#------------------------------------------------------------------------------ #$Date: 2018-03-28 08:10:12 +0300 (Wed, 28 Mar 2018) $ #$Revision: 207157 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/24/2242434.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2242434 loop_ _publ_author_name 'Vella-Zarb, L.' 'Baisch, U.' _publ_section_title ; Crystal water as the molecular glue for obtaining different co-crystal ratios: the case of gallic acid tris-caffeine hexahydrate ; _journal_coeditor_code LH5871 _journal_issue 4 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 559 _journal_page_last 562 _journal_paper_doi 10.1107/S2056989018004528 _journal_volume 74 _journal_year 2018 _chemical_formula_iupac 'C7 H6 O5, 3C8 H10 N4 O2, 6H2 O' _chemical_formula_moiety 'C7 H6 O5, 3(C8 H10 N4 O2), 6(H2 O)' _chemical_formula_sum 'C31 H48 N12 O17' _chemical_formula_weight 860.81 _chemical_name_systematic 'Gallic Acid Tris-Caffeine hexahydrate' _space_group_crystal_system monoclinic _space_group_IT_number 7 _space_group_name_Hall 'P -2yc' _space_group_name_H-M_alt 'P 1 c 1' _symmetry_space_group_name_Hall 'P -2yc' _symmetry_space_group_name_H-M 'P 1 c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _cell_angle_alpha 90 _cell_angle_beta 110.865(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 16.5434(3) _cell_length_b 6.79456(11) _cell_length_c 18.1390(4) _cell_measurement_reflns_used 27647 _cell_measurement_temperature 150.15 _cell_measurement_theta_max 29.6159 _cell_measurement_theta_min 2.9980 _cell_volume 1905.21(7) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2015) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2015) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2015) ; _computing_molecular_graphics ; DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 150.15 _diffrn_detector_area_resol_mean 10.3968 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.935 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku Oxford Diffraction Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 38532 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 29.616 _diffrn_reflns_theta_min 2.998 _exptl_absorpt_coefficient_mu 0.123 _exptl_absorpt_correction_T_max 0.994 _exptl_absorpt_correction_T_min 0.946 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2015) ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_density_diffrn 1.501 _exptl_crystal_description plate _exptl_crystal_F_000 908 _exptl_crystal_size_max 0.656 _exptl_crystal_size_mid 0.369 _exptl_crystal_size_min 0.062 _refine_diff_density_max 0.244 _refine_diff_density_min -0.226 _refine_ls_abs_structure_details ; Flack x determined using 4000 quotients [(I^+^)-(I^-^)]/[(I^+^)+(I^-^)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack -0.1(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 645 _refine_ls_number_reflns 9519 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0330 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.2608P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.0864 _reflns_number_gt 8931 _reflns_number_total 9519 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL euthba_caf_1_april2017_p2_a.res in Pc euthba_caf_1_april2017_p2.res created by SHELXL-2017/1 at 06:27:49 on 13-Feb-2018 CELL 0.71073 16.543389 6.794556 18.139003 90 110.8649 90 ZERR 2 0.000349 0.000105 0.000368 0 0.0023 0 LATT -1 SYMM +X,-Y,0.5+Z SFAC C H N O UNIT 62 96 24 34 EQIV $1 +X,1-Y,-0.5+Z EQIV $2 +X,-1+Y,+Z EQIV $3 +X,2-Y,0.5+Z EQIV $4 +X,1-Y,0.5+Z EQIV $5 1+X,1-Y,0.5+Z EQIV $6 1+X,+Y,+Z EQIV $7 -1+X,+Y,+Z EQIV $8 +X,1+Y,+Z L.S. 10 PLAN 6 TEMP -123 HTAB O12 O100_$1 HTAB O10 O104 HTAB O102 O101_$2 HTAB O102 O103 HTAB O11 O102 HTAB O1 O32_$1 HTAB O100 O10 HTAB O100 O102 HTAB O100 O105 HTAB O105 O74_$3 HTAB O105 N63 HTAB O104 O74_$4 HTAB O104 O1_$4 HTAB O104 O105 HTAB O101 O100 HTAB O101 N43_$3 HTAB O103 O34_$5 HTAB O103 N23_$6 HTAB C22 O72_$7 HTAB C42 O12_$8 HTAB C42 O72 HTAB C62 O52_$7 HTAB C30 O12_$7 HTAB C31 O2_$4 BOND $H list 4 fmap 2 acta 50 REM REM REM WGHT 0.051000 0.260800 FVAR 0.47093 O12 4 0.646010 0.342557 0.432983 11.00000 0.01476 0.03789 = 0.02044 0.00301 0.00886 0.00371 O74 4 0.398163 0.962197 0.290636 11.00000 0.02454 0.02983 = 0.02186 0.00244 0.01018 -0.00028 O10 4 0.530208 0.305381 0.633462 11.00000 0.01717 0.04129 = 0.01736 0.00422 0.00730 0.00253 O72 4 0.660764 0.822666 0.481109 11.00000 0.01653 0.03318 = 0.03579 -0.00036 0.01170 0.00215 O102 4 0.712992 0.314910 0.740977 11.00000 0.01742 0.03666 = 0.02311 -0.00072 0.00654 -0.00096 O11 4 0.666353 0.295529 0.583696 11.00000 0.01378 0.03907 = 0.01912 0.00175 0.00553 0.00559 O32 4 0.190130 0.383130 0.678000 11.00000 0.01436 0.03288 = 0.02642 -0.00364 0.00302 0.00304 O34 4 -0.000903 0.482786 0.427378 11.00000 0.01961 0.03839 = 0.02055 -0.00309 0.00812 0.00120 O54 4 1.062580 0.960415 0.708724 11.00000 0.02345 0.03727 = 0.02330 -0.00054 0.00488 0.00243 O1 4 0.333151 