+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 09:39:28 on 06-Oct-2003 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 11.1391 12.8788 14.1662 63.891 68.400 74.367 ZERR 2.00 0.0006 0.0006 0.0006 0.003 0.003 0.003 LATT 1 SFAC C H N O CL NI UNIT 36 56 36 32 4 2 V = 1682.62 F(000) = 904.0 Mu = 0.83 mm-1 Cell Wt = 1764.39 Rho = 1.741 MERG 2 OMIT -3.00 55.00 DFIX 0.84 0.02 O1W H1WA O1W H1WB O2W H2WA O2W H2WB DANG 1.35 0.02 H1WA H1WB H2WA H2WB SHEL 7 0.77 EQIV $1 X+1, Y, Z EQIV $2 -X+2, -Y+1, -Z EQIV $3 X-1, Y, Z EQIV $4 -X+2, -Y, -Z EQIV $5 -X+1, -Y+1, -Z EQIV $6 -X+2, -Y, -Z+1 EQIV $7 X, Y-1, Z EQIV $8 X, Y, Z-1 EQIV $9 -X+1, -Y, -Z+1 EQIV $10 -X+1, -Y+1, -Z+1 EQIV $11 -X+2, -Y+1, -Z+1 EQIV $12 X, Y, Z+1 HTAB N2 O2_$1 HTAB N2 O31_$2 HTAB N5 O1_$3 HTAB N5 O33_$3 HTAB O1 N16_$4 HTAB O2 O36_$5 HTAB O2 O21_$5 HTAB N12 O32_$6 HTAB N12 O1W_$7 HTAB N15 O2W_$8 HTAB O11 N26_$9 HTAB O12 O33_$4 HTAB N22 O38_$10 HTAB N22 O35_$10 HTAB N25 O2W_$9 HTAB O21 O31 HTAB O22 O32_$9 HTAB O1W O37 HTAB O1W O2W_$11 HTAB O2W O35 HTAB O2W N6_$12 FMAP 2 PLAN 5 SIZE 0.18 0.18 0.08 BOND $H ACTA WGHT 0.05480 0.84130 L.S. 10 TEMP -153.00 FVAR 0.35467 NI1 6 0.767820 0.185038 0.196922 11.00000 0.02217 0.01821 = 0.01875 -0.00873 -0.00516 -0.00398 MOLE 1 C1 1 0.903877 0.359825 0.000655 11.00000 0.02351 0.02152 = 0.02040 -0.01096 -0.00538 -0.00442 C2 1 0.776213 0.373696 -0.017039 11.00000 0.02176 0.01806 = 0.02358 -0.01080 -0.00550 -0.00157 C3 1 0.748357 0.445266 -0.115985 11.00000 0.02828 0.02370 = 0.02223 -0.00842 -0.00642 -0.00695 AFIX 43 H3 2 0.809552 0.492467 -0.176395 11.00000 -1.20000 AFIX 0 C4 1 0.629259 0.444599 -0.122334 11.00000 0.02751 0.02581 = 0.02276 -0.00801 -0.00880 -0.00406 AFIX 43 H4 2 0.604444 0.492022 -0.187511 11.00000 -1.20000 AFIX 0 C5 1 0.545145 0.372508 -0.030665 11.00000 0.02408 0.01892 = 0.02295 -0.01095 -0.00746 -0.00031 C6 1 0.416929 0.362189 -0.032440 11.00000 0.02471 0.02453 = 0.02565 -0.00897 -0.00871 -0.00330 N1 3 0.922349 0.270431 0.087058 11.00000 0.02067 0.02315 = 0.02328 -0.01170 -0.00767 -0.00424 N2 3 0.989207 0.433579 -0.069982 11.00000 0.02737 0.02873 = 0.02854 -0.00054 -0.01389 -0.00964 AFIX 93 H2A 2 1.065575 0.423755 -0.060007 11.00000 -1.20000 H2B 2 0.969492 0.492372 -0.126857 11.00000 -1.20000 AFIX 0 N3 3 0.690696 0.307771 0.069537 11.00000 0.02080 0.01925 = 0.02147 -0.01027 -0.00606 -0.00287 N4 3 0.574083 0.306849 0.063850 11.00000 0.02135 0.02206 = 0.02411 -0.01240 -0.00668 -0.00300 N5 3 0.330528 0.307900 0.062426 11.00000 0.02859 0.04731 = 0.02373 -0.00615 -0.00826 -0.01699 AFIX 93 H5A 2 0.254300 0.300527 0.062333 11.00000 -1.20000 H5B 2 0.350157 0.279709 0.124665 11.00000 -1.20000 AFIX 0 N6 3 0.399250 0.406888 -0.128421 11.00000 0.02351 0.05068 = 0.02803 -0.00661 -0.01053 -0.00951 O1 4 1.043285 0.264678 0.100766 11.00000 0.02331 0.02438 = 0.02780 -0.00925 -0.01158 -0.00449 AFIX 147 H1 2 1.077426 0.194865 0.122143 11.00000 -1.50000 AFIX 0 O2 4 0.276156 0.385081 -0.118405 11.00000 0.02999 0.07457 = 0.02986 -0.00640 -0.01347 -0.01944 AFIX 147 H2 2 0.259726 0.421544 -0.179009 11.00000 -1.50000 AFIX 0 MOLE 2 C11 1 0.898207 -0.049401 0.282837 11.00000 0.02330 0.02221 = 0.01937 -0.00811 -0.00518 -0.00582 C12 1 0.865096 -0.045818 0.188809 11.00000 0.02278 0.02337 = 0.02002 -0.00958 -0.00420 -0.00616 C13 1 0.885293 -0.141243 0.160340 11.00000 0.03311 0.01891 = 0.02357 -0.00842 -0.01031 -0.00261 AFIX 43 H13 2 0.919087 -0.216465 0.203157 11.00000 -1.20000 AFIX 0 C14 1 0.854699 -0.122728 0.068470 11.00000 0.03370 0.02319 = 0.02618 -0.01349 -0.00732 -0.00471 AFIX 43 H14 2 0.864344 -0.185205 0.046643 11.00000 -1.20000 AFIX 0 C15 1 0.808679 -0.008668 0.007576 11.00000 0.02314 0.02454 = 0.02326 -0.01171 -0.00623 -0.00429 C16 1 0.781720 0.026103 -0.098189 11.00000 0.02951 0.02608 = 0.02468 -0.01118 -0.00979 -0.00324 N11 3 0.865250 0.049302 0.296717 11.00000 0.02535 0.02337 = 0.01836 -0.01151 -0.00654 -0.00399 N12 3 0.959636 -0.145454 0.342150 11.00000 0.03993 0.02303 = 0.02687 -0.01242 -0.01714 0.00008 AFIX 93 H12A 2 0.981537 -0.145917 0.396027 11.00000 -1.20000 H12B 2 0.978520 -0.208765 0.327652 11.00000 -1.20000 AFIX 0 N13 3 0.813093 0.058968 0.131554 11.00000 0.02113 0.02077 = 0.01898 -0.00909 -0.00501 -0.00374 N14 3 0.785178 0.079271 0.040579 11.00000 0.02528 0.02195 = 0.02132 -0.01089 -0.00664 -0.00379 N15 3 0.715121 0.131949 -0.137143 11.00000 0.05518 0.03360 = 0.03575 -0.02197 -0.02695 0.01353 AFIX 93 H15A 2 0.698766 0.156000 -0.200262 11.00000 -1.20000 H15B 2 0.687882 0.177182 -0.099522 11.00000 -1.20000 AFIX 0 N16 3 0.825989 -0.046950 -0.146622 11.00000 0.03121 0.02893 = 0.02163 -0.01270 -0.01213 -0.00266 O11 4 0.913261 0.043758 0.378415 11.00000 0.03009 0.02962 = 0.02337 -0.01595 -0.01123 -0.00186 AFIX 147 H11 2 0.857057 0.078673 0.417001 11.00000 -1.50000 AFIX 0 O12 4 0.793506 0.002094 -0.245929 11.00000 0.04265 0.03276 = 0.02555 -0.01661 -0.01823 0.00225 AFIX 147 H12 2 0.825852 -0.043486 -0.279467 11.00000 -1.50000 AFIX 0 MOLE 3 C21 1 0.588894 0.286816 0.350536 11.00000 0.02415 0.01976 = 0.01776 -0.00760 -0.00716 -0.00310 C22 1 0.520780 0.194304 0.363777 11.00000 0.02389 0.01923 = 0.01866 -0.00824 -0.00927 -0.00128 C23 1 0.398535 0.170129 0.435977 11.00000 0.02346 0.02248 = 0.02300 -0.01262 -0.00693 -0.00039 AFIX 43 H23 2 0.349265 0.216206 0.477995 11.00000 -1.20000 AFIX 0 C24 1 0.351041 0.077434 0.444750 11.00000 0.02488 0.02159 = 0.02104 -0.00726 -0.00784 -0.00376 AFIX 43 H24 2 0.266992 0.058188 0.491810 11.00000 -1.20000 AFIX 0 C25 1 0.430732 0.012160 0.381940 11.00000 0.02206 0.01955 = 0.02006 -0.00701 -0.00802 -0.00353 C26 1 0.392346 -0.093648 0.389750 11.00000 0.02516 0.01806 = 0.02221 -0.00716 -0.00923 -0.00380 N21 3 0.707099 0.287084 0.287176 11.00000 0.02246 0.01904 = 0.02339 -0.00991 -0.00612 -0.00627 N22 3 0.528280 0.359890 0.402119 11.00000 0.02528 0.02484 = 0.03284 -0.01924 -0.00174 -0.00601 AFIX 93 H22A 2 0.569198 0.414131 0.394307 11.00000 -1.20000 H22B 2 0.447326 0.353914 0.444001 11.00000 -1.20000 AFIX 0 N23 3 0.589767 0.132739 0.301356 11.00000 0.02486 0.01725 = 0.01967 -0.00830 -0.00723 -0.00450 N24 3 0.546026 0.040415 0.310390 11.00000 0.02661 0.01865 = 0.02012 -0.00831 -0.00712 -0.00465 N25 3 0.474363 -0.149979 0.324810 11.00000 0.02933 0.02604 = 0.03644 -0.01957 0.00001 -0.00986 AFIX 93 H25A 2 0.455362 -0.214476 0.329557 11.00000 -1.20000 H25B 2 0.546883 -0.122240 0.277689 11.00000 -1.20000 AFIX 0 N26 3 0.283583 -0.126236 0.461620 11.00000 0.03110 0.01841 = 0.02611 -0.00954 -0.00952 -0.00770 O21 4 0.765432 0.376499 0.278534 11.00000 0.02438 0.02417 = 0.03841 -0.01662 -0.00593 -0.00942 AFIX 147 H21 2 0.845420 0.354829 0.271098 11.00000 -1.50000 AFIX 0 O22 4 0.264965 -0.229251 0.458939 11.00000 0.03351 0.02397 = 0.03643 -0.01505 -0.00471 -0.01346 AFIX 147 H22 2 0.191488 -0.248125 0.501167 11.00000 -1.50000 AFIX 0 MOLE 4 O31 4 1.022124 0.359129 0.265224 11.00000 0.03213 0.02763 = 0.02680 -0.00560 -0.01325 -0.00640 O32 4 1.001340 0.211119 0.440404 11.00000 0.03131 0.03192 = 0.02192 -0.00777 -0.00446 -0.00706 O33 4 1.181767 0.195379 0.293656 11.00000 0.03198 0.02988 = 0.02815 -0.01568 -0.00649 -0.00060 O34 4 1.163169 0.335045 0.363847 11.00000 0.03755 0.02941 = 0.04685 -0.01668 -0.02294 -0.00426 CL31 5 1.092833 0.275442 0.341153 11.00000 0.02571 0.02188 = 0.02176 -0.00823 -0.00820 -0.00422 MOLE 5 O35 4 0.645886 0.512769 0.448961 11.00000 0.04291 0.04720 = 0.05273 -0.03304 0.00707 -0.02028 O36 4 0.814307 0.590237 0.286974 11.00000 0.05564 0.03876 = 0.02707 -0.01456 -0.00595 -0.01820 O37 4 0.860977 0.479614 0.453876 11.00000 0.06781 0.05562 = 0.05020 -0.01475 -0.03030 0.01030 O38 4 0.742728 0.667321 0.422825 11.00000 0.04263 0.04330 = 0.05439 -0.03839 0.00176 -0.01505 CL35 5 0.765420 0.562690 0.402517 11.00000 0.03345 0.02746 = 0.02830 -0.01692 -0.00456 -0.00611 MOLE 6 O1W 4 1.088795 0.635686 0.315961 11.00000 0.05283 0.04426 = 0.05124 -0.02750 -0.02379 0.00635 H1WA 2 1.045679 0.583786 0.363586 11.00000 0.07153 H1WB 2 1.151694 0.634485 0.332795 11.00000 0.06170 MOLE 7 O2W 4 0.613496 0.349660 0.693889 11.00000 0.06423 0.03570 = 0.02984 -0.01460 -0.01127 0.00415 H2WA 2 0.618892 0.385271 0.628972 11.00000 0.07393 H2WB 2 0.544967 0.379434 0.728500 11.00000 0.07545 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 NI 1.250 Ni1 - N1 N11 N21 N23 N13 N3 C1 - N1 N2 C2 C2 - N3 C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - N4 C4 C6 C6 - N6 N5 C5 N1 - C1 O1 Ni1 N2 - C1 N3 - N4 C2 Ni1 N4 - N3 C5 N5 - C6 N6 - C6 O2 O1 - N1 O2 - N6 C11 - N11 N12 C12 C12 - N13 C13 C11 C13 - C14 C12 C14 - C13 C15 C15 - N14 C14 C16 C16 - N16 N15 C15 N11 - C11 O11 Ni1 N12 - C11 N13 - C12 N14 Ni1 N14 - N13 C15 N15 - C16 N16 - C16 O12 O11 - N11 O12 - N16 C21 - N21 N22 C22 C22 - N23 C23 C21 C23 - C24 C22 C24 - C23 C25 C25 - N24 C24 C26 C26 - N26 N25 C25 N21 - C21 O21 Ni1 N22 - C21 N23 - C22 N24 Ni1 N24 - C25 N23 N25 - C26 N26 - C26 O22 O21 - N21 O22 - N26 O31 - Cl31 O32 - Cl31 O33 - Cl31 O34 - Cl31 Cl31 - O34 O33 O32 O31 O35 - Cl35 O36 - Cl35 O37 - Cl35 O38 - Cl35 Cl35 - O36 O35 O38 O37 O1W - no bonds found O2W - no bonds found Operators for generating equivalent atoms: $1 x+1, y, z $2 -x+2, -y+1, -z $3 x-1, y, z $4 -x+2, -y, -z $5 -x+1, -y+1, -z $6 -x+2, -y, -z+1 $7 x, y-1, z $8 x, y, z-1 $9 -x+1, -y, -z+1 $10 -x+1, -y+1, -z+1 $11 -x+2, -y+1, -z+1 $12 x, y, z+1 31376 Reflections read, of which 6 rejected -14 =< h =< 14, -16 =< k =< 16, -18 =< l =< 18, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -3 7 0 33.36 0.89 6 4.87 -5 8 0 45.32 1.05 4 15.51 -3 8 0 114.68 1.06 7 13.41 5 -6 1 244.06 4.43 5 39.59 4 -5 1 158.97 2.01 6 26.85 3 -4 1 67.37 0.92 6 8.37 1 -7 3 54.44 0.90 8 16.69 7 -4 3 9.87 0.76 5 4.11 -1 -9 4 60.18 2.79 5 20.08 9 5 4 13.39 1.35 5 6.93 3 12 4 18.70 2.00 4 21.50 3 -2 5 168.30 1.02 11 9.78 2 3 5 455.07 6.13 6 38.12 -3 7 5 16.13 1.05 7 9.07 -2 13 5 119.34 5.41 3 37.41 11 -5 6 17.43 6.36 2 34.81 11 -4 6 44.29 6.31 2 36.58 4 -2 6 1546.33 13.67 9 84.96 0 13 7 8.79 1.91 5 11.89 5 -2 8 438.97 1.16 5 107.95 6 -2 10 157.69 4.87 4 45.29 9 3 10 21.09 1.57 5 46.01 -1 -2 11 11.29 2.29 4 12.00 -2 1 11 48.62 2.63 4 73.26 5 0 12 40.06 2.08 5 21.84 6 -2 13 16.76 2.04 3 23.74 26 Inconsistent equivalents 7687 Unique reflections, of which 0 suppressed R(int) = 0.0555 R(sigma) = 0.0530 Friedel opposites merged Maximum memory for data reduction = 4885 / 77812 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 = 6231 / 689892 wR2 = 0.1079 before cycle 1 for 7687 data and 518 / 518 