+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0072p21 started at 17:23:56 on 12-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0072p21 in P2(1) CELL 0.71073 11.6414 6.2915 22.2485 90.000 96.148 90.000 ZERR 4.00 0.0017 0.0008 0.0032 0.000 0.007 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O S UNIT 56 104 8 12 4 V = 1620.15 F(000) = 656.0 Mu = 0.21 mm-1 Cell Wt = 1209.71 Rho = 1.240 MERG 2 OMIT -3.00 55.00 EXTI 0.02691 SHEL 7 0.77 EADP C22A C22B EADP C21A C21B HTAB N25 O1A HTAB N34 O1A HTAB N45 O31C EQIV_$1 x-1, y, z HTAB N4 O31A_$1 EQIV_$2 x-1, y+1, z HTAB N4 O31B_$2 EQIV_$3 -x, y-1/2, -z HTAB N25 O1C_$3 HTAB N25 S1_$3 EQIV_$4 x, y-1, z HTAB N25 O1C_$4 HTAB N34 O1B_$4 HTAB N45 O31A_$4 EQIV_$5 -x+1, y-1/2, -z+1 HTAB N45 O31C_$5 DFIX 1.51 0.02 C22A C21A C22B C21B FMAP 2 PLAN 5 SIZE 0.02 0.11 0.23 ACTA BOND $H WGHT 0.07940 L.S. 4 TEMP -153.00 FVAR 0.66490 0.49424 MOLE 1 C1 1 -0.046025 0.644141 0.186761 11.00000 0.04273 0.02535 = 0.01391 -0.00573 -0.00353 0.00779 C2 1 -0.114544 0.496741 0.211208 11.00000 0.04706 0.01906 = 0.02454 -0.00763 0.00304 -0.01620 AFIX 43 H2 2 -0.113852 0.353841 0.197456 11.00000 -1.20000 AFIX 0 C3 1 -0.183384 0.549712 0.254574 11.00000 0.02728 0.02582 = 0.04306 0.00480 0.00458 -0.00390 AFIX 43 H3 2 -0.231288 0.444548 0.269717 11.00000 -1.20000 AFIX 0 C4 1 -0.184529 0.757630 0.277214 11.00000 0.03185 0.03995 = 0.02948 -0.00179 -0.00128 -0.00872 C5 1 -0.111819 0.908216 0.254876 11.00000 0.05753 0.02352 = 0.03172 -0.00632 -0.00418 -0.00618 AFIX 43 H5 2 -0.108115 1.048080 0.271059 11.00000 -1.20000 AFIX 0 C6 1 -0.043502 0.853126 0.208129 11.00000 0.02824 0.03636 = 0.02231 0.00014 0.00070 -0.00362 AFIX 43 H6 2 0.003342 0.956903 0.191568 11.00000 -1.20000 AFIX 0 N4 3 -0.254388 0.811720 0.319794 11.00000 0.05405 0.02522 = 0.04275 -0.00313 0.02413 0.00065 AFIX 93 H4A 2 -0.254200 0.942782 0.333619 11.00000 -1.20000 H4B 2 -0.299901 0.715752 0.333595 11.00000 -1.20000 AFIX 0 O1A 4 0.034625 0.351504 0.122512 11.00000 0.04946 0.02112 = 0.03447 -0.00442 0.00811 0.00056 O1B 4 0.155797 0.659415 0.146639 11.00000 0.02937 0.03746 = 0.04072 -0.01514 0.00312 -0.00984 O1C 4 -0.012735 0.681187 0.073699 11.00000 0.04330 0.03804 = 0.03170 0.00315 0.01409 0.00014 S1 5 0.039919 0.580644 0.129372 11.00000 0.03677 0.02772 = 0.02879 -0.00144 0.00870 0.00147 MOLE 2 PART 1 C21A 1 -0.386999 0.041754 0.170607 21.00000 0.03117 0.04640 = 0.01780 -0.02000 0.00214 -0.02024 AFIX 137 H21A 2 -0.468450 0.031767 0.177735 21.00000 -1.50000 H21B 2 -0.345138 0.128046 0.202458 21.00000 -1.50000 H21C 2 -0.353272 -0.101025 0.171019 21.00000 -1.50000 AFIX 0 C22A 1 -0.377953 0.144307 0.109840 21.00000 0.03384 0.06474 = 0.03455 0.01246 0.00544 0.01253 C28A 1 -0.475719 0.030652 0.072226 21.00000 0.07608 0.07418 = 0.02026 -0.00286 0.02273 -0.01158 AFIX 137 H28A 2 -0.549830 0.076369 0.085001 21.00000 -1.50000 H28B 2 -0.467091 -0.123190 0.077951 21.00000 -1.50000 H28C 2 -0.473369 0.065382 0.029436 21.00000 -1.50000 AFIX 0 C29A 1 -0.405676 0.374934 0.112616 21.00000 0.01953 0.05076 = 0.03658 -0.00841 -0.01480 -0.00112 AFIX 137 H29A 2 -0.487001 0.392505 0.119263 21.00000 -1.50000 H29B 2 -0.391773 0.443023 0.074444 21.00000 -1.50000 H29C 2 -0.356497 0.441047 0.145968 21.00000 -1.50000 AFIX 0 PART 2 C21B 1 -0.371673 0.102430 0.174580 -21.00000 0.03117 0.04640 = 0.01780 -0.02000 0.00214 -0.02024 AFIX 137 H21D 2 -0.347780 -0.018646 0.200686 -21.00000 -1.50000 H21E 2 -0.448288 0.150838 0.183100 -21.00000 -1.50000 H21F 2 -0.315918 0.218475 0.182398 -21.00000 -1.50000 AFIX 0 C22B 1 -0.376350 0.035554 0.109138 -21.00000 0.03384 0.06474 = 0.03455 0.01246 0.00544 0.01253 C28B 1 -0.467981 0.162533 0.070586 -21.00000 0.03371 0.04351 = 0.03649 0.02719 0.00260 0.00104 AFIX 137 H28D 2 -0.442941 0.310789 0.068403 -21.00000 -1.50000 H28E 2 -0.540968 0.156437 0.088757 -21.00000 -1.50000 H28F 2 -0.479045 0.102144 0.029773 -21.00000 -1.50000 AFIX 0 C29B 1 -0.405211 -0.203952 0.101273 -21.00000 0.06321 0.02906 = 0.07115 0.01391 0.03937 -0.00144 AFIX 137 H29D 2 -0.350275 -0.287509 0.128124 -21.00000 -1.50000 H29E 2 -0.399798 -0.245747 0.059237 -21.00000 -1.50000 H29F 2 -0.483812 -0.230060 0.111485 -21.00000 -1.50000 AFIX 0 PART 0 C23 1 -0.254785 0.087864 0.093588 11.00000 0.02817 0.04238 = 0.03174 -0.00033 0.00136 0.00036 AFIX 23 H23A 2 -0.199521 0.174068 0.120332 11.00000 -1.20000 H23B 2 -0.240512 -0.062550 0.105145 11.00000 -1.20000 AFIX 0 C24 1 -0.221152 0.113634 0.028696 11.00000 0.03379 0.03699 = 0.03595 0.00797 0.00330 0.00031 C26 1 -0.265567 -0.060305 -0.015167 11.00000 0.05102 0.03992 = 0.04143 -0.00790 0.01177 -0.01056 AFIX 137 H26A 2 -0.349986 -0.052118 -0.022362 11.00000 -1.50000 H26B 2 -0.242967 -0.199407 0.002058 11.00000 -1.50000 H26C 2 -0.232390 -0.041564 -0.053486 11.00000 -1.50000 AFIX 0 C27 1 -0.243950 0.330486 0.002737 11.00000 0.03930 0.02795 = 0.06748 0.00859 0.00751 0.00612 AFIX 137 H27A 2 -0.205777 0.345290 -0.034217 11.00000 -1.50000 H27B 2 -0.213652 0.437694 0.032232 11.00000 -1.50000 H27C 2 -0.327375 0.350704 -0.006829 11.00000 -1.50000 AFIX 0 N25 3 -0.090041 0.090820 0.036017 11.00000 0.03911 0.02352 = 0.02942 -0.00075 0.00319 -0.00306 AFIX 