0.497251 0.294022 11.00000 0.01494 0.04853 = 0.02138 0.00768 0.00310 0.00493 O100 4 0.619405 0.618135 0.777849 11.00000 0.02438 0.03390 = 0.02141 -0.00224 0.00810 0.00186 O105 4 0.442571 0.723414 0.699289 11.00000 0.03138 0.03529 = 0.02362 0.00289 0.01447 0.00568 O52 4 1.140779 0.901586 0.491468 11.00000 0.01973 0.03676 = 0.03781 -0.00233 0.01540 0.00173 O2 4 0.270184 0.470692 0.384113 11.00000 0.01503 0.04673 = 0.02820 0.00447 0.00747 0.00378 O104 4 0.387558 0.323810 0.667104 11.00000 0.02684 0.04259 = 0.02898 0.00028 0.01592 0.00200 O101 4 0.747906 0.935053 0.796216 11.00000 0.02791 0.03945 = 0.02882 0.00327 0.00851 -0.00247 N27 3 0.093916 0.438383 0.553577 11.00000 0.01353 0.02424 = 0.02329 -0.00247 0.00778 0.00013 N41 3 0.880458 1.059322 0.590974 11.00000 0.01720 0.02180 = 0.02624 -0.00165 0.01040 0.00098 N23 3 -0.097632 0.553361 0.636664 11.00000 0.01638 0.02504 = 0.02034 -0.00011 0.00741 0.00000 N67 3 0.529221 0.890479 0.387141 11.00000 0.01849 0.02216 = 0.02360 0.00057 0.01221 0.00046 N21 3 -0.136584 0.567681 0.505136 11.00000 0.01278 0.02323 = 0.01998 -0.00049 0.00581 0.00006 N61 3 0.324622 0.933010 0.424523 11.00000 0.01437 0.02783 = 0.02448 0.00001 0.00937 -0.00006 N63 3 0.413531 0.875902 0.548701 11.00000 0.01898 0.02813 = 0.02238 0.00081 0.01111 -0.00015 O103 4 0.867423 0.493526 0.776417 11.00000 0.02958 0.09546 = 0.02157 -0.00292 0.01019 -0.02514 N45 3 1.002010 0.987743 0.469223 11.00000 0.01641 0.02530 = 0.02337 -0.00112 0.00858 0.00101 N47 3 1.100758 0.932300 0.598873 11.00000 0.01214 0.02515 = 0.02705 -0.00264 0.00457 0.00047 N43 3 0.856461 1.076998 0.461634 11.00000 0.01546 0.02251 = 0.02676 -0.00122 0.00475 0.00098 N25 3 0.053321 0.468493 0.665828 11.00000 0.01458 0.02495 = 0.01868 0.00095 0.00381 0.00132 N65 3 0.546387 0.852588 0.521431 11.00000 0.01465 0.02312 = 0.02099 0.00153 0.00734 0.00106 C9 1 0.492728 0.403209 0.398526 11.00000 0.01662 0.02115 = 0.01771 0.00003 0.00731 -0.00029 C28 1 0.011599 0.481352 0.498045 11.00000 0.01559 0.01937 = 0.02076 -0.00140 0.00656 -0.00130 C68 1 0.439915 0.926446 0.360599 11.00000 0.01935 0.01704 = 0.02421 -0.00036 0.01102 -0.00073 C64 1 0.459279 0.880053 0.499965 11.00000 0.01675 0.01887 = 0.02232 -0.00101 0.00903 -0.00150 C5 1 0.432045 0.381774 0.501442 11.00000 0.01389 0.02153 = 0.02167 -0.00015 0.00840 -0.00072 C22 1 -0.161564 0.585391 0.567537 11.00000 0.01562 0.02446 = 0.02215 -0.00018 0.00781 -0.00046 C4 1 0.421925 0.413941 0.423098 11.00000 0.01508 0.01793 = 0.02115 -0.00055 0.00655 -0.00027 C26 1 0.116280 0.427782 0.635321 11.00000 0.01519 0.02039 = 0.02271 -0.00215 0.00530 -0.00030 C3 1 0.334449 0.462694 0.366768 11.00000 0.01612 0.02216 = 0.02140 0.00077 0.00561 0.00002 C42 1 0.823364 1.095527 0.518581 11.00000 0.01340 0.02364 = 0.03073 -0.00127 0.00761 0.00106 C62 1 0.332328 0.908193 0.499776 11.00000 0.01758 0.03289 = 0.02524 0.00080 0.01175 0.00005 C6 1 0.513535 0.339792 0.555604 11.00000 0.01867 0.01992 = 0.01896 -0.00090 0.00778 -0.00128 C29 1 -0.049573 0.519246 0.535277 11.00000 0.01280 0.01999 = 0.02057 0.00009 0.00496 -0.00059 C24 1 -0.028779 0.512825 0.615087 11.00000 0.01463 0.01797 = 0.02183 0.00026 0.00634 0.00002 C8 1 0.573937 0.360555 0.452613 11.00000 0.01576 0.01963 = 0.02223 -0.00048 0.00971 -0.00033 C69 1 0.407325 0.914977 0.422775 11.00000 0.01508 0.01931 = 0.02255 0.00025 0.00856 0.00036 C7 1 0.585462 0.331898 0.531865 11.00000 0.01447 0.01956 = 0.01927 -0.00006 0.00422 0.00158 C49 1 0.957741 1.013395 0.581301 11.00000 0.01318 0.02061 = 0.02382 -0.00153 0.00717 0.00034 C48 1 1.041313 0.968606 0.637086 11.00000 0.01775 0.01887 = 0.02820 -0.00206 0.00782 0.00018 C46 1 1.084286 0.938583 0.517908 11.00000 0.01673 0.02042 = 0.02905 -0.00223 0.00886 -0.00073 C30 1 -0.190916 0.591697 0.422518 11.00000 0.01444 0.02810 = 0.01747 0.00029 0.00275 0.00067 AFIX 137 H30A 2 -0.195314 0.465826 0.394977 11.00000 -1.50000 H30B 2 -0.165253 0.690518 0.398138 11.00000 -1.50000 H30C 2 -0.248743 0.634908 0.418844 11.00000 -1.50000 AFIX 0 C44 1 0.940047 1.024926 0.501653 11.00000 0.01590 0.01838 = 0.02528 -0.00252 0.00780 -0.00106 C66 1 0.583609 0.852915 0.464849 11.00000 0.01870 0.01809 = 0.02706 -0.00032 0.01073 0.00000 C71 1 0.600747 0.822735 0.604294 11.00000 0.01988 0.03157 = 0.02351 0.00047 0.00476 0.00173 AFIX 137 H71A 2 0.578830 0.903248 0.637924 11.00000 -1.50000 H71B 2 0.660364 0.861399 0.612352 11.00000 -1.50000 H71C 2 0.599411 0.683589 0.618036 11.00000 -1.50000 AFIX 0 C31 1 0.072883 0.463397 0.751201 11.00000 0.02048 0.03809 = 0.01820 0.00245 0.00441 0.00218 AFIX 137 H31A 2 0.049780 0.341920 0.765162 11.00000 -1.50000 H31B 2 0.046261 0.577200 0.766781 11.00000 -1.50000 H31C 2 0.135692 0.467660 0.778760 11.00000 -1.50000 AFIX 0 C51 1 0.982194 0.994984 0.383784 11.00000 0.02793 0.03595 = 0.02261 -0.00237 0.01192 -0.00082 AFIX 137 H51A 2 1.028745 1.063988 0.372886 11.00000 -1.50000 H51B 2 0.927512 1.065112 0.358458 11.00000 -1.50000 H51C 2 0.977081 