+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0992 started at 15:43:26 on 09-Oct-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0992 in P-1 CELL 0.71073 7.2720 7.4040 18.1310 86.128 78.470 89.295 ZERR 4.00 0.0015 0.0015 0.0036 0.030 0.030 0.030 LATT 1 SFAC C H O S MO ND UNIT 20 12 32 4 4 4 V = 954.32 F(000) = 860.0 Mu = 6.94 mm-1 Cell Wt = 1853.26 Rho = 3.225 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 DELU EADP O38 O32 EADP O39 O32 SIMU C23 C22 C21 C26 FMAP 2 PLAN 10 SIZE 0.01 0.02 0.14 ACTA BOND $H WGHT 0.02450 78.37310 L.S. 4 TEMP -153.00 FVAR 0.27286 C1 1 0.209317 0.438555 0.876338 11.00000 0.02279 0.01424 = 0.01818 -0.00145 -0.00416 0.00367 C2 1 0.018386 0.415840 0.904990 11.00000 0.02480 0.01830 = 0.00907 -0.00093 -0.01098 -0.00425 AFIX 43 H2 2 -0.059016 0.366083 0.875008 11.00000 -1.20000 AFIX 0 C3 1 -0.060450 0.465333 0.977217 11.00000 0.02203 0.01673 = 0.01697 0.00457 -0.00453 0.00428 C5 1 -0.248159 0.431587 1.010546 11.00000 0.02334 0.03444 = 0.03849 -0.00230 -0.00583 0.00754 AFIX 43 H5 2 -0.325361 0.374703 0.982394 11.00000 -1.20000 AFIX 0 C6 1 0.325082 0.523412 0.918534 11.00000 0.03302 0.00743 = 0.02970 -0.00728 -0.00498 -0.00077 AFIX 43 H6 2 0.453457 0.548055 0.897533 11.00000 -1.20000 AFIX 0 C21 1 -0.090331 0.899159 0.882048 11.00000 0.02354 0.01876 = 0.00601 0.00652 -0.00494 -0.00134 C22 1 -0.258275 0.895029 0.938918 11.00000 0.02917 0.02553 = 0.02730 -0.00510 0.00117 -0.00981 AFIX 43 H22 2 -0.372743 0.856419 0.927341 11.00000 -1.20000 AFIX 0 C23 1 -0.255457 0.945979 1.009519 11.00000 0.01113 0.03265 = 0.02929 -0.01605 0.00021 0.00514 AFIX 43 H23 2 -0.367061 0.942753 1.047194 11.00000 -1.20000 AFIX 0 C24 1 -0.080954 1.004844 1.026317 11.00000 0.01579 0.02360 = 0.01010 0.00115 0.00255 0.00881 C26 1 0.074913 0.944175 0.900666 11.00000 0.01904 0.02172 = 0.01312 -0.00743 -0.00024 0.00610 AFIX 43 H26 2 0.187846 0.941168 0.863873 11.00000 -1.20000 AFIX 0 O1 3 0.456821 0.233667 0.802005 11.00000 0.02075 0.01620 = 0.01986 0.00122 -0.00691 -0.00061 O2 3 0.170146 0.291266 0.754809 11.00000 0.01194 0.03169 = 0.01063 -0.00045 -0.00190 0.00077 O3 3 0.404269 0.527912 0.746079 11.00000 0.02510 0.01917 = 0.01738 0.00383 -0.00732 -0.00539 O21 3 -0.257377 0.724352 0.800304 11.00000 0.02001 0.01512 = 0.02006 -0.00275 -0.00109 -0.00399 O22 3 0.072540 0.769903 0.757299 11.00000 0.01210 0.03004 = 0.00606 -0.00452 -0.00339 -0.00164 O23 3 -0.137296 0.020549 0.750921 11.00000 0.02120 0.01914 = 0.01536 -0.00127 -0.00226 -0.00016 O30 3 0.444227 0.889351 0.748398 11.00000 0.01162 0.02020 = 0.01631 -0.00358 -0.00305 -0.00305 O31 3 -0.194530 0.377665 0.751996 11.00000 0.01127 0.02081 = 0.01614 -0.00397 0.00218 -0.00176 O32 3 -0.292402 0.223546 0.624733 11.00000 0.01511 0.02109 = 0.00961 -0.00015 0.00188 -0.00238 O33 3 0.032323 0.565315 0.623368 11.00000 0.01515 0.02029 = 0.01068 0.00138 -0.00119 -0.00177 O34 3 0.401252 0.445479 0.593835 11.00000 0.01812 0.01984 = 0.01220 -0.00370 -0.00030 0.00079 O35 3 0.075154 0.284288 0.515664 11.00000 0.01746 0.02205 = 0.00469 0.00065 -0.00607 -0.00509 O36 3 0.339884 0.074848 0.623604 11.00000 0.01644 0.02426 = 0.00194 0.00195 -0.00217 0.00041 O37 3 0.403699 0.795094 0.515379 11.00000 0.02403 0.02159 = 0.00845 0.00036 0.00034 -0.00533 O38 3 0.667848 0.736420 0.621969 11.00000 0.01511 0.02109 = 0.00961 -0.00015 0.00188 -0.00238 O39 3 0.012568 -0.065650 0.598238 11.00000 0.01511 0.02109 = 0.00961 -0.00015 0.00188 -0.00238 S1 4 0.316371 0.367450 0.788451 11.00000 0.01350 0.01768 = 0.01099 -0.00121 -0.00210 0.00174 S2 4 -0.103404 0.848200 0.790683 11.00000 0.01544 0.01447 = 0.01005 -0.00090 -0.00039 -0.00130 MO1 5 0.515173 0.237990 0.580708 11.00000 0.01227 0.01478 = 0.00898 -0.00112 -0.00207 0.00031 MO2 5 -0.094558 0.737167 0.580209 11.00000 0.01171 0.01513 = 0.01021 -0.00135 -0.00236 -0.00022 ND1 6 0.018400 0.236098 0.649355 11.00000 0.01355 0.01440 = 0.01021 -0.00148 -0.00274 0.00076 ND2 6 0.329952 0.743810 0.646870 11.00000 0.01250 0.01490 = 0.01016 -0.00150 -0.00122 -0.00006 HKLF 4 Covalent radii and connectivity table for 2008src0992 in P-1 C 0.770 H 0.320 O 0.660 S 1.030 MO 1.360 ND 1.810 C1 - C2 C6 S1 C2 - C1 C3 C3 - C2 C5 C3_$1 C5 - C6_$1 C3 C6 - C5_$1 C1 C21 - C26 C22 S2 C22 - C23 C21 C23 - C22 C24 C24 - C24_$2 C26_$2 C23 C26 - C21 C24_$2 O1 - S1 O2 - S1 Nd1 O3 - S1 Nd2 O21 - S2 O22 - S2 Nd2 O23 - S2_$8 Nd1 O30 - Nd2 O31 - Nd1 O32 - Mo1_$7 Nd1 O33 - Mo2 Nd1 Nd2 O34 - Mo1 Nd2 O35 - Mo2_$5 Nd1 O36 - Mo1 Nd2_$8 Nd1 O37 - Mo1_$6 Nd2 O38 - Mo2_$4 Nd2 O39 - Mo2_$8 Nd1 Nd2_$8 S1 - O3 O1 O2 C1 S2 - O21 O22 O23_$3 C21 Mo1 - O32_$4 O34 O37_$6 O36 Nd1 Mo2 - O35_$5 O38_$7 O39_$3 O33 Nd2 Nd1 - O35 O32 O2 O33 O31 O23 O39 O36 Mo1 Nd2 - O37 O38 O36_$3 O3 O22 O34 O30 O33 O39_$3 Mo2 Operators for generating equivalent atoms: $1 -x, -y+1, -z+2 $2 -x, -y+2, -z+2 $3 x, y+1, z $4 x+1, y, z $5 -x, -y+1, -z+1 $6 -x+1, -y+1, -z+1 $7 x-1, y, z $8 x, y-1, z 16841 Reflections read, of which 152 rejected -9 =< h =< 9, -9 =< k =< 9, -23 =< l =< 23, 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) 1 7 0 26.70 6.09 2 33.85 1 9 0 42.11 4.44 3 26.21 -1 -9 1 5.46 6.77 2 36.03 6 -5 2 7.67 4.46 3 23.03 0 8 3 4.52 4.10 3 24.46 -2 -8 4 3.64 5.92 2 50.74 6 -7 4 15.73 5.81 3 33.00 -3 7 5 -1.67 3.64 3 22.74 -2 -8 6 3.46 8.23 2 47.31 -2 -7 7 -1.49 3.80 3 25.92 6 -6 8 -9.40 3.53 5 18.88 9 2 8 8.33 7.61 2 39.05 2 9 8 31.70 4.27 3 30.67 2 -7 9 -14.04 7.57 2 38.17 5 0 9 1.37 1.17 6 6.85 -4 1 9 1.24 5.58 2 34.67 16 Inconsistent equivalents 4360 Unique reflections, of which 0 suppressed R(int) = 0.0885 R(sigma) = 0.0785 Friedel opposites merged Maximum memory for data reduction = 3283 / 43405 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 = 3980 / 347190 wR2 = 0.1690 before cycle 1 for 4360 data and 277 / 277 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 130. 18. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.010 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.052 for 148 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0245 * P )^2 + 78.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27287 0.00071 0.013 OSF Mean shift/su = 0.002 Maximum = 0.014 for z Nd2 Max. shift = 0.000 A for C23 Max. dU = 0.000 for O31 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3980 / 347190 wR2 = 0.1690 before cycle 2 for 4360 data and 277 / 277 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 130. 18. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.010 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.052 for 148 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0245 * P )^2 + 78.