+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - MSDOS 32-BIT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-1 + + TETRA started at 22:14:42 on 03-Jun-1998 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL Tetracycline Hydrochloride C22H25ClN2O8 P212121 Z=4 CELL 1.5406 10.980703 12.852671 15.733348 90.0 90.0 90.0 ZERR 4 0.001 0.001 0.001 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC CL C O N H UNIT 4 88 32 8 100 V = 2220.47 F(000) = 1008.0 Mu = 1.98 mm-1 Cell Wt = 1923.56 Rho = 1.439 ACTA L.S. 4 BOND FMAP 2 PLAN 20 FVAR 8.22329 CL1 1 0.07234 0.91608 0.50764 11.00000 0.17856 Q3 2 -0.18039 1.12112 0.80706 11.00000 0.02351 Q4 2 -0.26764 1.15385 0.85419 11.00000 0.08126 Q5 2 -0.00369 0.92802 0.71956 11.00000 0.04397 Q6 2 -0.22500 0.86983 0.61890 11.00000 0.05902 Q7 2 -0.12183 0.80769 0.96100 11.00000 0.11717 Q8 2 -0.53416 0.66021 0.81352 11.00000 0.05444 Q9 2 -0.00823 0.79760 0.81028 11.00000 0.06404 Q10 2 -0.71159 1.07787 0.74253 11.00000 0.21592 Q11 2 -0.30863 0.78392 1.02666 11.00000 0.12237 Q12 2 -0.11519 0.80659 0.82223 11.00000 0.10119 Q13 2 -0.56103 0.93086 0.65232 11.00000 0.11728 Q14 2 -0.44820 0.71181 0.94512 11.00000 0.14464 Q15 2 -0.19561 0.94753 0.83490 11.00000 0.13493 Q18 2 -0.66304 0.76280 0.76384 11.00000 0.03955 Q19 2 0.08573 0.82467 0.69243 11.00000 0.10621 Q20 2 -0.11782 1.00639 0.66990 11.00000 0.05444 Q24 2 -0.18522 1.04802 0.71212 11.00000 0.10947 Q25 2 -0.83118 1.02029 0.87738 11.00000 0.13181 Q27 2 -0.60797 1.02287 0.64588 11.00000 0.05076 Q28 2 -0.33168 0.88256 1.01467 11.00000 0.13540 Q30 2 -0.22302 0.73236 0.93784 11.00000 0.08146 Q31 2 -0.39088 0.72680 0.73689 11.00000 0.10614 Q32 2 -0.12425 0.88414 0.90903 11.00000 0.08430 Q33 2 -0.25460 0.65331 0.58267 11.00000 0.07747 Q35 2 -0.46355 0.94464 0.59416 11.00000 0.13240 Q36 2 -0.24348 0.66312 0.79321 11.00000 0.06439 Q38 2 -0.28514 1.23112 0.90560 11.00000 0.06157 Q39 2 -0.59900 0.59550 0.77531 11.00000 0.23972 Q42 2 -0.05539 0.97510 0.74611 11.00000 0.05651 HKLF 3 Covalent radii and connectivity table for Tetracycline Hydrochloride C22H25ClN2O8 P212121 Z=4 CL 0.990 C 0.770 O 0.660 N 0.700 H 0.320 Cl1 - no bonds found Q3 - Q4 Q24 Q4 - Q3 Q38 Q5 - Q42 Q19 Q20 Q6 - no bonds found Q7 - Q32 Q30 Q8 - Q39 Q9 - Q12 Q10 - Q36_$2 Q27 Q11 - Q28 Q30 Q12 - Q9 Q32 Q15 Q13 - Q27 Q35 Q14 - no bonds found Q15 - Q32 Q12 Q18 - no bonds found Q19 - Q5 Q20 - Q24 Q42 Q5 Q24 - Q20 Q3 Q42 Q25 - no bonds found Q27 - Q13 Q10 Q28 - Q11 Q30 - Q7 Q11 Q31 - Q36 Q32 - Q7 Q15 Q12 Q33 - no bonds found Q35 - Q13 Q36 - Q10_$1 Q31 Q38 - Q4 Q39 - Q8 Q42 - Q5 Q20 Q24 Operators for generating equivalent