0.860691 0.362901 11.00000 -1.50000 AFIX 0 C50 1 0.862609 1.058294 0.664090 11.00000 0.02801 0.03284 = 0.03121 -0.00035 0.01901 0.00348 C33 1 0.163796 0.406021 0.521763 11.00000 0.01480 0.03347 = 0.03268 -0.00348 0.01248 0.00184 AFIX 137 H33A 2 0.148733 0.294353 0.485177 11.00000 -1.50000 H33B 2 0.218050 0.377880 0.565271 11.00000 -1.50000 H33C 2 0.170850 0.524415 0.493788 11.00000 -1.50000 AFIX 0 C53 1 1.190538 0.888654 0.649402 11.00000 0.01456 0.03241 = 0.03760 -0.00386 0.00225 0.00307 AFIX 137 H53A 2 1.225454 1.008608 0.656930 11.00000 -1.50000 H53B 2 1.214230 0.787698 0.624216 11.00000 -1.50000 H53C 2 1.191737 0.840579 0.700719 11.00000 -1.50000 AFIX 0 C73 1 0.571110 0.889588 0.328200 11.00000 0.02658 0.03729 = 0.03146 0.00140 0.01978 0.00156 AFIX 137 H73A 2 0.573261 0.754593 0.309962 11.00000 -1.50000 H73B 2 0.630055 0.941262 0.351905 11.00000 -1.50000 H73C 2 0.538002 0.972313 0.283348 11.00000 -1.50000 AFIX 0 H5 2 0.384484 0.391227 0.520279 11.00000 0.02217 H9 2 0.487339 0.423927 0.342604 11.00000 0.01743 H22 2 -0.219806 0.629126 0.559596 11.00000 0.03004 H1 2 0.282104 0.520723 0.262918 11.00000 0.03512 H12 2 0.630662 0.368628 0.383234 11.00000 0.03095 H62 2 0.283595 0.911597 0.516973 11.00000 0.03516 H10 2 0.482127 0.307937 0.641272 11.00000 0.06148 C70 1 0.244178 0.965949 0.357954 11.00000 0.01749 0.03497 = 0.02552 0.00177 0.00563 0.00187 AFIX 137 H70A 2 0.194877 0.947555 0.375199 11.00000 -1.50000 H70B 2 0.240186 0.871975 0.315813 11.00000 -1.50000 H70C 2 0.243510 1.100411 0.338199 11.00000 -1.50000 AFIX 0 H42 2 0.766837 1.131175 0.509228 11.00000 0.03270 H11 2 0.668612 0.304424 0.630268 11.00000 0.04089 H10G 2 0.391981 0.448646 0.686447 11.00000 0.03616 H10E 2 0.425267 0.802355 0.727512 11.00000 0.06154 H10F 2 0.436058 0.780844 0.653850 11.00000 0.05255 H10A 2 0.718015 0.192059 0.759862 11.00000 0.05559 H10I 2 0.780914 0.914898 0.849549 11.00000 0.03886 H10C 2 0.568431 0.622457 0.746244 11.00000 0.05490 H10D 2 0.633784 0.518495 0.760424 11.00000 0.03387 H10B 2 0.762833 0.367350 0.755790 11.00000 0.03295 H10K 2 0.905462 0.515314 0.816069 11.00000 0.07605 H10L 2 0.880883 0.528122 0.737717 11.00000 0.07236 H10H 2 0.389045 0.243284 0.708927 11.00000 0.07657 H10J 2 0.713673 0.831806 0.788016 11.00000 0.05672 H50A 2 0.868383 0.928286 0.683217 11.00000 0.04387 H50B 2 0.803233 1.094329 0.650949 11.00000 0.06312 H50C 2 0.901858 1.155636 0.701121 11.00000 0.05459 HKLF 4 REM euthba_caf_1_april2017_p2_a.res in Pc REM R1 = 0.0330 for 8931 Fo > 4sig(Fo) and 0.0372 for all 9519 data REM 645 parameters refined using 2 restraints END WGHT 0.0509 0.2606 REM Highest difference peak 0.244, deepest hole -0.226, 1-sigma level 0.046 Q1 1 0.9978 1.0094 0.6082 11.00000 0.05 0.24 Q2 1 0.0113 0.4897 0.6421 11.00000 0.05 0.24 Q3 1 -0.0221 0.4996 0.5198 11.00000 0.05 0.23 Q4 1 0.3812 0.4297 0.3944 11.00000 0.05 0.21 Q5 1 0.5312 0.3785 0.4256 11.00000 0.05 0.21 Q6 1 1.0357 0.9496 0.4934 11.00000 0.05 0.20 REM The information below was added by Olex2. REM REM R1 = 0.0330 for 8931 Fo > 4sig(Fo) and 0.0372 for all 38532 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.24, deepest hole -0.23 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0372 REM R1_gt = 0.0330 REM wR_ref = 0.0864 REM GOOF = 1.043 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 38532 REM Reflections_gt = 8931 REM Parameters = n/a REM Hole = -0.23 REM Peak = 0.24 REM Flack = -0.1(2) ; _cod_data_source_file lh5871sup1.cif _cod_data_source_block I _cod_database_code 2242434 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, z+1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy O O12 0.64601(10) 0.3426(2) 0.43298(9) 0.0237(3) Uani d 1 O O74 0.39816(11) 0.9622(2) 0.29064(9) 0.0249(3) Uani d 1 O O10 0.53021(10) 0.3054(3) 0.63346(9) 0.0250(3) Uani d 1 O O72 0.66076(10) 0.8227(3) 0.48111(10) 0.0279(3) Uani d 1 O O102 0.71299(11) 0.3149(3) 0.74098(9) 0.0259(3) Uani d 1 O O11 0.66635(9) 0.2955(2) 0.58370(9) 0.0241(3) Uani d 1 O O32 0.19013(10) 0.3831(2) 0.67800(9) 0.0257(3) Uani d 1 O O34 -0.00090(10) 0.4828(2) 0.42738(9) 0.0259(3) Uani d 1 O O54 1.06258(11) 0.9604(3) 0.70872(10) 0.0289(3) Uani d 1 O O1 0.33315(11) 0.4973(3) 0.29402(10) 0.0292(4) Uani d 1 O O100 0.61941(12) 0.6181(3) 0.77785(10) 0.0266(3) Uani d 1 O O105 0.44257(11) 0.7234(3) 0.69929(10) 0.0288(3) Uani d 1 O O52 1.14078(10) 0.9016(3) 0.49147(10) 0.0300(4) Uani d 1 O O2 0.27018(10) 0.4707(3) 0.38411(10) 0.0300(4) Uani d 1 O O104 0.38756(11) 0.3238(3) 0.66710(11) 0.0312(4) Uani d 1 O O101 0.74791(12) 0.9351(3) 0.79622(11) 0.0325(4) Uani d 1 N N27 0.09392(11) 0.4384(3) 0.55358(11) 0.0200(3) Uani d 1 N N41 0.88046(12) 1.0593(3) 0.59097(11) 0.0210(3) Uani d 1 N N23 -0.09763(11) 0.5534(3) 0.63666(10) 0.0203(3) Uani d 1 N N67 0.52922(11) 0.8905(3) 0.38714(11) 0.0201(3) Uani d 1 N N21 -0.13658(11) 0.5677(3) 0.50514(10) 0.0187(3) Uani d 1 N N61 0.32462(12) 0.9330(3) 0.42452(11) 0.0216(4) Uani d 