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27287 0.00071 0.000 OSF Mean shift/su = 0.001 Maximum = 0.005 for z Nd2 Max. shift = 0.000 A for C23 Max. dU = 0.000 for C21 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3980 / 347190 wR2 = 0.1690 before cycle 3 for 4360 data and 277 / 277 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 130. 18. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.010 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.052 for 148 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0245 * P )^2 + 78.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27287 0.00071 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for z Nd1 Max. shift = 0.000 A for C21 Max. dU = 0.000 for C5 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3980 / 347190 wR2 = 0.1690 before cycle 4 for 4360 data and 277 / 277 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 130. 18. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.010 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.052 for 148 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0245 * P )^2 + 78.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27287 0.00071 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C5 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 H2 -0.0590 0.3661 0.8750 43 0.950 0.000 C2 C1 C3 H5 -0.3254 0.3747 0.9824 43 0.950 0.000 C5 C6_$1 C3 H6 0.4535 0.5481 0.8975 43 0.950 0.000 C6 C5_$1 C1 H22 -0.3728 0.8564 0.9273 43 0.950 0.000 C22 C23 C21 H23 -0.3671 0.9428 1.0472 43 0.950 0.000 C23 C22 C24 H26 0.1878 0.9411 0.8639 43 0.950 0.000 C26 C21 C24_$2 2008src0992 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.20931 0.43856 0.87634 1.00000 0.02279 0.01426 0.01819 -0.00146 -0.00416 0.00365 0.01842 0.02449 0.00223 0.00200 0.00090 0.00000 0.00641 0.00678 0.00599 0.00495 0.00457 0.00519 0.00265 C2 0.01838 0.41584 0.90499 1.00000 0.02481 0.01831 0.00908 -0.00094 -0.01099 -0.00426 0.01630 0.02165 0.00218 0.00197 0.00082 0.00000 0.00603 0.00706 0.00613 0.00532 0.00448 0.00573 0.00266 H2 -0.05902 0.36609 0.87501 1.00000 0.01956 0.00000 0.00000 C3 -0.06046 0.46534 0.97722 1.00000 0.02204 0.01673 0.01698 0.00456 -0.00455 0.00427 0.01879 0.02480 0.00220 0.00205 0.00090 0.00000 0.00689 0.00704 0.00688 0.00559 0.00526 0.00579 0.00292 C5 -0.24817 0.43160 1.01055 1.00000 0.02333 0.03445 0.03851 -0.00233 -0.00584 0.00757 0.03221 0.03181 0.00253 0.00259 0.00115 0.00000 0.00760 0.00987 0.01048 0.00819 0.00633 0.00724 0.00392 H5 -0.32538 0.37472 0.98239 1.00000 0.03865 0.00000 0.00000 C6 0.32509 0.52342 0.91854 1.00000 0.03302 0.00741 0.02969 -0.00729 -0.00496 -0.00081 0.02327 0.02464 0.00250 0.00195 0.00099 0.00000 0.00804 0.00660 0.00832 0.00585 0.00700 0.00593 0.00326 H6 0.45346 0.54807 0.89754 1.00000 0.02793 0.00000 0.00000 C21 -0.09034 0.89917 0.88205 1.00000 0.02353 0.01880 0.00602 0.00648 -0.00492 -0.00132 0.01617 0.02365 0.00219 0.00201 0.00081 0.00000 0.00668 0.00685 0.00519 0.00473 0.00444 0.00541 0.00258 C22 -0.25828 0.89503 0.93892 1.00000 0.02916 0.02558 0.02730 -0.00514 0.00119 -0.00983 0.02806 0.02729 0.00256 0.00234 0.00103 0.00000 0.00712 0.00807 0.00682 