137 H25A 2 -0.062661 0.111906 -0.000324 11.00000 -1.50000 H25B 2 -0.070535 -0.041992 0.049737 11.00000 -1.50000 H25C 2 -0.058654 0.188928 0.063007 11.00000 -1.50000 AFIX 0 MOLE 3 C31 1 0.484245 0.246093 0.320888 11.00000 0.03382 0.03092 = 0.03271 0.00293 0.01721 0.00710 C32 1 0.447367 0.408492 0.278743 11.00000 0.04666 0.02762 = 0.02029 -0.00296 0.01548 -0.00433 AFIX 43 H32 2 0.475009 0.550063 0.283999 11.00000 -1.20000 AFIX 0 C33 1 0.370930 0.353680 0.230536 11.00000 0.05050 0.02733 = 0.03252 0.00145 0.01506 0.01276 AFIX 43 H33 2 0.344702 0.460835 0.202255 11.00000 -1.20000 AFIX 0 C34 1 0.330149 0.150266 0.221051 11.00000 0.04119 0.03723 = 0.01979 0.00241 0.00348 0.00378 C35 1 0.367438 -0.003499 0.262961 11.00000 0.03924 0.03011 = 0.03979 -0.01735 0.00824 -0.00316 AFIX 43 H35 2 0.339071 -0.144607 0.257736 11.00000 -1.20000 AFIX 0 C36 1 0.443827 0.043676 0.311405 11.00000 0.04830 0.01631 = 0.04186 0.00604 0.01987 0.00474 AFIX 43 H36 2 0.469625 -0.065419 0.339145 11.00000 -1.20000 AFIX 0 N34 3 0.255234 0.103474 0.170943 11.00000 0.05563 0.03973 = 0.03527 -0.00099 -0.00157 0.00451 AFIX 93 H34A 2 0.233117 0.203983 0.144719 11.00000 -1.20000 H34B 2 0.229294 -0.027053 0.165024 11.00000 -1.20000 AFIX 0 O31A 4 0.579603 0.544192 0.389706 11.00000 0.05606 0.02639 = 0.03062 -0.00386 -0.00111 -0.00011 O31B 4 0.696442 0.236883 0.370370 11.00000 0.04311 0.04128 = 0.04629 -0.00957 0.00899 0.00631 O31C 4 0.546231 0.207731 0.435226 11.00000 0.04772 0.03818 = 0.02467 0.00623 0.01048 0.00830 S31 5 0.584568 0.314039 0.382541 11.00000 0.04410 0.02646 = 0.03426 -0.00082 0.00995 0.00306 MOLE 4 C41 1 0.827307 0.129192 0.666589 11.00000 0.06161 0.03692 = 0.06133 -0.00680 -0.01488 -0.00234 AFIX 137 H41A 2 0.891515 0.151699 0.698185 11.00000 -1.50000 H41B 2 0.759203 0.080687 0.685061 11.00000 -1.50000 H41C 2 0.809379 0.262926 0.645015 11.00000 -1.50000 AFIX 0 C42 1 0.861593 -0.040076 0.621817 11.00000 0.04072 0.03548 = 0.03534 0.00140 0.01126 -0.00387 C43 1 0.752832 -0.061210 0.574555 11.00000 0.03927 0.02646 = 0.04595 0.00473 0.01084 0.01150 AFIX 23 H43A 2 0.687895 -0.101112 0.597589 11.00000 -1.20000 H43B 2 0.735639 0.083465 0.558550 11.00000 -1.20000 AFIX 0 C44 1 0.746299 -0.205902 0.520968 11.00000 0.04163 0.03703 = 0.03827 -0.00155 -0.00538 0.02228 C46 1 0.968666 0.032691 0.594221 11.00000 0.04366 0.09804 = 0.04638 -0.02077 0.00639 -0.02749 AFIX 137 H46A 2 0.946542 0.134745 0.561757 11.00000 -1.50000 H46B 2 1.006310 -0.090271 0.577686 11.00000 -1.50000 H46C 2 1.022271 0.100580 0.625402 11.00000 -1.50000 AFIX 0 C47 1 0.885112 -0.246176 0.659091 11.00000 0.05684 0.04936 = 0.06384 -0.00385 -0.01867 0.01350 AFIX 137 H47A 2 0.811493 -0.311766 0.666340 11.00000 -1.50000 H47B 2 0.929273 -0.211882 0.697875 11.00000 -1.50000 H47C 2 0.929461 -0.345383 0.636658 11.00000 -1.50000 AFIX 0 C48 1 0.827945 -0.149905 0.473257 11.00000 0.04485 0.14506 = 0.03100 -0.01804 0.01413 0.02289 AFIX 137 H48A 2 0.825647 0.003678 0.465878 11.00000 -1.50000 H48B 2 0.803214 -0.225270 0.435532 11.00000 -1.50000 H48C 2 0.906944 -0.192479 0.487991 11.00000 -1.50000 AFIX 0 C49 1 0.757728 -0.443827 0.536431 11.00000 0.12478 0.02476 = 0.07993 -0.01433 -0.03480 0.02904 AFIX 137 H49A 2 0.838587 -0.476948 0.550073 11.00000 -1.50000 H49B 2 0.732352 -0.528258 0.500428 11.00000 -1.50000 H49C 2 0.709525 -0.477827 0.568643 11.00000 -1.50000 AFIX 0 N45 3 0.626396 -0.181896 0.489219 11.00000 0.04461 0.01809 = 0.03566 -0.00168 0.01412 -0.00682 AFIX 137 H45A 2 0.573756 -0.214303 0.515235 11.00000 -1.50000 H45B 2 0.617225 -0.271409 0.456933 11.00000 -1.50000 H45C 2 0.615611 -0.045440 0.476266 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0072p21 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - C2 C6 S1 C2 - C3 C1 C3 - C2 C4 C4 - N4 C5 C3 C5 - C4 C6 C6 - C1 C5 N4 - C4 O1A - S1 O1B - S1 O1C - S1 S1 - O1B O1A O1C C1 C21A_a - C22A_a C22A_a - C29A_a C21A_a C28A_a C23 C28A_a - C22A_a C29A_a - C22A_a C21B_b - C22B_b C22B_b - C21B_b C28B_b C23 C29B_b C28B_b - C22B_b C29B_b - C22B_b C23 - C22B_b C24 C22A_a C24 - C27 C26 N25 C23 C26 - C24 C27 - C24 N25 - C24 C31 - C36 C32 S31 C32 - C33 C31 C33 - C32 C34 C34 - N34 C33 C35 C35 - C36 C34 C36 - C35 C31 N34 - C34 O31A - S31 O31B - S31 O31C - S31 S31 - O31B O31A O31C C31 C41 - C42 C42 - C46 C41 C47 C43 C43 - C44 C42 C44 - C43 N45 C49 C48 C46 - C42 C47 - C42 C48 - C44 C49 - C44 N45 - C44 Operators for generating equivalent atoms: $1 x-1, y, z $2 x-1, y+1, z $3 -x, y-1/2, -z $4 x, y-1, z $5 -x+1, y-1/2, -z+1 Floating origin restraints generated h k l Fo^2 Sigma Why rejected 0 1 0 40.29 8.24 observed but should be systematically absent 14684 Reflections read, of which 26 rejected -13 =< h =< 15, -8 =< k =< 8, -28 =< l =< 23, Max. 2-theta = 54.96 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 10 3 4 -46.27 24.49 2 142.40 9 4 4 106.39 22.08 3 145.61 2 7 9 0.03 0.18 3 6.16 0 -3 14 199.77 24.36 3 233.65 8 4 14 157.84 40.38 2 385.70 0 1 15 169.36 36.33 2 188.34 6 Inconsistent equivalents 6849 Unique reflections, of which 0 suppressed R(int) = 0.2133 R(sigma) = 0.3756 Friedel opposites not merged Maximum memory for data reduction = 5232 / 69359 