#------------------------------------------------------------------------------ #$Date: 2015-12-09 13:16:15 +0200 (Wed, 09 Dec 2015) $ #$Revision: 170942 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/52/90/1529086.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1529086 loop_ _publ_author_name 'Sanna, Elena' 'Escudero-Ad\'an, Eduardo C.' 'Bauz\'a, Antonio' 'Ballester, Pablo' 'Frontera, Antonio' 'Rotger, Carmen' 'Costa, Antonio' _publ_section_title ; A crystalline sponge based on dispersive forces suitable for X-ray structure determination of included molecular guests ; _journal_issue 10 _journal_name_full 'Chem. Sci.' _journal_page_first 5466 _journal_paper_doi 10.1039/C5SC01838B _journal_volume 6 _journal_year 2015 _chemical_formula_sum 'C74 H72 N4' _chemical_formula_weight 1017.35 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _space_group_name_Hall '-P 1' _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2012 _audit_update_record ; 2014-07-07 deposited with the CCDC. 2015-07-14 downloaded from the CCDC. ; _cell_angle_alpha 82.080(6) _cell_angle_beta 89.417(6) _cell_angle_gamma 83.086(6) _cell_formula_units_Z 2 _cell_length_a 5.8111(13) _cell_length_b 17.553(4) _cell_length_c 28.328(5) _cell_measurement_reflns_used 1304 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.46 _cell_measurement_theta_min 2.36 _cell_volume 2841.1(10) _computing_cell_refinement 'Bruker APEX2 v2011.4-0' _computing_data_collection 'Bruker APEX2 v2011.4-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _computing_structure_solution Sir2011 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 512 _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.868 _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_measurement_specimen_support 'magnetic support with MicroMount' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.0858 _diffrn_reflns_laue_measured_fraction_full 0.994 _diffrn_reflns_laue_measured_fraction_max 0.868 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 21469 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.868 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.572 _diffrn_reflns_theta_min 0.726 _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_current 70 _diffrn_source_power 50 _diffrn_source_size '0.3 mm x 0.3 mm fine focus' _diffrn_source_type 'Bruker-Nonius FR 591' _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.189 _exptl_crystal_description plate _exptl_crystal_F_000 1088 _exptl_crystal_recrystallization_method 'Inmersion in Stilbene' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.594 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.082 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 818 _refine_ls_number_reflns 21469 _refine_ls_number_restraints 246 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.1388 _refine_ls_R_factor_gt 0.0949 _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^)+(0.1083P)^2^+3.1100P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2375 _refine_ls_wR_factor_ref 0.2665 _reflns_Friedel_coverage 0.000 _reflns_number_gt 14509 _reflns_number_total 21469 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c5sc01838b2.cif _cod_data_source_block 3_Stilbene _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to /usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius Adding full bibliography for 1529078--1529087.cif. ; _cod_cif_authors_sg_H-M P-1 _cod_original_cell_volume 2841.2(10) _cod_database_code 1529086 _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. ; _shelx_estimated_absorpt_t_min 0.983 _shelx_estimated_absorpt_t_max 0.998 _shelxl_version_number 2012-9 _shelx_res_file ; TITL E66_St-04 in P-1 CELL 0.71073 5.8111 17.5534 28.3283 82.080 89.417 83.086 ZERR 2.00 0.0013 0.0036 0.0047 0.006 0.006 0.006 LATT 1 SFAC C H N UNIT 148 144 8 MERG 0 L.S. 20 ACTA BOND FMAP 2 PLAN 25 SIZE 0.030 0.100 0.250 conf TEMP -173.000 WGHT 0.108300 3.110000 BASF 0.50024 FVAR 0.38542 C1 1 0.910573 0.132101 0.381507 11.00000 0.02449 0.01516 = 0.01877 0.00122 0.00171 0.00039 C2 1 1.031134 0.081746 0.425317 11.00000 0.02635 0.01924 = 0.01692 0.00051 -0.00067 -0.00355 AFIX 23 H2A 2 1.192746 0.093637 0.427278 11.00000 -1.20000 H2B 2 0.950007 0.094925 0.454549 11.00000 -1.20000 AFIX 0 C3 1 1.032870 -0.004580 0.423109 11.00000 0.03522 0.01824 = 0.02234 0.00215 -0.00202 0.00057 AFIX 23 H3A 2 1.130526 -0.019145 0.396163 11.00000 -1.20000 H3B 2 1.102145 -0.034373 0.452848 11.00000 -1.20000 AFIX 0 C4 1 0.791830 -0.025513 0.416860 11.00000 0.04016 0.01975 = 0.02730 0.00159 0.00283 -0.00592 AFIX 23 H4A 2 0.698113 -0.015934 0.445296 11.00000 -1.20000 H4B 2 0.800229 -0.081310 0.413868 11.00000 -1.20000 AFIX 0 C5 1 0.675347 0.022325 0.372541 11.00000 0.02517 0.02317 = 0.02958 -0.00008 -0.00001 -0.00606 AFIX 23 H5A 2 0.514966 0.009636 0.369853 11.00000 -1.20000 H5B 2 0.761169 0.009231 0.343801 11.00000 -1.20000 AFIX 0 C6 1 0.670435 0.108821 0.375255 11.00000 0.02291 0.02152 = 0.02409 0.00033 -0.00202 0.00024 AFIX 23 H6A 2 0.599190 0.138620 0.345703 11.00000 -1.20000 H6B 2 0.572283 0.122396 0.402352 11.00000 -1.20000 AFIX 0 C7 1 1.044653 0.124722 0.337353 11.00000 0.02686 0.01708 = 0.02171 0.00080 -0.00337 -0.00167 C8 1 1.139210 0.123369 0.299660 11.00000 0.02340 0.02261 = 0.02168 0.00067 -0.00189 0.00008 C9 1 1.246187 0.127423 0.253672 11.00000 0.02604 0.02508 = 0.01619 0.00006 0.00013 -0.00273 C10 1 1.463842 0.089318 0.246968 11.00000 0.02800 0.02662 = 0.01780 0.00231 -0.00223 -0.00063 AFIX 43 H10 2 1.543529 0.057364 0.272979 11.00000 -1.20000 AFIX 0 C11 1 1.566415 0.097521 0.202443 11.00000 0.02135 0.02861 = 0.02643 -0.00184 0.00406 0.00203 AFIX 43 H11 2 1.715793 0.071026 0.197987 11.00000 -1.20000 AFIX 0 C12 1 1.450742 0.144551 0.164246 11.00000 0.03272 