0.00674 0.00556 0.00677 0.00335 H22 -0.37275 0.85642 0.92735 1.00000 0.03367 0.00000 0.00000 C23 -0.25547 0.94599 1.00953 1.00000 0.01115 0.03267 0.02926 -0.01607 0.00022 0.00515 0.02435 0.02498 0.00216 0.00234 0.00101 0.00000 0.00661 0.00874 0.00738 0.00710 0.00585 0.00616 0.00338 H23 -0.36707 0.94278 1.04720 1.00000 0.02922 0.00000 0.00000 C24 -0.08097 1.00483 1.02632 1.00000 0.01579 0.02360 0.01011 0.00117 0.00254 0.00883 0.01739 0.02594 0.00208 0.00212 0.00085 0.00000 0.00697 0.00781 0.00708 0.00553 0.00549 0.00555 0.00288 C26 0.07490 0.94417 0.90067 1.00000 0.01905 0.02173 0.01313 -0.00743 -0.00026 0.00609 0.01814 0.02398 0.00219 0.00208 0.00087 0.00000 0.00620 0.00729 0.00717 0.00570 0.00528 0.00568 0.00286 H26 0.18784 0.94113 0.86388 1.00000 0.02177 0.00000 0.00000 O1 0.45682 0.23367 0.80200 1.00000 0.02073 0.01620 0.01985 0.00123 -0.00692 -0.00061 0.01863 0.01657 0.00151 0.00141 0.00063 0.00000 0.00521 0.00483 0.00580 0.00397 0.00425 0.00377 0.00211 O2 0.17014 0.29127 0.75482 1.00000 0.01193 0.03167 0.01064 -0.00046 -0.00190 0.00078 0.01818 0.01672 0.00142 0.00153 0.00059 0.00000 0.00426 0.00564 0.00433 0.00373 0.00333 0.00370 0.00193 O3 0.40426 0.52793 0.74608 1.00000 0.02513 0.01916 0.01738 0.00383 -0.00734 -0.00539 0.02031 0.01664 0.00156 0.00144 0.00062 0.00000 0.00531 0.00448 0.00456 0.00359 0.00382 0.00369 0.00197 O21 -0.25738 0.72435 0.80031 1.00000 0.01998 0.01513 0.02005 -0.00276 -0.00108 -0.00398 0.01869 0.01630 0.00151 0.00139 0.00062 0.00000 0.00496 0.00509 0.00584 0.00416 0.00429 0.00391 0.00218 O22 0.07254 0.76991 0.75730 1.00000 0.01210 0.03004 0.00607 -0.00453 -0.00339 -0.00165 0.01568 0.01535 0.00139 0.00147 0.00056 0.00000 0.00385 0.00565 0.00411 0.00381 0.00310 0.00366 0.00194 O23 -0.13729 0.02056 0.75092 1.00000 0.02120 0.01915 0.01536 -0.00128 -0.00226 -0.00016 0.01875 0.01666 0.00152 0.00143 0.00061 0.00000 0.00490 0.00459 0.00457 0.00352 0.00360 0.00378 0.00195 O30 0.44423 0.88935 0.74840 1.00000 0.01163 0.02020 0.01631 -0.00357 -0.00305 -0.00306 0.01588 0.01536 0.00139 0.00140 0.00060 0.00000 0.00447 0.00469 0.00485 0.00381 0.00368 0.00383 0.00195 O31 -0.19453 0.37767 0.75199 1.00000 0.01125 0.02080 0.01613 -0.00397 0.00218 -0.00176 0.01660 0.01605 0.00139 0.00142 0.00060 0.00000 0.00421 0.00472 0.00475 0.00368 0.00344 0.00364 0.00192 O32 -0.29240 0.22355 0.62473 1.00000 0.01510 0.02110 0.00960 -0.00015 0.00188 -0.00239 0.01589 0.01607 0.00142 0.00140 0.00057 0.00000 0.00237 0.00278 0.00269 0.00211 0.00204 0.00215 0.00109 O33 0.03233 0.56531 0.62337 1.00000 0.01515 0.02030 0.01068 0.00138 -0.00121 -0.00177 0.01566 0.01600 0.00142 0.00140 0.00058 0.00000 0.00390 0.00386 0.00459 0.00314 0.00335 0.00287 0.00165 O34 0.40125 0.44547 0.59384 1.00000 0.01811 0.01986 0.01217 -0.00368 -0.00029 0.00079 0.01698 0.01623 0.00146 0.00140 0.00059 0.00000 0.00436 0.00410 0.00474 0.00349 0.00392 0.00329 0.00185 O35 0.07516 0.28429 0.51566 1.00000 0.01745 0.02207 0.00467 0.00065 -0.00607 -0.00510 0.01422 0.01481 0.00141 0.00139 0.00054 0.00000 0.00458 0.00478 0.00375 0.00332 0.00335 0.00392 0.00184 O36 0.33990 0.07484 0.62360 1.00000 0.01642 0.02427 0.00191 0.00196 -0.00216 0.00042 0.01429 0.01582 0.00141 0.00142 0.00054 0.00000 0.00383 0.00457 0.00436 0.00344 0.00327 