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 = 6528 / 516668 wR2 = 0.2561 before cycle 1 for 6849 data and 402 / 402 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.966; Restrained GooF = 0.965 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0794 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66496 0.00275 0.021 OSF 2 0.49412 0.01653 -0.007 FVAR 2 3 0.02696 0.00335 0.014 EXTI Mean shift/esd = 0.010 Maximum = -0.273 for tors H21D_b Max. shift = 0.032 A for H21F_b Max. dU = 0.000 for C21A_a Least-squares cycle 2 Maximum vector length = 511 Memory required = 6528 / 516668 wR2 = 0.2562 before cycle 2 for 6849 data and 402 / 402 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.966; Restrained GooF = 0.965 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0794 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66499 0.00276 0.012 OSF 2 0.49402 0.01656 -0.007 FVAR 2 3 0.02699 0.00335 0.009 EXTI Mean shift/esd = 0.010 Maximum = -0.253 for tors H21D_b Max. shift = 0.030 A for H21F_b Max. dU = 0.000 for C21A_a Least-squares cycle 3 Maximum vector length = 511 Memory required = 6528 / 516668 wR2 = 0.2562 before cycle 3 for 6849 data and 402 / 402 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.966; Restrained GooF = 0.965 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0794 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66500 0.00276 0.004 OSF 2 0.49398 0.01659 -0.002 FVAR 2 3 0.02700 0.00336 0.003 EXTI Mean shift/esd = 0.006 Maximum = -0.134 for tors H21D_b Max. shift = 0.016 A for H21F_b Max. dU = 0.000 for C21A_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 6528 / 516668 wR2 = 0.2561 before cycle 4 for 6849 data and 402 / 402 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.966; Restrained GooF = 0.965 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0794 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66501 0.00276 0.003 OSF 2 0.49398 0.01662 0.000 FVAR 2 3 0.02700 0.00336 0.001 EXTI Mean shift/esd = 0.004 Maximum = -0.067 for tors H21D_b Max. shift = 0.008 A for H21F_b Max. dU = 0.000 for C21A_a Largest correlation matrix elements -0.957 x C21B_b / x C21A_a -0.855 U12 C22A_a / x C22A_a -0.779 y C21B_b / y C21A_a -0.911 x C21B_b / U11 C21A_a 0.831 z C22B_b / z C21B_b -0.776 U23 C22A_a / z C22A_a 0.909 U11 C21A_a / x C21A_a -0.827 z C22B_b / z C22A_a -0.775 z C21B_b / z C22A_a -0.906 x C22B_b / x C22A_a 0.820 U23 C21A_a / z C21A_a 0.775 z C22A_a / z C21A_a -0.891 z C21B_b / z C21A_a 0.806 U12 C21A_a / x C21A_a -0.766 z C22B_b / z C21A_a 0.859 x C22B_b / U12 C22A_a -0.802 z C21B_b / U23 C21A_a 0.736 U12 C21A_a / U11 C21A_a 0.857 U22 C21A_a / y C21A_a -0.800 x C21B_b / U12 C21A_a -0.703 z C22B_b / U23 C21A_a -0.855 y C21B_b / U22 C21A_a 0.787 z C22B_b / U23 C22A_a 0.691 z C21B_b / U23 C22A_a Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.1138 0.3538 0.1975 43 0.950 0.000 C2 C3 C1 H3 -0.2313 0.4445 0.2697 43 0.950 0.000 C3 C2 C4 H5 -0.1081 1.0481 0.2711 43 0.950 0.000 C5 C4 C6 H6 0.0033 0.9569 0.1916 43 0.950 0.000 C6 C1 C5 H4A -0.2541 0.9429 0.3336 93 0.880 0.000 N4 C4 C5 H4B -0.2999 0.7159 0.3336 93 0.880 0.000 N4 C4 C5 H21A -0.4686 0.0339 0.1780 137 0.980 0.000 C21A_a C22A_a H21A_a H21B -0.3451 0.1299 0.2026 137 0.980 0.001 C21A_a C22A_a H21A_a H21C -0.3536 -0.0997 0.1715 137 0.980 0.001 C21A_a C22A_a H21A_a H28A -0.5498 0.0767 0.0850 137 0.980 0.000 C28A_a C22A_a H28A_a H28B -0.4671 -0.1231 0.0781 137 0.980 0.000 C28A_a C22A_a H28A_a H28C -0.4731 0.0651 0.0295 137 0.980 0.000 C28A_a C22A_a H28A_a H29A -0.4871 0.3923 0.1192 137 0.980 0.000 C29A_a C22A_a H29A_a H29B -0.3917 0.4429 0.0745 137 0.980 0.000 C29A_a C22A_a H29A_a H29C -0.3567 0.4411 0.1460 137 0.980 0.000 C29A_a C22A_a H29A_a H21D -0.3538 -0.0235 0.2003 137 0.980 0.001 C21B_b C22B_b H21D_b H21E -0.4460 0.1606 0.1824 137 0.980 0.000 C21B_b C22B_b H21D_b H21F -0.3108 0.2083 0.1832 137 0.980 0.000 C21B_b C22B_b H21D_b H28D -0.4417 0.3101 0.0675 137 0.980 0.000 C28B_b C22B_b H28D_b H28E -0.5402 0.1602 0.0895 137 0.980 0.000 C28B_b C22B_b H28D_b H28F -0.4808 0.1002 0.0301 137 0.980 0.000 C28B_b C22B_b H28D_b H29D -0.3502 -0.2870 0.1283 137 0.980 0.001 C29B_b C22B_b H29D_b H29E -0.3995 -0.2464 0.0594 137 0.980 0.001 C29B_b C22B_b H29D_b H29F -0.4838 -0.2301 0.1115 137 0.980 0.000 C29B_b C22B_b H29D_b H23A -0.1994 0.1738 0.1203 23 0.990 0.000 C23 C24 C22A_a H23B -0.2406 -0.0626 0.1051 23 0.990 0.000 C23 C24 C22A_a H26A -0.3500 -0.0522 -0.0223 137 0.980 0.000 C26 C24 H26A H26B -0.2429 -0.1994 0.0020 137 0.980 0.000 C26 C24 H26A H26C -0.2325 -0.0414 -0.0535 137 0.980 0.000 C26 C24 H26A H27A -0.2056 0.3454 -0.0342 137 0.980 0.000 C27 C24 H27A H27B -0.2138 0.4377 0.0323 137 0.980 0.000 C27 C24 H27A H27C -0.3273 0.3506 -0.0069 137 0.980 0.000 C27 C24 H27A H25A -0.0626 0.1116 -0.0003 137 0.910 0.000 N25 C24 H25A H25B -0.0705 -0.0419 0.0498 137 0.910 0.000 N25 C24 H25A H25C -0.0586 0.1891 0.0630 137 0.910 0.000 N25 C24 H25A H32 0.4750 0.5500 0.2840 43 0.950 0.000 C32 C33 C31 H33 0.3447 0.4609 0.2022 43 0.950 0.000 C33 C32 C34 H35 0.3391 -0.1446 0.2577 43 0.950 0.000 C35 C36 C34 H36 0.4696 -0.0653 0.3392 43 0.950 0.000 C36 C35 C31 