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.021 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.018; Restrained GooF = 1.018 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35474 0.00047 0.151 OSF Mean shift/esd = 0.015 Maximum = -0.521 for z H2WA Max. shift = 0.009 A for H2WA Max. dU = 0.000 for H2WB Least-squares cycle 2 Maximum vector length = 511 Memory required = 6231 / 689892 wR2 = 0.1079 before cycle 2 for 7687 data and 518 / 518 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.018; Restrained GooF = 1.018 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35474 0.00047 0.005 OSF Mean shift/esd = 0.005 Maximum = -0.177 for z H2WA Max. shift = 0.003 A for H2WA Max. dU = 0.000 for H1WB Least-squares cycle 3 Maximum vector length = 511 Memory required = 6231 / 689892 wR2 = 0.1079 before cycle 3 for 7687 data and 518 / 518 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.018; Restrained GooF = 1.018 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35474 0.00047 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.013 for U11 H1WB Max. shift = 0.001 A for H2WA Max. dU = 0.000 for H1WB Least-squares cycle 4 Maximum vector length = 511 Memory required = 6231 / 689892 wR2 = 0.1079 before cycle 4 for 7687 data and 518 / 518 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.018; Restrained GooF = 1.018 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35474 0.00047 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.003 for x H2WA Max. shift = 0.000 A for H2WA Max. dU = 0.000 for H1WB Least-squares cycle 5 Maximum vector length = 511 Memory required = 6231 / 689892 wR2 = 0.1079 before cycle 5 for 7687 data and 518 / 518 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.018; Restrained GooF = 1.018 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35474 0.00047 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for x H2WA Max. shift = 0.000 A for H2WA Max. dU = 0.000 for H1WB Least-squares cycle 6 Maximum vector length = 511 Memory required = 6231 / 689892 wR2 = 0.1079 before cycle 6 for 7687 data and 518 / 518 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.018; Restrained GooF = 1.018 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35474 0.00047 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Cl35 Max. shift = 0.000 A for H2WA Max. dU = 0.000 for H1WB Least-squares cycle 7 Maximum vector length = 511 Memory required = 6231 / 689892 wR2 = 0.1079 before cycle 7 for 7687 data and 518 / 518 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.018; Restrained GooF = 1.018 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35474 0.00047 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Cl35 Max. shift = 0.000 A for H2WA Max. dU = 0.000 for H1WB Least-squares cycle 8 Maximum vector length = 511 Memory required = 6231 / 689892 wR2 = 0.1079 before cycle 8 for 7687 data and 518 / 518 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.018; Restrained GooF = 1.018 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35474 0.00047 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Cl35 Max. shift = 0.000 A for H12 Max. dU = 0.000 for H1WA Least-squares cycle 9 Maximum vector length = 511 Memory required = 6231 / 689892 wR2 = 0.1079 before cycle 9 for 7687 data and 518 / 518 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.018; Restrained GooF = 1.018 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35474 0.00047 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Cl35 Max. shift = 0.000 A for H2WA Max. dU = 0.000 for H1WA Least-squares cycle 10 Maximum vector length = 511 Memory required = 6231 / 689892 wR2 = 0.1079 before cycle 10 for 7687 data and 518 / 518 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.018; Restrained GooF = 1.018 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35474 0.00047 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H2 Max. dU = 0.000 for H2WB Largest correlation matrix elements -0.719 y H1WA / x H1WA -0.560 z H1WB / x H1WB -0.518 U23 N22 / U22 N22 -0.617 U23 O38 / U33 O38 -0.535 U23 N15 / U33 N15 -0.517 U23 Cl35 / U22 Cl35 -0.610 U23 O38 / U22 O38 -0.531 U23 N15 / U22 N15 -0.515 U13 O1W / U33 O1W -0.596 z H2WB / y H2WB -0.524 U23 N22 / U33 N22 -0.511 U12 O38 / U13 O38 -0.583 U23 O1W / U22 O1W -0.523 U23 N25 / U22 N25 -0.506 U13 N15 / U33 N15 -0.579 U23 O1W / U33 O1W -0.521 z O38 / y O38 -0.505 U23 O11 / U33 O11 -0.572 U23 O35 / U22 O35 -0.519 U23 Cl35 / U33 Cl35 -0.504 U23 O22 / U33 O22 -0.569 U23 O35 / U33 O35 -0.519 U23 N25 / U33 N25 -0.502 U23 O2W / U33 O2W Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.8096 0.4925 -0.1764 43 0.950 0.000 C3 C4 C2 H4 0.6044 0.4920 -0.1875 43 0.950 0.000 C4 C3 C5 H2A 1.0656 0.4238 -0.0600 93 0.880 0.000 N2 C1 N1 H2B 0.9695 0.4924 -0.1269 93 0.880 0.000 N2 C1 N1 H5A 0.2543 0.3005 0.0623 93 0.880 0.000 N5 C6 N6 H5B 0.3502 0.2797 0.1247 93 0.880 0.000 N5 C6 N6 H1 1.0774 0.1949 0.1221 147 0.840 0.000 O1 N1 H1 H2 0.2597 0.4216 -0.1790 147 0.840 0.000 O2 N6 H2 H13 0.9191 -0.2165 0.2031 43 0.950 0.000 C13 C14 C12 H14 0.8643 -0.1852 0.0466 43 0.950 0.000 C14 C13 C15 H12A 0.9815 -0.1459 0.3960 93 0.880 0.000 N12 C11 N11 H12B 0.9785 -0.2088 0.3276 93 0.880 