1 N N63 0.41353(12) 0.8759(3) 0.54870(11) 0.0221(4) Uani d 1 O O103 0.86742(14) 0.4935(4) 0.77642(12) 0.0486(6) Uani d 1 N N45 1.00201(12) 0.9877(3) 0.46922(11) 0.0213(4) Uani d 1 N N47 1.10076(11) 0.9323(3) 0.59887(11) 0.0221(4) Uani d 1 N N43 0.85646(11) 1.0770(3) 0.46163(11) 0.0223(4) Uani d 1 N N25 0.05332(11) 0.4685(3) 0.66583(10) 0.0200(3) Uani d 1 N N65 0.54639(11) 0.8526(3) 0.52143(10) 0.0193(3) Uani d 1 C C9 0.49273(13) 0.4032(3) 0.39853(12) 0.0182(4) Uani d 1 C C28 0.01160(13) 0.4814(3) 0.49805(12) 0.0185(4) Uani d 1 C C68 0.43992(14) 0.9264(3) 0.36060(12) 0.0193(4) Uani d 1 C C64 0.45928(13) 0.8801(3) 0.49996(12) 0.0188(4) Uani d 1 C C5 0.43204(13) 0.3818(3) 0.50144(12) 0.0185(4) Uani d 1 C C22 -0.16156(14) 0.5854(3) 0.56754(12) 0.0204(4) Uani d 1 C C4 0.42193(13) 0.4139(3) 0.42310(12) 0.0180(4) Uani d 1 C C26 0.11628(13) 0.4278(3) 0.63532(12) 0.0198(4) Uani d 1 C C3 0.33445(14) 0.4627(3) 0.36677(12) 0.0202(4) Uani d 1 C C42 0.82336(14) 1.0955(3) 0.51858(13) 0.0227(4) Uani d 1 C C62 0.33233(14) 0.9082(3) 0.49978(13) 0.0241(4) Uani d 1 C C6 0.51354(13) 0.3398(3) 0.55560(12) 0.0189(4) Uani d 1 C C29 -0.04957(13) 0.5192(3) 0.53528(12) 0.0181(4) Uani d 1 C C24 -0.02878(13) 0.5128(3) 0.61509(12) 0.0182(4) Uani d 1 C C8 0.57394(13) 0.3606(3) 0.45261(12) 0.0184(4) Uani d 1 C C69 0.40732(13) 0.9150(3) 0.42277(12) 0.0185(4) Uani d 1 C C7 0.58546(13) 0.3319(3) 0.53187(12) 0.0183(4) Uani d 1 C C49 0.95774(13) 1.0134(3) 0.58130(13) 0.0190(4) Uani d 1 C C48 1.04131(14) 0.9686(3) 0.63709(13) 0.0217(4) Uani d 1 C C46 1.08429(14) 0.9386(3) 0.51791(13) 0.0219(4) Uani d 1 C C30 -0.19092(13) 0.5917(3) 0.42252(12) 0.0208(4) Uani d 1 H H30A -0.195314 0.465826 0.394977 0.031 Uiso calc 1 H H30B -0.165253 0.690518 0.398138 0.031 Uiso calc 1 H H30C -0.248743 0.634908 0.418844 0.031 Uiso calc 1 C C44 0.94005(13) 1.0249(3) 0.50165(12) 0.0197(4) Uani d 1 C C66 0.58361(14) 0.8529(3) 0.46485(13) 0.0206(4) Uani d 1 C C71 0.60075(14) 0.8227(3) 0.60429(13) 0.0258(4) Uani d 1 H H71A 0.578830 0.903248 0.637924 0.039 Uiso calc 1 H H71B 0.660364 0.861399 0.612352 0.039 Uiso calc 1 H H71C 0.599411 0.683589 0.618036 0.039 Uiso calc 1 C C31 0.07288(15) 0.4634(4) 0.75120(13) 0.0263(4) Uani d 1 H H31A 0.049780 0.341920 0.765162 0.039 Uiso calc 1 H H31B 0.046261 0.577200 0.766781 0.039 Uiso calc 1 H H31C 0.135692 0.467660 0.778760 0.039 Uiso calc 1 C C51 0.98219(16) 0.9950(4) 0.38378(14) 0.0280(5) Uani d 1 H H51A 1.028745 1.063988 0.372886 0.042 Uiso calc 1 H H51B 0.927512 1.065112 0.358458 0.042 Uiso calc 1 H H51C 0.977081 0.860691 0.362901 0.042 Uiso calc 1 C C50 0.86261(17) 1.0583(4) 0.66409(15) 0.0284(5) Uani d 1 C C33 0.16380(14) 0.4060(4) 0.52176(14) 0.0259(5) Uani d 1 H H33A 0.148733 0.294353 0.485177 0.039 Uiso calc 1 H H33B 0.218050 0.377880 0.565271 0.039 Uiso calc 1 H H33C 0.170850 0.524415 0.493788 0.039 Uiso calc 1 C C53 1.19054(14) 0.8887(4) 0.64940(15) 0.0301(5) Uani d 1 H H53A 1.225454 1.008608 0.656930 0.045 Uiso calc 1 H H53B 1.214230 0.787698 0.624216 0.045 Uiso calc 1 H H53C 1.191737 0.840579 0.700719 0.045 Uiso calc 1 C C73 0.57111(16) 0.8896(4) 0.32820(15) 0.0292(5) Uani d 1 H H73A 0.573261 0.754593 0.309962 0.044 Uiso calc 1 H H73B 0.630055 0.941262 0.351905 0.044 Uiso calc 1 H H73C 0.538002 0.972313 0.283348 0.044 Uiso calc 1 H H5 0.3845(19) 0.391(4) 0.5203(16) 0.022(6) Uiso d 1 H H9 0.4873(17) 0.424(4) 0.3426(16) 0.017(6) Uiso d 1 H H22 -0.220(2) 0.629(4) 0.5596(17) 0.030(7) Uiso d 1 H H1 0.282(2) 0.521(5) 0.2629(19) 0.035(8) Uiso d 1 H H12 0.631(2) 0.369(4) 0.3832(19) 0.031(7) Uiso d 1 H H62 0.284(2) 0.912(5) 0.5170(18) 0.035(8) Uiso d 1 H H10 0.482(3) 0.308(6) 0.641(2) 0.061(11) Uiso d 1 C C70 0.24418(15) 0.9659(4) 0.35795(14) 0.0265(4) Uani d 1 H H70A 0.194877 0.947555 0.375199 0.040 Uiso calc 1 H H70B 0.240186 0.871975 0.315813 0.040 Uiso calc 1 H H70C 0.243510 1.100411 0.338199 0.040 Uiso calc 1 H H42 0.767(2) 1.131(4) 0.5092(18) 0.033(7) Uiso d 1 H H11 0.669(2) 0.304(5) 0.630(2) 0.041(9) Uiso d 1 H H10G 0.392(2) 0.449(5) 0.6864(19) 0.036(8) Uiso d 1 H H10E 0.425(3) 0.802(6) 0.728(3) 0.062(11) Uiso d 1 H H10F 0.436(2) 0.781(6) 0.654(2) 0.053(10) Uiso d 1 H H10A 0.718(2) 0.192(6) 0.760(2) 0.056(10) Uiso d 1 H H10I 0.781(2) 0.915(5) 0.850(2) 0.039(8) Uiso d 1 H H10C 0.568(3) 0.622(6) 0.746(2) 0.055(11) Uiso d 1 H H10D 0.634(2) 0.518(5) 0.7604(19) 0.034(8) Uiso d 1 H H10B 0.763(2) 0.367(5) 0.7558(19) 0.033(8) Uiso d 1 H H10K 0.905(3) 0.515(7) 0.816(3) 0.076(14) Uiso d 1 H H10L 0.881(3) 0.528(6) 0.738(3) 0.072(13) Uiso d 1 H H10H 0.389(3) 0.243(7) 0.709(3) 0.077(13) Uiso d 1 H H10J 0.714(3) 0.832(6) 0.788(2) 0.057(11) Uiso d 1 H H50A 0.868(2) 0.928(5) 0.683(2) 0.044(9) Uiso d 1 H H50B 0.803(3) 1.094(6) 0.651(2) 0.063(11) Uiso d 1 H H50C 0.902(3) 1.156(5) 0.701(2) 0.055(10) Uiso d 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O12 0.0148(7) 0.0379(8) 0.0204(7) 0.0037(6) 0.0089(6) 0.0030(6) O74 0.0245(8) 0.0298(7) 