k =< 12, -19 =< l =< 19, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 4897 Unique reflections, of which 0 suppressed R(int) = 0.0290 R(sigma) = 0.0369 Friedel opposites merged Maximum memory for data reduction = 2450 / 49038 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 = 3242 / 378411 wR2 = 0.0819 before cycle 1 for 4897 data and 300 / 300 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0376 * P )^2 + 0.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43450 0.00054 0.007 OSF Mean shift/esd = 0.007 Maximum = -0.150 for z Co Max. shift = 0.000 A for H18C Max. dU = 0.000 for N21 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3242 / 378411 wR2 = 0.0819 before cycle 2 for 4897 data and 300 / 300 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0376 * P )^2 + 0.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43450 0.00054 -0.002 OSF Mean shift/esd = 0.002 Maximum = -0.049 for z Co Max. shift = 0.000 A for H28A Max. dU = 0.000 for F12 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3242 / 378411 wR2 = 0.0819 before cycle 3 for 4897 data and 300 / 300 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0376 * P )^2 + 0.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43450 0.00054 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y F12 Max. shift = 0.000 A for H28A Max. dU = 0.000 for C18 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3242 / 378411 wR2 = 0.0819 before cycle 4 for 4897 data and 300 / 300 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0376 * P )^2 + 0.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43450 0.00054 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H18C Max. dU = 0.000 for F12 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 H22A 0.2778 0.0391 0.0419 23 0.970 0.000 C22 N21 C23 H22B 0.3646 0.1816 0.0300 23 0.970 0.000 C22 N21 C23 H24 0.1309 0.2180 -0.0895 43 0.930 0.000 C24 C25 C23 H25 -0.1283 0.3582 -0.1104 43 0.930 0.000 C25 C26 C24 H26 -0.3051 0.4393 0.0171 43 0.930 0.000 C26 C25 C27 H28A -0.2861 0.3097 0.2382 137 0.960 0.000 C28 C27 H28A H28B -0.3644 0.4497 0.1811 137 0.960 0.000 C28 C27 H28A H28C -0.2006 0.4524 0.2274 137 0.960 0.000 C28 C27 H28A H12A -0.1190 0.3988 0.4180 23 0.970 0.000 C12 N11 C13 H12B 0.0226 0.3189 0.4767 23 0.970 0.000 C12 N11 C13 H14 -0.2294 0.1750 0.5522 43 0.930 0.000 C14 C15 C13 H15 -0.3399 -0.0403 0.5491 43 0.930 0.000 C15 C14 C16 H16 -0.2729 -0.1610 0.4176 43 0.930 0.000 C16 C17 C15 H18A -0.1426 -0.0328 0.2097 137 0.960 0.000 C18 C17 H18A H18C -0.1077 -0.1850 0.2664 137 0.960 0.000 C18 C17 H18A H18B 0.0402 -0.0889 0.2359 137 0.960 0.000 C18 C17 H18A Co110 in P-1 #2 