0.02797 = 0.02039 0.00006 0.00375 0.00062 AFIX 43 H12 2 1.522600 0.150536 0.133906 11.00000 -1.20000 AFIX 0 C13 1 1.232479 0.182517 0.170162 11.00000 0.03050 0.02616 = 0.01874 0.00079 -0.00171 -0.00131 C14 1 1.129058 0.173284 0.215089 11.00000 0.02334 0.03143 = 0.02016 0.00064 -0.00050 0.00421 AFIX 43 H14 2 0.977716 0.198471 0.219357 11.00000 -1.20000 AFIX 0 C15 1 1.112376 0.231584 0.131097 11.00000 0.03444 0.02722 = 0.02083 -0.00116 0.00130 -0.00215 C16 1 1.010846 0.271742 0.098821 11.00000 0.02972 0.02109 = 0.01926 -0.00138 -0.00044 -0.00091 C17 1 0.876687 0.316642 0.057977 11.00000 0.02611 0.01881 = 0.01946 0.00298 0.00025 0.00101 C18 1 0.661074 0.278395 0.050321 11.00000 0.02960 0.02361 = 0.03393 0.00021 -0.00218 0.00072 AFIX 23 H18A 2 0.566173 0.276628 0.079586 11.00000 -1.20000 H18B 2 0.567166 0.309985 0.024069 11.00000 -1.20000 AFIX 0 C19 1 0.721503 0.196574 0.038265 11.00000 0.03012 0.02346 = 0.04660 -0.00267 -0.00805 -0.00184 AFIX 23 H19A 2 0.803228 0.163627 0.065664 11.00000 -1.20000 H19B 2 0.577149 0.174522 0.032380 11.00000 -1.20000 AFIX 0 C20 1 0.874254 0.196084 -0.005521 11.00000 0.04981 0.02678 = 0.02952 -0.00626 -0.01330 0.00785 AFIX 23 H20A 2 0.921911 0.141909 -0.010913 11.00000 -1.20000 H20B 2 0.784958 0.223073 -0.033799 11.00000 -1.20000 AFIX 0 C21 1 1.087053 0.235446 0.000331 11.00000 0.04215 0.02707 = 0.02224 0.00540 0.00848 0.00812 AFIX 23 H21A 2 1.176732 0.237837 -0.029629 11.00000 -1.20000 H21B 2 1.186493 0.204451 0.025934 11.00000 -1.20000 AFIX 0 C22 1 1.024723 0.316873 0.012587 11.00000 0.02699 0.02687 = 0.02328 0.00522 0.00258 -0.00057 AFIX 23 H22A 2 0.937742 0.349308 -0.014333 11.00000 -1.20000 H22B 2 1.168540 0.339932 0.017422 11.00000 -1.20000 AFIX 0 C23 1 0.929368 0.431869 0.087837 11.00000 0.03476 0.03004 = 0.04247 -0.00730 -0.00756 0.00446 AFIX 43 H23 2 1.069050 0.403946 0.101243 11.00000 -1.20000 AFIX 0 C24 1 0.870151 0.513911 0.095216 11.00000 0.03907 0.02558 = 0.03473 -0.00380 -0.00427 0.00114 C25 1 0.655152 0.555363 0.081211 11.00000 0.03693 0.02419 = 0.02903 0.00053 -0.00341 -0.00361 AFIX 43 H25 2 0.545995 0.531927 0.065028 11.00000 -1.20000 AFIX 0 C26 1 0.602234 0.630138 0.090935 11.00000 0.03055 0.02323 = 0.03001 0.00179 -0.00278 0.00105 AFIX 43 H26 2 0.455886 0.658038 0.081527 11.00000 -1.20000 AFIX 0 C27 1 0.761208 0.665332 0.114446 11.00000 0.03342 0.02535 = 0.02660 -0.00040 -0.00301 0.00044 C28 1 0.974845 0.625254 0.126778 11.00000 0.03715 0.03754 = 0.05556 -0.01669 -0.00912 0.00017 AFIX 43 H28 2 1.086797 0.649834 0.141371 11.00000 -1.20000 AFIX 0 C29 1 1.028888 0.548972 0.118099 11.00000 0.03813 0.03706 = 0.06615 -0.01818 -0.01670 0.00613 AFIX 43 H29 2 1.174733 0.521083 0.127903 11.00000 -1.20000 AFIX 0 C30 1 0.709419 0.745709 0.125048 11.00000 0.03107 0.02831 = 0.03132 -0.00474 -0.00284 -0.00406 AFIX 43 H30 2 0.819044 0.766353 0.142805 11.00000 -1.20000 AFIX 0 C31 1 0.493843 0.870190 0.119292 11.00000 0.02649 0.01987 = 0.01571 -0.00027 -0.00019 -0.00279 C32 1 0.586749 0.915814 0.074260 11.00000 0.02648 0.02110 = 0.01728 -0.00005 0.00113 -0.00136 AFIX 23 H32A 2 0.757533 0.903815 0.073568 11.00000 -1.20000 H32B 2 0.522896 0.898603 0.045780 11.00000 -1.20000 AFIX 0 C33 1 0.524191 1.003509 0.071749 11.00000 0.03288 0.02208 = 0.02019 0.00385 0.00201 -0.00086 AFIX 23 H33A 2 0.604191 1.022160 0.097844 11.00000 -1.20000 H33B 2 0.577866 1.029573 0.041093 11.00000 -1.20000 AFIX 0 C34 1 0.264612 1.024286 0.076003 11.00000 0.03382 0.02400 = 0.02374 0.00323 -0.00375 0.00252 AFIX 23 H34A 2 0.185245 1.010057 0.048300 11.00000 -1.20000 H34B 2 0.228748 1.080888 0.075920 11.00000 -1.20000 AFIX 0 C35 1 0.176387 0.981780 0.121819 11.00000 0.02390 0.02608 = 0.02615 -0.00335 -0.00033 0.00065 AFIX 23 H35A 2 0.006316 0.994892 0.123702 11.00000 -1.20000 H35B 2 0.247695 0.998897 0.149536 11.00000 -1.20000 AFIX 0 C36 1 0.234706 0.894068 0.123814 11.00000 0.02454 0.02464 = 0.02062 -0.00043 -0.00049 -0.00481 AFIX 23 H36A 2 0.179797 0.868139 0.154394 11.00000 -1.20000 H36B 2 0.151826 0.876521 0.097695 11.00000 -1.20000 AFIX 0 C37 1 0.615622 0.882745 0.162746 11.00000 0.02047 0.01797 = 0.02351 0.00268 0.00129 -0.00229 C38 1 0.708272 0.887779 0.199267 11.00000 0.02192 0.02122 = 0.01981 0.00201 0.00026 -0.00406 C39 1 0.830803 0.885603 0.243673 11.00000 0.02587 0.02036 = 0.01786 -0.00094 0.00008 -0.00028 C40 1 0.766768 0.837683 0.283616 11.00000 0.02104 0.02360 = 0.01989 -0.00086 0.00055 -0.00416 AFIX 43 H40 2 0.633852 0.811400 0.282210 11.00000 -1.20000 AFIX 0 C41 1 0.895510 0.827784 0.325714 11.00000 0.02846 0.01976 = 0.01614 0.00025 -0.00085 -0.00027 C42 1 1.090283 0.866507 0.327472 11.00000 0.03182 0.02472 = 0.01918 -0.00220 -0.00528 -0.00242 AFIX 43 H42 2 1.182791 0.858702 0.355576 11.00000 -1.20000 AFIX 0 C43 1 1.148640 0.916340 0.288203 11.00000 0.02172 0.02485 = 0.02761 -0.00214 -0.00018 -0.00792 AFIX 43 H43 2 1.277783 0.944311 0.289899 11.00000 -1.20000 AFIX 0 C44 1 1.020044 0.925802 0.246350 11.00000 0.02809 0.02453 = 0.01934 -0.00030 0.00135 -0.00676 AFIX 43 H44 2 1.061940 0.959919 0.219494 11.00000 -1.20000 AFIX 0 C45 1 0.830035 0.776617 0.366367 11.00000 0.02839 0.02013 = 0.01907 -0.00206 -0.00268 -0.00142 C46 1 0.771091 0.734911 0.400022 11.00000 0.02503 0.01904 = 0.02024 -0.00185 -0.00145 -0.00060 C47 1 0.668361 0.687047 0.440363 11.00000 0.02519 0.01674 = 0.01954 0.00231 -0.00090 -0.00445 C48 1 0.408827 0.713738 0.440914 11.00000 0.02190 0.02427 = 0.03419 0.00291 -0.00197 -0.00206 AFIX 23 H48A 2 0.334424 0.679441 0.465634 11.00000 -1.20000 H48B 2 0.340293 0.709445 0.409677 11.00000 -1.20000 AFIX 0 C49 1 0.359654 0.797290 0.451065 11.00000 0.01987 0.02527 = 0.04217 0.00254 0.00566 0.00211 AFIX 23 H49A 2 0.421070 0.832158 0.424724 11.00000 -1.20000 H49B 2 0.189998 0.811827 0.452470 11.00000 -1.20000 AFIX 