0.0219(7) -0.0003(6) 0.0102(6) 0.0024(6) O10 0.0172(7) 0.0413(9) 0.0174(7) 0.0025(6) 0.0073(6) 0.0042(6) O72 0.0165(7) 0.0332(8) 0.0358(9) 0.0021(6) 0.0117(6) -0.0004(7) O102 0.0174(8) 0.0367(9) 0.0231(7) -0.0010(7) 0.0065(6) -0.0007(7) O11 0.0138(7) 0.0391(9) 0.0191(7) 0.0056(6) 0.0055(6) 0.0018(6) O32 0.0144(7) 0.0329(8) 0.0264(8) 0.0030(6) 0.0030(6) -0.0036(6) O34 0.0196(7) 0.0384(9) 0.0206(7) 0.0012(6) 0.0081(6) -0.0031(6) O54 0.0235(8) 0.0373(8) 0.0233(8) 0.0024(7) 0.0049(7) -0.0005(7) O1 0.0149(7) 0.0485(10) 0.0214(7) 0.0049(7) 0.0031(6) 0.0077(7) O100 0.0244(9) 0.0339(9) 0.0214(8) 0.0019(7) 0.0081(7) -0.0022(7) O105 0.0314(9) 0.0353(9) 0.0236(8) 0.0057(7) 0.0145(7) 0.0029(7) O52 0.0197(8) 0.0368(9) 0.0378(9) 0.0017(6) 0.0154(7) -0.0023(7) O2 0.0150(7) 0.0467(10) 0.0282(8) 0.0038(7) 0.0075(7) 0.0045(7) O104 0.0268(8) 0.0426(10) 0.0290(8) 0.0020(7) 0.0159(7) 0.0003(8) O101 0.0279(9) 0.0394(10) 0.0288(9) -0.0025(8) 0.0085(7) 0.0033(7) N27 0.0135(8) 0.0242(8) 0.0233(9) 0.0001(6) 0.0078(7) -0.0025(6) N41 0.0172(8) 0.0218(8) 0.0262(9) 0.0010(7) 0.0104(7) -0.0017(7) N23 0.0164(8) 0.0250(8) 0.0203(8) 0.0000(7) 0.0074(7) -0.0001(7) N67 0.0185(9) 0.0222(8) 0.0236(8) 0.0005(7) 0.0122(7) 0.0006(7) N21 0.0128(8) 0.0232(8) 0.0200(8) 0.0001(6) 0.0058(7) -0.0005(6) N61 0.0144(8) 0.0278(9) 0.0245(9) -0.0001(7) 0.0094(7) 0.0000(7) N63 0.0190(9) 0.0281(9) 0.0224(8) -0.0001(7) 0.0111(7) 0.0008(7) O103 0.0296(10) 0.0955(18) 0.0216(9) -0.0251(11) 0.0102(8) -0.0029(10) N45 0.0164(8) 0.0253(9) 0.0234(9) 0.0010(7) 0.0086(7) -0.0011(7) N47 0.0121(8) 0.0251(8) 0.0270(9) 0.0005(7) 0.0046(7) -0.0026(7) N43 0.0155(9) 0.0225(8) 0.0268(9) 0.0010(6) 0.0047(7) -0.0012(7) N25 0.0146(8) 0.0250(8) 0.0187(8) 0.0013(6) 0.0038(7) 0.0010(6) N65 0.0147(8) 0.0231(8) 0.0210(8) 0.0011(6) 0.0073(7) 0.0015(7) C9 0.0166(9) 0.0211(9) 0.0177(9) -0.0003(7) 0.0073(8) 0.0000(7) C28 0.0156(9) 0.0194(9) 0.0208(9) -0.0013(7) 0.0066(8) -0.0014(7) C68 0.0194(10) 0.0170(9) 0.0242(10) -0.0007(7) 0.0110(8) -0.0004(7) C64 0.0168(9) 0.0189(9) 0.0223(10) -0.0015(7) 0.0090(8) -0.0010(7) C5 0.0139(9) 0.0215(9) 0.0217(10) -0.0007(7) 0.0084(8) -0.0001(7) C22 0.0156(10) 0.0245(10) 0.0221(10) -0.0005(8) 0.0078(8) -0.0002(8) C4 0.0151(9) 0.0179(9) 0.0211(9) -0.0003(7) 0.0066(8) -0.0006(7) C26 0.0152(9) 0.0204(9) 0.0227(10) -0.0003(7) 0.0053(8) -0.0022(8) C3 0.0161(9) 0.0222(9) 0.0214(10) 0.0000(7) 0.0056(8) 0.0008(8) C42 0.0134(10) 0.0236(10) 0.0307(11) 0.0011(7) 0.0076(8) -0.0013(8) C62 0.0176(10) 0.0329(11) 0.0252(10) 0.0001(8) 0.0118(8) 0.0008(8) C6 0.0187(9) 0.0199(9) 0.0190(9) -0.0013(7) 0.0078(8) -0.0009(7) C29 0.0128(9) 0.0200(9) 0.0206(9) -0.0006(7) 0.0050(7) 0.0001(7) C24 0.0146(9) 0.0180(9) 0.0218(10) 0.0000(7) 0.0063(8) 0.0003(7) C8 0.0158(9) 0.0196(9) 0.0222(10) -0.0003(7) 0.0097(8) -0.0005(7) C69 0.0151(9) 0.0193(9) 0.0225(10) 0.0004(7) 0.0086(8) 0.0003(7) C7 0.0145(9) 0.0196(9) 0.0193(9) 0.0016(7) 0.0042(7) -0.0001(7) C49 0.0132(9) 0.0206(9) 0.0238(10) 0.0003(7) 0.0072(8) -0.0015(7) C48 0.0178(10) 0.0189(9) 0.0282(11) 0.0002(8) 0.0078(9) -0.0021(8) C46 0.0167(10) 0.0204(9) 0.0291(11) -0.0007(7) 0.0089(8) -0.0022(8) C30 0.0144(9) 0.0281(10) 0.0175(9) 0.0007(7) 0.0028(8) 0.0003(8) C44 0.0159(9) 0.0184(9) 0.0253(10) -0.0011(7) 0.0078(8) -0.0025(8) C66 0.0187(9) 0.0181(9) 0.0271(10) 0.0000(7) 0.0107(8) -0.0003(8) C71 0.0199(10) 0.0316(11) 0.0235(10) 0.0017(9) 0.0048(8) 0.0005(9) C31 0.0205(10) 0.0381(12) 0.0182(10) 0.0022(9) 0.0044(8) 0.0024(9) C51 0.0279(12) 0.0360(12) 0.0226(10) -0.0008(9) 0.0119(9) -0.0024(9) C50 0.0280(12) 0.0328(12) 0.0312(12) 0.0035(10) 0.0190(10) -0.0003(10) C33 0.0148(10) 0.0335(11) 0.0327(12) 0.0018(8) 0.0125(9) -0.0035(9) C53 0.0146(10) 0.0324(11) 0.0376(13) 0.0031(8) 0.0023(9) -0.0039(10) C73 0.0266(12) 0.0373(12) 0.0315(12) 0.0016(9) 0.0198(10) 0.0014(10) C70 0.0175(10) 0.0350(11) 0.0255(10) 0.0019(9) 0.0056(8) 0.0018(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 10 -1 0.2177 1 0 -24 0.0308 -1 0 24 0.0308 -22 1 7 0.2931 1 -10 -1 0.1209 23 1 -8 0.3323 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C8 O12 H12 107(2) C6 O10 H10 108(3) H10A O102 H10B 109(3) C7 O11 H11 111(2) C3 O1 H1 111(2) H10C O100 H10D 97(3) H10E O105 H10F 109(4) H10G O104 H10H 105(3) H10I O101 H10J 99(3) C28 N27 C33 116.29(17) C26 N27 C28 126.45(17) C26 N27 C33 117.24(17) C42 N41 C49 106.10(18) C42 N41 C50 126.3(2) C49 N41 C50 127.5(2) C22 N23 C24 103.11(17) C68 N67 C73 117.64(18) C66 N67 C68 126.75(17) C66 N67 C73 115.61(18) C22 N21 C29 106.10(17) C22 N21 C30 126.55(18) C29 N21 C30 127.34(17) C62 N61 C69 106.06(18) C62 N61 C70 126.25(19) C69 N61 C70 127.66(18) C62 N63 C64 103.07(18) H10K O103 H10L 110(5) C46 N45 C44 119.25(18) C46 N45 C51 119.00(18) C44 N45 C51 121.74(18) C48 N47 C53 117.03(19) C46 N47 C48 127.02(18) C46 N47 C53 115.92(18) C42 N43 C44 103.33(18) C26 N25 C24 119.03(17) C26 N25 C31 120.56(18) C24 N25 C31 120.40(17) C64 N65 C66 119.72(17) C64 N65 