0.00301 0.00172 O37 0.40369 0.79509 0.51538 1.00000 0.02401 0.02162 0.00844 0.00036 0.00033 -0.00532 0.01854 0.01640 0.00153 0.00145 0.00058 0.00000 0.00487 0.00504 0.00398 0.00368 0.00364 0.00421 0.00200 O38 0.66785 0.73642 0.62198 1.00000 0.01510 0.02110 0.00960 -0.00015 0.00188 -0.00239 0.01589 0.01611 0.00143 0.00140 0.00057 0.00000 0.00237 0.00278 0.00269 0.00211 0.00204 0.00215 0.00109 O39 0.01258 -0.06565 0.59824 1.00000 0.01510 0.02110 0.00960 -0.00015 0.00188 -0.00239 0.01589 0.01606 0.00142 0.00141 0.00057 0.00000 0.00237 0.00278 0.00269 0.00211 0.00204 0.00215 0.00109 S1 0.31637 0.36745 0.78845 1.00000 0.01350 0.01768 0.01099 -0.00121 -0.00211 0.00174 0.01411 0.00558 0.00050 0.00049 0.00020 0.00000 0.00166 0.00169 0.00168 0.00128 0.00130 0.00130 0.00068 S2 -0.10341 0.84820 0.79068 1.00000 0.01544 0.01447 0.01005 -0.00090 -0.00039 -0.00130 0.01360 0.00548 0.00050 0.00048 0.00020 0.00000 0.00168 0.00162 0.00165 0.00126 0.00130 0.00127 0.00068 Mo1 0.51517 0.23799 0.58071 1.00000 0.01227 0.01479 0.00897 -0.00112 -0.00207 0.00031 0.01200 0.00187 0.00017 0.00016 0.00007 0.00000 0.00057 0.00058 0.00059 0.00044 0.00045 0.00043 0.00026 Mo2 -0.09456 0.73717 0.58021 1.00000 0.01171 0.01514 0.01021 -0.00136 -0.00236 -0.00022 0.01230 0.00187 0.00017 0.00016 0.00007 0.00000 0.00057 0.00058 0.00060 0.00044 0.00045 0.00044 0.00026 Nd1 0.01840 0.23610 0.64935 1.00000 0.01355 0.01440 0.01021 -0.00148 -0.00274 0.00076 0.01265 0.00118 0.00011 0.00010 0.00004 0.00000 0.00038 0.00037 0.00039 0.00027 0.00028 0.00027 0.00019 Nd2 0.32995 0.74381 0.64687 1.00000 0.01250 0.01490 0.01016 -0.00150 -0.00122 -0.00006 0.01263 0.00118 0.00011 0.00010 0.00004 0.00000 0.00038 0.00038 0.00039 0.00028 0.00028 0.00027 0.00019 Final Structure Factor Calculation for 2008src0992 in P-1 Total number of l.s. parameters = 277 Maximum vector length = 511 Memory required = 3703 / 25039 wR2 = 0.1690 before cycle 5 for 4360 data and 0 / 277 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 130. 18. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.010 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.052 for 148 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0245 * P )^2 + 78.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0728 for 3500 Fo > 4sig(Fo) and 0.1004 for all 4360 data wR2 = 0.1690, GooF = S = 1.067, Restrained GooF = 1.052 for all data Occupancy sum of asymmetric unit = 32.00 for non-hydrogen and 6.00 for hydrogen atoms Principal mean square atomic displacements U 0.0242 0.0181 0.0129 C1 0.0284 0.0170 0.0036 C2 0.0263 0.0204 0.0097 C3 0.0397 0.0375 0.0194 C5 0.0342 0.0303 0.0053 C6 0.0244 0.0215 0.0026 C21 0.0428 0.0240 0.0174 C22 0.0444 0.0208 0.0079 C23 0.0322 0.0127 0.0073 C24 0.0268 0.0200 0.0077 C26 0.0234 0.0177 0.0148 O1 0.0319 0.0121 0.0106 O2 0.0299 0.0176 0.0135 O3 0.0253 0.0180 0.0128 O21 0.0305 0.0122 0.0044 O22 0.0219 0.0191 0.0152 O23 0.0222 0.0154 0.0100 O30 0.0239 0.0169 0.0090 O31 0.0220 0.0178 0.0078 O32 0.0212 0.0158 0.0100 O33 0.0206 0.0197 0.0106 O34 0.0257 0.0145 0.0025 O35 0.0249 0.0165 0.0015 O36 0.0289 0.0187 0.0080 O37 0.0220 0.0178 0.0078 O38 0.0220 0.0178 0.0078 O39 0.0183 0.0130 0.0109 S1 0.0173 0.0139 0.0096 S2 0.0148 0.0123 0.0089 Mo1 0.0152 0.0117 0.0100 Mo2 0.0149 0.0131 0.0099 Nd1 0.0150 0.0131 0.0098 Nd2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.023 0.045 0.072 0.098 0.128 0.157 0.193 0.236 0.305 1.000 Number in group 438. 