0 C50 1 0.469737 0.807954 0.497836 11.00000 0.04648 0.02382 = 0.02642 -0.00063 0.01103 -0.00170 AFIX 23 H50A 2 0.447432 0.863541 0.501740 11.00000 -1.20000 H50B 2 0.391640 0.779189 0.524644 11.00000 -1.20000 AFIX 0 C51 1 0.726553 0.779271 0.499423 11.00000 0.04634 0.02763 = 0.01774 0.00052 -0.00419 -0.00456 AFIX 23 H51A 2 0.788330 0.781574 0.531570 11.00000 -1.20000 H51B 2 0.808233 0.813880 0.476200 11.00000 -1.20000 AFIX 0 C52 1 0.775547 0.696263 0.487955 11.00000 0.02882 0.02388 = 0.01909 0.00081 -0.00324 -0.00022 AFIX 23 H52A 2 0.945252 0.681591 0.486911 11.00000 -1.20000 H52B 2 0.712373 0.660647 0.513656 11.00000 -1.20000 AFIX 0 C53 1 0.880222 0.575024 0.416892 11.00000 0.03600 0.02121 = 0.03060 0.00034 0.00209 -0.00609 AFIX 43 H53 2 0.993836 0.608001 0.406186 11.00000 -1.20000 AFIX 0 C54 1 0.923044 0.492145 0.410899 11.00000 0.03720 0.01962 = 0.03024 -0.00134 -0.00034 -0.00276 C55 1 0.757587 0.442573 0.424626 11.00000 0.03379 0.02155 = 0.03302 -0.00098 0.00735 -0.00176 AFIX 43 H55 2 0.622334 0.460625 0.440860 11.00000 -1.20000 AFIX 0 C56 1 0.789351 0.367141 0.414719 11.00000 0.03256 0.01859 = 0.03200 0.00185 0.00266 -0.00517 AFIX 43 H56 2 0.675632 0.333594 0.424242 11.00000 -1.20000 AFIX 0 C57 1 0.987631 0.339678 0.390771 11.00000 0.03409 0.02036 = 0.02455 0.00078 -0.00049 -0.00141 C58 1 1.154407 0.388358 0.378408 11.00000 0.03309 0.02775 = 0.04107 -0.00493 0.00862 -0.00592 AFIX 43 H58 2 1.292021 0.369902 0.363074 11.00000 -1.20000 AFIX 0 C59 1 1.121922 0.464615 0.388322 11.00000 0.03613 0.02412 = 0.04657 -0.00190 0.00502 -0.00879 AFIX 43 H59 2 1.237229 0.497859 0.379503 11.00000 -1.20000 AFIX 0 C60 1 1.017070 0.260181 0.378119 11.00000 0.02846 0.02196 = 0.02384 0.00055 0.00239 0.00144 AFIX 43 H60 2 1.142998 0.244632 0.358554 11.00000 -1.20000 AFIX 0 N1 3 0.877370 0.212739 0.392934 11.00000 0.03037 0.01783 = 0.02009 -0.00027 0.00032 0.00041 N2 3 0.697831 0.603372 0.435748 11.00000 0.03704 0.01817 = 0.02165 0.00188 -0.00103 -0.00281 N3 3 0.800004 0.398074 0.064323 11.00000 0.03499 0.02157 = 0.02198 0.00195 -0.00077 -0.00004 N4 3 0.524801 0.787724 0.111322 11.00000 0.03099 0.01821 = 0.02223 -0.00003 -0.00166 -0.00063 rem eadp c6s c14' PART 1 10.5 DELU 0.005 C1S > C14S SIMU 0.005 C1S > C14S C1S 1 0.609977 0.421727 0.263093 10.50000 0.06248 0.04190 = 0.04605 -0.00364 -0.00846 -0.00767 C2S 1 0.616769 0.344224 0.275806 10.50000 0.05233 0.04709 = 0.04592 0.00077 0.00144 -0.00264 AFIX 43 H2S 2 0.655454 0.321533 0.307567 10.50000 -1.20000 AFIX 0 C3S 1 0.565508 0.297114 0.241213 10.50000 0.05436 0.03854 = 0.06108 -0.00784 0.00585 -0.01230 AFIX 43 H3S 2 0.553233 0.243621 0.250340 10.50000 -1.20000 AFIX 0 C4S 1 0.534166 0.329499 0.194823 10.50000 0.05900 0.04433 = 0.05336 -0.01793 0.00188 -0.01045 AFIX 43 H4S 2 0.514035 0.296896 0.171432 10.50000 -1.20000 AFIX 0 C5S 1 0.530898 0.403610 0.181501 10.50000 0.05497 0.05076 = 0.04459 -0.00703 -0.00228 -0.01148 AFIX 43 H5S 2 0.504186 0.424209 0.148953 10.50000 -1.20000 AFIX 0 C6S 1 0.566126 0.452846 0.214457 10.50000 0.06218 0.04252 = 0.04545 -0.00103 -0.00701 -0.01681 AFIX 43 H6S 2 0.560992 0.506995 0.204603 10.50000 -1.20000 AFIX 0 C7S 1 0.672240 0.470135 0.297289 10.50000 0.07649 0.05471 = 0.05196 -0.00607 -0.02228 0.00253 AFIX 43 H7S1 2 0.785213 0.445557 0.320225 10.50000 -1.20000 AFIX 0 C8S 1 0.596230 0.544129 0.301849 10.50000 0.08597 0.05310 = 0.05472 -0.01501 -0.02862 -0.00104 AFIX 43 H8S1 2 0.682994 0.567826 0.322757 10.50000 -1.20000 AFIX 0 C9S 1 0.397684 0.592087 0.278676 10.50000 0.09284 0.04568 = 0.06458 -0.00780 -0.02394 -0.00075 C10S 1 0.181121 0.564479 0.270637 10.50000 0.08629 0.05467 = 0.06397 -0.00615 -0.01797 -0.00178 AFIX 43 H10S 2 0.169838 0.510764 0.279006 10.50000 -1.20000 AFIX 0 C11S 1 -0.005489 0.610024 0.252054 10.50000 0.08659 0.06445 = 0.07080 -0.01096 -0.00973 0.00252 AFIX 43 H11S 2 -0.146573 0.589062 0.248467 10.50000 -1.20000 AFIX 0 C12S 1 0.008385 0.690134 0.237666 10.50000 0.09677 0.06096 = 0.07105 -0.01404 -0.01329 0.01309 AFIX 43 H12S 2 -0.125187 0.724698 0.227020 10.50000 -1.20000 AFIX 0 C13S 1 0.244456 0.718610 0.239904 10.50000 0.10722 0.04822 = 0.07383 -0.00665 -0.02139 0.00364 AFIX 43 H13S 2 0.270843 0.769057 0.225720 10.50000 -1.20000 AFIX 0 C14S 1 0.409936 0.670105 0.262380 10.50000 0.10096 0.04599 = 0.08094 -0.01022 -0.02461 -0.00190 AFIX 43 H14S 2 0.550679 0.689931 0.268055 10.50000 -1.20000 AFIX 0 PART 2 10.5 DELU 0.005 C1' > C14' SIMU 0.005 C1' > C14' C1' 1 0.236168 0.561524 0.255619 10.50000 0.09058 0.07176 = 0.07936 -0.01569 -0.02243 0.00280 C2' 1 0.392639 0.541228 0.288807 10.50000 0.08514 0.06892 = 0.07024 -0.01042 -0.01413 -0.00142 AFIX 43 H2' 2 0.453028 0.488330 0.296916 10.50000 -1.20000 AFIX 0 C3' 1 0.476415 0.601686 0.314016 10.50000 0.08046 0.07314 = 0.05890 -0.00911 -0.01115 -0.00039 AFIX 43 H3' 2 0.596241 0.587727 0.337266 10.50000 -1.20000 AFIX 0 C4' 1 0.389975 0.670525 0.304736 10.50000 0.08416 0.06898 = 0.06018 -0.02323 -0.00421 0.00094 AFIX 43 H4' 2 0.427737 0.706536 0.324714 10.50000 -1.20000 AFIX 0 C5' 1 0.236191 0.697690 0.265263 10.50000 0.08915 0.07027 = 0.07145 -0.02809 -0.01098 0.01350 AFIX 43 H5' 2 0.200242 0.751103 0.253448 10.50000 -1.20000 AFIX 0 C6' 1 0.147185 0.641905 0.246348 10.50000 0.09570 0.07401 = 0.08086 -0.02162 -0.02304 0.01070 AFIX 43 H6' 2 0.017374 0.656391 0.225547 10.50000 -1.20000 AFIX 0 C7' 1 0.115902 0.507452 0.229599 10.50000 0.09099 0.07847 = 0.08135 -0.01813 -0.01682 -0.00214 AFIX 43 H7'1 2 -0.037070 0.524023 0.217860 10.50000 -1.20000 AFIX 0 C8' 1 0.217724 0.436370 0.222384 10.50000 0.09602 0.07893 = 0.08482 -0.01652 -0.00852 -0.00623 AFIX 43 H8'1 2 0.115150 0.404455 0.211207 10.50000 -1.20000 AFIX 66 C9' 1 0.447580 0.401651 0.228501 10.50000 0.09943 0.07215 = 0.07841 -0.00842 -0.00069 -0.00264 