0.000 N12 C11 N11 H15A 0.6988 0.1560 -0.2003 93 0.880 0.000 N15 C16 N16 H15B 0.6879 0.1772 -0.0995 93 0.880 0.000 N15 C16 N16 H11 0.8571 0.0788 0.4169 147 0.840 0.000 O11 N11 H11 H12 0.8259 -0.0434 -0.2795 147 0.840 0.000 O12 N16 H12 H23 0.3493 0.2162 0.4780 43 0.950 0.000 C23 C24 C22 H24 0.2670 0.0582 0.4918 43 0.950 0.000 C24 C23 C25 H22A 0.5692 0.4141 0.3943 93 0.880 0.000 N22 C21 N21 H22B 0.4473 0.3539 0.4440 93 0.880 0.000 N22 C21 N21 H25A 0.4554 -0.2145 0.3296 93 0.880 0.000 N25 C26 N26 H25B 0.5469 -0.1222 0.2777 93 0.880 0.000 N25 C26 N26 H21 0.8454 0.3549 0.2710 147 0.840 0.000 O21 N21 H21 H22 0.1915 -0.2481 0.5011 147 0.840 0.000 O22 N26 H22 s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Ni1 0.76782 0.18504 0.19692 1.00000 0.02217 0.01821 0.01876 -0.00874 -0.00516 -0.00398 0.01899 0.00040 0.00003 0.00003 0.00002 0.00000 0.00018 0.00016 0.00017 0.00013 0.00013 0.00013 0.00010 C1 0.90387 0.35981 0.00066 1.00000 0.02351 0.02151 0.02039 -0.01096 -0.00538 -0.00441 0.02062 0.00319 0.00024 0.00020 0.00019 0.00000 0.00132 0.00120 0.00121 0.00103 0.00104 0.00104 0.00052 C2 0.77621 0.37370 -0.01704 1.00000 0.02177 0.01806 0.02356 -0.01080 -0.00550 -0.00157 0.02057 0.00326 0.00024 0.00020 0.00020 0.00000 0.00130 0.00114 0.00126 0.00101 0.00104 0.00100 0.00052 C3 0.74837 0.44526 -0.11599 1.00000 0.02824 0.02370 0.02227 -0.00844 -0.00639 -0.00696 0.02434 0.00339 0.00026 0.00022 0.00020 0.00000 0.00142 0.00125 0.00127 0.00106 0.00109 0.00108 0.00055 H3 0.80957 0.49245 -0.17639 1.00000 0.02921 0.00000 0.00000 C4 0.62926 0.44460 -0.12234 1.00000 0.02752 0.02580 0.02276 -0.00801 -0.00879 -0.00407 0.02522 0.00350 0.00026 0.00022 0.00021 0.00000 0.00144 0.00130 0.00129 0.00108 0.00111 0.00112 0.00056 H4 0.60444 0.49202 -0.18752 1.00000 0.03026 0.00000 0.00000 C5 0.54514 0.37250 -0.03066 1.00000 0.02407 0.01892 0.02294 -0.01095 -0.00745 -0.00033 0.02116 0.00327 0.00024 0.00020 0.00020 0.00000 0.00134 0.00114 0.00125 0.00102 0.00106 0.00101 0.00052 C6 0.41692 0.36219 -0.03244 1.00000 0.02469 0.02454 0.02568 -0.00900 -0.00869 -0.00332 0.02471 0.00343 0.00025 0.00022 0.00021 0.00000 0.00138 0.00128 0.00134 0.00110 0.00111 0.00109 0.00056 N1 0.92236 0.27043 0.08706 1.00000 0.02065 0.02316 0.02328 -0.01171 -0.00765 -0.00424 0.02054 0.00261 0.00020 0.00017 0.00016 0.00000 0.00109 0.00104 0.00106 0.00089 0.00088 0.00086 0.00044 N2 0.98921 0.43358 -0.06999 1.00000 0.02735 0.02873 0.02856 -0.00054 -0.01386 -0.00966 0.02907 0.00296 0.00022 0.00019 0.00017 0.00000 0.00122 0.00115 0.00119 0.00097 0.00101 0.00098 0.00052 H2A 1.06558 0.42376 -0.06002 1.00000 0.03488 0.00000 0.00000 H2B 0.96949 0.49237 -0.12686 1.00000 0.03488 0.00000 0.00000 N3 0.69069 0.30777 0.06954 1.00000 0.02081 0.01928 0.02149 -0.01028 -0.00608 -0.00287 0.01950 0.00262 0.00019 0.00017 0.00016 0.00000 0.00110 0.00098 0.00104 0.00085 0.00087 0.00085 0.00044 N4 0.57408 0.30685 0.06385 1.00000 0.02134 0.02206 0.02413 -0.01241 -0.00669 -0.00297 0.02105 0.00269 0.00020 0.00017 0.00016 0.00000 0.00110 0.00103 0.00108 0.00089 0.00090 0.00086 0.00044 N5 0.33053 0.30790 0.06243 1.00000 0.02860 0.04729 0.02376 -0.00615 -0.00830 -0.01698 0.03317 0.00311 0.00022 0.00021 0.00018 0.00000 0.00128 0.00142 0.00117 0.00107 0.00101 0.00112 0.00056 H5A 0.25430 0.30052 0.06233 1.00000 0.03980 0.00000 0.00000 H5B 0.35015 0.27971 0.12467 1.00000 0.03980 0.00000 0.00000 N6 0.39925 0.40689 -0.12842 1.00000 0.02353 0.05069 0.02805 -0.00663 -0.01055 -0.00954 0.03529 0.00325 0.00022 0.00022 0.00018 0.00000 0.00124 0.00152 0.00124 0.00113 0.00102 0.00112 0.00058 O1 1.04328 0.26468 0.10077 1.00000 0.02333 0.02437 0.02779 -0.00925 -0.01159 -0.00449 0.02381 0.00223 0.00017 0.00015 0.00014 0.00000 0.00095 0.00088 0.00094 0.00079 0.00077 0.00075 0.00039 H1 1.07743 0.19487 0.12212 1.00000 0.03571 0.00000 0.00000 O2 0.27615 0.38508 -0.11840 1.00000 0.02998 0.07458 0.02989 -0.00638 -0.01348 -0.01942 0.04572 0.00289 0.00020 0.00021 0.00016 0.00000 0.00114 0.00161 0.00109 0.00108 0.00093 0.00110 0.00058 H2 0.25966 0.42164 -0.17897 1.00000 0.06857 0.00000 0.00000 C11 0.89822 -0.04940 0.28283 1.00000 0.02331 0.02221 0.01939 -0.00812 -0.00516 -0.00583 0.02123 0.00326 0.00024 0.00021 0.00019 0.00000 0.00132 0.00122 0.00120 0.00101 0.00103 0.00104 0.00052 C12 0.86510 -0.04581 0.18881 1.00000 0.02277 0.02335 0.02002 -0.00957 -0.00421 -0.00615 0.02145 0.00327 0.00024 0.00021 0.00019 0.00000 0.00132 0.00123 0.00121 0.00103 0.00103 0.00104 0.00052 C13 0.88530 -0.14124 0.16033 1.00000 0.03312 0.01888 0.02358 -0.00841 -0.01031 -0.00261 0.02457 0.00339 0.00026 0.00021 0.00020 0.00000 0.00150 0.00118 0.00128 0.00104 0.00114 0.00108 0.00056 H13 0.91909 -0.21646 0.20315 1.00000 0.02948 0.00000 0.00000 C14 0.85470 -0.12272 0.06847 1.00000 0.03370 0.02320 0.02617 -0.01349 -0.00731 -0.00472 0.02630 0.00350 0.00026 0.00022 0.00021 0.00000 0.00153 0.00126 0.00134 0.00110 0.00117 0.00114 0.00058 H14 0.86434 -0.18520 0.04664 1.00000 0.03156 0.00000 0.00000 C15 0.80868 -0.00868 0.00758 1.00000 0.02314 0.02456 0.02326 -0.01172 -0.00621 -0.00428 0.02254 0.00332 0.00025 0.00021 0.00020 0.00000 0.00133 0.00125 0.00126 0.00106 0.00106 0.00106 0.00053 C16 0.78172 0.02611 -0.09819 1.00000 0.02949 0.02608 0.02470 -0.01119 -0.00980 -0.00323 0.02563 0.00348 0.00026 0.00022 0.00021 0.00000 0.00146 0.00130 0.00132 0.00111 0.00114 0.00113 0.00057 N11 0.86525 0.04931 0.29671 1.00000 0.02536 0.02334 0.01839 -0.01148 -0.00656 -0.00399 0.02074 0.00264 0.00020 0.00017 0.00016 0.00000 0.00114 0.00104 0.00101 0.00086 0.00088 0.00088 0.00044 N12 0.95963 -0.14546 0.34215 1.00000 0.03995 0.02303 0.02688 -0.01246 -0.01713 0.00009 0.02741 0.00289 0.00022 0.00018 0.00017 0.00000 0.00137 0.00109 0.00115 0.00095 0.00104 0.00099 0.00050 H12A 0.98151 -0.14592 0.39604 1.00000 0.03289 0.00000 0.00000 H12B 0.97852 -0.20877 0.32765 1.00000 0.03289 0.00000 0.00000 N13 0.81308 0.05897 0.13155 1.00000 0.02114 0.02077 0.01899 -0.00911 -0.00500 -0.00375 0.01973 0.00265 0.00020 0.00017 0.00016 0.00000 0.00109 0.00101 0.00101 0.00084 0.00086 0.00085 0.00043 N14 0.78518 0.07927 0.04058 1.00000 0.02529 0.02194 0.02133 -0.01089 -0.00665 -0.00379 0.02169 0.00268 0.00020 0.00017 0.00016 0.00000 0.00115 0.00103 0.00105 0.00088 0.00090 0.00089 0.00045 N15 0.71512 0.13194 -0.13715 1.00000 0.05520 0.03356 0.03575 -0.02195 -0.02696 0.01352 0.03807 0.00332 0.00025 0.00020 0.00020 0.00000 0.00167 0.00129 0.00132 0.00112 0.00125 0.00119 0.00062 H15A 0.69877 0.15599 -0.20027 1.00000 0.04569 0.00000 0.00000 H15B 0.68788 0.17718 -0.09953 1.00000 0.04569 0.00000 0.00000 N16 0.82599 -0.04695 -0.14663 1.00000 0.03117 0.02893 0.02163 -0.01270 -0.01212 -0.00265 0.02494 0.00277 0.00022 0.00019 0.00017 0.00000 0.00125 0.00113 0.00107 0.00093 0.00095 0.00096 0.00048 O11 0.91326 0.04376 0.37841 1.00000 0.03008 0.02960 0.02340 -0.01596 -0.01123 -0.00185 0.02479 0.00222 0.00017 0.00015 0.00014 0.00000 0.00102 0.00096 0.00092 0.00078 0.00080 0.00080 0.00040 H11 0.85710 0.07876 0.41694 1.00000 0.03718 0.00000 0.00000 O12 0.79350 0.00209 -0.24593 1.00000 0.04265 0.03275 0.02557 -0.01661 -0.01822 0.00228 0.03051 0.00243 0.00019 0.00016 0.00014 0.00000 0.00119 0.00102 0.00096 0.00083 0.00090 0.00089 0.00044 H12 0.82594 -0.04344 -0.27951 1.00000 0.04577 0.00000 0.00000 C21 0.58890 0.28681 0.35054 1.00000 0.02416 0.01974 0.01777 -0.00760 -0.00714 -0.00310 0.01998 0.00319 0.00024 0.00020 0.00019 0.00000 0.00134 0.00117 0.00117 0.00099 0.00104 0.00101 0.00052 C22 0.52078 0.19430 0.36377 1.00000 0.02389 0.01923 0.01866 -0.00825 -0.00927 -0.00126 0.01956 0.00316 0.00024 0.00020 0.00019 0.00000 0.00133 0.00115 0.00119 0.00098 0.00104 0.00101 0.00051 C23 0.39853 0.17013 0.43598 1.00000 0.02346 0.02246 0.02301 -0.01260 -0.00694 -0.00039 0.02196 0.00329 0.00024 0.00021 0.00020 0.00000 0.00135 0.00122 0.00125 0.00104 0.00106 0.00104 0.00053 H23 0.34926 0.21620 0.47801 1.00000 0.02635 0.00000 0.00000 C24 0.35104 0.07744 0.44474 1.00000 0.02487 0.02160 0.02103 -0.00728 -0.00782 -0.00376 0.02228 0.00332 0.00025 0.00021 0.00020 0.00000 0.00135 0.00121 0.00123 0.00102 0.00106 0.00104 0.00053 H24 0.26698 0.05820 0.49179 1.00000 0.02674 0.00000 0.00000 C25 0.43073 0.01216 0.38194 1.00000 0.02203 0.01956 0.02007 -0.00701 -0.00804 -0.00353 0.01997 0.00320 0.00024 0.00020 0.00019 0.00000 0.00130 0.00116 0.00120 0.00099 0.00104 0.00100 0.00051 C26 0.39235 -0.09365 0.38974 1.00000 0.02517 0.01807 0.02222 -0.00716 -0.00923 -0.00380 0.02105 0.00323 0.00025 0.00020 0.00019 0.00000 0.00136 0.00115 0.00125 0.00101 0.00108 0.00103 0.00052 N21 0.70710 0.28708 0.28718 1.00000 0.02248 0.01904 0.02340 -0.00993 -0.00613 -0.00626 0.02029 0.00262 0.00020 0.00017 0.00016 0.00000 0.00111 0.00098 0.00106 0.00086 0.00090 0.00085 0.00044 N22 0.52828 0.35989 0.40212 1.00000 0.02529 0.02484 0.03281 -0.01921 -0.00174 -0.00602 0.02594 0.00285 0.00021 0.00018 0.00017 0.00000 0.00118 0.00108 0.00119 0.00097 0.00096 0.00092 0.00048 H22A 0.56920 0.41414 0.39431 1.00000 0.03112 0.00000 0.00000 H22B 0.44732 0.35392 0.44401 1.00000 0.03112 0.00000 0.00000 N23 0.58976 0.13274 0.30136 1.00000 0.02484 0.01726 0.01967 -0.00829 -0.00721 -0.00452 0.01947 0.00260 0.00020 0.00016 0.00016 0.00000 0.00113 0.00096 0.00101 0.00083 0.00087 0.00085 0.00043 N24 0.54603 0.04042 0.31039 1.00000 0.02662 0.01865 0.02015 -0.00834 -0.00714 -0.00463 0.02095 0.00267 0.00020 0.00017 0.00016 0.00000 0.00117 0.00099 0.00103 0.00085 0.00090 0.00088 0.00045 N25 0.47436 -0.14998 0.32482 1.00000 0.02932 0.02607 0.03644 -0.01958 0.00002 -0.00988 0.02923 0.00296 0.00022 0.00019 0.00018 0.00000 0.00125 0.00113 0.00126 0.00102 0.00103 0.00098 0.00051 H25A 0.45536 -0.21448 0.32957 1.00000 0.03508 0.00000 0.00000 H25B 0.54688 -0.12224 0.27769 1.00000 0.03508 0.00000 0.00000 N26 0.28357 -0.12624 0.46162 1.00000 0.03107 0.01842 0.02609 -0.00952 -0.00953 -0.00769 0.02340 0.00269 0.00021 0.00017 0.00017 0.00000 0.00125 0.00100 0.00113 0.00090 0.00098 0.00092 0.00047 O21 0.76544 0.37650 0.27853 1.00000 0.02438 0.02418 0.03842 -0.01663 -0.00592 -0.00943 0.02678 0.00225 0.00017 0.00014 0.00015 0.00000 0.00097 0.00091 0.00105 0.00083 0.00088 0.00077 0.00041 H21 0.84544 0.35486 0.27100 1.00000 0.04017 0.00000 0.00000 O22 0.26497 -0.22925 0.45893 1.00000 0.03350 0.02397 0.03643 -0.01504 -0.00472 -0.01345 0.02947 0.00238 0.00019 0.00015 0.00015 0.00000 0.00109 0.00091 0.00109 0.00084 0.00087 0.00082 0.00042 H22 0.19149 -0.24812 0.50115 1.00000 0.04420 0.00000 0.00000 