H34A 0.2331 0.2039 0.1447 93 0.880 0.000 N34 C34 C33 H34B 0.2293 -0.0271 0.1650 93 0.880 0.000 N34 C34 C33 H41A 0.8915 0.1516 0.6982 137 0.980 0.000 C41 C42 H41A H41B 0.7592 0.0806 0.6851 137 0.980 0.000 C41 C42 H41A H41C 0.8094 0.2628 0.6450 137 0.980 0.000 C41 C42 H41A H43A 0.6879 -0.1011 0.5976 23 0.990 0.000 C43 C44 C42 H43B 0.7356 0.0835 0.5585 23 0.990 0.000 C43 C44 C42 H46A 0.9465 0.1347 0.5618 137 0.980 0.000 C46 C42 H46A H46B 1.0063 -0.0903 0.5777 137 0.980 0.000 C46 C42 H46A H46C 1.0223 0.1006 0.6254 137 0.980 0.000 C46 C42 H46A H47A 0.8115 -0.3116 0.6665 137 0.980 0.000 C47 C42 H47A H47B 0.9295 -0.2121 0.6978 137 0.980 0.000 C47 C42 H47A H47C 0.9292 -0.3457 0.6366 137 0.980 0.000 C47 C42 H47A H48A 0.8260 0.0039 0.4660 137 0.980 0.000 C48 C44 H48A H48B 0.8029 -0.2244 0.4354 137 0.980 0.000 C48 C44 H48A H48C 0.9069 -0.1932 0.4878 137 0.980 0.000 C48 C44 H48A H49A 0.8385 -0.4771 0.5500 137 0.980 0.000 C49 C44 H49A H49B 0.7322 -0.5283 0.5004 137 0.980 0.000 C49 C44 H49A H49C 0.7095 -0.4778 0.5687 137 0.980 0.000 C49 C44 H49A H45A 0.5738 -0.2147 0.5152 137 0.910 0.000 N45 C44 H45A H45B 0.6173 -0.2714 0.4569 137 0.910 0.000 N45 C44 H45A H45C 0.6155 -0.0455 0.4763 137 0.910 0.000 N45 C44 H45A 06skc0072p21 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.04604 0.64416 0.18677 1.00000 0.04260 0.02531 0.01402 -0.00574 -0.00343 0.00797 0.02778 0.01452 0.00071 0.00128 0.00039 0.00000 0.00507 0.00475 0.00528 0.00388 0.00401 0.00419 0.00213 C2 -0.11454 0.49675 0.21122 1.00000 0.04717 0.01910 0.02443 -0.00755 0.00309 -0.01637 0.03029 0.01403 0.00071 0.00128 0.00041 0.00000 0.00542 0.00441 0.00576 0.00394 0.00435 0.00417 0.00220 H2 -0.11383 0.35384 0.19748 1.00000 0.03635 0.00000 0.00000 C3 -0.18341 0.54969 0.25459 1.00000 0.02741 0.02590 0.04289 0.00471 0.00442 -0.00390 0.03202 0.01541 0.00067 0.00136 0.00043 0.00000 0.00451 0.00510 0.00660 0.00452 0.00413 0.00396 0.00226 H3 -0.23132 0.44453 0.26973 1.00000 0.03843 0.00000 0.00000 C4 -0.18453 0.75764 0.27721 1.00000 0.03192 0.03999 0.02964 -0.00153 -0.00127 -0.00869 0.03418 0.01554 0.00071 0.00145 0.00043 0.00000 0.00495 0.00585 0.00625 0.00451 0.00437 0.00438 0.00231 C5 -0.11181 0.90827 0.25489 1.00000 0.05729 0.02352 0.03184 -0.00637 -0.00433 -0.00634 0.03821 0.01536 0.00075 0.00141 0.00043 0.00000 0.00608 0.00473 0.00630 0.00430 0.00476 0.00456 0.00239 H5 -0.10808 1.04812 0.27109 1.00000 0.04585 0.00000 0.00000 C6 -0.04351 0.85317 0.20813 1.00000 0.02836 0.03617 0.02234 0.00003 0.00078 -0.00365 0.02910 0.01480 0.00066 0.00138 0.00040 0.00000 0.00460 0.00567 0.00554 0.00416 0.00382 0.00401 0.00215 H6 0.00332 0.95694 0.19155 1.00000 0.03492 0.00000 0.00000 N4 -0.25437 0.81180 0.31981 1.00000 0.05414 0.02542 0.04276 -0.00321 0.02426 0.00069 0.03940 0.01360 0.00057 0.00124 0.00034 0.00000 0.00471 0.00389 0.00547 0.00418 0.00397 0.00408 0.00197 H4A -0.25413 0.94286 0.33364 1.00000 0.04728 0.00000 0.00000 H4B -0.29990 0.71587 0.33361 1.00000 0.04728 0.00000 0.00000 O1A 0.03467 0.35151 0.12252 1.00000 0.04939 0.02111 0.03471 -0.00436 0.00813 0.00058 0.03481 0.01034 0.00048 0.00087 0.00028 0.00000 0.00375 0.00331 0.00432 0.00278 0.00305 0.00278 0.00160 O1B 0.15579 0.65937 0.14664 1.00000 0.02938 0.03743 0.04075 -0.01521 0.00308 -0.00971 0.03590 0.00972 0.00044 0.00089 0.00029 0.00000 0.00322 0.00350 0.00460 0.00305 0.00289 0.00272 0.00163 O1C -0.01274 0.68121 0.07370 1.00000 0.04323 0.03817 0.03173 0.00311 0.01401 0.00013 0.03699 0.01100 0.00049 0.00090 0.00030 0.00000 0.00363 0.00365 0.00441 0.00298 0.00315 0.00288 0.00165 S1 0.03991 0.58064 0.12937 1.00000 0.03680 0.02771 0.02882 -0.00140 0.00873 0.00151 0.03073 0.00401 0.00018 0.00033 0.00011 0.00000 0.00127 0.00116 0.00152 0.00113 0.00104 0.00109 0.00058 C21A_a -0.38709 0.04329 0.17084 0.49398 0.03130 0.04971 0.01857 -0.01778 0.00321 -0.01954 0.03315 0.07716 0.00549 0.00675 0.00183 0.01662 0.01365 0.02013 0.00724 0.01157 0.00693 0.01356 0.00656 H21A_a -0.46856 0.03392 0.17797 0.49398 0.04973 0.01662 0.00000 H21B_a -0.34512 0.12992 0.20257 0.49398 0.04973 0.01662 0.00000 H21C_a -0.35357 -0.09968 0.17146 0.49398 0.04973 0.01662 0.00000 C22A_a -0.37785 0.14461 0.10995 0.49398 0.03396 0.06421 0.03453 0.01046 0.00560 0.01126 0.04409 0.07759 0.00388 0.00494 0.00179 0.01662 0.00585 0.01868 0.00796 0.01827 0.00533 0.02091 0.00599 C28A_a -0.47563 0.03076 0.07229 0.49398 0.07522 0.07460 0.01989 -0.00272 0.02215 -0.01151 0.05534 0.04904 0.00247 0.00495 0.00118 0.01662 0.01821 0.02040 0.01483 0.01482 0.01277 0.01824 0.00800 H28A_a -0.54978 0.07673 0.08496 0.49398 0.08301 0.01662 0.00000 H28B_a -0.46710 -0.12305 0.07812 0.49398 0.08301 0.01662 0.00000 H28C_a -0.47311 0.06514 0.02949 0.49398 0.08301 0.01662 0.00000 C29A_a -0.40569 0.37483 0.11264 0.49398 0.01978 0.05105 0.03643 -0.00832 -0.01427 -0.00078 0.03700 0.03120 0.00139 0.00295 0.00092 0.01662 0.00985 0.01485 0.01361 0.00956 0.00854 0.00833 0.00640 H29A_a -0.48707 0.39226 0.11920 0.49398 0.05550 0.01662 0.00000 H29B_a -0.39168 0.44285 0.07448 0.49398 0.05550 0.01662 0.00000 H29C_a -0.35667 0.44112 0.14602 0.49398 0.05550 0.01662 0.00000 C21B_b -0.37132 0.10099 0.17444 0.50602 0.03130 0.04971 