C10' 1 0.483324 0.329614 0.256419 10.50000 0.10303 0.06651 = 0.07278 -0.01645 0.00710 -0.00611 AFIX 43 H10' 2 0.354784 0.303036 0.266705 10.50000 -1.20000 AFIX 65 C11' 1 0.707140 0.296464 0.269288 10.50000 0.10753 0.06531 = 0.06936 -0.01030 0.00130 -0.00290 AFIX 43 H11' 2 0.731568 0.247229 0.288368 10.50000 -1.20000 AFIX 65 C12' 1 0.895214 0.335350 0.254238 10.50000 0.10404 0.07099 = 0.07694 -0.00775 0.00127 -0.00121 AFIX 43 H12' 2 1.048182 0.312693 0.263033 10.50000 -1.20000 AFIX 65 C13' 1 0.859473 0.407387 0.226320 10.50000 0.10128 0.07459 = 0.08246 -0.00354 0.00587 -0.00176 AFIX 43 H13' 2 0.988014 0.433964 0.216034 10.50000 -1.20000 AFIX 65 C14' 1 0.635658 0.440538 0.213451 10.50000 0.10205 0.07556 = 0.08091 -0.00080 0.00492 -0.00254 AFIX 43 H14' 2 0.611230 0.489772 0.194370 10.50000 -1.20000 PART 0 AFIX 0 HKLF 5 REM E66_St-04 in P-1 REM R1 = 0.0949 for 14509 Fo > 4sig(Fo) and 0.1388 for all 21469 data REM 818 parameters refined using 246 restraints END WGHT 0.1075 3.0118 REM Highest difference peak 0.594, deepest hole -0.471, 1-sigma level 0.082 Q1 1 0.3803 0.6726 0.2222 11.00000 0.05 0.59 Q2 1 0.1683 0.3703 0.2399 11.00000 0.05 0.53 Q3 1 0.4525 0.5945 0.2342 11.00000 0.05 0.52 Q4 1 0.4922 0.6272 0.2237 11.00000 0.05 0.44 Q5 1 0.6741 0.5916 0.2741 11.00000 0.05 0.40 Q6 1 0.5473 0.7102 0.4394 11.00000 0.05 0.39 Q7 1 0.6270 0.6472 0.1275 11.00000 0.05 0.39 Q8 1 0.6474 0.3587 0.1826 11.00000 0.05 0.37 Q9 1 0.6595 0.4888 0.1177 11.00000 0.05 0.36 Q10 1 0.7242 0.4738 0.5114 11.00000 0.05 0.34 Q11 1 1.0408 0.2998 0.3896 11.00000 0.05 0.33 Q12 1 0.7553 0.5108 0.2864 11.00000 0.05 0.33 Q13 1 0.3333 0.3475 0.2090 11.00000 0.05 0.33 Q14 1 0.2114 0.6698 0.3089 11.00000 0.05 0.32 Q15 1 -0.3770 0.6044 0.2394 11.00000 0.05 0.32 Q16 1 0.3654 0.8899 0.1182 11.00000 0.05 0.32 Q17 1 0.5207 0.4499 0.4264 11.00000 0.05 0.32 Q18 1 0.7600 0.0581 0.3708 11.00000 0.05 0.32 Q19 1 -0.3865 0.5844 0.2394 11.00000 0.05 0.32 Q20 1 0.7480 0.2504 0.3815 11.00000 0.05 0.31 Q21 1 0.4678 0.5643 0.4582 11.00000 0.05 0.31 Q22 1 0.6590 0.5967 0.1667 11.00000 0.05 0.31 Q23 1 0.8736 0.3694 0.3923 11.00000 0.05 0.31 Q24 1 0.7045 0.4197 0.1028 11.00000 0.05 0.30 Q25 1 1.1975 0.5806 0.4195 11.00000 0.05 0.30 ; _shelx_res_checksum 93771 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-2 4 36 2.73720 1.64138 1 1 5 36 25.6014 2.70328 -2 -1 4 36 25.6014 2.70328 1 -1 4 36 5.13649 1.83954 1 -1 4 36 4.55793 2.02040 2 0 4 36 13.1196 1.44610 -2 0 4 36 13.1196 1.44610 1 1 4 36 0.94356 1.81462 2 1 4 36 -0.8228 1.74361 1 2 4 36 2.13034 1.97993 1 2 4 36 3.95120 1.45089 2 -2 5 36 2.58996 1.24383 1 -2 5 36 3.39860 1.52556 2 1 6 36 0.98134 2.32925 -2 -1 5 36 0.98134 2.32925 1 -1 5 36 -0.0636 1.72915 2 -1 5 36 3.36483 1.80613 1 0 5 36 11.6112 1.39131 -2 0 5 36 11.6112 1.39131 1 -1 4 36 16.8851 3.44552 -2 1 5 36 16.8851 3.44552 1 1 5 36 15.2787 2.41230 1 1 5 36 10.9661 2.09953 2 2 5 36 1.18269 1.45151 1 2 5 36 -1.7371 1.45196 2 -2 6 36 1.37526 1.21089 1 -1 6 36 -1.0533 1.73449 1 -1 6 36 -1.5616 1.75315 2 1 7 36 -2.2925 2.32446 -2 -1 6 36 -2.2925 2.32446 1 0 6 36 8.45261 1.29613 -2 0 6 36 8.45261 1.29613 1 1 6 36 -1.4488 1.79482 1 -1 5 36 5.55661 3.30166 -2 1 6 36 5.55661 3.30166 1 1 6 36 1.71385 1.74710 2 2 6 36 11.8378 1.76484 1 2 6 36 10.0044 1.39981 2 1 8 36 4.89730 2.51401 -2 -1 7 36 4.89730 2.51401 1 -1 7 36 1.95652 1.89101 2 -1 7 36 -0.1492 1.72855 1 0 7 36 4.47122 1.29403 -2 0 7 36 4.47122 1.29403 1 1 7 36 0.48458 1.86433 1 1 7 36 -3.8294 1.72307 2 -1 6 36 -2.9112 3.26483 -2 1 7 36 -2.9112 3.26483 1 2 7 36 0.04746 1.43426 1 2 7 36 -0.5924 1.22554 2 1 9 36 4.29062 2.56198 -2 -1 8 36 4.29062 2.56198 1 -1 8 36 1.68362 1.81324 1 -1 8 36 -0.4588 1.82109 2 0 8 36 4.04913 1.30410 -2 0 8 36 4.04913 1.30410 1 1 8 36 4.14606 1.92070 1 -1 7 36 3.79280 3.26529 -2 1 8 36 3.79280 3.26529 1 1 8 36 4.83254 1.92821 2 2 8 36 0.47042 1.21351 2 2 8 36 -0.8989 1.40338 1 1 10 36 27.1843 3.05584 -2 -1 9 36 27.1843 3.05584 1 -1 9 36 6.24800 2.08504 1 -1 9 36 6.06204 2.24232 2 0 9 36 83.8482 3.71915 -2 0 9 36 83.8482 3.71915 1 -1 8 36 3.50093 3.41060 -2 1 9 36 3.50093 3.41060 1 1 9 36 3.34844 1.90033 1 1 9 36 1.81120 1.91660 2 0 10 36 2.95960 1.33570 -2 0 10 36 2.95960 1.33570 1 1 10 36 20.7077 2.78488 1 1 10 36 24.6811 3.01105 2 -1 9 36 23.5079 4.02259 -2 1 10 36 23.5079 4.02259 1 0 -2 37 2.77826 2.29055 -2 0 -2 37 2.77826 2.29055 1 1 0 37 1.70287 2.26686 -2 -1 -1 37 1.70287 2.26686 1 0 -1 37 3.31144 1.50400 -2 0 -1 37 3.31144 1.50400 1 1 -1 37 5.36544 2.40289 2 1 -1 37 6.25078 2.38457 1 1 1 37 -1.3448 2.20571 -2 -1 0 37 -1.3448 2.20571 1 0 0 37 1.99731 1.58148 -2 0 0 37 1.99731 1.58148 1 -1 -1 37 4.28252 2.21949 -2 1 0 37 4.28252 2.21949 1 1 2 37 4.29496 2.21090 -2 -1 1 37 4.29496 2.21090 1 -1 1 37 7.35561 2.07333 2 0 1 37 1.12765 1.18414 -2 0 1 37 1.12765 1.18414 1 -1 0 37 -4.1274 2.65434 -2 1 1 37 -4.1274 2.65434 1 -1 2 37 -0.0970 1.73782 1 -1 2 37 -0.4454 1.82644 2 0 2 37 4.58000 1.24096 -2 0 2 37 4.58000 1.24096 1 1 2 37 3.32743 1.90539 1 -1 3 37 1.20762 1.88891 1 -1 3 37 3.45493 1.91834 2 1 4 37 4.12993 3.70310 -2 -1 3 37 4.12993 3.70310 1 0 3 37 4.19315 1.27154 -2 0 3 37 4.19315 1.27154 1 1 3 37 2.87846 2.01642 2 1 3 37 -2.1650 1.73663 1 -1 4 37 -1.9234 1.77111 2 -1 4 37 -0.5364 1.70451 1 1 5 37 2.52702 2.36219 -2 -1 4 37 2.52702 2.36219 1 0 4 37 2.91423 1.23759 -2 0 4 37 2.91423 1.23759 1 1 4 37 2.68232 1.89243 1 1 4 37 2.93664 1.94605 2 1 6 37 6.95866 2.41491 -2 -1 5 37 6.95866 2.41491 1 -1 5 37 2.69467 1.88527 1 -1 5 37 -1.1302 1.87320 2 0 5 37 0.38590 1.22327 -2 0 5 37 0.38590 1.22327 1 1 5 37 1.01358 1.78917 2 1 5 37 1.08907 1.94757 1 -1 6 37 -2.2912 1.72648 2 1 7 37 -3.8289 2.35294 -2 -1 6 37 -3.8289 2.35294 1 -1 6 37 -0.7493 1.73224 1 0 6 37 1.05880 1.25007 -2 0 6 37 1.05880 1.25007 1 -1 5 37 3.63308 3.29414 -2 1 6 37 3.63308 3.29414 1 1 6 37 1.73594 1.94107 1 1 6 37 -1.5849 1.68851 2 0 7 37 11.6468 1.46365 -2 0 7 37 11.6468 1.46365 1 -1 6 37 -5.4821 3.28921 -2 1 7 37 -5.4821 3.28921 1 1 7 37 1.63575 1.98672 1 1 7 37 1.84663 1.90764 2 0 8 37 -0.8461 1.25970 -2 0 8 37 -0.8461 1.25970 1 0 3 38 2.82755 2.33593 -2 0 3 38 2.82755 2.33593 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 20647 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9106(7) 0.13210(17) 0.38151(11) 0.0200(7) Uani 1 1 d . . . . . C2 C 1.0311(7) 0.08175(18) 0.42532(11) 0.0210(7) Uani 1 1 d . . . . . H2A H 1.1927 0.0936 0.4273 0.025 Uiso 1 1 calc R U . . . H2B H 0.9500 0.0949 0.4545 0.025 Uiso 1 1 calc R U . . . C3 C 1.0329(7) -0.00458(19) 0.42311(12) 0.0260(8) Uani 1 1 d . . . . . H3A H 1.1305 -0.0191 0.3962 0.031 Uiso 1 1 calc R U . . . H3B H 1.1021 -0.0344 0.4528 0.031 Uiso 1 1 calc R U . . . C4 C 0.7918(8) -0.0255(2) 0.41686(13) 0.0294(9) Uani 1 1 d . . . . . H4A H 0.6981 -0.0159 0.4453 0.035 Uiso 1 1 calc R U . . . H4B H 0.8002 -0.0813 0.4139 0.035 Uiso 1 1 calc R U . . . C5 C 0.6753(7) 0.02232(19) 0.37254(12) 0.0260(8) Uani 1 1 d . . . . . H5A H 0.5150 0.0096 0.3699 0.031 Uiso 1 1 calc R U . . . H5B H 0.7612 0.0092 0.3438 0.031 Uiso 1 1 calc R U . . . C6 C 0.6704(7) 0.10882(19) 0.37526(12) 0.0234(7) Uani 1 1 d . . . . . H6A H 0.5992 0.1386 0.3457 0.028 Uiso 1 1 calc R U . . . H6B H 0.5723 0.1224 0.4024 0.028 Uiso 1 1 calc R U . . . C7 C 1.0447(7) 0.12472(18) 0.33735(11) 0.0223(7) Uani 1 1 d . . . . . C8 C 1.1392(7) 0.12337(19) 0.29966(11) 0.0231(7) Uani 1 1 d . . . . . C9 C 1.2462(7) 0.12742(19) 0.25367(11) 0.0227(7) Uani 1 1 d . . . . . C10 C 1.4638(7) 0.0893(2) 0.24697(12) 0.0248(8) Uani 1 1 d . . . . . H10 H 1.5435 0.0574 0.2730 0.030 Uiso 1 1 calc R U . . . C11 C 1.5664(7) 0.0975(2) 0.20244(12) 0.0261(8) Uani 1 1 d . . . . . H11 H 1.7158 0.0710 0.1980 0.031 Uiso 1 1 calc R U . . . C12 C 1.4507(7) 0.1446(2) 0.16425(12) 0.0277(8) Uani 1 1 d . . . . . H12 H 1.5226 0.1505 0.1339 0.033 Uiso 1 1 calc R U . . . C13 C 1.2325(7) 0.1825(2) 0.17016(11) 0.0257(8) Uani 1 1 d . . . . . C14 C 1.1291(7) 0.1733(2) 0.21509(11) 0.0260(8) Uani 1 1 d . . . . . H14 H 0.9777 0.1985 0.2194 0.031 Uiso 1 1 calc R U . . . C15 C 1.1124(7) 0.2316(2) 0.13110(12) 0.0278(8) Uani 1 1 d . . . . . C16 C 1.0108(7) 0.27174(19) 0.09882(11) 0.0237(8) Uani 1 1 d . . . . . C17 C 0.8767(7) 0.31664(18) 0.05798(11) 0.0223(7) Uani 1 1 d . . . . . C18 C 0.6611(7) 0.2784(2) 0.05032(14) 0.0297(8) Uani 1 1 d . . . . . H18A H 0.5662 0.2766 0.0796 0.036 Uiso 1 1 calc R U . . . H18B H 0.5672 0.3100 0.0241 0.036 Uiso 1 1 calc R U . . . C19 C 0.7215(8) 0.1966(2) 0.03827(15) 0.0337(9) Uani 1 1 d . . . . . H19A H 0.8032 0.1636 0.0657 0.040 Uiso 1 1 calc R U . . . H19B H 0.5771 0.1745 0.0324 0.040 Uiso 1 1 calc R U . . . C20 C 0.8743(8) 0.1961(2) -0.00552(13) 0.0361(10) Uani 1 1 d . . . . . H20A H 0.9219 0.1419 -0.0109 0.043 Uiso 1 1 calc R U . . . H20B H 0.7850 0.2231 -0.0338 0.043 Uiso 1 1 calc R U . . . C21 C 1.0871(8) 0.2354(2) 0.00033(13) 0.0324(9) Uani 1 1 d . . . . . H21A H 1.1767 0.2378 -0.0296 0.039 Uiso 1 1 calc R U . . . H21B H 1.1865 0.2045 0.0259 0.039 Uiso 1 1 calc R U . . . C22 C 1.0247(7) 0.3169(2) 0.01259(12) 0.0268(8) Uani 1 1 d . . . . . H22A H 0.9377 0.3493 -0.0143 0.032 Uiso 1 1 calc R U . . . H22B H 1.1685 0.3399 0.0174 0.032 Uiso 1 1 calc R U . . . C23 C 0.9294(8) 0.4319(2) 0.08784(14) 0.0362(10) Uani 1 1 d . . . . . H23 H 1.0690 0.4039 0.1012 0.043 Uiso 1 1 calc R U . . . C24 C 0.8702(8) 0.5139(2) 0.09522(14) 0.0335(9) Uani 1 1 d . . . . . C25 C 0.6552(8) 0.5554(2) 0.08121(13) 0.0304(9) Uani 1 1 d . . . . . H25 H 0.5460 0.5319 0.0650 0.037 Uiso 1 1 calc R U . . . C26 C 0.6022(7) 0.6301(2) 0.09094(13) 0.0288(8) Uani 1 1 d . . . . . H26 H 0.4559 0.6580 0.0815 0.035 Uiso 1 1 calc R U . . . C27 C 0.7612(7) 0.6653(2) 0.11445(13) 0.0291(9) Uani 1 1 d . . . . . C28 C 0.9748(9) 0.6253(2) 0.12678(16) 0.0428(11) Uani 1 1 d . . . . . H28 H 1.0868 0.6498 0.1414 0.051 Uiso 1 1 calc R U . . . C29 C 1.0289(9) 0.5490(3) 0.11810(17) 0.0468(12) Uani 1 1 d . . . . . H29 H 1.1747 0.5211 0.1279 0.056 Uiso 1 1 calc R U . . . C30 C 0.7094(7) 0.7457(2) 0.12505(13) 0.0301(9) Uani 1 1 d . . . . . H30 H 0.8190 0.7664 0.1428 0.036 Uiso 1 1 calc R U . . . C31 C 0.4938(7) 0.87019(18) 0.11929(11) 0.0209(7) Uani 1 1 d . . . . . C32 C 0.5867(7) 0.91581(18) 0.07426(11) 0.0220(7) Uani 1 1 d . . . . . H32A H 0.7575 0.9038 0.0736 0.026 Uiso 1 1 calc R U . . . H32B H 0.5229 0.8986 0.0458 0.026 Uiso 1 1 calc R U . . . C33 C 0.5242(7) 1.00351(19) 0.07175(12) 0.0259(8) Uani 1 1 d . . . . . H33A H 0.6042 1.0222 0.0978 0.031 Uiso 1 1 calc R U . . . H33B H 0.5779 1.0296 0.0411 0.031 Uiso 1 1 calc R U . . . C34 C 0.2646(7) 1.0243(2) 0.07600(12) 0.0283(8) Uani 1 1 d . . . . . H34A H 0.1852 1.0101 0.0483 0.034 Uiso 1 1 calc R U . . . H34B H 0.2287 1.0809 0.0759 0.034 Uiso 1 1 calc R U . . . C35 C 0.1764(7) 0.98178(19) 0.12182(12) 0.0257(8) Uani 1 1 d . . . . . H35A H 0.0063 0.9949 0.1237 0.031 Uiso 1 1 calc R U . . . H35B H 0.2477 0.9989 0.1495 0.031 Uiso 1 1 calc R U . . . C36 C 0.2347(7) 0.89407(19) 0.12381(12) 0.0234(7) Uani 1 1 d . . . . . H36A H 0.1798 0.8681 0.1544 0.028 Uiso 1 1 calc R U . . . H36B H 0.1518 0.8765 0.0977 0.028 Uiso 1 1 calc R U . . . C37 C 0.6156(7) 0.88274(18) 0.16275(11) 0.0212(7) Uani 1 1 d . . . . . C38 C 0.7083(7) 0.88778(18) 0.19927(11) 0.0213(7) Uani 1 1 d . . . . . C39 C 0.8308(7) 0.88560(18) 0.24367(11) 0.0217(7) Uani 1 1 d . . . . . C40 C 0.7668(7) 0.83768(19) 0.28362(11) 0.0216(7) Uani 1 1 d . . . . . H40 H 0.6339 0.8114 0.2822 0.026 Uiso 1 1 calc R U . . . C41 C 0.8955(7) 0.82778(18) 0.32571(11) 0.0219(7) Uani 1 1 d . . . . . C42 C 1.0903(7) 0.86651(19) 0.32747(12) 