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Co 0.09892 0.20544 0.24465 1.00000 0.01565 0.01883 0.01150 -0.00482 -0.00034 0.00174 0.01559 0.00040 0.00003 0.00003 0.00002 0.00000 0.00014 0.00015 0.00013 0.00010 0.00010 0.00010 0.00008 S21 0.46587 0.03684 0.19103 1.00000 0.01587 0.02008 0.01634 -0.00578 -0.00118 0.00194 0.01761 0.00075 0.00006 0.00005 0.00003 0.00000 0.00025 0.00025 0.00024 0.00019 0.00018 0.00018 0.00011 F21 0.41241 -0.19766 0.12419 1.00000 0.05055 0.03570 0.03668 -0.01720 0.00121 -0.01614 0.03945 0.00211 0.00020 0.00016 0.00010 0.00000 0.00095 0.00080 0.00082 0.00065 0.00069 0.00069 0.00036 F22 0.59649 -0.23720 0.22085 1.00000 0.02130 0.02328 0.06944 -0.00392 -0.00140 0.00584 0.03944 0.00240 0.00017 0.00014 0.00012 0.00000 0.00072 0.00070 0.00109 0.00068 0.00068 0.00055 0.00037 F23 0.32913 -0.19334 0.26977 1.00000 0.02547 0.03061 0.03583 0.00409 0.00633 -0.00371 0.03236 0.00227 0.00017 0.00015 0.00010 0.00000 0.00072 0.00072 0.00078 0.00058 0.00058 0.00055 0.00032 O21 0.60667 0.05366 0.11929 1.00000 0.01780 0.02650 0.02576 -0.00463 0.00153 -0.00085 0.02384 0.00235 0.00019 0.00016 0.00011 0.00000 0.00075 0.00079 0.00079 0.00062 0.00060 0.00060 0.00033 O22 0.48136 0.06054 0.28342 1.00000 0.02593 0.03060 0.01992 -0.00880 -0.00718 0.00603 0.02548 0.00232 0.00020 0.00017 0.00010 0.00000 0.00083 0.00083 0.00076 0.00063 0.00062 0.00065 0.00034 N21 0.29065 0.11210 0.16349 1.00000 0.01909 0.02866 0.01263 -0.00661 -0.00083 0.00631 0.02080 0.00273 0.00022 0.00020 0.00011 0.00000 0.00089 0.00095 0.00081 0.00070 0.00066 0.00071 0.00037 N22 0.00158 0.26831 0.12326 1.00000 0.01740 0.01995 0.01528 -0.00295 -0.00301 0.00009 0.01761 0.00255 0.00021 0.00018 0.00011 0.00000 0.00086 0.00084 0.00081 0.00066 0.00065 0.00066 0.00035 C21 0.45036 -0.15836 0.20231 1.00000 0.01886 0.02419 0.02820 -0.00469 0.00131 0.00010 0.02432 0.00349 0.00028 0.00024 0.00016 0.00000 0.00106 0.00108 0.00114 0.00089 0.00086 0.00084 0.00045 C22 0.27198 0.13279 0.06430 1.00000 0.02964 0.05802 0.01293 -0.00942 -0.00398 0.01603 0.03507 0.00415 0.00031 0.00031 0.00015 0.00000 0.00130 0.00167 0.00102 0.00104 0.00089 0.00115 0.00061 H22A 0.27779 0.03910 0.04185 1.00000 0.04208 0.00000 0.00000 H22B 0.36457 0.18160 0.03003 1.00000 0.04208 0.00000 0.00000 C23 0.10403 0.22182 0.04888 1.00000 0.02218 0.02735 0.01608 -0.00405 -0.00299 -0.00056 0.02193 0.00324 0.00028 0.00024 0.00014 0.00000 0.00109 0.00111 0.00099 0.00083 0.00080 0.00086 0.00044 C24 0.05878 0.25248 -0.03938 1.00000 0.03326 0.03947 0.01553 -0.00417 -0.00321 -0.00216 0.02956 0.00360 0.00032 0.00027 0.00015 0.00000 0.00130 0.00135 0.00103 0.00094 0.00090 0.00104 