0.01857 -0.01778 0.00321 -0.01954 0.03315 0.07016 0.00547 0.00699 0.00182 0.01662 0.01365 0.02013 0.00724 0.01157 0.00693 0.01356 0.00656 H21D_b -0.35377 -0.02346 0.20029 0.50602 0.04973 0.01662 0.00000 H21E_b -0.44600 0.16059 0.18237 0.50602 0.04973 0.01662 0.00000 H21F_b -0.31080 0.20827 0.18320 0.50602 0.04973 0.01662 0.00000 C22B_b -0.37652 0.03562 0.10891 0.50602 0.03396 0.06421 0.03453 0.01046 0.00560 0.01126 0.04409 0.06916 0.00383 0.00433 0.00170 0.01662 0.00585 0.01868 0.00796 0.01827 0.00533 0.02091 0.00599 C28B_b -0.46789 0.16280 0.07061 0.50602 0.03367 0.04414 0.03650 0.02730 0.00232 0.00094 0.03820 0.04843 0.00194 0.00406 0.00114 0.01662 0.01246 0.01337 0.01550 0.01333 0.01032 0.01223 0.00649 H28D_b -0.44172 0.31006 0.06752 0.50602 0.05731 0.01662 0.00000 H28E_b -0.54020 0.16022 0.08946 0.50602 0.05731 0.01662 0.00000 H28F_b -0.48075 0.10023 0.03011 0.50602 0.05731 0.01662 0.00000 C29B_b -0.40514 -0.20400 0.10133 0.50602 0.06323 0.02897 0.07187 0.01343 0.04007 -0.00143 0.05232 0.03984 0.00167 0.00302 0.00105 0.01662 0.01376 0.01171 0.01793 0.01137 0.01183 0.01060 0.00692 H29D_b -0.35023 -0.28702 0.12834 0.50602 0.07848 0.01662 0.00000 H29E_b -0.39951 -0.24643 0.05936 0.50602 0.07848 0.01662 0.00000 H29F_b -0.48378 -0.23011 0.11148 0.50602 0.07848 0.01662 0.00000 C23 -0.25479 0.08785 0.09360 1.00000 0.02798 0.04260 0.03169 -0.00037 0.00137 0.00038 0.03422 0.01577 0.00062 0.00158 0.00040 0.00000 0.00437 0.00527 0.00603 0.00492 0.00388 0.00455 0.00215 H23A_a -0.19940 0.17380 0.12034 1.00000 0.04107 0.00000 0.00000 H23B_a -0.24064 -0.06264 0.10511 1.00000 0.04107 0.00000 0.00000 C24 -0.22116 0.11363 0.02870 1.00000 0.03369 0.03715 0.03582 0.00802 0.00304 0.00039 0.03560 0.01650 0.00068 0.00142 0.00044 0.00000 0.00478 0.00588 0.00645 0.00469 0.00419 0.00455 0.00235 C26 -0.26560 -0.06028 -0.01516 1.00000 0.05100 0.04022 0.04124 -0.00804 0.01171 -0.01019 0.04367 0.01585 0.00078 0.00158 0.00044 0.00000 0.00591 0.00560 0.00681 0.00528 0.00487 0.00516 0.00253 H26A -0.35003 -0.05218 -0.02231 1.00000 0.06550 0.00000 0.00000 H26B -0.24292 -0.19938 0.00203 1.00000 0.06550 0.00000 0.00000 H26C -0.23252 -0.04142 -0.05350 1.00000 0.06550 0.00000 0.00000 C27 -0.24393 0.33049 0.00273 1.00000 0.03931 0.02791 0.06706 0.00848 0.00724 0.00619 0.04465 0.01810 0.00074 0.00149 0.00048 0.00000 0.00515 0.00479 0.00823 0.00547 0.00491 0.00483 0.00266 H27A -0.20562 0.34535 -0.03418 1.00000 0.06697 0.00000 0.00000 H27B -0.21375 0.43770 0.03225 1.00000 0.06697 0.00000 0.00000 H27C -0.32734 0.35064 -0.00691 1.00000 0.06697 0.00000 0.00000 N25 -0.09000 0.09081 0.03603 1.00000 0.03922 0.02343 0.02958 -0.00066 0.00325 -0.00308 0.03077 0.01166 0.00049 0.00109 0.00032 0.00000 0.00392 0.00368 0.00482 0.00361 0.00329 0.00361 0.00173 H25A -0.06262 0.11164 -0.00032 1.00000 0.04616 0.00000 0.00000 H25B -0.07050 -0.04192 0.04983 1.00000 0.04616 0.00000 0.00000 H25C -0.05862 0.18909 0.06297 1.00000 0.04616 0.00000 0.00000 C31 0.48421 0.24603 0.32086 1.00000 0.03363 0.03095 0.03267 0.00299 0.01715 0.00718 0.03143 0.01638 0.00069 0.00137 0.00042 0.00000 0.00503 0.00487 0.00650 0.00440 0.00437 0.00419 0.00229 C32 0.44738 0.40847 0.27873 1.00000 0.04663 0.02774 0.02020 -0.00293 0.01537 -0.00441 0.03067 0.01621 0.00073 0.00138 0.00040 0.00000 0.00538 0.00475 0.00575 0.00432 0.00440 0.00424 0.00218 H32 0.47505 0.55002 0.28399 1.00000 0.03681 0.00000 0.00000 C33 0.37095 0.35372 0.23053 1.00000 0.05064 0.02741 0.03252 0.00150 0.01520 0.01281 0.03608 0.01754 0.00076 0.00133 0.00044 0.00000 0.00569 0.00558 0.00631 0.00428 0.00477 0.00443 0.00236 H33 0.34473 0.46088 0.20225 1.00000 0.04330 0.00000 0.00000 C34 0.33013 0.15025 0.22105 1.00000 0.04124 0.03706 0.01981 0.00246 0.00354 0.00371 0.03268 0.01627 0.00074 0.00143 0.00042 0.00000 0.00522 0.00521 0.00596 0.00449 0.00443 0.00456 0.00221 C35 0.36742 -0.00346 0.26295 1.00000 0.03933 0.02983 0.03983 -0.01728 0.00830 -0.00326 0.03604 0.01634 0.00072 0.00145 0.00046 0.00000 0.00520 0.00505 0.00668 0.00471 0.00473 0.00418 0.00234 H35 0.33907 -0.14458 0.25773 1.00000 0.04324 0.00000 0.00000 C36 0.44382 0.04375 0.31141 1.00000 0.04846 0.01648 0.04175 0.00600 0.01998 0.00493 0.03447 0.01755 0.00076 0.00126 0.00045 0.00000 0.00541 0.00487 0.00680 0.00416 0.00482 0.00398 0.00232 H36 0.46961 -0.06531 0.33916 1.00000 0.04136 0.00000 0.00000 N34 0.25523 0.10345 0.17094 1.00000 0.05570 0.03978 0.03516 -0.00094 -0.00144 0.00448 0.04400 0.01380 0.00060 0.00134 0.00036 0.00000 0.00463 0.00481 0.00565 0.00404 0.00400 0.00420 0.00208 H34A 0.23313 0.20394 0.14471 1.00000 0.05280 0.00000 0.00000 H34B 0.22928 -0.02707 0.16503 1.00000 0.05280 0.00000 0.00000 O31A 0.57959 0.54423 0.38971 1.00000 0.05617 0.02647 0.03046 -0.00384 -0.00111 -0.00007 0.03811 0.01020 0.00049 0.00091 0.00028 0.00000 0.00384 0.00342 0.00419 0.00291 0.00310 0.00288 0.00163 O31B 0.69643 0.23690 0.37038 1.00000 0.04315 0.04126 0.04614 -0.00965 0.00898 0.00639 0.04321 0.01101 0.00049 0.00094 0.00031 0.00000 0.00387 0.00382 0.00490 0.00336 0.00334 0.00301 0.00180 O31C 0.54626 0.20774 0.43524 1.00000 0.04768 0.03846 0.02455 0.00619 0.01039 0.00833 0.03642 0.01104 0.00050 