0.0254(8) Uani 1 1 d . . . . . H42 H 1.1828 0.8587 0.3556 0.030 Uiso 1 1 calc R U . . . C43 C 1.1486(7) 0.9163(2) 0.28820(12) 0.0244(8) Uani 1 1 d . . . . . H43 H 1.2778 0.9443 0.2899 0.029 Uiso 1 1 calc R U . . . C44 C 1.0200(7) 0.92580(19) 0.24635(12) 0.0240(8) Uani 1 1 d . . . . . H44 H 1.0619 0.9599 0.2195 0.029 Uiso 1 1 calc R U . . . C45 C 0.8300(7) 0.77662(18) 0.36637(11) 0.0227(7) Uani 1 1 d . . . . . C46 C 0.7711(7) 0.73491(18) 0.40002(11) 0.0217(7) Uani 1 1 d . . . . . C47 C 0.6684(7) 0.68705(18) 0.44036(11) 0.0208(7) Uani 1 1 d . . . . . C48 C 0.4088(7) 0.7137(2) 0.44091(13) 0.0275(8) Uani 1 1 d . . . . . H48A H 0.3344 0.6794 0.4656 0.033 Uiso 1 1 calc R U . . . H48B H 0.3403 0.7094 0.4097 0.033 Uiso 1 1 calc R U . . . C49 C 0.3597(7) 0.7973(2) 0.45106(14) 0.0302(8) Uani 1 1 d . . . . . H49A H 0.4211 0.8322 0.4247 0.036 Uiso 1 1 calc R U . . . H49B H 0.1900 0.8118 0.4525 0.036 Uiso 1 1 calc R U . . . C50 C 0.4697(8) 0.8080(2) 0.49784(13) 0.0328(9) Uani 1 1 d . . . . . H50A H 0.4474 0.8635 0.5017 0.039 Uiso 1 1 calc R U . . . H50B H 0.3916 0.7792 0.5246 0.039 Uiso 1 1 calc R U . . . C51 C 0.7266(8) 0.7793(2) 0.49942(12) 0.0309(9) Uani 1 1 d . . . . . H51A H 0.7883 0.7816 0.5316 0.037 Uiso 1 1 calc R U . . . H51B H 0.8082 0.8139 0.4762 0.037 Uiso 1 1 calc R U . . . C52 C 0.7755(7) 0.69626(19) 0.48795(11) 0.0245(8) Uani 1 1 d . . . . . H52A H 0.9453 0.6816 0.4869 0.029 Uiso 1 1 calc R U . . . H52B H 0.7124 0.6606 0.5137 0.029 Uiso 1 1 calc R U . . . C53 C 0.8802(8) 0.5750(2) 0.41689(13) 0.0294(8) Uani 1 1 d . . . . . H53 H 0.9938 0.6080 0.4062 0.035 Uiso 1 1 calc R U . . . C54 C 0.9230(8) 0.49214(19) 0.41090(13) 0.0293(8) Uani 1 1 d . . . . . C55 C 0.7576(8) 0.4426(2) 0.42463(13) 0.0299(9) Uani 1 1 d . . . . . H55 H 0.6223 0.4606 0.4409 0.036 Uiso 1 1 calc R U . . . C56 C 0.7894(7) 0.36714(19) 0.41472(13) 0.0281(8) Uani 1 1 d . . . . . H56 H 0.6756 0.3336 0.4242 0.034 Uiso 1 1 calc R U . . . C57 C 0.9876(7) 0.33968(19) 0.39077(12) 0.0268(8) Uani 1 1 d . . . . . C58 C 1.1544(8) 0.3884(2) 0.37841(14) 0.0338(9) Uani 1 1 d . . . . . H58 H 1.2920 0.3699 0.3631 0.041 Uiso 1 1 calc R U . . . C59 C 1.1219(8) 0.4646(2) 0.38832(15) 0.0355(9) Uani 1 1 d . . . . . H59 H 1.2372 0.4979 0.3795 0.043 Uiso 1 1 calc R U . . . C60 C 1.0171(7) 0.26018(19) 0.37812(12) 0.0255(8) Uani 1 1 d . . . . . H60 H 1.1430 0.2446 0.3586 0.031 Uiso 1 1 calc R U . . . N1 N 0.8774(6) 0.21274(15) 0.39293(9) 0.0233(7) Uani 1 1 d . . . . . N2 N 0.6978(6) 0.60337(16) 0.43575(10) 0.0261(7) Uani 1 1 d . . . . . N3 N 0.8000(6) 0.39807(16) 0.06432(10) 0.0269(7) Uani 1 1 d . . . . . N4 N 0.5248(6) 0.78772(15) 0.11132(10) 0.0242(7) Uani 1 1 d . . . . . C1S C 0.610(2) 0.4217(5) 0.2631(3) 0.0502(17) Uani 0.5 1 d . U P A 1 C2S C 0.617(2) 0.3442(6) 0.2758(4) 0.0494(18) Uani 0.5 1 d . U P A 1 H2S H 0.6555 0.3215 0.3076 0.059 Uiso 0.5 1 calc R U P A 1 C3S C 0.566(2) 0.2971(6) 0.2412(4) 0.0507(18) Uani 0.5 1 d . U P A 1 H3S H 0.5532 0.2436 0.2503 0.061 Uiso 0.5 1 calc R U P A 1 C4S C 0.534(2) 0.3295(5) 0.1948(3) 0.0508(18) Uani 0.5 1 d . U P A 1 H4S H 0.5140 0.2969 0.1714 0.061 Uiso 0.5 1 calc R U P A 1 C5S C 0.5309(19) 0.4036(6) 0.1815(3) 0.0496(18) Uani 0.5 1 d . U P A 1 H5S H 0.5042 0.4242 0.1490 0.060 Uiso 0.5 1 calc R U P A 1 C6S C 0.566(2) 0.4528(6) 0.2145(4) 0.0496(19) Uani 0.5 1 d . U P A 1 H6S H 0.5610 0.5070 0.2046 0.060 Uiso 0.5 1 calc R U P A 1 C7S C 0.672(2) 0.4701(6) 0.2973(4) 0.062(2) Uani 0.5 1 d . U P A 1 H7S1 H 0.7852 0.4456 0.3202 0.074 Uiso 0.5 1 calc R U P A 1 C8S C 0.596(2) 0.5441(6) 0.3018(4) 0.064(2) Uani 0.5 1 d . U P A 1 H8S1 H 0.6830 0.5678 0.3228 0.077 Uiso 0.5 1 calc R U P A 1 C9S C 0.398(3) 0.5921(7) 0.2787(4) 0.068(2) Uani 0.5 1 d . U P A 1 C10S C 0.181(3) 0.5645(10) 0.2706(5) 0.069(2) Uani 0.5 1 d . U P A 1 H10S H 0.1698 0.5108 0.2790 0.083 Uiso 0.5 1 calc R U P A 1 C11S C -0.005(3) 0.6100(7) 0.2521(4) 0.075(2) Uani 0.5 1 d . U P A 1 H11S H -0.1466 0.5891 0.2485 0.090 Uiso 0.5 1 calc R U P A 1 C12S C 0.008(3) 0.6901(7) 0.2377(4) 0.078(2) Uani 0.5 1 d . U P A 1 H12S H -0.1252 0.7247 0.2270 0.093 Uiso 0.5 1 calc R U P A 1 C13S C 0.244(3) 0.7186(7) 0.2399(5) 0.078(3) Uani 0.5 1 d . U P A 1 H13S H 0.2708 0.7691 0.2257 0.093 Uiso 0.5 1 calc R U P A 1 C14S C 0.410(3) 0.6701(6) 0.2624(5) 0.076(2) Uani 0.5 1 d . U P A 1 H14S H 0.5507 0.6899 0.2681 0.091 Uiso 0.5 1 calc R U P A 1 C1' C 0.236(4) 0.5615(12) 0.2556(6) 0.081(2) Uani 0.5 1 d . U P B 2 C2' C 0.393(3) 0.5412(8) 0.2888(5) 0.075(2) Uani 0.5 1 d . U P B 2 H2' H 0.4530 0.4883 0.2969 0.090 Uiso 0.5 1 calc R U P B 2 C3' C 0.476(3) 0.6017(7) 0.3140(4) 0.071(2) Uani 0.5 1 d . U P B 2 H3' H 0.5962 0.5877 0.3373 0.086 Uiso 0.5 1 calc R U P B 2 C4' C 0.390(3) 0.6705(7) 0.3047(4) 0.071(2) Uani 0.5 1 d . U P B 2 H4' H 0.4277 0.7065 0.3247 0.085 Uiso 0.5 1 calc R U P B 2 C5' C 0.236(3) 0.6977(9) 0.2653(5) 0.077(3) Uani 0.5 1 d . U P B 2 H5' H 0.2002 0.7511 0.2534 0.092 Uiso 0.5 1 calc R U P B 2 C6' C 0.147(3) 0.6419(8) 0.2463(5) 0.084(2) Uani 0.5 1 d . U P B 2 H6' H 0.0174 0.6564 0.2255 0.101 Uiso 0.5 1 calc R U P B 2 C7' C 0.116(3) 0.5075(8) 0.2296(5) 0.083(2) Uani 0.5 1 d . U P B 2 H7'1 H -0.0371 0.5240 0.2179 0.100 Uiso 0.5 1 calc R U P B 2 C8' C 0.218(3) 0.4364(8) 0.2224(5) 0.086(2) Uani 0.5 1 d . U P B 2 H8'1 H 0.1151 0.4045 0.2112 0.104 Uiso 0.5 1 calc R U P B 2 C9' C 0.4476(15) 0.4017(5) 0.2285(4) 0.084(2) Uani 0.5 1 d G U P B 2 C10' C 0.4833(15) 0.3296(5) 0.2564(3) 0.081(2) Uani 0.5 1 d G U P B 2 H10' H 0.3548 0.3030 0.2667 0.097 Uiso 0.5 1 calc R U P B 2 C11' C 0.7071(18) 0.2965(4) 0.2693(3) 0.081(3) Uani 0.5 1 d G U P B 2 H11' H 0.7316 0.2472 0.2884 0.098 Uiso 0.5 1 calc R U P B 2 C12' C 0.8952(14) 0.3354(5) 0.2542(3) 0.085(3) Uani 0.5 1 d G U P B 2 H12' H 1.0482 0.3127 0.2630 0.102 Uiso 0.5 1 calc