452. 430. 424. 443. 435. 438. 426. 438. 436. GooF 1.245 1.155 1.077 1.075 1.012 0.943 1.054 1.007 0.992 1.077 K 7.652 2.007 1.174 1.055 1.037 1.009 0.992 0.989 1.007 1.007 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.66 inf Number in group 448. 428. 439. 432. 433. 436. 439. 433. 437. 435. GooF 1.244 1.185 1.166 1.122 1.068 1.008 0.976 0.948 0.897 1.002 K 1.018 1.075 1.030 1.025 1.024 1.009 1.015 1.011 0.999 1.005 R1 0.191 0.171 0.141 0.124 0.116 0.081 0.080 0.062 0.051 0.044 Recommended weighting scheme: WGHT 0.0267 77.0818 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) 5 -3 1 6672.58 12836.04 5.55 0.327 1.24 -1 -2 1 5980.42 2840.73 4.88 0.154 3.14 5 -7 11 804.93 4147.62 4.57 0.186 0.77 -3 -1 10 741.73 5.02 4.16 0.006 1.27 6 4 17 6482.27 11643.51 4.14 0.311 0.81 2 -1 18 10284.99 16397.56 4.08 0.369 0.98 6 1 15 2124.43 4877.11 4.07 0.201 0.93 6 3 18 1297.71 2.32 3.96 0.004 0.81 -1 -4 2 718.47 46.21 3.82 0.020 1.71 7 -5 12 912.03 3873.60 3.81 0.179 0.77 -1 -2 15 1644.85 364.06 3.70 0.055 1.06 -6 4 0 1345.63 3561.55 3.62 0.172 1.00 -5 -3 6 11927.86 17227.61 3.51 0.378 1.06 3 -8 4 -84.30 1491.09 3.49 0.111 0.85 5 3 15 2857.64 5297.79 3.44 0.210 0.96 3 -1 10 578.68 47.85 3.40 0.020 1.53 4 4 21 1291.19 0.49 3.35 0.002 0.78 8 1 9 648.67 8.71 3.30 0.009 0.88 -5 -2 9 613.24 57.27 3.30 0.022 1.01 -7 0 3 498.72 3.33 3.25 0.005 0.97 7 -1 4 1109.98 11.50 3.24 0.010 1.03 -1 -2 2 1641.16 665.47 3.22 0.074 2.93 -4 -1 10 9621.65 13571.95 3.18 0.336 1.13 1 -2 2 17338.96 22208.89 3.16 0.430 3.11 -2 -3 16 7308.03 11370.50 3.16 0.307 0.91 -5 0 13 1124.99 186.65 3.14 0.039 0.90 7 -3 15 3217.60 88.39 3.11 0.027 0.80 -4 -5 12 4668.59 7388.14 3.08 0.248 0.83 5 -1 18 3550.35 5937.70 3.08 0.222 0.89 4 3 15 5452.61 8160.15 3.05 0.260 1.02 -5 2 16 -696.21 1850.34 3.04 0.124 0.79 2 9 2 12629.61 9021.87 3.03 0.274 0.80 3 -3 3 5976.81 8678.21 3.02 0.269 1.69 -3 5 13 1542.59 482.44 3.01 0.063 0.90 -4 1 18 892.04 52.60 3.01 0.021 0.80 2 -2 11 1085.16 363.09 3.00 0.055 1.43 -5 -2 14 3838.28 1328.57 2.99 0.105 0.83 0 -6 3 12038.17 16637.18 2.97 0.372 1.19 -3 -2 16 2539.16 6025.65 2.91 0.224 0.89 -4 -1 14 667.98 3018.80 2.87 0.158 0.93 -6 -1 13 1790.68 106.91 2.86 0.030 0.81 5 0 21 1180.10 165.54 2.86 0.037 0.80 5 -7 10 1378.38 3477.69 2.85 0.170 0.79 7 6 1 670.03 1968.56 2.83 0.128 0.79 6 4 16 4114.09 6586.61 2.83 0.234 0.83 -6 4 12 2366.22 948.93 2.83 0.089 0.78 -6 -1 12 1749.14 22.77 2.81 0.014 0.84 6 -4 14 2343.44 99.74 2.79 0.029 0.84 -9 0 2 1098.51 10.84 2.79 0.009 0.77 9 -1 2 10423.42 7035.72 2.76 0.242 0.80 Bond lengths and angles C1 - Distance Angles C2 1.3898 (0.0222) C6 1.4229 (0.0215) 120.42 (1.46) S1 1.7406 (0.0162) 122.23 (1.17) 117.35 (1.24) C1 - C2 C6 C2 - Distance Angles C1 1.3898 (0.0223) C3 1.3919 (0.0217) 120.60 (1.34) H2 0.9500 119.70 119.70 C2 - C1 C3 C3 - Distance Angles C2 1.3919 (0.0217) C5 1.3961 (0.0243) 122.50 (1.55) C3_$1 1.4414 (0.0311) 118.83 (1.81) 118.26 (1.94) C3 - C2 C5 C5 - Distance Angles C6_$1 1.3575 (0.0255) C3 1.3961 (0.0242) 122.81 (1.78) H5 0.9500 118.60 118.60 