0.00091 0.00029 0.00000 0.00372 0.00371 0.00414 0.00289 0.00304 0.00286 0.00164 S31 0.58458 0.31403 0.38254 1.00000 0.04411 0.02647 0.03428 -0.00082 0.00993 0.00302 0.03454 0.00424 0.00019 0.00035 0.00011 0.00000 0.00139 0.00117 0.00163 0.00115 0.00111 0.00112 0.00062 C41 0.82730 0.12910 0.66658 1.00000 0.06170 0.03727 0.06153 -0.00676 -0.01469 -0.00259 0.05504 0.01671 0.00084 0.00145 0.00052 0.00000 0.00651 0.00636 0.00866 0.00545 0.00572 0.00547 0.00308 H41A 0.89152 0.15162 0.69817 1.00000 0.08256 0.00000 0.00000 H41B 0.75921 0.08057 0.68506 1.00000 0.08256 0.00000 0.00000 H41C 0.80935 0.26283 0.64501 1.00000 0.08256 0.00000 0.00000 C42 0.86156 -0.04007 0.62183 1.00000 0.04070 0.03547 0.03528 0.00157 0.01110 -0.00370 0.03664 0.01665 0.00075 0.00152 0.00043 0.00000 0.00515 0.00548 0.00634 0.00473 0.00441 0.00463 0.00229 C43 0.75281 -0.06120 0.57454 1.00000 0.03938 0.02641 0.04580 0.00476 0.01081 0.01157 0.03675 0.01615 0.00071 0.00140 0.00043 0.00000 0.00510 0.00484 0.00675 0.00481 0.00453 0.00433 0.00231 H43A 0.68786 -0.10111 0.59756 1.00000 0.04410 0.00000 0.00000 H43B 0.73563 0.08348 0.55854 1.00000 0.04410 0.00000 0.00000 C44 0.74632 -0.20582 0.52097 1.00000 0.04188 0.03711 0.03831 -0.00154 -0.00524 0.02228 0.03979 0.01701 0.00074 0.00151 0.00045 0.00000 0.00529 0.00569 0.00658 0.00485 0.00453 0.00473 0.00245 C46 0.96865 0.03266 0.59422 1.00000 0.04343 0.09708 0.04683 -0.02120 0.00639 -0.02747 0.06234 0.01781 0.00078 0.00202 0.00050 0.00000 0.00575 0.00996 0.00794 0.00663 0.00511 0.00621 0.00358 H46A 0.94653 0.13470 0.56175 1.00000 0.09350 0.00000 0.00000 H46B 1.00628 -0.09032 0.57769 1.00000 0.09350 0.00000 0.00000 H46C 1.02227 0.10055 0.62539 1.00000 0.09350 0.00000 0.00000 C47 0.88508 -0.24628 0.65911 1.00000 0.05681 0.04967 0.06366 -0.00373 -0.01872 0.01356 0.05853 0.01914 0.00086 0.00163 0.00056 0.00000 0.00668 0.00687 0.00900 0.00586 0.00613 0.00546 0.00331 H47A 0.81145 -0.31162 0.66647 1.00000 0.08780 0.00000 0.00000 H47B 0.92945 -0.21207 0.69784 1.00000 0.08780 0.00000 0.00000 H47C 0.92921 -0.34567 0.63662 1.00000 0.08780 0.00000 0.00000 C48 0.82794 -0.14976 0.47323 1.00000 0.04470 0.14483 0.03098 -0.01848 0.01409 0.02201 0.07278 0.02261 0.00081 0.00248 0.00049 0.00000 0.00605 0.01242 0.00703 0.00767 0.00501 0.00733 0.00410 H48A 0.82602 0.00394 0.46605 1.00000 0.10917 0.00000 0.00000 H48B 0.80288 -0.22438 0.43542 1.00000 0.10917 0.00000 0.00000 H48C 0.90687 -0.19318 0.48783 1.00000 0.10917 0.00000 0.00000 C49 0.75768 -0.44390 0.53644 1.00000 0.12452 0.02454 0.08023 -0.01434 -0.03524 0.02923 0.07977 0.02034 0.00108 0.00160 0.00059 0.00000 0.01008 0.00561 0.01038 0.00602 0.00804 0.00656 0.00428 H49A 0.83854 -0.47714 0.55004 1.00000 0.11965 0.00000 0.00000 H49B 0.73220 -0.52830 0.50044 1.00000 0.11965 0.00000 0.00000 H49C 0.70953 -0.47782 0.56868 1.00000 0.11965 0.00000 0.00000 N45 0.62641 -0.18201 0.48922 1.00000 0.04459 0.01800 0.03569 -0.00167 0.01407 -0.00682 0.03205 0.01236 0.00053 0.00116 0.00032 0.00000 0.00416 0.00333 0.00511 0.00375 0.00351 0.00362 0.00177 H45A 0.57379 -0.21467 0.51522 1.00000 0.04808 0.00000 0.00000 H45B 0.61732 -0.27140 0.45690 1.00000 0.04808 0.00000 0.00000 H45C 0.61553 -0.04552 0.47630 1.00000 0.04808 0.00000 0.00000 Final Structure Factor Calculation for 06skc0072p21 in P2(1) Total number of l.s. parameters = 402 Maximum vector length = 511 Memory required = 6128 / 26068 wR2 = 0.2561 before cycle 5 for 6849 data and 2 / 402 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.966; Restrained GooF = 0.965 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0794 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1006 for 2674 Fo > 4sig(Fo) and 0.2587 for all 6849 data wR2 = 0.2561, GooF = S = 0.966, Restrained GooF = 0.965 for all data Flack x parameter = -0.0980 with esd 0.1862 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 40.00 for non-hydrogen and 52.00 for hydrogen atoms Principal mean square atomic displacements U 0.0487 0.0231 0.0116 C1 0.0547 0.0270 0.0092 C2 0.0442 0.0303 0.0215 C3 0.0458 0.0331 0.0237 C4 0.0617 0.0347 0.0182 C5 0.0377 0.0277 0.0219 C6 0.0665 0.0290 0.0227 N4 0.0499 0.0349 0.0196 O1A 0.0552 0.0335 0.0190 O1B 0.0483 0.0385 0.0242 O1C 0.0389 0.0289 0.0244 S1 0.0659 0.0253 0.0083 C21A_a 0.0704 0.0322 0.0297 C22A_a 0.0882 0.0648 0.0130 C28A_a 0.0574 0.0436 0.0100 C29A_a 0.0659 0.0253 0.0083 C21B_b 0.0704 0.0322 0.0297 C22B_b 0.0681 0.0338 0.0128 C28B_b 0.0986 0.0397 0.0186 C29B_b 0.0426 0.0326 0.0274 C23 0.0446 0.0338 0.0284 C24 0.0610 0.0377 0.0323 C26 0.0689 0.0408 0.0243 C27 0.0399 0.0296 0.0228 N25 0.0482 0.0289 0.0172 C31 0.0510 0.0268 0.0142 C32 0.0592 0.0292 0.0199 C33 0.0434 0.0352 0.0194 C34 0.0539 0.0374 0.0168 C35 0.0603 0.0280 0.0151 C36 0.0594 0.0387 0.0340 N34 0.0581 0.0322 0.0240 O31A 0.0539 0.0472 0.0286 O31B 0.0543 0.0338 0.0212 O31C 0.0465 0.0318 0.0253 S31 0.0857 0.0465 0.0329 C41 0.0454 0.0367 0.0278 C42 0.0529 0.0377 0.0196 C43 0.0658 0.0371 0.0165 C44 0.1133 0.0442 0.0295 C46 0.0924 0.0500 0.0332 C47 0.1523 0.0481 0.0180 C48 0.1673 0.0558 0.0163 C49 0.0512 0.0288 0.0162 N45 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.028 0.036 0.045 0.054 0.065 0.080 0.103 0.143 1.000 Number in group 687. 