C71 120.76(17) C66 N65 C71 119.51(18) C4 C9 H9 122.5(15) C8 C9 C4 119.88(18) C8 C9 H9 117.6(15) O34 C28 N27 120.75(18) O34 C28 C29 127.67(19) N27 C28 C29 111.58(17) O74 C68 N67 121.51(19) O74 C68 C69 126.7(2) N67 C68 C69 111.75(18) N63 C64 N65 126.15(19) N63 C64 C69 112.08(18) N65 C64 C69 121.77(18) C4 C5 H5 122.4(16) C6 C5 C4 119.37(19) C6 C5 H5 118.2(16) N23 C22 N21 113.42(19) N23 C22 H22 126.9(17) N21 C22 H22 119.4(17) C9 C4 C3 121.08(18) C5 C4 C9 120.66(18) C5 C4 C3 118.26(18) O32 C26 N27 120.64(19) O32 C26 N25 121.57(19) N25 C26 N27 117.80(18) O1 C3 C4 112.93(18) O2 C3 O1 122.85(19) O2 C3 C4 124.22(19) N41 C42 H42 123(2) N43 C42 N41 113.62(19) N43 C42 H42 123(2) N61 C62 N63 113.97(19) N61 C62 H62 122.8(19) N63 C62 H62 123.2(19) O10 C6 C5 123.93(18) O10 C6 C7 115.58(18) C5 C6 C7 120.49(19) N21 C29 C28 131.99(19) C24 C29 N21 105.09(17) C24 C29 C28 122.92(18) N23 C24 N25 125.54(18) N23 C24 C29 112.27(18) C29 C24 N25 122.19(18) O12 C8 C9 123.47(18) O12 C8 C7 116.40(18) C9 C8 C7 120.14(18) N61 C69 C68 132.3(2) C64 C69 N61 104.82(17) C64 C69 C68 122.86(19) O11 C7 C6 121.96(18) O11 C7 C8 118.61(18) C8 C7 C6 119.43(18) N41 C49 C48 131.5(2) C44 C49 N41 105.08(18) C44 C49 C48 123.34(19) O54 C48 N47 121.84(19) O54 C48 C49 127.2(2) N47 C48 C49 110.97(19) O52 C46 N45 121.3(2) O52 C46 N47 121.2(2) N45 C46 N47 117.47(18) N21 C30 H30A 109.5 N21 C30 H30B 109.5 N21 C30 H30C 109.5 H30A C30 H30B 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 N43 C44 N45 126.21(19) N43 C44 C49 111.87(18) C49 C44 N45 121.92(18) O72 C66 N67 121.06(19) O72 C66 N65 121.9(2) N65 C66 N67 117.06(18) N65 C71 H71A 109.5 N65 C71 H71B 109.5 N65 C71 H71C 109.5 H71A C71 H71B 109.5 H71A C71 H71C 109.5 H71B C71 H71C 109.5 N25 C31 H31A 109.5 N25 C31 H31B 109.5 N25 C31 H31C 109.5 H31A C31 H31B 109.5 H31A C31 H31C 109.5 H31B C31 H31C 109.5 N45 C51 H51A 109.5 N45 C51 H51B 109.5 N45 C51 H51C 109.5 H51A C51 H51B 109.5 H51A C51 H51C 109.5 H51B C51 H51C 109.5 N41 C50 H50A 108(2) N41 C50 H50B 107(3) N41 C50 H50C 108(2) H50A C50 H50B 107(3) H50A C50 H50C 115(3) H50B C50 H50C 111(3) N27 C33 H33A 109.5 N27 C33 H33B 109.5 N27 C33 H33C 109.5 H33A C33 H33B 109.5 H33A C33 H33C 109.5 H33B C33 H33C 109.5 N47 C53 H53A 109.5 N47 C53 H53B 109.5 N47 C53 H53C 109.5 H53A C53 H53B 109.5 H53A C53 H53C 109.5 H53B C53 H53C 109.5 N67 C73 H73A 109.5 N67 C73 H73B 109.5 N67 C73 H73C 109.5 H73A C73 H73B 109.5 H73A C73 H73C 109.5 H73B C73 H73C 109.5 N61 C70 H70A 109.5 N61 C70 H70B 109.5 N61 C70 H70C 109.5 H70A C70 H70B 109.5 H70A C70 H70C 109.5 H70B C70 H70C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O12 C8 1.366(2) O12 H12 0.86(3) O74 C68 1.234(3) O10 C6 1.359(2) O10 H10 0.86(4) O72 C66 1.221(3) O102 H10A 0.89(4) O102 H10B 0.85(4) O11 C7 1.356(2) O11 H11 0.83(4) O32 C26 1.229(3) O34 C28 1.224(3) O54 C48 1.221(3) O1 C3 1.333(3) O1 H1 0.85(3) O100 H10C 0.83(4) O100 H10D 0.82(4) O105 H10E 0.86(5) O105 H10F 0.88(4) O52 C46 1.219(3) O2 C3 1.213(3) O104 H10G 0.91(3) O104 H10H 0.93(5) O101 H10I 0.94(4) O101 H10J 0.88(4) N27 C28 1.406(3) N27 C26 1.396(3) N27 C33 1.481(3) N41 C42 1.339(3) N41 C49 1.387(3) N41 C50 1.458(3) N23 C22 1.339(3) N23 C24 1.358(3) N67 C68 1.403(3) N67 C66 1.399(3) N67 C73 1.467(3) N21 C22 1.342(3) N21 C29 1.385(3) N21 C30 1.456(3) N61 C62 1.336(3) N61 C69 1.385(3) N61 C70 1.461(3) N63 C64 1.353(3) N63 C62 1.338(3) O103 H10K 0.78(5) O103 H10L 0.84(5) N45 C46 1.374(3) N45 C44 1.375(3) N45 C51 1.466(3) N47 C48 1.412(3) N47 C46 1.396(3) N47 C53 1.471(3) N43 C42 1.336(3) N43 C44 1.360(3) N25 C26 1.370(3) N25 C24 1.376(3) N25 C31 1.465(3) N65 C64 1.365(3) N65 C66 1.372(3) N65 C71 1.465(3) C9 C4 1.396(3) C9 C8 1.383(3) C9 H9 1.00(3) C28 C29 1.426(3) C68 C69 1.415(3) C64 C69 1.378(3) C5 C4 1.388(3) C5 C6 1.386(3) C5 H5 0.97(3) C22 H22 0.97(3) C4 C3 1.481(3) C42 H42 0.92(3) C62 H62 0.96(3) C6 C7 1.403(3) C29 C24 1.364(3) C8 C7 1.395(3) C49 C48 1.425(3) C49 C44 1.370(3) C30 H30A 0.9800 C30 H30B 0.9800 C30 H30C 0.9800 C71 H71A 0.9800 C71 H71B 0.9800 C71 H71C 0.9800 C31 H31A 0.9800 C31 H31B 0.9800 C31 H31C 0.9800 C51 H51A 0.9800 C51 H51B 0.9800 C51 H51C 0.9800 C50 H50A 0.94(3) C50 H50B 0.96(4) C50 H50C 1.00(4) C33 H33A 0.9800 C33 H33B 0.9800 C33 H33C 0.9800 C53 H53A 0.9800 C53 H53B 0.9800 C53 H53C 0.9800 C73 H73A 0.9800 C73 H73B 0.9800 C73 H73C 0.9800 C70 H70A 0.9800 C70 H70B 0.9800 C70 H70C 0.9800 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1 O32 2_564 0.85(3) 1.86(3) 2.672(2) 161(3) yes O10 H10 O104 . 0.86(4) 1.79(4) 2.643(2) 174(4) yes O11 H11 O10 . 0.83(3) 2.32(4) 2.709(2) 109(3) yes O11 H11 O102 . 0.83(4) 1.88(4) 2.680(2) 161(3) yes O12 H12 O100 2_564 0.86(3) 1.86(3) 2.702(2) 166(3) yes O100 H10C O105 . 0.83(4) 2.07(4) 2.851(3) 157(4) yes O100 H10D O10 . 0.82(4) 2.74(3) 3.286(2) 126(3) yes O100 H10D O102 . 0.82(4) 2.02(4) 2.798(3) 158(3) yes O101 H10I N43 2_575 0.94(4) 1.97(4) 2.898(3) 170(3) yes O101 H10J O100 . 