atoms: $1 -x-1, y-1/2, -z+3/2 $2 -x-1, y+1/2, -z+3/2 699 Reflections read, of which 0 rejected 0 =< h =< 10, 0 =< k =< 12, 0 =< l =< 15, Max. 2-theta = 95.08 0 Systematic absence violations 0 Inconsistent equivalents 699 Unique reflections, of which 0 suppressed R(int) = 0.0000 R(sigma) = 0.2064 Friedel opposites not merged Maximum memory for data reduction = 1673 / 7749 ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. CL 4.00 4.00 C 88.00 116.00 O 32.00 0.00 N 8.00 0.00 H 100.00 0.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 1974 / 155302 wR2 = 0.7127 before cycle 1 for 699 data and 121 / 121 parameters GooF = S = 3.955; Restrained GooF = 3.955 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 7.89336 0.30230 -1.091 OSF Mean shift/esd = 0.429 Maximum = 2.368 for y Q10 Max. shift = 0.478 A for Q10 Max. dU = 0.034 for Q39 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1974 / 155302 wR2 = 0.6939 before cycle 2 for 699 data and 121 / 121 parameters GooF = S = 3.668; Restrained GooF = 3.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 8.19385 0.28882 1.040 OSF Mean shift/esd = 0.291 Maximum = 1.040 for OSF Max. shift = 0.163 A for Q39 Max. dU =-0.075 for Q39 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1974 / 155302 wR2 = 0.6819 before cycle 3 for 699 data and 121 / 121 parameters GooF = S = 3.601; Restrained GooF = 3.601 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 8.25093 0.27906 0.205 OSF Mean shift/esd = 0.252 Maximum = -0.895 for x Q32 Max. shift = 0.113 A for Q14 Max. dU = 0.048 for Q10 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1974 / 155302 wR2 = 0.6748 before cycle 4 for 699 data and 121 / 121 parameters GooF = S = 3.500; Restrained GooF = 3.500 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 8.25178 0.28042 0.003 OSF Mean shift/esd = 0.251 Maximum = -0.785 for U11 Q5 Max. shift = 0.121 A for Q35 Max. dU =-0.054 for Q39 Largest correlation matrix elements -0.633 x Q28 / x Q11 0.507 U11 Cl1 / OSF Tetracycline Hydrochloride C22H25ClN2O8 P212121 Z=4 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Cl1 0.07420 0.91797 0.50886 1.00000 0.18399 0.06470 0.00285 0.00298 0.00257 0.00000 0.01663 Q3 -0.17817 1.11685 0.80648 1.00000 0.02418 0.09598 0.00583 0.00382 0.00340 0.00000 0.01315 Q4 -0.27756 1.16319 0.84561 1.00000 0.07260 0.13789 0.00786 0.00637 0.00494 0.00000 0.02615 Q5 -0.00964 0.93437 0.72141 1.00000 0.02989 0.11906 0.00682 0.00544 0.00391 0.00000 0.01719 Q6 -0.23071 0.86127 0.62141 1.00000 0.05276 0.11335 0.00532 0.00524 0.00381 0.00000 0.01777 Q7 -0.11003 0.80557 0.95942 1.00000 0.13853 