760. 676. 669. 656. 674. 696. 682. 665. 684. GooF 0.843 0.843 0.942 0.929 0.963 0.938 1.013 1.072 1.048 1.048 K 5.573 1.563 1.082 1.167 1.070 1.005 1.020 1.026 1.028 1.028 Resolution(A) 0.77 0.81 0.84 0.88 0.93 0.99 1.07 1.17 1.34 1.68 inf Number in group 714. 675. 684. 677. 673. 686. 685. 696. 674. 685. GooF 0.887 0.846 0.899 0.919 0.903 0.987 1.051 1.022 1.061 1.052 K 0.713 1.190 1.160 1.164 1.056 1.057 1.073 1.060 1.031 1.021 R1 0.516 0.480 0.444 0.378 0.271 0.238 0.169 0.126 0.110 0.059 Recommended weighting scheme: WGHT 0.0793 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)/esd Fc/Fc(max) Resolution(A) 1 -1 1 10954.52 21976.92 5.62 0.921 5.30 3 1 6 201.09 33.27 5.57 0.036 2.35 2 -5 2 121.10 658.44 5.32 0.159 1.22 -2 0 1 991.16 1675.44 4.67 0.254 5.75 0 -3 12 142.24 355.24 4.59 0.117 1.38 -3 -5 17 -95.90 250.66 4.38 0.098 0.90 -1 -3 17 18.07 267.19 4.30 0.102 1.11 1 0 19 2228.46 164.39 4.29 0.080 1.15 0 4 2 115.90 45.64 4.18 0.042 1.56 -7 -2 3 178.39 77.26 4.05 0.055 1.46 3 -1 6 180.74 35.07 4.00 0.037 2.35 -4 5 8 -61.74 107.30 3.97 0.064 1.08 -1 0 16 3221.74 47.19 3.96 0.043 1.39 1 1 7 195.44 81.10 3.90 0.056 2.68 8 -4 4 45.18 95.59 3.89 0.061 1.03 -6 4 7 -5.80 77.72 3.68 0.055 1.16 3 3 6 181.11 292.30 3.67 0.106 1.62 -1 8 1 -41.58 64.49 3.62 0.050 0.78 1 -2 12 455.68 753.92 3.55 0.171 1.56 0 5 20 450.80 16.86 3.40 0.026 0.83 -1 4 17 -48.14 198.91 3.38 0.088 1.01 0 1 20 680.42 210.36 3.37 0.090 1.09 -4 -5 16 -126.84 140.62 3.36 0.074 0.91 2 -2 9 124.66 27.95 3.36 0.033 1.79 2 0 3 34406.32 25887.28 3.36 1.000 4.33 -2 -4 2 21.65 124.65 3.33 0.069 1.51 -1 -5 1 -77.74 164.96 3.32 0.080 1.25 5 5 3 301.88 122.61 3.30 0.069 1.09 4 -4 11 92.93 187.80 3.27 0.085 1.11 -6 -3 3 106.29 29.69 3.24 0.034 1.42 7 3 18 307.83 9.75 3.22 0.019 0.86 -7 -1 15 1022.85 671.87 3.13 0.161 1.14 0 -6 10 62.41 153.85 3.13 0.077 0.95 -2 0 5 29321.79 22129.45 3.12 0.925 3.71 -7 -2 15 119.76 311.30 3.06 0.110 1.09 -10 2 14 239.87 75.28 3.05 0.054 0.94 1 -2 19 757.18 459.48 3.04 0.133 1.08 -13 0 8 -27.80 109.55 3.03 0.065 0.88 -11 3 3 -39.75 65.92 3.01 0.050 0.94 -1 2 3 341.42 236.26 3.00 0.096 2.84 -10 -3 1 4.58 81.20 2.98 0.056 1.02 -5 6 1 1028.95 701.82 2.97 0.165 0.96 4 3 12 337.24 508.80 2.95 0.140 1.21 9 2 5 -3.72 144.71 2.93 0.075 1.12 2 0 19 2529.61 1688.85 2.92 0.255 1.12 -1 1 23 306.83 58.05 2.91 0.047 0.96 -6 0 13 514.70 814.60 2.90 0.177 1.35 -11 2 1 217.79 49.45 2.89 0.044 1.00 0 -2 14 101.20 226.67 2.88 0.094 1.41 -5 1 25 394.85 87.09 2.86 0.058 0.85 Bond lengths and angles C1 - Distance Angles C2 1.3730 (0.0109) C6 1.3974 (0.0113) 119.53 (0.77) S1 1.7507 (0.0089) 122.44 (0.62) 118.03 (0.69) C1 - C2 C6 C2 - Distance Angles C3 1.3602 (0.0115) C1 1.3730 (0.0109) 121.82 (0.75) H2 0.9500 119.09 119.09 C2 - C3 C1 C3 - Distance Angles C2 1.3602 (0.0115) C4 1.4024 (0.0121) 120.79 (0.82) H3 0.9500 119.61 119.61 C3 - C2 C4 C4 - Distance Angles N4 1.3566 (0.0108) C5 1.3969 (0.0119) 120.61 (0.83) C3 1.4024 (0.0121) 120.96 (0.83) 118.43 (0.87) C4 - N4 C5 C5 - Distance Angles C4 1.3969 (0.0119) C6 1.4185 (0.0118) 120.23 (0.84) H5 0.9500 119.88 119.88 C5 - C4 C6 C6 - Distance Angles C1 1.3974 (0.0113) C5 1.4185 (0.0118) 119.10 (0.80) H6 0.9500 120.45 120.45 C6 - C1 C5 N4 - Distance Angles C4 1.3566 (0.0108) H4A 0.8800 120.00 H4B 0.8800 120.00 120.00 N4 - C4 H4A O1A - Distance Angles S1 1.4502 (0.0058) O1A - O1B - Distance Angles S1 1.4497 (0.0054) O1B - O1C - Distance Angles S1 1.4655 (0.0066) O1C - S1 - Distance Angles O1B 1.4497 (0.0054) O1A 1.4502 (0.0058) 113.27 (0.35) O1C 1.4655 (0.0066) 111.69 (0.36) 109.34 (0.38) C1 1.7507 (0.0089) 108.48 (0.37) 106.42 (0.38) 107.33 (0.37) S1 - O1B O1A O1C C21A_a - Distance Angles C22A_a 1.5113 (0.0189) H21A_a 0.9800 109.46 H21B_a 0.9800 109.51 109.47 H21C_a 0.9800 109.44 109.47 109.47 C21A_a - C22A_a H21A_a H21B_a C22A_a - Distance Angles C29A_a 1.4869 (0.0351) C21A_a 1.5113 (0.0189) 109.76 (3.03) C28A_a 1.5187 (0.0541) 109.14 (2.87) 100.05 (3.27) C23 1.5570 (0.0430) 116.28 (2.74) 105.56 (3.45) 114.64 (2.60) C22A_a - C29A_a C21A_a C28A_a C28A_a - Distance Angles C22A_a 1.5187 (0.0541) H28A_a 0.9800 109.47 H28B_a 0.9800 109.47 109.47 H28C_a 0.9800 109.48 109.47 109.47 C28A_a - C22A_a H28A_a H28B_a C29A_a - Distance Angles C22A_a 1.4869 (0.0351) H29A_a 0.9800 109.47 H29B_a 0.9800 109.49 109.47 H29C_a 0.9800 109.45 109.47 109.47 C29A_a - C22A_a H29A_a H29B_a C21B_b - Distance Angles C22B_b 1.5098 (0.0186) H21D_b 0.9800 109.52 H21E_b 0.9800 109.45 109.47 H21F_b 0.9800 109.45 109.47 109.47 C21B_b - C22B_b H21D_b H21E_b C22B_b - Distance Angles C21B_b 1.5098 (0.0186) C28B_b 1.5178 (0.0455) 110.60 (3.60) C23 1.5283 (0.0439) 102.38 (3.36) 111.86 (2.36) C29B_b 1.5492 (0.0329) 110.87 (2.60) 108.80 (2.85) 112.25 (2.29) C22B_b - C21B_b C28B_b C23 C28B_b - Distance Angles C22B_b 1.5178 (0.0455) H28D_b 0.9800 109.49 H28E_b 0.9800 109.48 109.47 H28F_b 0.9800 109.45 109.47 109.47 C28B_b - C22B_b H28D_b H28E_b C29B_b - Distance Angles C22B_b 1.5492 (0.0330) H29D_b 0.9800 109.50 H29E_b 0.9800 109.44 109.47 H29F_b 0.9800 109.47 109.47 109.47 C29B_b - C22B_b H29D_b H29E_b C23 - Distance Angles C22B_b 1.5283 (0.0439) C24 1.5445 (0.0121) 124.40 (1.57) C22A_a 1.5570 (0.0430) 25.68 (1.17) 121.75 (1.53) H23A_a 0.9900 122.89 106.90 106.88 H23B_a 0.9900 82.49 106.90 106.90 106.69 C23 - C22B_b C24 C22A_a H23A_a C24 - Distance Angles C27 1.4942 (0.0125) C26 1.5195 (0.0128) 112.03 (0.84) N25 1.5248 (0.0095) 105.16 (0.68) 105.61 (0.72) C23 1.5445 (0.0121) 113.90 (0.78) 114.95 (0.72) 103.96 (0.66) C24 - C27 C26 N25 C26 - Distance Angles C24 1.5195 (0.0128) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C24 H26A H26B C27 - Distance Angles C24 1.4942 (0.0125) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C24 H27A H27B N25 - Distance Angles C24 1.5248 (0.0095) H25A 0.9100 109.47 H25B 0.9100 109.47 109.47 H25C 0.9100 109.47 109.47 109.47 N25 - C24 H25A H25B C31 - Distance Angles C36 1.3652 (0.0116) C32 1.4216 (0.0115) 119.61 (0.85) S31 1.7573 (0.0094) 122.44 (0.72) 117.92 (0.66) C31 - C36 C32 C32 - Distance Angles C33 1.3623 (0.0122) C31 1.4216 (0.0115) 117.56 (0.81) H32 0.9500 121.22 121.22 C32 - C33 C31 C33 - Distance Angles C32 1.3623 (0.0122) C34 1.3738 (0.0117) 122.85 (0.87) H33 0.9500 118.58 118.57 C33 - C32 C34 C34 - Distance Angles N34 1.3718 (0.0111) C33 1.3738 (0.0117) 120.27 (0.87) C35 1.3806 (0.0126) 121.66 (0.87) 118.07 (0.84) C34 - N34 C33 C35 - Distance Angles C36 1.3551 (0.0126) C34 1.3806 (0.0126) 121.05 (0.84) H35 0.9500 119.48 119.47 C35 - C36 C34 C36 - Distance Angles C35 1.3551 (0.0126) C31 1.3652 (0.0116) 120.85 (0.85) H36 0.9500 119.57 119.58 C36 - C35 C31 N34 - Distance Angles C34 1.3718 (0.0111) H34A 0.8800 120.00 H34B 0.8800 120.00 120.00 N34 - C34 H34A O31A - Distance Angles S31 1.4589 (0.0061) O31A - O31B - Distance Angles S31 1.4422 (0.0059) O31B - O31C - Distance Angles S31 1.4603 (0.0064) O31C - S31 - Distance Angles O31B 1.4422 (0.0059) O31A 1.4589 (0.0061) 113.69 (0.38) O31C 1.4603 (0.0064) 110.86 (0.38) 110.35 (0.38) C31 1.7573 (0.0095) 108.04 (0.40) 107.22 (0.39) 106.30 (0.40) S31 - O31B O31A O31C C41 - Distance Angles C42 1.5389 (0.0129) H41A 0.9800 109.47 H41B 0.9800 109.47 109.47 H41C 0.9800 109.47 109.47 109.47 C41 - C42 H41A H41B C42 - Distance Angles C46 1.5182 (0.0120) C41 1.5389 (0.0129) 109.53 (0.81) C47 1.5484 (0.0138) 111.32 (0.85) 106.03 (0.81) C43 1.5627 (0.0121) 113.23 (0.81) 104.30 (0.73) 111.93 (0.78) C42 - C46 C41 C47 C43 - Distance Angles C44 1.4950 (0.0125) C42 1.5627 (0.0122) 123.82 (0.74) H43A 0.9900 106.37 106.37 H43B 0.9900 106.37 106.37 106.45 C43 - C44 C42 H43A C44 - Distance Angles C43 1.4950 (0.0125) N45 1.5030 (0.0102) 106.21 (0.67) C49 1.5394 (0.0137) 114.72 (0.87) 104.79 (0.79) C48 1.5400 (0.0136) 115.36 (0.90) 105.28 (0.76) 109.42 (0.96) C44 - C43 N45 C49 C46 - Distance Angles C42 1.5182 (0.0120) H46A 0.9800 109.47 H46B 0.9800 109.47 109.47 H46C 0.9800 109.47 109.47 109.47 C46 - C42 H46A H46B C47 - Distance Angles C42 1.5484 (0.0138) H47A 0.9800 109.47 H47B 0.9800 109.47 109.47 H47C 0.9800 109.47 109.47 109.47 C47 - C42 H47A H47B C48 - Distance Angles C44 1.5400 (0.0136) H48A 0.9800 109.47 H48B 0.9800 109.47 109.47 H48C 0.9800 109.47 109.47 109.47 C48 - C44 H48A H48B C49 - Distance Angles C44 1.5394 (0.0137) H49A 0.9800 109.47 H49B 0.9800 109.47 109.47 H49C 0.9800 109.47 109.47 109.47 C49 - C44 H49A H49B N45 - Distance Angles C44 1.5030 (0.0102) H45A 0.9100 109.47 H45B 0.9100 109.48 109.47 H45C 0.9100 109.47 109.47 109.47 N45 - C44 H45A H45B Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.92 2.811(9) 167.3 N25-H25C...O1A 0.88 2.49 3.098(10) 126.8 N34-H34A...O1A 0.91 1.97 2.844(9) 161.4 N45-H45C...O31C 0.88 2.25 3.104(9) 163.1 N4-H4B...O31A_$1 0.88 2.13 2.981(10) 163.5 N4-H4A...O31B_$2 0.91 1.98 2.888(9) 172.4 N25-H25A...O1C_$3 0.91 2.92 3.788(7) 160.4 N25-H25A...S1_$3 0.91 1.92 2.827(9) 172.9 N25-H25B...O1C_$4 0.88 2.17 3.050(10) 176.3 N34-H34B...O1B_$4 0.91 1.91 2.812(9) 173.4 N45-H45B...O31A_$4 0.91 1.93 2.841(9) 175.3 N45-H45A...O31C_$5 FMAP and GRID set by program FMAP 2 2 30 GRID -3.704 -1 -2 3.704 1 2 R1 = 0.2223 for 3964 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.44 at 0.0452 0.0786 0.1346 [ 1.60 A from H6 ] Deepest hole -0.44 at 0.6572 0.0817 0.2521 [ 1.14 A from H21B ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 6150 / 49422 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0452 1.0786 0.1346 1.00000 0.05 0.44 1.60 H6 1.74 O1A 2.02 H25C 2.28 H34B Q2 1 -0.0952 1.0935 0.2582 1.00000 0.05 0.43 0.44 H5 1.18 C5 2.01 C6 2.12 H2 Q3 1 -0.1884 0.5081 -0.0682 1.00000 0.05 0.42 1.30 H27A 2.09 C27 2.12 H34A 2.17 H34B Q4 1 -0.3984 -0.2728 0.1804 1.00000 0.05 0.41 1.23 H21C 1.34 H29D 1.70 H21D 1.76 H29F Q5 1 0.6620 0.0952 0.3978 1.00000 0.05 0.40 1.18 O31B 1.66 S31 1.80 O31C 2.05 H4A Shortest distances between peaks (including symmetry equivalents) 1 3 2.38 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.66: 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 3.55: Structure factors and derivatives 6.89: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 0.53: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0072p21 finished at 17:24:08 Total CPU time: 12.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++