R U P B 2 C13' C 0.8595(16) 0.4074(5) 0.2263(3) 0.088(3) Uani 0.5 1 d G U P B 2 H13' H 0.9880 0.4340 0.2160 0.105 Uiso 0.5 1 calc R U P B 2 C14' C 0.6357(19) 0.4405(4) 0.2135(4) 0.088(3) Uani 0.5 1 d G U P B 2 H14' H 0.6112 0.4898 0.1944 0.105 Uiso 0.5 1 calc R U P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(2) 0.0152(14) 0.0188(15) 0.0012(11) 0.0017(14) 0.0004(13) C2 0.026(2) 0.0192(15) 0.0169(14) 0.0005(11) -0.0007(14) -0.0036(14) C3 0.035(2) 0.0182(15) 0.0223(16) 0.0021(12) -0.0020(16) 0.0006(15) C4 0.040(3) 0.0198(16) 0.0273(17) 0.0016(13) 0.0028(17) -0.0059(16) C5 0.025(2) 0.0232(16) 0.0296(18) -0.0001(13) 0.0000(15) -0.0061(15) C6 0.023(2) 0.0215(16) 0.0241(16) 0.0003(13) -0.0020(14) 0.0002(15) C7 0.027(2) 0.0171(14) 0.0217(16) 0.0008(12) -0.0034(15) -0.0017(14) C8 0.023(2) 0.0226(16) 0.0217(16) 0.0007(13) -0.0019(14) 0.0001(14) C9 0.026(2) 0.0251(16) 0.0162(14) 0.0001(12) 0.0001(14) -0.0027(15) C10 0.028(2) 0.0266(17) 0.0178(15) 0.0023(13) -0.0022(14) -0.0006(15) C11 0.021(2) 0.0286(17) 0.0264(17) -0.0018(14) 0.0041(15) 0.0020(15) C12 0.033(2) 0.0280(18) 0.0204(16) 0.0001(13) 0.0038(15) 0.0006(16) C13 0.031(2) 0.0262(17) 0.0187(15) 0.0008(13) -0.0017(15) -0.0013(16) C14 0.023(2) 0.0314(18) 0.0202(16) 0.0006(13) -0.0005(14) 0.0042(16) C15 0.034(2) 0.0272(17) 0.0208(16) -0.0012(13) 0.0013(16) -0.0022(16) C16 0.030(2) 0.0211(15) 0.0193(15) -0.0014(12) -0.0004(15) -0.0009(15) C17 0.026(2) 0.0188(15) 0.0195(15) 0.0030(12) 0.0002(14) 0.0010(14) C18 0.030(2) 0.0236(17) 0.0339(19) 0.0002(14) -0.0022(17) 0.0007(16) C19 0.030(2) 0.0235(17) 0.047(2) -0.0027(15) -0.0081(19) -0.0018(17) C20 0.050(3) 0.0268(18) 0.0295(19) -0.0063(15) -0.0133(19) 0.0078(19) C21 0.042(3) 0.0271(18) 0.0222(17) 0.0054(14) 0.0085(17) 0.0081(18) C22 0.027(2) 0.0269(17) 0.0233(16) 0.0052(13) 0.0026(15) -0.0006(16) C23 0.035(3) 0.0300(19) 0.042(2) -0.0073(16) -0.0076(19) 0.0045(18) C24 0.039(3) 0.0256(18) 0.035(2) -0.0038(15) -0.0043(18) 0.0011(18) C25 0.037(3) 0.0242(17) 0.0290(18) 0.0005(14) -0.0034(17) -0.0036(17) C26 0.031(2) 0.0232(17) 0.0300(18) 0.0018(14) -0.0028(16) 0.0011(16) C27 0.033(2) 0.0254(17) 0.0266(18) -0.0004(14) -0.0030(16) 0.0004(16) C28 0.037(3) 0.038(2) 0.056(3) -0.0167(19) -0.009(2) 0.000(2) C29 0.038(3) 0.037(2) 0.066(3) -0.018(2) -0.017(2) 0.006(2) C30 0.031(2) 0.0283(18) 0.0313(19) -0.0047(15) -0.0028(17) -0.0041(17) C31 0.026(2) 0.0199(15) 0.0157(14) -0.0003(12) -0.0002(14) -0.0028(14) C32 0.026(2) 0.0211(15) 0.0173(14) 0.0000(12) 0.0011(14) -0.0014(14) C33 0.033(2) 0.0221(16) 0.0202(16) 0.0039(12) 0.0020(15) -0.0009(15) C34 0.034(2) 0.0240(17) 0.0237(17) 0.0032(13) -0.0037(16) 0.0025(16) C35 0.024(2) 0.0261(17) 0.0262(17) -0.0033(13) -0.0003(15) 0.0006(15) C36 0.025(2) 0.0246(16) 0.0206(15) -0.0004(13) -0.0005(14) -0.0048(15) C37 0.0205(19) 0.0180(15) 0.0235(16) 0.0027(12) 0.0013(14) -0.0023(14) C38 0.022(2) 0.0212(15) 0.0198(15) 0.0020(12) 0.0003(14) -0.0041(14) C39 0.026(2) 0.0204(15) 0.0179(15) -0.0009(12) 0.0001(14) -0.0003(14) C40 0.0210(19) 0.0236(16) 0.0199(15) -0.0009(12) 0.0005(14) -0.0042(14) C41 0.028(2) 0.0198(15) 0.0161(14) 0.0003(12) -0.0008(14) -0.0003(14) C42 0.032(2) 0.0247(16) 0.0192(15) -0.0022(13) -0.0053(15) -0.0024(16) C43 0.022(2) 0.0248(16) 0.0276(17) -0.0021(13) -0.0002(15) -0.0079(15) C44 0.028(2) 0.0245(16) 0.0193(15) -0.0003(12) 0.0013(14) -0.0068(15) C45 0.028(2) 0.0201(15) 0.0191(15) -0.0021(12) -0.0027(14) -0.0014(15) C46 0.025(2) 0.0190(15) 0.0202(15) -0.0018(12) -0.0015(14) -0.0006(14) C47 0.025(2) 0.0167(14) 0.0195(15) 0.0023(11) -0.0009(14) -0.0044(14) C48 0.022(2) 0.0243(17) 0.0342(19) 0.0029(14) -0.0020(16) -0.0021(15) C49 0.020(2) 0.0253(17) 0.042(2) 0.0025(15) 0.0057(17) 0.0021(15) C50 0.046(3) 0.0238(17) 0.0264(17) -0.0006(14) 0.0110(18) -0.0017(18) C51 0.046(3) 0.0276(18) 0.0177(16) 0.0005(13) -0.0042(16) -0.0046(18) C52 0.029(2) 0.0239(16) 0.0191(15) 0.0008(12) -0.0032(15) -0.0002(15) C53 0.036(2) 0.0212(16) 0.0306(18) 0.0003(14) 0.0021(17) -0.0061(16) C54 0.037(2) 0.0196(16) 0.0302(18) -0.0013(13) -0.0003(17) -0.0028(16) C55 0.034(2) 0.0215(17) 0.0330(19) -0.0010(14) 0.0073(17) -0.0018(16) C56 0.033(2) 0.0186(16) 0.0320(18) 0.0018(13) 0.0027(17) -0.0052(16) C57 0.034(2) 0.0204(16) 0.0246(16) 0.0008(13) -0.0005(16) -0.0014(16) C58 0.033(2) 0.0277(18) 0.041(2) -0.0049(16) 0.0086(18) -0.0059(17) C59 0.036(3) 0.0241(17) 0.047(2) -0.0019(16) 0.005(2) -0.0088(17) C60 0.028(2) 0.0220(16) 0.0238(16) 0.0005(13) 0.0024(15) 0.0014(15) N1 0.0304(19) 0.0178(13) 0.0201(13) -0.0003(10) 0.0003(12) 0.0004(13) N2 0.037(2) 0.0182(13) 0.0216(14) 0.0019(11) -0.0010(14) -0.0028(13) N3 0.035(2) 0.0216(14) 0.0220(14) 0.0019(11) -0.0008(14) 0.0000(14) N4 0.0310(19) 0.0182(13) 0.0222(14) 0.0000(11) -0.0017(13) -0.0006(13) C1S 0.062(4) 0.042(3) 0.046(3) -0.004(3) -0.008(3) -0.008(3) C2S 0.052(5) 0.047(3) 0.046(3) 0.001(3) 0.001(4) -0.003(4) C3S 0.054(5) 0.039(3) 0.061(4) -0.008(3) 0.006(4) -0.012(4) C4S 0.059(5) 0.044(3) 0.053(3) -0.018(3) 0.002(4) -0.010(4) C5S 0.055(5) 0.051(3) 0.045(3) -0.007(3) -0.002(4) -0.011(4) C6S 0.062(5) 0.043(3) 0.045(3) -0.001(3) -0.007(4) -0.017(4) C7S 0.076(5) 0.055(3) 0.052(4) -0.006(3) -0.022(4) 0.003(4) C8S 0.086(5) 0.053(4) 0.055(4) -0.015(3) -0.029(4) -0.001(4) C9S 0.093(5) 0.046(3) 0.065(4) -0.008(3) -0.024(4) -0.001(4) C10S 0.086(5) 0.055(4) 0.064(5) -0.006(4) -0.018(5) -0.002(4) C11S 0.087(5) 0.064(4) 0.071(5) -0.011(4) -0.010(5) 0.003(4) C12S 0.097(6) 0.061(4) 0.071(5) -0.014(4) -0.013(5) 0.013(4) C13S 0.107(6) 0.048(4) 0.074(5) -0.007(4) -0.021(5) 0.004(4) C14S 0.101(6) 0.046(4) 0.081(5) -0.010(4) -0.025(5) -0.002(4) C1' 0.091(5) 0.072(4) 0.079(5) -0.016(4) -0.022(4) 0.003(4) C2' 0.085(6) 0.069(4) 0.070(5) -0.010(4) -0.014(4) -0.001(4) C3' 0.080(6) 0.073(5) 