0.22309 0.01177 0.00995 0.00815 0.00000 0.04242 Q8 -0.53280 0.66492 0.81713 1.00000 0.03780 0.11487 0.00627 0.00481 0.00383 0.00000 0.01671 Q9 -0.00539 0.79459 0.81265 1.00000 0.07027 0.13710 0.00749 0.00616 0.00603 0.00000 0.02261 Q10 -0.71753 1.11514 0.73410 1.00000 0.24787 0.36995 0.01908 0.01600 0.01455 0.00000 0.10496 Q11 -0.31125 0.77810 1.02624 1.00000 0.20151 0.29442 0.01620 0.01194 0.01041 0.00000 0.05898 Q12 -0.12096 0.80113 0.81424 1.00000 0.09371 0.19563 0.00873 0.00894 0.00793 0.00000 0.03446 Q13 -0.55587 0.93253 0.64422 1.00000 0.09966 0.17971 0.00904 0.00889 0.00687 0.00000 0.03298 Q14 -0.42235 0.70260 0.93597 1.00000 0.17520 0.26008 0.01323 0.01139 0.00878 0.00000 0.05372 Q15 -0.19244 0.93275 0.83215 1.00000 0.13181 0.20961 0.01085 0.00850 0.00748 0.00000 0.03638 Q18 -0.66912 0.75982 0.76089 1.00000 0.03500 0.10697 0.00642 0.00387 0.00374 0.00000 0.01494 Q19 0.07299 0.82383 0.68815 1.00000 0.10655 0.18021 0.00823 0.00896 0.00690 0.00000 0.03439 Q20 -0.12248 1.00279 0.67072 1.00000 0.07822 0.12056 0.00670 0.00528 0.00479 0.00000 0.02407 Q24 -0.18519 1.04682 0.70853 1.00000 0.11379 0.17694 0.01009 0.00838 0.00688 0.00000 0.03340 Q25 -0.83406 1.01995 0.87378 1.00000 0.07804 0.14162 0.00769 0.00606 0.00540 0.00000 0.02607 Q27 -0.60991 1.02955 0.65065 1.00000 0.04370 0.11823 0.00618 0.00527 0.00415 0.00000 0.01794 Q28 -0.32851 0.87421 1.01441 1.00000 0.12716 0.22850 0.01386 0.00921 0.00825 0.00000 0.04487 Q30 -0.23052 0.73451 0.93230 1.00000 0.09423 0.15906 0.00885 0.00718 0.00538 0.00000 0.02680 Q31 -0.37623 0.73282 0.74113 1.00000 0.10793 0.21649 0.01056 0.00948 0.00816 0.00000 0.04183 Q32 -0.13430 0.88240 0.89826 1.00000 0.09957 0.19262 0.01099 0.00794 0.00669 0.00000 0.02886 Q33 -0.24124 0.65018 0.58306 1.00000 0.09287 0.17558 0.01015 0.00762 0.00558 0.00000 0.03292 Q35 -0.46223 0.91922 0.58110 1.00000 0.14607 0.20983 0.01158 0.01079 0.00730 0.00000 0.05072 Q36 -0.25537 0.66630 0.79799 1.00000 0.06686 0.15502 0.00789 0.00609 0.00537 0.00000 0.02182 Q38 -0.29112 1.24073 0.90339 1.00000 0.07773 0.14168 0.00800 0.00649 0.00487 0.00000 0.02601 Q39 -0.57832 0.61010 0.76484 1.00000 0.15251 0.30956 0.01349 0.01365 0.01131 0.00000 0.07938 Q42 -0.07250 0.97903 0.74243 1.00000 0.06222 0.11896 0.00710 0.00561 0.00488 0.00000 0.02301 Final Structure Factor Calculation for Tetracycline Hydrochloride C22H25ClN2O8 P212121 Z=4 Total number of l.s. parameters = 121 Maximum vector length = 511 Memory required = 1855 / 26068 wR2 = 0.6584 before cycle 5 for 699 data and 2 / 121 parameters GooF = S = 3.294; Restrained GooF = 3.294 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.3540 