O31 1.02213 0.35912 0.26522 1.00000 0.03214 0.02761 0.02681 -0.00558 -0.01326 -0.00641 0.02865 0.00240 0.00018 0.00015 0.00014 0.00000 0.00105 0.00094 0.00095 0.00079 0.00082 0.00081 0.00042 O32 1.00134 0.21112 0.44040 1.00000 0.03135 0.03192 0.02192 -0.00777 -0.00445 -0.00708 0.02969 0.00247 0.00018 0.00016 0.00014 0.00000 0.00106 0.00099 0.00092 0.00079 0.00080 0.00083 0.00043 O33 1.18177 0.19538 0.29365 1.00000 0.03197 0.02989 0.02815 -0.01570 -0.00647 -0.00060 0.02965 0.00249 0.00018 0.00016 0.00014 0.00000 0.00106 0.00096 0.00097 0.00082 0.00083 0.00082 0.00042 O34 1.16317 0.33505 0.36384 1.00000 0.03757 0.02944 0.04684 -0.01672 -0.02293 -0.00429 0.03378 0.00240 0.00019 0.00016 0.00016 0.00000 0.00114 0.00098 0.00118 0.00090 0.00097 0.00087 0.00046 Cl31 1.09283 0.27544 0.34115 1.00000 0.02572 0.02188 0.02176 -0.00823 -0.00820 -0.00422 0.02248 0.00079 0.00006 0.00005 0.00005 0.00000 0.00033 0.00029 0.00030 0.00024 0.00025 0.00025 0.00014 O35 0.64589 0.51277 0.44896 1.00000 0.04292 0.04721 0.05274 -0.03305 0.00707 -0.02032 0.04553 0.00284 0.00021 0.00019 0.00018 0.00000 0.00129 0.00125 0.00134 0.00111 0.00105 0.00104 0.00056 O36 0.81431 0.59024 0.28698 1.00000 0.05567 0.03877 0.02706 -0.01456 -0.00596 -0.01824 0.03891 0.00266 0.00021 0.00017 0.00015 0.00000 0.00138 0.00112 0.00102 0.00089 0.00096 0.00101 0.00050 O37 0.86097 0.47961 0.45387 1.00000 0.06781 0.05566 0.05021 -0.01478 -0.03029 0.01030 0.05984 0.00357 0.00026 0.00021 0.00019 0.00000 0.00171 0.00148 0.00142 0.00121 0.00131 0.00129 0.00069 O38 0.74273 0.66733 0.42282 1.00000 0.04266 0.04329 0.05442 -0.03839 0.00176 -0.01505 0.04200 0.00263 0.00020 0.00018 0.00018 0.00000 0.00126 0.00119 0.00131 0.00108 0.00104 0.00100 0.00053 Cl35 0.76542 0.56269 0.40252 1.00000 0.03346 0.02746 0.02830 -0.01692 -0.00456 -0.00612 0.02819 0.00086 0.00007 0.00005 0.00005 0.00000 0.00037 0.00032 0.00034 0.00027 0.00028 0.00028 0.00016 O1W 1.08880 0.63568 0.31597 1.00000 0.05287 0.04414 0.05105 -0.02740 -0.02378 0.00644 0.04585 0.00351 0.00027 0.00021 0.00020 0.00000 0.00157 0.00139 0.00150 0.00125 0.00133 0.00125 0.00057 H1WA 1.04559 0.58325 0.36427 1.00000 0.07135 0.04447 0.00311 0.00280 0.00259 0.00000 0.01497 H1WB 1.15238 0.63401 0.33328 1.00000 0.06272 0.03266 0.00254 0.00314 0.00282 0.00000 0.01307 O2W 0.61350 0.34967 0.69386 1.00000 0.06416 0.03567 0.02983 -0.01463 -0.01119 0.00412 0.04543 0.00335 0.00025 0.00019 0.00018 0.00000 0.00169 0.00119 0.00120 0.00105 0.00115 0.00112 0.00058 H2WA 0.61937 0.38582 0.62793 1.00000 0.07483 0.05280 0.00359 0.00315 0.00148 0.00000 0.01370 H2WB 0.54489 0.37930 0.72861 1.00000 0.07478 0.05519 0.00271 0.00328 0.00247 0.00000 0.01401 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 518 Maximum vector length = 511 Memory required = 5713 / 25039 wR2 = 0.1079 before cycle 11 for 7687 data and 0 / 518 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.018; Restrained GooF = 1.018 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0448 for 5825 Fo > 4sig(Fo) and 0.0702 for all 7687 data wR2 = 0.1079, GooF = S = 1.018, Restrained GooF = 1.018 for all data Occupancy sum of asymmetric unit = 55.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0229 0.0194 0.0147 Ni1 0.0252 0.0218 0.0149 C1 0.0245 0.0222 0.0150 C2 0.0299 0.0223 0.0209 C3 0.0282 0.0258 0.0216 C4 0.0256 0.0225 0.0155 C5 0.0267 0.0245 0.0229 C6 0.0253 0.0222 0.0141 N1 0.0462 0.0214 0.0197 N2 0.0225 0.0208 0.0152 N3 0.0259 0.0214 0.0158 N4 0.0559 0.0234 0.0202 N5 0.0588 0.0278 0.0193 N6 0.0301 0.0246 0.0168 O1 0.0873 0.0306 0.0193 O2 0.0255 0.0196 0.0187 C11 0.0265 0.0196 0.0182 C12 0.0333 0.0222 0.0182 C13 0.0346 0.0277 0.0166 C14 0.0264 0.0229 0.0183 C15 0.0299 0.0264 0.0207 C16 0.0258 0.0237 0.0127 N11 0.0425 0.0233 0.0164 N12 0.0225 0.0200 0.0167 N13 0.0256 0.0234 0.0161 N14 0.0697 0.0251 0.0194 N15 0.0326 0.0285 0.0137 N16 0.0334 0.0283 0.0126 O11 0.0479 0.0299 0.0138 O12 0.0242 0.0197 0.0161 C21 0.0250 0.0190 0.0147 C22 0.0265 0.0230 0.0163 C23 0.0252 0.0214 0.0202 C24 0.0232 0.0194 0.0173 C25 0.0263 0.0200 0.0169 C26 0.0250 0.0229 0.0130 N21 0.0405 0.0233 0.0140 N22 0.0251 0.0198 0.0136 N23 0.0268 0.0203 0.0157 N24 0.0477 0.0249 0.0152 N25 0.0322 0.0255 0.0126 N26 0.0409 0.0274 0.0120 O21 0.0439 0.0323 0.0123 O22 0.0374 0.0265 0.0221 O31 0.0344 0.0332 0.0215 O32 0.0356 0.0322 0.0212 O33 0.0516 0.0313 0.0185 O34 0.0262 0.0218 0.0195 Cl31 0.0806 0.0311 0.0249 O35 0.0622 0.0309 0.0237 O36 0.0851 0.0601 0.0343 O37 0.0764 0.0360 0.0136 O38 0.0384 0.0292 0.0170 Cl35 0.0659 0.0398 0.0319 O1W 0.0748 0.0338 0.0277 O2W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.021 0.031 0.042 0.054 0.068 0.086 0.111 0.155 1.000 Number in group 802. 776. 758. 777. 757. 759. 761. 772. 763. 762. GooF 1.023 1.050 0.984 1.039 1.011 1.053 1.015 0.994 1.015 0.995 K 4.353 1.614 1.148 1.049 0.998 0.991 0.983 0.991 1.013 1.022 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 773. 776. 762. 769. 764. 767. 777. 766. 765. 