0.88(4) 2.09(4) 2.960(3) 170(4) yes O102 H10A O101 1_545 0.89(4) 1.87(4) 2.754(3) 169(4) yes O102 H10B O103 . 0.85(4) 1.85(4) 2.691(3) 173(3) yes O103 H10K O34 2_665 0.78(5) 2.06(5) 2.832(3) 168(5) yes O103 H10L N23 1_655 0.84(5) 1.99(5) 2.823(3) 168(4) yes O104 H10G O1 2_565 0.91(3) 2.50(3) 3.011(2) 116(2) yes O104 H10G O105 . 0.91(3) 2.03(3) 2.857(3) 151(3) yes O104 H10H O74 2_565 0.93(5) 2.00(5) 2.924(2) 171(4) yes O105 H10E O74 2_575 0.86(5) 2.11(5) 2.952(2) 169(4) yes O105 H10F N63 . 0.88(4) 1.92(4) 2.798(2) 173(4) yes C22 H22 O72 1_455 0.97(3) 2.38(3) 3.227(3) 146(2) yes C30 H30C O12 1_455 0.98 2.71 3.247(3) 114.7 yes C31 H31C O2 2_565 0.98 2.40 3.326(3) 157.8 yes C42 H42 O12 1_565 0.92(3) 2.45(3) 3.254(3) 146(3) yes C42 H42 O72 . 0.92(3) 2.66(3) 3.136(3) 113(2) yes C62 H62 O52 1_455 0.96(3) 2.24(3) 3.119(3) 151(3) yes loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas 0 0 4 189.37 0 0 4 187.9 0 0 4 200.04 0 0 -4 189.96 0 0 4 203.15 0 0 -4 181.79 0 0 6 269.56 0 0 -6 261.86 0 0 6 247.87 0 0 6 263.3 0 0 -6 268.85 0 0 -6 258.49 0 0 6 267.81 0 0 -6 262.18 0 0 8 1179.69 0 0 8 1321.49 0 0 -8 1214.42 0 0 -8 1266.23 0 0 8 1260.53 0 0 -8 1268.85 0 0 -8 1280.59 0 0 8 1233.62 0 0 -10 233.54 0 0 -10 237.53 0 0 10 245.09 0 0 10 209 0 0 10 218.32 0 0 -10 220.06 0 0 -10 230.02 0 0 -10 222.33 0 0 12 67.87 0 0 -12 72.23 0 0 -12 62.89 0 0 -12 68.53 0 0 -12 66.66 0 0 12 63.07 0 0 12 68.72 0 0 -12 65.83 0 0 14 245.17 0 0 -14 256.94 0 0 -14 246.76 0 0 -14 234.53 0 0 16 14.35 0 0 -16 16.88 0 0 -16 12.96 0 0 -16 16.65 0 0 18 2.06 0 0 -18 4 0 0 18 3.09 0 0 -18 1.08 0 0 18 1.49 0 0 -20 8.15 0 0 20 6.18 0 0 -20 9.51 0 0 -22 36.96 0 0 22 27.67 0 1 0 4.76 0 -1 1 151.01 0 -1 1 152.92 0 -1 1 156.72 0 -1 2 470.4 0 1 -2 491.7 0 -1 -2 528.33 0 -1 2 514.55 0 -1 -2 528 0 -1 2 526.36 0 1 2 499.92 0 1 2 523.02 0 1 2 526.1 0 1 3 163.03 0 -1 -3 151.5 0 -1 3 146.12 0 1 -3 150.04 0 -1 3 151.87 0 -1 3 147.76 0 -1 -3 152.45 0 1 3 162.09 0 1 -3 159.64 0 -1 4 38.94 0 -1 -4 43.83 0 1 -4 38.76 0 1 4 43.68 0 1 4 42.07 0 1 4 38.5 0 1 -4 39.94 0 -1 4 40.7 0 -1 -4 38.58 0 1 -4 37.84 0 -1 -4 39.84 0 -1 -5 81.93 0 -1 -5 84.76 0 1 5 86.38 0 -1 5 82.87 0 -1 -5 83.61 0 1 5 86.26 0 -1 -5 88.6 0 1 -5 82.05 0 -1 -5 67.12 0 1 5 85.36 0 1 -5 84.11 0 -1 5 87.96 0 -1 -6 629.15 0 1 6 638.03 0 1 6 634.69 0 -1 -6 603.84 0 -1 -6 594.24 0 1 -6 625.03 0 -1 -6 630.02 0 -1 -6 622.88 0 1 6 646.58 0 -1 6 616.8 0 -1 6 652.72 0 1 -6 642.77 0 1 7 141.05 0 -1 7 137.59 0 -1 7 125.54 0 -1 -7 133.94 0 1 7 135.58 0 1 7 132.82 0 1 -7 129.95 0 -1 7 130.01 0 1 -7 132.72 0 -1 -7 133.34 0 -1 7 134 0 1 -7 139.42 0 -1 -7 137.57 0 -1 -8 1370.03 0 -1 -8 1335.21 0 1 8 1281.25 0 -1 8 1347.21 0 -1 -8 1284.6 0 -1 8 1316.09 0 -1 8 1289.3 0 1 -8 1342.06 0 -1 8 1286.3 0 -1 -8 1308.38 0 1 8 1409.09 0 1 -8 1249.26 0 -1 -9 293.75 0 -1 -9 275.09 0 1 -9 288.39 0 -1 9 282.19 0 1 -9 289.71 0 -1 -9 288.22 0 1 9 285.37 0 -1 9 277.12 0 1 9 279.97 0 1 -9 272.57 0 -1 -9 279.26 0 -1 9 277.36 0 -1 -10 286.02 0 1 10 309.21 0 -1 -10 281.49 0 1 -10 301.7 0 1 -10 289.59 0 -1 10 300.95 0 1 -10 276 0 -1 -10 275.85 0 1 10 291.84 0 -1 -10 291.52 0 1 10 274.34 0 -1 10 293.84 0 -1 10 271.77 0 -1 11 108.39 0 1 -11 124.44 0 1 -11 94.09 0 1 11 112.94 0 -1 11 115.62 0 1 -11 109.64 0 1 -11 110.95 0 -1 -11 115.2 0 1 11 110.14 0 1 -11 117.81 0 -1 -11 115.26 0 1 11 127.5 0 -1 11 120.24 0 -1 -11 110.34 0 1 -12 23.36 0 -1 -12 23.46 0 1 -12 23.3 0 1 -12 27.09 0 1 12 23.89 0 -1 12 22.32 0 -1 -12 23.44 0 1 12 23.94 0 -1 -12 23.74 0 -1 12 23.4 0 1 -12 19.69 0 -1 -12 23.18 0 1 -12 27.92 0 -1 -13 137.84 0 1 13 123.06 0 -1 -13 131.94 0 -1 13 131.81 0 -1 -13 128.92 0 -1 13 122.61 0 -1 -13 136.94 0 1 -13 137.23 0 -1 13 126.2 0 1 -13 127.9 0 -1 -13 123.79 0 -1 -14 51.38 0 -1 -14 51.39 0 1 -14 36.61 0 1 14 46.52 0 -1 14 44.21 0 1 -14 45.64 0 -1 14 43.36 0 1 -14 47.26 0 -1 -14 45.61 0 -1 -14 47.54 0 -1 -14 46.17 0 -1 -15 14.78 0 1 -15 13.41 0 -1 15 11.69 0 -1 -15 12.87 0 1 -15 14.24 0 -1 -15 12.87 0 1 -15 13.59 0 -1 -15 16.48 0 -1 -15 11.34 0 -1 15 12.99 0 1 -15 10.83 0 1 15 12.38 0 -1 16 87.12 0 1 16 86.7 0 -1 -16 83.5 0 -1 -16 96.22 0 -1 -16 86.66 0 1 -16 98.83 0 -1 -16 94.82 0 -1 16 83.61 0 1 -16 62.58 0 -1 -16 99.56 0 1 16 83.19 0 1 -16 80.18 0 1 -16 92.31 0 1 -17 27.23 0 1 -17 34.06 0 -1 -17 30.68 0 1 -17 23.11 0 -1 17 28.21 0 -1 -17 29.4 0 1 17 26.5 0 -1 -17 31.68 0 -1 -17 23.38 0 1 17 28.13 0 -1 17 26.81 0 1 18 25.12 0 -1 -18 28.56 0 1 18 25.67 0 1 -18 24.33 0 -1 18 22.5 0 -1 -18 25.9 0 1 -18 29.85 0 -1 -18 26.2 0 -1 18 21.67 0 1 -19 8.58 0 1 19 5.89 0 -1 -19 8.81 0 -1 19 7.05 0 -1 -19 8.46 0 1 -19 9.55 0 1 19 7.36 0 -1 19 5.95 0 -1 -19 8.31 0 1 -20 20.33 0 -1 -20 18.49 0 -1 -20 17.28 0 -1 20 15.22 0 -1 20 11.48 0 1 20 11.51 0 1 -20 16.99 0 -1 -21 24.85 0 -1 21 20.12 0 1 -21 23.62 0 1 -21 28.66 0 -1 -21 23.47 0 1 21 20.69 0 1 -22 5.96 0 1 22 4.26 0 1 23 12.4 0 -2 0 9858.18 0 -2 0 9748.33 0 -2 0 9588.9 0 -2 0 9906.97 0 -2 0 9846.8 0 2 0 9680.76 0 2 0 9590.02 0 -2 0 9999 0 2 1 6450.59 