for 507 Fo > 4sig(Fo) and 0.3733 for all 699 data wR2 = 0.6584, GooF = S = 3.294, Restrained GooF = 3.294 for all data Flack x parameter = 0.6946 with esd 0.5480 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 Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 30.00 for non-hydrogen and 0.00 for hydrogen atoms Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.020 0.037 0.047 0.059 0.072 0.087 0.110 0.157 0.221 1.000 Number in group 72. 75. 66. 71. 67. 69. 70. 69. 71. 69. GooF 5.087 2.232 2.456 2.680 2.028 1.907 2.179 2.218 2.665 3.463 K 85.579 18.551 11.156 6.052 4.330 2.812 2.679 1.721 1.769 1.266 Resolution(A) 1.04 1.10 1.17 1.24 1.32 1.43 1.55 1.72 2.02 2.67 inf Number in group 74. 67. 72. 68. 71. 69. 68. 70. 70. 70. GooF 2.386 2.989 3.051 2.029 2.241 2.132 2.406 3.005 4.270 3.233 K 6.054 4.626 6.115 3.730 3.059 2.324 2.254 1.881 1.935 1.252 R1 0.612 0.555 0.615 0.510 0.509 0.506 0.420 0.339 0.328 0.173 ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** Recommended weighting scheme: WGHT 0.2000 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) 8 4 4 0.00 3.03 5.01 0.014 1.20 0 4 4 0.00 0.48 5.01 0.005 2.49 3 4 0 0.00 0.44 5.01 0.005 2.41 2 7 11 0.01 1.65 4.95 0.010 1.11 1 12 3 0.14 4.61 4.36 0.017 1.04 5 1 3 3.18 53.64 4.02 0.058 2.00 9 3 4 0.22 4.33 3.99 0.016 1.12 2 1 3 7802.92 2766.92 2.94 0.416 3.64 5 1 0 8736.21 396.31 2.72 0.157 2.16 0 0 6 3526.03 682.82 2.39 0.206 2.62 1 1 1 1423.07 598.56 2.24 0.193 7.37 4 1 3 1633.23 130.99 2.22 0.090 2.39 1 2 5 3396.01 1510.03 2.03 0.307 2.74 2 3 4 3376.94 1031.82 2.02 0.254 2.56 0 7 3 932.17 207.72 2.01 0.114 1.73 1 2 6 2443.34 459.15 1.91 0.169 2.37 0 1 1 1877.82 944.53 1.89 0.243 9.95 7 6 5 1.77 10.88 1.87 0.026 1.17 3 2 8 842.29 155.06 1.86 0.098 1.67 2 7 0 655.95 23.95 1.83 0.039 1.74 1 0 1 2710.18 1524.69 1.73 0.308 9.00 1 4 0 3067.86 982.31 1.72 0.248 3.08 0 4 5 3182.86 432.78 1.71 0.164 2.25 1 6 1 825.84 273.07 1.69 0.131 2.08 1 2 4 3722.95 2099.37 1.65 0.362 3.21 4 1 6 1272.67 340.45 1.59 0.146 1.88 2 4 1 2945.93 1658.18 1.58 0.322 2.73 1 1 2 3232.75 1957.18 1.55 0.349 5.73 5 0 3 1746.37 39.04 1.52 0.049 2.03 6 2 3 658.49 81.37 1.51 0.071 1.67 2 4 8 307.41 4.05 1.49 0.016 1.60 5 2 3 1237.09 22.53 1.48 0.037 1.93 2 1 5 2891.95 1404.73 1.46 0.296 2.67 2 8 8 628.79 18.18 1.45 0.034 1.21 2 2 2 5272.77 3188.16 1.45 0.446 3.69 2 3 3 2717.60 1071.65 1.44 0.259 2.84 0 2 3 4064.05 2288.23 1.43 0.378 4.06 1 0 2 6445.30 4089.65 1.42 0.505 6.39 0 2 7 500.35 168.53 1.42 0.103 2.12 2 3 1 1132.56 2085.45 1.41 0.361 3.30 6 0 4 436.06 33.03 1.41 0.045 1.66 0 2 0 1388.73 841.93 1.39 0.229 