C5 - C6_$1 C3 C6 - Distance Angles C5_$1 1.3575 (0.0255) C1 1.4229 (0.0215) 118.58 (1.66) H6 0.9500 120.71 120.71 C6 - C5_$1 C1 C21 - Distance Angles C26 1.3624 (0.0216) C22 1.4315 (0.0230) 119.06 (1.43) S2 1.7446 (0.0149) 121.88 (1.22) 119.06 (1.20) C21 - C26 C22 C22 - Distance Angles C23 1.3628 (0.0239) C21 1.4315 (0.0230) 120.60 (1.56) H22 0.9500 119.70 119.70 C22 - C23 C21 C23 - Distance Angles C22 1.3628 (0.0239) C24 1.4418 (0.0220) 119.16 (1.50) H23 0.9500 120.42 120.42 C23 - C22 C24 C24 - Distance Angles C24_$2 1.3640 (0.0290) C26_$2 1.4100 (0.0210) 119.96 (1.87) C23 1.4418 (0.0219) 119.82 (1.87) 119.94 (1.38) C24 - C24_$2 C26_$2 C26 - Distance Angles C21 1.3624 (0.0215) C24_$2 1.4100 (0.0211) 121.05 (1.44) H26 0.9500 119.47 119.47 C26 - C21 C24_$2 O1 - Distance Angles S1 1.4585 (0.0111) O1 - O2 - Distance Angles S1 1.4633 (0.0107) Nd1 2.4496 (0.0103) 153.70 (0.67) O2 - S1 O3 - Distance Angles S1 1.4524 (0.0109) Nd2 2.4621 (0.0108) 135.86 (0.64) O3 - S1 O21 - Distance Angles S2 1.4320 (0.0106) O21 - O22 - Distance Angles S2 1.4349 (0.0107) Nd2 2.4688 (0.0101) 149.43 (0.66) O22 - S2 O23 - Distance Angles S2_$8 1.4656 (0.0112) Nd1 2.4564 (0.0109) 140.79 (0.66) O23 - S2_$8 O30 - Distance Angles Nd2 2.4783 (0.0099) O30 - O31 - Distance Angles Nd1 2.4558 (0.0102) O31 - O32 - Distance Angles Mo1_$7 1.7430 (0.0104) Nd1 2.3938 (0.0103) 163.23 (0.57) O32 - Mo1_$7 O33 - Distance Angles Mo2 1.7911 (0.0105) Nd1 2.4506 (0.0104) 137.82 (0.52) Nd2 2.6698 (0.0100) 103.06 (0.43) 118.67 (0.40) O33 - Mo2 Nd1 O34 - Distance Angles Mo1 1.7442 (0.0104) Nd2 2.4763 (0.0102) 156.83 (0.57) O34 - Mo1 O35 - Distance Angles Mo2_$5 1.7336 (0.0096) Nd1 2.3791 (0.0097) 165.18 (0.57) O35 - Mo2_$5 O36 - Distance Angles Mo1 1.7898 (0.0103) Nd2_$8 2.4583 (0.0105) 135.51 (0.53) Nd1 2.5845 (0.0102) 108.39 (0.46) 115.53 (0.39) O36 - Mo1 Nd2_$8 O37 - Distance Angles Mo1_$6 1.7568 (0.0104) Nd2 2.3424 (0.0103) 161.60 (0.63) O37 - Mo1_$6 O38 - Distance Angles Mo2_$4 1.7422 (0.0102) Nd2 2.4086 (0.0102) 165.40 (0.58) O38 - Mo2_$4 O39 - Distance Angles Mo2_$8 1.7434 (0.0102) Nd1 2.4799 (0.0103) 154.66 (0.56) Nd2_$8 2.9427 (0.0106) 94.46 (0.42) 103.43 (0.34) O39 - Mo2_$8 Nd1 S1 - Distance Angles O3 1.4524 (0.0110) O1 1.4585 (0.0111) 111.03 (0.66) O2 1.4633 (0.0108) 113.15 (0.65) 112.50 (0.65) C1 1.7406 (0.0162) 105.60 (0.71) 106.47 (0.70) 107.56 (0.70) S1 - O3 O1 O2 S2 - Distance Angles O21 1.4320 (0.0108) O22 1.4349 (0.0108) 112.98 (0.64) O23_$3 1.4656 (0.0113) 113.07 (0.66) 111.63 (0.66) C21 1.7446 (0.0149) 104.73 (0.70) 107.74 (0.68) 106.04 (0.68) S2 - O21 O22 O23_$3 Mo1 - Distance Angles O32_$4 1.7430 (0.0105) O34 1.7442 (0.0105) 111.02 (0.49) O37_$6 1.7568 (0.0104) 107.83 (0.50) 111.73 (0.51) O36 1.7898 (0.0104) 110.83 (0.46) 103.99 (0.49) 111.48 (0.47) Nd1 3.5779 (0.0017) 133.51 (0.34) 61.79 (0.35) 117.47 (0.36) 43.27 (0.33) Mo1 - O32_$4 O34 O37_$6 O36 Mo2 - Distance Angles O35_$5 1.7336 (0.0096) O38_$7 1.7422 (0.0102) 108.17 (0.48) O39_$3 1.7434 (0.0103) 111.87 (0.48) 110.39 (0.48) O33 1.7911 (0.0105) 112.52 (0.49) 111.89 (0.48) 101.97 (0.48) Nd2 3.5350 (0.0016) 116.52 (0.34) 135.17 (0.34) 56.09 (0.35) 47.37 (0.32) Mo2 - O35_$5 O38_$7 O39_$3 O33 Nd1 - Distance Angles O35 2.3791 (0.0097) O32 2.3938 (0.0103) 