768. GooF 0.999 0.944 0.945 0.838 0.888 0.967 0.955 0.990 1.060 1.466 K 1.066 1.060 1.058 1.032 1.021 1.016 1.011 1.008 1.019 1.013 R1 0.229 0.163 0.129 0.081 0.072 0.059 0.049 0.037 0.032 0.033 Recommended weighting scheme: WGHT 0.0545 0.8560 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 3 7 49.17 18.80 4.80 0.017 1.98 5 4 5 716.00 521.35 4.69 0.089 1.96 -5 -5 3 43.14 0.51 4.52 0.003 1.31 -3 6 2 308.06 438.18 4.48 0.082 1.61 2 5 4 2047.88 1585.58 4.36 0.156 2.44 5 5 4 114.99 62.78 4.26 0.031 1.89 5 2 3 1836.21 1430.92 4.18 0.148 2.21 4 -13 2 152.06 1.72 4.07 0.005 0.77 8 -3 13 24.69 164.52 3.87 0.050 0.79 -3 -2 4 80.04 43.04 3.86 0.026 1.80 4 3 6 388.17 291.09 3.80 0.067 2.10 5 1 3 221.37 311.13 3.78 0.069 2.19 0 16 6 216.03 104.36 3.70 0.040 0.77 -3 1 0 424.10 324.87 3.68 0.071 3.17 3 7 3 341.36 255.51 3.59 0.063 1.78 6 2 3 36.67 11.56 3.56 0.013 1.86 -4 2 1 6.02 25.32 3.55 0.020 2.16 8 -2 1 42.45 97.59 3.52 0.039 1.24 3 4 4 74.56 41.52 3.42 0.025 2.62 -3 -5 2 154.01 214.46 3.39 0.057 1.69 2 -2 3 41.40 70.80 3.38 0.033 2.65 6 5 6 4037.55 3319.29 3.38 0.225 1.62 1 0 4 810.97 1011.26 3.37 0.124 3.18 2 4 0 271.39 205.55 3.35 0.056 2.65 3 2 8 1287.90 1050.90 3.35 0.127 1.72 4 4 7 1038.02 837.08 3.35 0.113 1.87 3 4 0 1653.40 1349.92 3.34 0.144 2.35 3 1 8 826.47 1028.58 3.34 0.125 1.66 3 6 4 3769.94 3120.50 3.34 0.219 2.04 1 6 3 22.10 6.68 3.33 0.010 2.14 3 -1 2 302.63 392.88 3.32 0.078 3.02 4 -1 5 48.76 26.90 3.31 0.020 1.92 5 2 4 155.84 110.83 3.27 0.041 2.14 1 3 5 1062.96 1307.70 3.26 0.142 2.72 -4 -4 2 643.36 805.70 3.25 0.111 1.70 -8 -5 1 78.28 15.86 3.23 0.016 1.13 5 5 6 557.49 441.94 3.22 0.082 1.79 -3 -1 14 164.25 0.26 3.20 0.002 0.77 2 3 8 273.45 353.34 3.18 0.074 1.77 4 2 7 665.08 538.27 3.17 0.091 1.86 -8 -1 3 118.89 175.85 3.12 0.052 1.13 -2 -2 3 447.45 558.94 3.10 0.093 2.35 1 -3 2 727.46 591.57 3.08 0.095 2.72 -1 3 4 249.24 192.40 3.08 0.054 2.62 13 2 3 64.09 171.84 3.07 0.051 0.84 -6 -3 4 95.87 140.10 3.07 0.046 1.24 3 -3 5 240.41 317.28 3.04 0.070 1.68 -4 -2 4 1095.99 1345.59 3.03 0.144 1.60 -8 -9 3 112.74 3.85 3.02 0.008 0.85 1 -1 4 118.88 85.62 3.02 0.036 2.77 Bond lengths and angles Ni1 - Distance Angles N1 2.0338 (0.0021) N11 2.0406 (0.0020) 98.15 (0.08) N21 2.0451 (0.0020) 95.29 (0.08) 97.27 (0.08) N23 2.0637 (0.0021) 168.08 (0.08) 91.97 (0.08) 77.09 (0.08) N13 2.0703 (0.0020) 93.98 (0.08) 76.88 (0.08) 169.68 (0.08) 94.46 (0.08) N3 2.0957 (0.0020) 77.27 (0.08) 167.55 (0.08) 94.69 (0.08) 94.05 (0.08) 91.78 (0.08) Ni1 - N1 N11 N21 N23 N13 C1 - Distance Angles N1 1.2974 (0.0030) N2 1.3256 (0.0032) 125.30 (0.23) C2 1.4842 (0.0035) 114.25 (0.21) 120.43 (0.21) C1 - N1 N2 C2 - Distance Angles N3 1.3386 (0.0031) C3 1.3926 (0.0034) 122.41 (0.23) C1 1.4842 (0.0035) 114.08 (0.21) 123.46 (0.22) C2 - N3 C3 C3 - Distance Angles C4 1.3650 (0.0037) C2 1.3926 (0.0034) 117.06 (0.24) H3 0.9500 121.47 121.47 C3 - C4 C2 C4 - Distance Angles C3 1.3650 (0.0037) C5 1.3922 (0.0035) 118.16 (0.24) H4 0.9500 120.92 120.92 C4 - C3 C5 C5 - Distance Angles N4 1.3364 (0.0031) C4 1.3922 (0.0035) 123.12 (0.23) C6 1.4798 (0.0036) 115.25 (0.21) 121.62 (0.22) C5 - N4 C4 C6 - Distance Angles N6 1.2907 (0.0032) N5 1.3433 (0.0033) 125.60 (0.25) C5 1.4798 (0.0036) 115.23 (0.23) 119.16 (0.22) C6 - N6 N5 N1 - Distance Angles C1 1.2974 (0.0030) O1 1.4084 (0.0026) 111.23 (0.19) Ni1 2.0338 (0.0021) 118.30 (0.17) 128.82 (0.14) N1 - C1 O1 N2 - Distance Angles C1 1.3256 (0.0032) H2A 0.8800 120.00 H2B 0.8800 120.00 120.00 N2 - C1 H2A N3 - Distance Angles N4 1.3342 (0.0028) C2 1.3386 (0.0031) 120.80 (0.20) Ni1 2.0957 (0.0020) 123.27 (0.15) 114.73 (0.16) N3 - N4 C2 N4 - Distance Angles N3 1.3342 (0.0028) C5 1.3364 (0.0031) 118.41 (0.20) N4 - N3 N5 - Distance Angles C6 1.3433 (0.0033) H5A 0.8800 120.00 H5B 0.8800 120.00 120.00 N5 - C6 H5A N6 - Distance Angles C6 1.2907 (0.0032) O2 1.4172 (0.0029) 109.07 (0.21) N6 - C6 O1 - Distance Angles N1 1.4084 (0.0026) H1 0.8400 109.47 O1 - N1 O2 - Distance Angles N6 1.4172 (0.0029) H2 0.8400 109.47 O2 - N6 C11 - Distance Angles N11 1.3057 (0.0031) N12 1.3254 (0.0031) 125.41 (0.23) C12 1.4869 (0.0034) 113.90 (0.21) 120.65 (0.22) C11 - N11 N12 C12 - Distance Angles N13 1.3326 (0.0031) C13 1.3943 (0.0034) 121.47 (0.22) C11 1.4869 (0.0034) 113.87 (0.21) 124.66 (0.22) C12 - N13 C13 C13 - Distance Angles C14 1.3698 (0.0035) C12 1.3943 (0.0034) 117.66 (0.23) H13 0.9500 121.17 121.17 C13 - C14 C12 C14 - Distance Angles C13 1.3698 (0.0035) C15 1.4031 (0.0035) 117.99 (0.23) H14 0.9500 121.01 121.01 C14 - C13 C15 C15 - Distance Angles N14 1.3365 (0.0031) C14 1.4031 (0.0035) 122.28 (0.22) C16 1.4845 (0.0035) 113.77 (0.21) 123.95 (0.23) C15 - N14 C14 C16 - Distance Angles N16 1.2917 (0.0033) N15 1.3443 (0.0033) 125.01 (0.24) C15 1.4845 (0.0035) 117.43 (0.22) 117.55 (0.23) C16 - N16 N15 N11 - Distance Angles C11 1.3057 (0.0031) O11 1.4117 (0.0025) 110.79 (0.19) Ni1 2.0406 (0.0020) 118.49 (0.16) 130.59 (0.14) N11 - C11 O11 N12 - Distance Angles C11 1.3254 (0.0031) H12A 0.8800 120.00 H12B 0.8800 120.00 120.00 N12 - C11 H12A N13 - Distance Angles C12 1.3326 (0.0031) N14 1.3343 (0.0027) 121.66 (0.20) Ni1 2.0703 (0.0020) 116.21 (0.16) 122.02 (0.15) N13 - C12 N14 N14 - Distance Angles N13 1.3343 (0.0027) C15 1.3365 (0.0031) 118.69 (0.20) N14 - N13 N15 - Distance Angles C16 1.3443 (0.0033) H15A 0.8800 120.00 H15B 0.8800 120.00 120.00 N15 - C16 H15A N16 - Distance Angles C16 1.2917 (0.0033) O12 1.4065 (0.0025) 109.15 (0.20) N16 - C16 O11 - Distance Angles