0 -2 -1 6695.58 0 -2 1 6480.85 0 2 -1 6482 0 -2 1 6228.51 0 2 1 6599.55 0 -2 1 6365.03 0 -2 -1 6467.18 0 -2 1 6267.42 0 2 -1 6503.62 0 2 -1 6495.67 0 -2 1 6525.17 0 -2 1 6205.61 0 -2 -1 6539.27 0 -2 -1 6581.75 0 -2 1 6201.43 0 2 1 6442.61 0 -2 -1 6583.86 0 -2 -2 709.72 0 2 -2 689.91 0 2 2 700.1 0 2 -2 707.09 0 -2 2 731.81 0 2 -2 749.95 0 -2 -2 720.21 0 -2 -2 698.86 0 -2 2 712.85 0 -2 2 701.22 0 -2 -2 720.71 0 2 2 738.68 0 -2 2 723.27 0 -2 2 737.2 0 -2 3 180.52 0 -2 -3 169.81 0 2 3 176.6 0 -2 3 173.62 0 2 -3 172.04 0 -2 -3 173.84 0 2 3 171.74 0 -2 3 180.62 0 -2 3 167.77 0 -2 -3 173.81 0 2 3 170.1 0 2 -3 187.77 0 -2 -4 126.12 0 2 4 120.33 0 2 4 117.38 0 2 -4 111.87 0 -2 -4 116.15 0 -2 4 115.47 0 -2 4 119.51 0 -2 -4 120.42 0 -2 4 116.86 0 -2 4 106.2 0 2 4 117.53 0 2 4 108.64 0 2 -4 117.4 0 2 5 83.15 0 2 -5 82.07 0 -2 5 77.78 0 2 5 76.35 0 -2 5 76.88 0 2 5 82.07 0 2 5 77.65 0 -2 -5 76.98 0 -2 5 73.32 0 -2 5 72.8 0 -2 5 64.64 0 -2 -5 82.93 0 2 -5 78.31 0 -2 -6 69.85 0 -2 6 61.64 0 2 -6 62.7 0 2 6 70.08 0 -2 6 64.4 0 -2 6 64.42 0 2 6 66.74 0 -2 -6 64.48 0 2 7 180.7 0 -2 7 171.79 0 -2 7 182.39 0 -2 -7 180.5 0 2 -7 182.86 0 2 -7 177.79 0 -2 -7 189.71 0 2 7 184.56 0 -2 8 470.5 0 2 8 474.13 0 -2 -8 483.55 0 -2 -8 480.34 0 2 -8 480.57 0 2 -8 466.08 0 2 8 464.54 0 -2 -9 76.39 0 -2 9 70.07 0 2 9 78.24 0 2 -9 78.21 0 2 9 81.84 0 2 -9 78.7 0 2 9 77.69 0 -2 -9 81.77 0 -2 9 78.3 0 2 -9 76.46 0 -2 9 69.4 0 -2 -9 75.98 0 -2 9 77.09 0 -2 -9 76.93 0 -2 -9 78.78 0 -2 -10 138.83 0 2 10 111.02 0 -2 -10 123.46 0 -2 10 114.29 0 -2 10 125.18 0 2 10 130.37 0 -2 -10 123.1 0 -2 10 121.69 0 -2 -10 120.47 0 2 -10 120.11 0 2 -10 123.47 0 -2 10 124.79 0 2 10 126.43 0 -2 -10 129.36 0 2 -10 132.96 0 2 10 116.46 0 -2 11 8.82 0 -2 11 8.15 0 -2 -11 8.4 0 -2 -11 10.3 0 -2 -11 7.6 0 2 -11 8.83 0 2 -11 7.66 0 -2 -11 8.79 0 2 -11 8.24 0 -2 11 7.96 0 2 11 8.98 0 -2 -11 8.89 0 -2 11 8.76 0 2 11 8.55 0 2 11 7.97 0 2 11 8.52 0 2 -11 9.4 0 2 12 20.2 0 -2 -12 21.2 0 -2 -12 21.69 0 2 -12 21.86 0 -2 -12 20.1 0 -2 -12 21.98 0 2 -12 22 0 2 12 19.63 0 -2 -12 20.84 0 -2 12 20.57 0 -2 12 20.89 0 -2 12 19.71 0 2 -12 19.73 0 -2 13 25.02 0 -2 -13 27.42 0 -2 -13 29.99 0 2 13 26.05 0 -2 13 29.09 0 2 -13 30.53 0 2 -13 29.31 0 2 -13 26.94 0 -2 -13 27.31 0 -2 -13 27.99 0 -2 13 26.29 0 2 13 27.04 0 -2 -13 27.98 0 -2 -14 141.19 0 -2 14 133.28 0 -2 14 135.99 0 -2 -14 142.69 0 2 -14 150.76 0 2 -14 141.88 0 2 14 136.62 0 2 -14 148.99 0 2 14 140.03 0 -2 -14 128.82 0 -2 -14 143.83 0 -2 -15 27.36 0 2 15 22.73 0 2 15 26.17 0 -2 -15 27.97 0 2 -15 26.44 0 2 -15 25.09 0 -2 15 27.33 0 2 -15 29.36 0 -2 15 22.83 0 -2 -15 29.77 0 2 16 12.54 0 2 16 12.79 0 2 -16 12.71 0 2 -16 13.1 0 -2 16 11.17 0 2 -16 11.52 0 -2 -16 15.18 0 -2 -16 13.4 0 -2 16 12.22 0 -2 -16 13.6 0 -2 17 29.75 0 2 17 26.67 0 -2 17 30.56 0 2 -17 34.28 0 -2 -17 32.06 0 -2 -17 31.63 0 2 17 27.8 0 -2 -17 31.57 0 2 -17 33.02 0 2 -17 27.7 0 -2 18 0.66 0 -2 -18 2.04 0 -2 18 0.14 0 2 18 1.64 0 -2 -18 2.36 0 2 -18 1.61 0 -2 -18 2.36 0 2 -18 1.27 0 2 18 0.28 0 2 -18 1.4 0 -2 -19 26.34 0 2 -19 32.77 0 -2 -19 31.29 0 -2 19 30.18 0 -2 -19 29.83 0 2 19 24.22 0 2 19 26.44 0 -2 19 25.07 0 -2 20 1.8 0 -2 -20 0.93 0 -2 20 3.88 0 2 20 1.76 0 2 20 2.89 0 -2 -20 2.37 0 -2 -20 2.11 0 2 -20 5.66 0 -2 21 1.98 0 -2 21 0.87 0 2 21 2.25 0 -3 0 81.61 0 -3 0 86.18 0 3 0 81.88 0 3 0 80.07 0 -3 0 86.56 0 -3 0 86.95 0 -3 0 82.46 0 3 0 78.41 0 -3 0 76.99 0 -3 0 76.47 0 -3 0 78.79 0 -3 -1 108.69 0 -3 1 117.77 0 -3 1 110.33 0 -3 1 108.98 0 -3 1 111.33 0 -3 -1 107.51 0 -3 -1 106.87 0 -3 1 113.75 0 3 1 106.77 0 3 -1 107.33 0 -3 1 111.11 0 -3 -1 118.19 0 -3 -1 115.74 0 -3 -1 109.58 0 3 -1 109.8 0 3 1 116.16 0 3 1 112.39 0 -3 -1 101.07 0 -3 1 109.02 0 3 -1 113.59 0 -3 -2 211.08 0 3 2 212.06 0 3 2 204.08 0 -3 2 201.99 0 -3 2 207.21 0 -3 -2 219.42 0 -3 -2 228.08 0 3 2 217.13 0 -3 2 202.05 0 3 -2 201.05 0 -3 2 216.5 0 -3 2 216.64 0 -3 -2 214.66 0 -3 2 210.5 0 3 -2 210.76 0 3 -2 207.82 0 -3 -2 207.34 0 -3 2 203.87 0 -3 3 43.3 0 -3 3 43.57 0 -3 -3 45.19 0 3 3 46.37 0 3 -3 46.23 0 -3 -3 50.15 0 -3 -3 44.65 0 -3 3 45.13 0 3 -3 41.02 0 -3 3 45.18 0 3 3 45.92 0 -3 -3 47.2 0 -3 3 45.51 0 -3 3 45.37 0 3 -3 46.6 0 3 -4 122.11 0 -3 4 113.52 0 3 -4 119.83 0 -3 -4 126.97 0 3 4 122.68 0 -3 4 121.16 0 -3 4 116.79 0 -3 4 123.04 0 -3 -4 121.93 0 -3 -4 117.92 0 3 4 112.32 0 -3 4 115.92 0 -3 5 83 0 -3 -5 83.68 0 -3 -5 83.63 0 -3 5 80.7 0 3 5 81.82 0 -3 -5 88.51 0 -3 5 86.86 0 -3 5 83.87 0 -3 5 85.69 0 3 -5 77.73 0 -3 5 79.06 0 3 5 81.28 0 3 5 88.77 0 -3 6 67.17 0 -3 -6 65.39 0 -3 6 71.52 0 -3 6 67.77 0 -3 6 69.68 0 -3 6 74.2 0 3 6 68.81 0 -3 -6 72.14 0 3 -6 67.69 0 -3 -6 82.15 0 -3 -6 75.86 0 -3 6 68.32 0 3 6 69.39 0 3 6 64.76 0 -3 -6 70.86 0 3 6 71.25 0 3 6 71.94 0 -3 6 66.38 0 3 7 120.99 0 -3 7 112.12 0 -3 -7 131.34 0 -3 7 112.79 0 3 7 119.77 0 -3 7 115.82 0 3 -7 127.48 0 3 7 117.87 0 -3 7 114.46 0 -3 -7 122.31 0 3 -7 114.56 0 3 7 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