0.00051 H24 0.13092 0.21803 -0.08950 1.00000 0.03548 0.00000 0.00000 C25 -0.09569 0.33529 -0.05168 1.00000 0.03585 0.03792 0.02178 0.00550 -0.01383 -0.00792 0.03128 0.00369 0.00032 0.00027 0.00016 0.00000 0.00136 0.00133 0.00113 0.00097 0.00098 0.00106 0.00053 H25 -0.12830 0.35820 -0.11037 1.00000 0.03754 0.00000 0.00000 C26 -0.20097 0.38356 0.02446 1.00000 0.02579 0.02935 0.03409 0.00335 -0.01398 0.00059 0.02973 0.00365 0.00031 0.00026 0.00017 0.00000 0.00121 0.00120 0.00129 0.00098 0.00099 0.00094 0.00051 H26 -0.30508 0.43929 0.01714 1.00000 0.03568 0.00000 0.00000 C27 -0.15120 0.34881 0.11168 1.00000 0.02004 0.02133 0.02575 0.00018 -0.00465 -0.00141 0.02257 0.00334 0.00027 0.00023 0.00015 0.00000 0.00107 0.00104 0.00111 0.00085 0.00085 0.00082 0.00044 C28 -0.26034 0.39422 0.19727 1.00000 0.02440 0.03901 0.03275 -0.00597 -0.00295 0.01344 0.03369 0.00419 0.00031 0.00028 0.00017 0.00000 0.00122 0.00136 0.00131 0.00106 0.00098 0.00102 0.00056 H28A -0.28605 0.30968 0.23820 1.00000 0.05054 0.00000 0.00000 H28B -0.36437 0.44973 0.18114 1.00000 0.05054 0.00000 0.00000 H28C -0.20060 0.45238 0.22736 1.00000 0.05054 0.00000 0.00000 S11 0.19328 0.47445 0.32335 1.00000 0.02126 0.01818 0.01539 -0.00333 -0.00392 0.00042 0.01828 0.00076 0.00007 0.00005 0.00003 0.00000 0.00026 0.00024 0.00024 0.00018 0.00019 0.00019 0.00011 F11 0.30005 0.41636 0.48616 1.00000 0.03642 0.03642 0.01787 -0.00649 -0.00792 0.00375 0.03032 0.00202 0.00018 0.00015 0.00009 0.00000 0.00078 0.00075 0.00063 0.00054 0.00055 0.00060 0.00031 F12 0.45741 0.54592 0.38626 1.00000 0.04690 0.03497 0.04594 0.00499 -0.02557 -0.01880 0.04010 0.00206 0.00020 0.00016 0.00011 0.00000 0.00093 0.00080 0.00089 0.00066 0.00074 0.00068 0.00037 F13 0.46955 0.31706 0.37815 1.00000 0.02592 0.03402 0.03060 -0.00814 -0.00683 0.00787 0.03062 0.00208 0.00017 0.00015 0.00009 0.00000 0.00071 0.00074 0.00073 0.00058 0.00056 0.00057 0.00031 O11 0.09088 0.59904 0.35914 1.00000 0.03060 0.01855 0.02634 -0.00472 -0.00469 0.00351 0.02553 0.00237 0.00020 0.00016 0.00011 0.00000 0.00088 0.00075 0.00081 0.00061 0.00066 0.00063 0.00034 O12 0.28304 0.48773 0.23125 1.00000 0.02559 0.02644 0.01698 -0.00050 -0.00240 -0.00307 0.02323 0.00228 0.00019 0.00016 0.00010 0.00000 0.00081 0.00080 0.00073 0.00060 0.00060 0.00063 0.00032 N11 0.10194 0.33481 0.33928 1.00000 0.01936 0.02094 0.01364 -0.00557 0.00047 -0.00120 0.01806 0.00256 0.00022 0.00018 0.00011 0.00000 0.00087 0.00086 0.00079 0.00066 0.00065 0.00067 0.00035 N12 -0.05977 0.10746 0.34684 1.00000 0.01627 0.02013 0.01575 -0.00192 -0.00323 0.00081 0.01758 0.00257 0.00021 0.00018 0.00011 0.00000 0.00085 0.00085 0.00081 0.00066 