78.16 (0.34) O2 2.4496 (0.0103) 139.39 (0.35) 138.40 (0.35) O33 2.4506 (0.0104) 74.40 (0.35) 91.76 (0.35) 85.45 (0.36) O31 2.4558 (0.0102) 133.21 (0.37) 72.19 (0.34) 67.63 (0.35) 71.27 (0.35) O23 2.4564 (0.0109) 140.47 (0.34) 77.86 (0.36) 76.44 (0.36) 137.11 (0.35) 65.92 (0.36) O39 2.4799 (0.0103) 73.18 (0.34) 77.60 (0.35) 122.87 (0.36) 147.29 (0.34) 131.48 (0.34) 71.28 (0.34) O36 2.5845 (0.0103) 83.58 (0.33) 142.27 (0.33) 73.31 (0.33) 114.77 (0.33) 139.92 (0.33) 96.90 (0.34) 65.54 (0.33) Mo1 3.5779 (0.0017) 71.91 (0.25) 149.34 (0.25) 72.03 (0.25) 86.57 (0.24) 134.94 (0.24) 122.55 (0.26) 87.43 (0.24) Nd1 - O35 O32 O2 O33 O31 O23 O39 Nd2 - Distance Angles O37 2.3424 (0.0104) O38 2.4086 (0.0103) 78.11 (0.37) O36_$3 2.4583 (0.0105) 74.83 (0.35) 89.80 (0.34) O3 2.4621 (0.0108) 139.34 (0.39) 76.03 (0.36) 135.26 (0.33) O22 2.4688 (0.0102) 142.44 (0.37) 137.27 (0.33) 90.47 (0.35) 74.05 (0.37) O34 2.4763 (0.0102) 72.95 (0.37) 77.28 (0.34) 147.10 (0.34) 71.10 (0.36) 119.54 (0.36) O30 2.4783 (0.0100) 131.51 (0.36) 70.69 (0.34) 69.02 (0.33) 66.24 (0.35) 69.64 (0.32) 131.28 (0.35) O33 2.6698 (0.0101) 85.21 (0.34) 141.96 (0.33) 118.57 (0.32) 96.36 (0.33) 71.63 (0.32) 65.15 (0.33) 140.59 (0.33) O39_$3 2.9427 (0.0106) 71.79 (0.34) 141.81 (0.32) 60.24 (0.31) 141.78 (0.33) 70.92 (0.31) 114.32 (0.32) 113.62 (0.32) Mo2 3.5350 (0.0016) 72.35 (0.27) 149.63 (0.25) 89.23 (0.23) 123.62 (0.25) 73.10 (0.23) 87.35 (0.25) 136.13 (0.24) Nd2 - O37 O38 O36_$3 O3 O22 O34 O30 FMAP and GRID set by program FMAP 2 1 35 GRID -3.125 -2 -1 3.125 2 1 R1 = 0.0982 for 4360 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 4.77 at 0.6628 0.3615 0.3446 [ 0.79 A from ND2 ] Deepest hole -2.25 at 0.1589 0.3217 0.4389 [ 0.79 A from MO2 ] Mean = 0.00, Rms deviation from mean = 0.46 e/A^3, Highest memory used = 3764 / 33391 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3372 0.6385 0.6554 1.00000 0.05 4.77 0.79 ND2 1.87 O34 1.93 O3 2.47 O38 Q2 1 0.0276 0.3500 0.6381 1.00000 0.05 4.16 0.85 ND1 1.60 O33 2.26 O35 2.37 O31 Q3 1 -0.0908 0.8435 0.5710 1.00000 0.05 2.78 0.79 MO2 1.21 O39 1.87 O35 1.96 O38 Q4 1 0.2830 0.6592 0.7134 1.00000 0.05 2.36 1.30 ND2 1.48 O3 1.79 O22 2.27 O30 Q5 1 -0.2472 1.0340 0.9122 1.00000 0.05 2.29 1.10 C22 1.55 C21 1.59 H22 1.83 C23 Q6 1 0.0673 0.3424 0.5773 1.00000 0.05 2.10 1.21 O35 1.46 ND1 1.89 O33 2.63 O34 Q7 1 -0.3768 0.1493 0.6534 1.00000 0.05 2.10 0.89 O32 1.75 MO1 2.31 O36 2.66 O30 Q8 1 0.0253 0.1313 0.6333 1.00000 0.05 2.05 0.84 ND1 1.64 O39 2.29 O36 2.31 O35 Q9 1 -0.2261 1.0796 0.9722 1.00000 0.05 2.03 1.16 C23 1.57 C22 1.65 C24 1.79 H23 Q10 1 0.3423 0.7417 0.6072 1.00000 0.05 1.98 0.71 ND2 1.66 O37 2.25 O34 2.43 O38 Shortest distances between peaks (including symmetry equivalents) 1 4 1.07 2 6 1.09 1 10 1.12 5 9 1.20 2 8 1.63 6 8 1.80 4 10 1.94 3 8 2.70 7 8 2.88 Time profile in seconds ----------------------- 0.00: 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. 0.78: 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 0.72: Structure factors and derivatives 2.11: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 0.17: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0992 finished at 15:43:31 Total CPU time: 4.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++