6.43 3 10 0 889.06 20.87 1.38 0.036 1.21 2 4 4 590.53 82.30 1.36 0.072 2.27 3 4 4 2645.01 1117.80 1.34 0.264 2.06 2 8 0 376.50 1401.29 1.33 0.296 1.54 0 5 4 2097.82 169.61 1.33 0.103 2.15 1 10 4 684.45 54.61 1.33 0.058 1.21 3 3 4 1252.34 513.38 1.30 0.179 2.27 6 3 9 856.85 38.93 1.30 0.049 1.21 Bond lengths and angles Q3 - Distance Angles Q4 1.3873 (0.0916) Q24 1.7864 (0.1203) 124.41 (6.20) Q3 - Q4 Q4 - Distance Angles Q3 1.3873 (0.0916) Q38 1.3572 (0.1048) 134.33 (8.31) Q4 - Q3 Q5 - Distance Angles Q42 0.9567 (0.0787) Q19 1.7651 (0.1235) 162.99 (8.81) Q20 1.7160 (0.0980) 48.11 (6.61) 130.24 (5.94) Q5 - Q42 Q19 Q7 - Distance Angles Q32 1.4043 (0.1325) Q30 1.6634 (0.1409) 93.40 (9.62) Q7 - Q32 Q8 - Distance Angles Q39 1.1930 (0.1750) Q8 - Q9 - Distance Angles Q12 1.2721 (0.1198) Q9 - Q10 - Distance Angles Q36_$2 0.8809 (0.2187) Q27 2.0810 (0.2110) 102.99 (9.99) Q10 - Q36_$2 Q11 - Distance Angles Q28 1.2636 (0.1561) Q30 1.8123 (0.1626) 104.79 (9.99) Q11 - Q28 Q12 - Distance Angles Q9 1.2721 (0.1196) Q32 1.6911 (0.1393) 98.20 (9.89) Q15 1.8860 (0.1534) 118.51 (9.16) 45.03 (5.48) Q12 - Q9 Q32 Q13 - Distance Angles Q27 1.3846 (0.1114) Q35 1.4397 (0.1268) 117.61 (9.99) Q13 - Q27 Q15 - Distance Angles Q32 1.3814 (0.1450) Q12 1.8860 (0.1534) 60.00 (7.04) Q15 - Q32 Q19 - Distance Angles Q5 1.7651 (0.1235) Q19 - Q20 - Distance Angles Q24 1.0715 (0.1102) Q42 1.2913 (0.0979) 85.00 (8.22) Q5 1.7160 (0.0981) 118.46 (8.71) 33.47 (3.72) Q20 - Q24 Q42 Q24 - Distance Angles Q20 1.0715 (0.1102) Q3 1.7864 (0.1202) 135.83 (9.99) Q42 1.6045 (0.1253) 53.29 (6.82) 87.34 (6.08) Q24 - Q20 Q3 Q27 - Distance Angles Q13 1.3846 (0.1114) Q10 2.0810 (0.2108) 139.96 (9.44) Q27 - Q13 Q28 - Distance Angles Q11 1.2636 (0.1562) Q28 - Q30 - Distance Angles Q7 1.6634 (0.1416) Q11 1.8123 (0.1625) 90.58 (7.70) Q30 - Q7 Q31 - Distance Angles Q36 1.8145 (0.1279) Q31 - Q32 - Distance Angles Q7 1.4043 (0.1325) Q15 1.3814 (0.1450) 158.92 (9.99) Q12 1.6911 (0.1394) 94.87 (7.13) 74.98 (7.49) Q32 - Q7 Q15 Q35 - Distance Angles Q13 1.4397 (0.1268) Q35 - Q36 - Distance Angles Q10_$1 0.8809 (0.2197) Q31 1.8145 (0.1280) 79.75 (9.99) Q36 - Q10_$1 Q38 - Distance Angles Q4 1.3572 (0.1048) Q38 - Q39 - Distance Angles Q8 1.1930 (0.1738) Q39 - Q42 - Distance Angles Q5 0.9567 (0.0787) Q20 1.2913 (0.0979) 98.42 (8.47) Q24 1.6045 (0.1254) 140.10 (9.44) 41.70 (4.61) Q42 - Q5 Q20 FMAP and GRID set by program FMAP 2 1 12 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.4003 for 699 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.52 at 0.0802 0.9111 0.5133 [ 0.13 A from CL1 ] Deepest hole -0.51 at 0.0843 0.9395 0.4060 [ 1.65 A from CL1 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 2095 / 14781 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.3605 1.0191 0.8617 1.00000 0.05 0.36 2.08 Q4 2.20 Q15 2.40 Q39 2.52 Q3 Q2 1 0.0042 1.0266 0.5173 1.00000 0.05 0.34 1.60 CL1 2.31 Q28 2.80 Q20 3.29 Q11 Q3 1 -0.4442 1.2107 0.9881 1.00000 0.05 0.32 2.18 Q38 2.21 CL1 2.96 Q4 2.99 Q6 Q4 1 -0.4165 0.7923 1.1081 1.00000 0.05 0.29 1.74 Q11 1.94 Q9 2.05 Q28 2.69 Q7 Q5 1 -0.2853 0.6983 0.9468 1.00000 0.05 0.29 0.79 Q30 1.52 Q14 1.64 Q11 2.38 Q7 Q6 1 -0.3302 0.9089 0.6894 1.00000 0.05 0.28 1.65 Q6 2.24 Q35 2.40 Q24 2.46 Q31 Q7 1 -0.6339 0.7296 0.7456 1.00000 0.05 0.26 0.60 Q18 1.68 Q39 1.79 Q8 1.93 Q4 Q8 1 -0.2351 0.7594 0.9451 1.00000 0.05 0.26 0.38 Q30 1.51 Q7 1.54 Q11 2.07 Q32 Q9 1 -0.3400 0.9211 0.9667 1.00000 0.05 0.26 0.97 Q28 2.09 Q11 2.55 Q32 2.67 Q15 Q10 1 -0.2125 0.9545 0.7789 1.00000 0.05 0.25 0.91 Q15 1.65 Q24 1.67 Q42 2.06 Q20 Q11 1 -0.1946 0.9820 0.7661 1.00000 0.05 0.25 1.22 Q15 1.23 Q24 1.39 Q42 1.72 Q20 Q12 1 -0.4695 0.7544 0.5385 1.00000 0.05 0.24 2.22 Q35 2.39 CL1 2.79 Q38 2.93 Q33 Q13 1 -0.0747 0.6283 0.9252 1.00000 0.05 0.23 2.19 Q30 2.37 Q7 2.86 Q36 2.87 Q28 Q14 1 -0.4405 0.7412 0.9195 1.00000 0.05 0.22 0.59 Q14 2.14 Q8 2.25 Q11 2.32 Q30 Q15 1 0.0966 0.8185 0.7006 1.00000 0.05 0.22 0.33 Q19 1.92 Q5 2.11 Q9 2.74 Q3 Q16 1 -0.2314 0.7999 0.9999 1.00000 0.05 0.21 1.01 Q11 1.36 Q30 1.45 Q28 1.48 Q7 Q17 1 -0.5941 0.7538 0.6968 1.00000 0.05 0.21 1.30 Q18 1.95 Q4 2.03 Q38 2.14 Q39 Q18 1 -0.0367 0.6285 0.8585 1.00000 0.05 0.21 2.28 Q9 2.42 Q20 2.50 Q12 2.63 Q36 Q19 1 -0.4512 0.6548 0.7374 1.00000 0.05 0.20 1.30 Q31 1.55 Q8 1.57 Q39 1.97 Q10 Q20 1 -0.4334 0.6615 0.9269 1.00000 0.05 0.20 0.56 Q14 2.04 Q8 2.14 Q27 2.42 Q30 Shortest distances between peaks (including symmetry equivalents) 10 11 0.45 7 17 0.94 5 8 0.96 8 16 1.01 14 20 1.03 13 18 1.13 3 12 1.18 5 16 1.66 5 20 1.72 4 18 1.75 2 13 1.77 5 14 1.84 6 10 2.00 9 16 2.03 2 9 2.08 4 13 2.08 1 9 2.09 17 19 2.12 6 11 2.13 7 19 2.23 1 10 2.24 8 14 2.30 2 18 2.38 8 9 2.40 1 11 2.41 8 13 2.46 5 13 2.50 8 20 2.53 4 16 2.65 9 14 2.67 14 16 2.73 12 17 2.84 2 4 2.90 4 9 2.90 5 9 2.94 1 2 2.97 19 20 2.99 3 17 2.99 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.11: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.98: Structure factors and derivatives 0.56: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.17: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.17: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + tetra finished at 22:14:44 Total elapsed time: 2.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++