0.00065 0.00065 0.00034 C11 0.36514 0.43619 0.39719 1.00000 0.02624 0.02240 0.02062 -0.00313 -0.00619 -0.00196 0.02281 0.00327 0.00029 0.00023 0.00015 0.00000 0.00114 0.00105 0.00103 0.00083 0.00085 0.00085 0.00044 C12 -0.02822 0.31833 0.42093 1.00000 0.02295 0.02550 0.01734 -0.00852 0.00372 0.00019 0.02236 0.00332 0.00028 0.00023 0.00014 0.00000 0.00109 0.00109 0.00099 0.00083 0.00081 0.00085 0.00044 H12A -0.11899 0.39877 0.41797 1.00000 0.02683 0.00000 0.00000 H12B 0.02258 0.31887 0.47671 1.00000 0.02683 0.00000 0.00000 C13 -0.09943 0.17788 0.42322 1.00000 0.01597 0.02506 0.01693 -0.00326 -0.00237 0.00209 0.01968 0.00320 0.00026 0.00023 0.00014 0.00000 0.00099 0.00105 0.00097 0.00080 0.00077 0.00079 0.00042 C14 -0.20402 0.12508 0.50026 1.00000 0.02032 0.03529 0.01541 -0.00068 -0.00113 0.00244 0.02458 0.00356 0.00027 0.00025 0.00015 0.00000 0.00109 0.00122 0.00098 0.00087 0.00080 0.00090 0.00046 H14 -0.22942 0.17497 0.55222 1.00000 0.02949 0.00000 0.00000 C15 -0.26962 -0.00279 0.49834 1.00000 0.01943 0.04173 0.02267 0.00921 -0.00258 -0.00540 0.02894 0.00377 0.00029 0.00027 0.00016 0.00000 0.00113 0.00137 0.00113 0.00098 0.00088 0.00097 0.00051 H15 -0.33987 -0.04031 0.54913 1.00000 0.03473 0.00000 0.00000 C16 -0.22947 -0.07480 0.41966 1.00000 0.02369 0.03048 0.02952 0.00696 -0.01075 -0.00797 0.02762 0.00357 0.00029 0.00026 0.00016 0.00000 0.00117 0.00121 0.00121 0.00096 0.00094 0.00093 0.00049 H16 -0.27291 -0.16102 0.41760 1.00000 0.03314 0.00000 0.00000 C17 -0.12489 -0.01823 0.34442 1.00000 0.01703 0.02382 0.02392 0.00126 -0.00938 -0.00067 0.02144 0.00321 0.00027 0.00023 0.00015 0.00000 0.00102 0.00106 0.00109 0.00085 0.00083 0.00081 0.00043 C18 -0.07969 -0.08750 0.25616 1.00000 0.02460 0.02336 0.02958 -0.00524 -0.00988 -0.00240 0.02506 0.00327 0.00029 0.00024 0.00016 0.00000 0.00114 0.00109 0.00117 0.00090 0.00091 0.00087 0.00046 H18A -0.14265 -0.03283 0.20973 1.00000 0.03759 0.00000 0.00000 H18C -0.10769 -0.18501 0.26640 1.00000 0.03759 0.00000 0.00000 H18B 0.04017 -0.08894 0.23593 1.00000 0.03759 0.00000 0.00000 Final Structure Factor Calculation for Co110 in P-1 #2 Total number of l.s. parameters = 300 Maximum vector length = 511 Memory required = 2942 / 26061 wR2 = 0.0819 before cycle 5 for 4897 data and 0 / 300 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0376 * P )^2 + 0.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0312 for 4121 Fo > 4sig(Fo) and 0.0410 for all 4897 data wR2 = 0.0819, GooF = S = 1.047, Restrained GooF = 1.047 for all data Occupancy sum of asymmetric unit = 33.