N11 1.4117 (0.0025) H11 0.8400 109.47 O11 - N11 O12 - Distance Angles N16 1.4065 (0.0025) H12 0.8400 109.47 O12 - N16 C21 - Distance Angles N21 1.2918 (0.0031) N22 1.3325 (0.0031) 125.59 (0.23) C22 1.4886 (0.0034) 114.01 (0.21) 120.40 (0.22) C21 - N21 N22 C22 - Distance Angles N23 1.3376 (0.0030) C23 1.3858 (0.0034) 121.94 (0.22) C21 1.4886 (0.0034) 113.98 (0.21) 124.05 (0.22) C22 - N23 C23 C23 - Distance Angles C24 1.3718 (0.0035) C22 1.3858 (0.0034) 117.76 (0.23) H23 0.9500 121.12 121.12 C23 - C24 C22 C24 - Distance Angles C23 1.3718 (0.0035) C25 1.4003 (0.0034) 117.71 (0.23) H24 0.9500 121.15 121.15 C24 - C23 C25 C25 - Distance Angles N24 1.3335 (0.0031) C24 1.4003 (0.0034) 122.85 (0.22) C26 1.4828 (0.0033) 114.92 (0.21) 122.23 (0.22) C25 - N24 C24 C26 - Distance Angles N26 1.2926 (0.0032) N25 1.3484 (0.0032) 125.33 (0.23) C25 1.4828 (0.0033) 116.50 (0.21) 118.13 (0.22) C26 - N26 N25 N21 - Distance Angles C21 1.2918 (0.0031) O21 1.4086 (0.0025) 110.92 (0.19) Ni1 2.0451 (0.0020) 118.04 (0.16) 129.98 (0.15) N21 - C21 O21 N22 - Distance Angles C21 1.3325 (0.0031) H22A 0.8800 120.00 H22B 0.8800 120.00 120.00 N22 - C21 H22A N23 - Distance Angles C22 1.3376 (0.0030) N24 1.3416 (0.0027) 121.06 (0.20) Ni1 2.0637 (0.0021) 115.86 (0.16) 123.04 (0.15) N23 - C22 N24 N24 - Distance Angles C25 1.3335 (0.0031) N23 1.3416 (0.0027) 118.52 (0.20) N24 - C25 N25 - Distance Angles C26 1.3484 (0.0032) H25A 0.8800 120.00 H25B 0.8800 120.00 120.00 N25 - C26 H25A N26 - Distance Angles C26 1.2926 (0.0032) O22 1.4152 (0.0025) 108.40 (0.19) N26 - C26 O21 - Distance Angles N21 1.4086 (0.0025) H21 0.8400 109.47 O21 - N21 O22 - Distance Angles N26 1.4152 (0.0025) H22 0.8400 109.47 O22 - N26 O31 - Distance Angles Cl31 1.4438 (0.0018) O31 - O32 - Distance Angles Cl31 1.4410 (0.0018) O32 - O33 - Distance Angles Cl31 1.4377 (0.0018) O33 - O34 - Distance Angles Cl31 1.4259 (0.0019) O34 - Cl31 - Distance Angles O34 1.4259 (0.0019) O33 1.4377 (0.0018) 109.80 (0.12) O32 1.4410 (0.0018) 110.68 (0.11) 108.78 (0.11) O31 1.4438 (0.0018) 109.44 (0.11) 109.40 (0.11) 108.72 (0.11) Cl31 - O34 O33 O32 O35 - Distance Angles Cl35 1.4364 (0.0022) O35 - O36 - Distance Angles Cl35 1.4276 (0.0020) O36 - O37 - Distance Angles Cl35 1.4416 (0.0023) O37 - O38 - Distance Angles Cl35 1.4376 (0.0019) O38 - Cl35 - Distance Angles O36 1.4276 (0.0020) O35 1.4364 (0.0022) 111.50 (0.13) O38 1.4376 (0.0019) 109.13 (0.12) 109.04 (0.12) O37 1.4416 (0.0023) 108.62 (0.14) 108.75 (0.15) 109.78 (0.15) Cl35 - O36 O35 O38 O1W - Distance Angles H1WA 0.8258 (0.0175) H1WB 0.8230 (0.0175) 109.70 (2.62) O1W - H1WA O2W - Distance Angles H2WA 0.8259 (0.0178) H2WB 0.8386 (0.0177) 107.02 (2.59) O2W - H2WA Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.18 2.960(3) 148.1 N2-H2A...O2_$1 0.88 2.04 2.893(3) 162.3 N2-H2B...O31_$2 0.88 2.34 3.203(3) 168.4 N5-H5A...O1_$3 0.88 2.44 2.949(3) 117.6 N5-H5B...O33_$3 0.84 1.87 2.701(3) 170.4 O1-H1...N16_$4 0.84 2.06 2.784(3) 144.0 O2-H2...O36_$5 0.84 2.34 2.944(3) 128.7 O2-H2...O21_$5 0.88 2.15 2.981(3) 156.5 N12-H12A...O32_$6 0.88 2.09 2.914(3) 155.8 N12-H12B...O1W_$7 0.88 2.42 3.042(3) 128.0 N15-H15A...O2W_$8 0.84 2.05 2.877(3) 166.8 O11-H11...N26_$9 0.84 2.08 2.828(3) 148.2 O12-H12...O33_$4 0.88 2.24 3.111(3) 168.7 N22-H22B...O38_$10 0.88 2.55 3.037(3) 115.8 N22-H22B...O35_$10 0.88 2.27 3.129(3) 165.6 N25-H25A...O2W_$9 0.84 1.95 2.749(3) 157.5 O21-H21...O31 0.84 2.00 2.774(3) 152.1 O22-H22...O32_$9 0.826(18) 2.38(2) 3.153(4) 155(3) O1W-H1WA...O37 0.823(17) 2.55(2) 3.321(4) 157(3) O1W-H1WB...O2W_$11 0.826(18) 2.29(2) 3.107(3) 169(4) O2W-H2WA...O35 0.839(18) 2.18(2) 2.973(3) 157(3) O2W-H2WB...N6_$12 FMAP and GRID set by program FMAP 2 2 69 GRID -1.515 -1 -2 1.515 1 2 R1 = 0.0672 for 7687 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.68 at 0.6197 0.5729 0.3789 [ 1.04 A from O35 ] Deepest hole -0.52 at 0.8190 0.2244 0.1825 [ 0.78 A from NI1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 5456 / 62220 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6197 0.5729 0.3789 1.00000 0.05 0.68 1.04 O35 1.74 CL35 2.09 O36 2.16 H22A Q2 1 0.7671 0.4817 0.4882 1.00000 0.05 0.55 0.98 O37 1.21 CL35 1.53 O35 2.13 O38 Q3 1 0.8016 0.1076 0.2693 1.00000 0.05 0.41 0.94 N11 1.17 NI1 1.98 C11 2.09 O11 Q4 1 0.8406 0.1209 0.2227 1.00000 0.05 0.38 1.03 NI1 1.12 N11 1.93 N13 1.99 C11 Q5 1 0.7005 0.1824 0.2661 1.00000 0.05 0.38 0.98 NI1 1.37 N23 1.53 N21 1.98 C22 Shortest distances between peaks (including symmetry equivalents) 3 4 0.62 3 5 1.27 4 5 1.58 1 2 2.39 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.02: 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. 2.58: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.06: Set up l.s. refinement 0.00: Generate idealized H-atoms 11.63: Structure factors and derivatives 47.27: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.08: Apply other restraints 5.64: Solve l.s. equations 0.00: Generate HTAB table 0.08: Other dependent quantities, CIF, tables 0.19: Analysis of variance 0.08: Merge reflections for Fourier and .fcf 0.22: Fourier summations 0.09: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 09:40:40 Total CPU time: 68.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++