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0221 0.0154 0.0092 Co 0.0238 0.0172 0.0119 S21 0.0612 0.0380 0.0191 F21 0.0716 0.0322 0.0145 F22 0.0492 0.0291 0.0188 F23 0.0284 0.0272 0.0159 O21 0.0407 0.0195 0.0163 O22 0.0358 0.0168 0.0098 N21 0.0219 0.0162 0.0148 N22 0.0307 0.0258 0.0165 C21 0.0729 0.0208 0.0115 C22 0.0288 0.0214 0.0155 C23 0.0408 0.0327 0.0152 C24 0.0462 0.0332 0.0145 C25 0.0411 0.0326 0.0155 C26 0.0274 0.0220 0.0183 C27 0.0535 0.0330 0.0146 C28 0.0236 0.0168 0.0144 S11 0.0463 0.0290 0.0157 F11 0.0700 0.0309 0.0194 F12 0.0448 0.0281 0.0189 F13 0.0346 0.0260 0.0160 O11 0.0273 0.0256 0.0168 O12 0.0222 0.0208 0.0112 N11 0.0223 0.0162 0.0142 N12 0.0277 0.0222 0.0186 C11 0.0282 0.0281 0.0108 C12 0.0278 0.0168 0.0145 C13 0.0394 0.0191 0.0153 C14 0.0499 0.0198 0.0171 C15 0.0432 0.0221 0.0176 C16 0.0287 0.0241 0.0115 C17 0.0336 0.0231 0.0184 C18 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.028 0.041 0.054 0.071 0.088 0.109 0.138 0.186 1.000 Number in group 519. 493. 485. 470. 504. 473. 482. 491. 486. 494. GooF 0.959 1.033 1.126 1.033 1.075 1.059 0.965 1.152 0.991 1.065 K 0.687 0.948 1.004 1.036 1.035 1.019 1.012 1.002 0.991 1.004 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.65 inf Number in group 491. 499. 494. 475. 490. 495. 488. 489. 482. 494. GooF 0.887 0.907 0.915 0.886 0.935 0.914 0.935 0.893 1.161 1.730 K 1.027 1.019 1.020 1.012 0.991 0.988 0.986 0.985 0.995 1.018 R1 0.070 0.071 0.060 0.049 0.044 0.038 0.034 0.025 0.026 0.029 Recommended weighting scheme: WGHT 0.0376 0.5789 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 0 0 1 314.10 688.60 10.90 0.135 14.49 1 4 6 125.42 2.33 9.22 0.008 1.80 1 -1 8 83.00 40.09 5.42 0.033 1.74 -3 -3 6 192.92 106.69 5.33 0.053 1.47 0 2 7 331.16 234.43 5.31 0.079 1.97 -1 4 5 2377.49 1895.81 5.10 0.224 1.78 0 -1 7 30.33 9.18 4.66 0.016 1.97 -1 1 5 819.84 634.48 4.61 0.129 2.55 -1 2 4 982.27 788.05 4.49 0.144 2.65 3 4 3 104.52 62.30 4.39 0.041 1.84 1 0 7 201.07 140.11 4.04 0.061 2.07 0 -1 5 24.68 8.39 3.92 0.015 2.68 3 3 3 95.28 60.41 3.86 0.040 2.10 -2 1 3 322.27 245.62 3.80 0.080 2.72 4 2 13 190.00 133.52 3.79 0.059 1.04 -2 3 2 275.98 214.08 3.72 0.075 2.18 3 -3 1 75.61 46.92 3.65 0.035 1.87 0 3 4 3252.87 2785.11 3.59 0.271 2.48 -3 5 4 362.53 284.82 3.58 0.087 1.33 2 -4 2 649.10 786.15 3.56 0.144 1.81 2 -3 1 232.29 180.53 3.51 0.069 2.25 1 1 9 509.83 625.96 3.45 0.128 1.63 4 -1 1 622.92 514.09 3.45 0.116 1.88 3 4 8 996.74 826.94 3.32 0.148 1.43 2 -2 2 2721.15 2344.90 3.31 0.249 2.65 -2 3 4 1051.42 899.49 3.21 0.154 1.94 -1 -2 7 30.17 51.51 3.21 0.037 1.74 -3 -3 1 183.34 232.80 3.20 0.078 2.05 9 1 8 202.87 138.93 3.16 0.061 0.84 1 5 1 223.03 176.60 3.13 0.068 1.87 0 -4 7 40.61 21.61 3.13 0.024 1.46 1 -2 2 70.58 45.45 3.12 0.035 3.31 4 3 0 1010.45 1180.08 3.10 0.176 1.76 2 -3 2 398.41 330.97 3.10 0.093 2.17 -1 2 5 16.18 31.83 3.08 0.029 2.33 4 0 2 26.81 9.97 3.08 0.016 1.96 9 1 3 97.78 43.32 3.08 0.034 0.89 -2 1 5 71.06 42.95 3.08 0.034 2.14 -2 4 1 95.12 68.90 3.08 0.043 1.88 2 6 3 595.75 489.26 3.02 0.114 1.50 -3 2 0 521.95 435.95 3.02 0.107 2.16 -1 -1 9 52.65 83.23 3.01 0.047 1.50 0 3 3 9.12 21.19 2.98 0.024 2.73 7 3 15 184.35 127.61 2.98 0.058 0.79 -1 1 4 1381.95 1190.12 2.97 0.177 3.01 3 -2 5 453.98 380.70 2.93 0.100 1.78 -1 -1 12 26.39 53.57 2.92 0.038 1.15 -1 3 4 7368.56 6524.66 2.91 0.415 2.24 7 -3 4 489.57 406.36 2.88 0.104 1.00 -5 1 13 214.94 163.31 2.88 0.066 0.85 Bond lengths and angles Co - Distance Angles N11 1.9667 (0.0016) N21 1.9723 (0.0016) 129.33 (0.07) N12 2.0346 (0.0017) 82.16 (0.07) 127.66 (0.07) N22 2.0398 (0.0017) 124.50 (0.07) 82.85 (0.07) 115.16 (0.07) Co - N11 N21 N12 S21 - Distance Angles O22 1.4331 (0.0015) O21 1.4383 (0.0015) 119.72 (0.10) N21 1.5610 (0.0018) 110.37 (0.09) 113.89 (0.09) C21 1.8360 (0.0023) 102.48 (0.10) 103.24 (0.09) 105.05 (0.10) S21 - O22 O21 N21 F21 - Distance Angles C21 1.3406 (0.0026) F21 - F22 - Distance Angles C21 1.3345 (0.0025) F22 - F23 - Distance Angles C21 1.3267 (0.0025) F23 - O21 - Distance Angles S21 1.4383 (0.0015) O21 - O22 - Distance Angles S21 1.4331 (0.0015) O22 - N21 - Distance Angles C22 1.4763 (0.0027) S21 1.5610 (0.0018) 117.20 (0.14) Co 1.9723 (0.0016) 115.23 (0.13) 127.10 (0.10) N21 - C22 S21 N22 - Distance Angles C23 1.3484 (0.0025) C27 1.3621 (0.0027) 119.25 (0.18) Co 2.0398 (0.0017) 113.83 (0.14) 126.92 (0.14) N22 - C23 C27 C21 - Distance Angles F23 1.3267 (0.0025) F22 1.3345 (0.0025) 107.95 (0.18) F21 1.3406 (0.0026) 107.74 (0.18) 107.61 (0.18) S21 1.8360 (0.0023) 110.78 (0.14) 111.58 (0.15) 111.02 (0.16) C21 - F23 F22 F21 C22 - Distance Angles N21 1.4763 (0.0027) C23 1.5073 (0.0031) 110.28 (0.17) C22 - N21 C23 - Distance Angles N22 1.3484 (0.0025) C24 1.3848 (0.0030) 122.17 (0.20) C22 1.5073 (0.0031) 117.80 (0.18) 120.03 (0.19) C23 - N22 C24 C24 - Distance Angles C25 1.3842 (0.0034) C23 1.3848 (0.0030) 118.84 (0.21) C24 - C25 C25 - Distance Angles C26 1.3840 (0.0035) C24 1.3842 (0.0034) 119.16 (0.21) C25 - C26 C26 - Distance Angles C25 1.3840 (0.0035) C27 1.3865 (0.0032) 119.98 (0.22) C26 - C25 C27 - Distance Angles N22 1.3621 (0.0027) C26 1.3865 (0.0032) 120.60 (0.20) C28 1.4969 (0.0031) 116.53 (0.19) 122.86 (0.21) C27 - N22 C26 C28 - Distance Angles C27 1.4969 (0.0031) C28 - S11 - Distance Angles O11 1.4381 (0.0015) O12 1.4381 (0.0015) 119.80 (0.09) N11 1.5644 (0.0018) 113.93 (0.09) 109.52 (0.09) C11 1.8442 (0.0023) 102.71 (0.10) 103.66 (0.10) 105.36 (0.10) S11 - O11 O12 N11 F11 - Distance Angles C11 1.3374 (0.0025) F11 - F12 - Distance Angles C11 1.3302 (0.0025) F12 - F13 - Distance Angles C11 1.3289 (0.0025) F13 - O11 - Distance Angles S11 1.4381 (0.0015) O11 - O12 - Distance Angles S11 1.4381 (0.0015) O12 - N11 - Distance Angles C12 1.4782 (0.0025) S11 1.5644 (0.0018) 117.99 (0.13) Co 1.9667 (0.0016) 115.10 (0.13) 124.80 (0.10) N11 - C12 S11 N12 - Distance Angles C13 1.3521 (0.0025) C17 1.3613 (0.0027) 119.48 (0.18) Co 2.0346 (0.0017) 114.19 (0.14) 126.33 (0.14) N12 - C13 C17 C11 - Distance Angles F13 1.3289 (0.0025) F12 1.3302 (0.0025) 107.98 (0.19) F11 1.3374 (0.0025) 107.43 (0.17) 108.06 (0.17) S11 1.8442 (0.0023) 111.89 (0.14) 110.85 (0.15) 110.48 (0.15) C11 - F13 F12 F11 C12 - Distance Angles N11 1.4782 (0.0025) C13 1.5024 (0.0030) 109.38 (0.16) C12 - N11 C13 - Distance Angles N12 1.3521 (0.0025) C14 1.3888 (0.0029) 121.91 (0.20) C12 1.5024 (0.0030) 117.16 (0.18) 120.91 (0.18) C13 - N12 C14 C14 - Distance Angles C15 1.3807 (0.0034) C13 1.3888 (0.0029) 118.82 (0.20) C14 - C15 C15 - Distance Angles C14 1.3807 (0.0034) C16 1.3899 (0.0034) 119.25 (0.20) C15 - C14 C16 - Distance Angles C17 1.3834 (0.0031) C15 1.3899 (0.0034) 120.00 (0.21) C16 - C17 C17 - Distance Angles N12 1.3613 (0.0027) C16 1.3834 (0.0031) 120.52 (0.20) C18 1.5014 (0.0030) 116.36 (0.18) 123.10 (0.20) C17 - N12 C16 C18 - Distance Angles C17 1.5014 (0.0030) C18 - FMAP and GRID set by program FMAP 2 1 21 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0398 for 4897 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.63 at 0.2829 0.4569 0.3627 [ 0.87 A from C11 ] Deepest hole -0.38 at -0.0051 0.7618 0.7188 [ 0.90 A from CO ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2972 / 23778 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2829 0.4569 0.3627 1.00000 0.05 0.63 0.87 C11 0.97 S11 1.82 F12 1.83 F11 Q2 1 0.0281 0.1439 0.2968 1.00000 0.05 0.48 1.00 N12 1.05 CO 2.03 C13 2.08 C17 Q3 1 -0.0096 0.1781 0.2352 1.00000 0.05 0.48 0.97 CO 1.71 N12 1.75 N22 2.37 H28A Q4 1 0.0550 0.2536 0.1774 1.00000 0.05 0.45 0.95 N22 1.12 CO 1.93 C23 2.07 C27 Q5 1 0.3623 0.0538 0.1741 1.00000 0.05 0.39 0.75 N21 0.89 S21 1.89 C22 2.00 O22 Shortest distances between peaks (including symmetry equivalents) 2 3 1.00 3 4 1.15 2 4 1.92 4 5 2.87 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. 0.03: 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 0.39: Structure factors and derivatives 1.20: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + co110 finished at 15:29:08 Total CPU time: 1.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++