0.059(4) -0.009(4) -0.011(4) 0.000(4) C4' 0.084(6) 0.069(4) 0.060(4) -0.023(4) -0.004(4) 0.001(5) C5' 0.089(6) 0.070(4) 0.071(5) -0.028(4) -0.011(5) 0.014(5) C6' 0.096(6) 0.074(4) 0.081(5) -0.022(4) -0.023(5) 0.011(5) C7' 0.091(6) 0.078(4) 0.081(5) -0.018(4) -0.017(4) -0.002(4) C8' 0.096(5) 0.079(4) 0.085(5) -0.017(4) -0.009(5) -0.006(4) C9' 0.099(5) 0.072(4) 0.078(5) -0.008(4) -0.001(5) -0.003(4) C10' 0.103(6) 0.067(5) 0.073(5) -0.016(4) 0.007(5) -0.006(4) C11' 0.108(6) 0.065(5) 0.069(5) -0.010(4) 0.001(5) -0.003(4) C12' 0.104(6) 0.071(5) 0.077(5) -0.008(4) 0.001(5) -0.001(5) C13' 0.101(6) 0.075(5) 0.082(5) -0.004(4) 0.006(5) -0.002(5) C14' 0.102(6) 0.076(5) 0.081(5) -0.001(5) 0.005(5) -0.003(5) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C7 C1 N1 112.7(3) C7 C1 C6 109.2(3) N1 C1 C6 106.8(3) C7 C1 C2 112.0(3) N1 C1 C2 106.3(2) C6 C1 C2 109.7(3) C3 C2 C1 112.2(3) C4 C3 C2 111.7(3) C3 C4 C5 110.7(3) C4 C5 C6 110.5(3) C1 C6 C5 112.6(3) C8 C7 C1 174.4(4) C7 C8 C9 175.9(4) C10 C9 C14 119.4(3) C10 C9 C8 121.9(3) C14 C9 C8 118.6(3) C9 C10 C11 120.3(3) C10 C11 C12 120.1(4) C13 C12 C11 120.5(3) C12 C13 C14 119.1(3) C12 C13 C15 120.9(3) C14 C13 C15 120.0(4) C9 C14 C13 120.6(4) C16 C15 C13 179.3(5) C15 C16 C17 175.8(4) C16 C17 N3 113.9(3) C16 C17 C18 109.3(3) N3 C17 C18 107.6(3) C16 C17 C22 109.5(3) N3 C17 C22 108.1(3) C18 C17 C22 108.4(3) C19 C18 C17 111.9(3) C20 C19 C18 111.1(3) C21 C20 C19 111.1(3) C20 C21 C22 111.8(3) C21 C22 C17 111.3(3) N3 C23 C24 122.0(4) C29 C24 C25 119.6(4) C29 C24 C23 118.7(4) C25 C24 C23 121.7(4) C26 C25 C24 119.9(4) C25 C26 C27 120.7(4) C28 C27 C26 119.3(3) C28 C27 C30 119.0(4) C26 C27 C30 121.8(4) C27 C28 C29 120.7(4) C24 C29 C28 119.9(4) N4 C30 C27 122.2(4) C37 C31 N4 112.4(3) C37 C31 C36 109.8(3) N4 C31 C36 107.2(3) C37 C31 C32 111.5(3) N4 C31 C32 105.9(2) C36 C31 C32 109.9(3) C33 C32 C31 112.9(3) C34 C33 C32 110.9(3) C33 C34 C35 110.4(3) C34 C35 C36 111.0(3) C31 C36 C35 112.1(3) C38 C37 C31 175.1(3) C37 C38 C39 174.1(3) C44 C39 C40 119.5(3) C44 C39 C38 121.4(3) C40 C39 C38 118.9(3) C39 C40 C41 120.7(3) C42 C41 C40 119.3(3) C42 C41 C45 120.7(3) C40 C41 C45 120.0(3) C43 C42 C41 119.8(3) C42 C43 C44 120.5(3) C39 C44 C43 120.1(3) C46 C45 C41 178.6(4) C45 C46 C47 173.0(4) N2 C47 C46 112.9(3) N2 C47 C48 107.6(3) C46 C47 C48 107.9(3) N2 C47 C52 107.7(3) C46 C47 C52 111.3(3) C48 C47 C52 109.3(3) C47 C48 C49 111.6(3) C50 C49 C48 111.5(3) C51 C50 C49 111.5(3) C50 C51 C52 112.1(3) C47 C52 C51 112.0(3) N2 C53 C54 122.2(4) C59 C54 C55 119.4(3) C59 C54 C53 119.8(4) C55 C54 C53 120.6(4) C56 C55 C54 120.2(4) C55 C56 C57 120.6(4) C58 C57 C56 119.0(3) C58 C57 C60 120.2(4) C56 C57 C60 120.8(3) C57 C58 C59 120.3(4) C54 C59 C58 120.5(4) N1 C60 C57 120.9(3) C60 N1 C1 121.0(3) C53 N2 C47 118.8(3) C23 N3 C17 118.0(3) C30 N4 C31 119.2(3) C2S C1S C6S 118.5(9) C2S C1S C7S 120.2(9) C6S C1S C7S 120.9(9) C1S C2S C3S 119.4(9) C4S C3S C2S 119.3(9) C5S C4S C3S 122.2(9) C4S C5S C6S 120.6(10) C5S C6S C1S 119.7(9) C8S C7S C1S 130.5(10) C7S C8S C9S 127.7(11) C14S C9S C10S 115.7(13) C14S C9S C8S 120.3(14) C10S C9S C8S 124.0(12) C11S C10S C9S 123.6(16) C10S C11S C12S 119.5(17) C11S C12S C13S 117.7(13) C14S C13S C12S 116.7(13) C13S C14S C9S 125.8(16) C2' C1' C6' 117.4(17) C2' C1' C7' 126.3(17) C6' C1' C7' 115.9(16) C1' C2' C3' 119.3(15) C4' C3' C2' 120.2(13) C3' C4' C5' 122.8(12) C6' C5' C4' 114.6(14) C5' C6' C1' 123.8(16) C8' C7' C1' 122.7(16) C7' C8' C9' 131.4(15) C10' C9' C14' 120.0 C10' C9' C8' 116.9(9) C14' C9' C8' 122.5(9) C11' C10' C9' 120.0 C10' C11' C12' 120.0 C13' C12' C11' 120.0 C12' C13' C14' 120.0 C13' C14' C9' 120.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C7 1.479(5) C1 N1 1.485(4) C1 C6 1.519(5) C1 C2 1.542(4) C2 C3 1.524(4) C3 C4 1.508(6) C4 C5 1.526(5) C5 C6 1.528(4) C7 C8 1.198(5) C8 C9 1.434(5) C9 C10 1.382(5) C9 C14 1.395(5) C10 C11 1.386(5) C11 C12 1.393(5) C12 C13 1.380(5) C13 C14 1.399(5) C13 C15 1.436(5) C15 C16 1.189(5) C16 C17 1.479(5) C17 N3 1.480(4) C17 C18 1.522(5) C17 C22 1.540(5) C18 C19 1.521(5) C19 C20 1.518(6) C20 C21 1.508(6) C21 C22 1.518(5) C23 N3 1.260(5) C23 C24 1.483(5) C24 C29 1.382(6) C24 C25 1.400(6) C25 C26 1.376(5) C26 C27 1.394(6) C27 C28 1.374(6) C27 C30 1.478(5) C28 C29 1.393(6) C30 N4 1.259(5) C31 C37 1.481(5) C31 N4 1.485(4) C31 C36 1.523(5) C31 C32 1.539(4) C32 C33 1.531(4) C33 C34 1.516(5) C34 C35 1.522(5) C35 C36 1.529(5) C37 C38 1.190(5) C38 C39 1.445(5) C39 C44 1.384(5) C39 C40 1.390(5) C40 C41 1.394(5) C41 C42 1.393(5) C41 C45 1.437(5) C42 C43 1.383(5) C43 C44 1.388(5) C45 C46 1.193(5) C46 C47 1.487(5) C47 N2 1.482(4) C47 C48 1.525(5) C47 C52 1.527(4) C48 C49 1.526(5) C49 C50 1.521(5) C50 C51 1.516(6) C51 C52 1.529(5) C53 N2 1.261(5) C53 C54 1.479(5) C54 C59 1.383(6) C54 C55 1.390(6) C55 C56 1.382(5) C56 C57 1.400(6) C57 C58 1.379(6) C57 C60 1.478(5) C58 C59 1.396(5) C60 N1 1.260(5) C1S C2S 1.354(13) C1S C6S 1.424(14) C1S C7S 1.449(14) C2S C3S 1.422(14) C3S C4S 1.363(14) C4S C5S 1.302(13) C5S C6S 1.389(15) C7S C8S 1.344(14) C8S C9S 1.449(17) C9S C14S 1.394(16) C9S C10S 1.43(2) C10S C11S 1.33(2) C11S C12S 1.421(18) C12S C13S 1.52(2) C13S C14S 1.312(19) C1' C2' 1.30(2) C1' C6' 1.43(2) C1' C7' 1.52(2) C2' C3' 1.488(18) C3' C4' 1.245(16) C4' C5' 1.431(19) C5' C6' 1.34(2) C7' C8' 1.356(18) C8' C9' 1.402(17) C9' C10' 1.3900 C9' C14' 1.3900 C10' C11' 1.3900 C11' C12' 1.3900 C12' C13' 1.3900 C13' C14' 1.3900 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C7 C1 C2 C3 -68.1(4) N1 C1 C2 C3 168.4(3) C6 C1 C2 C3 53.3(4) C1 C2 C3 C4 -55.2(4) C2 C3 C4 C5 56.2(4) C3 C4 C5 C6 -56.5(4) C7 C1 C6 C5 68.6(3) N1 C1 C6 C5 -169.3(3) C2 C1 C6 C5 -54.5(4) C4 C5 C6 C1 56.8(4) C14 C9 C10 C11 1.0(6) C8 C9 C10 C11 -176.9(3) C9 C10 C11 C12 0.3(6) C10 C11 C12 C13 -0.8(6) C11 C12 C13 C14 0.1(6) C11 C12 C13 C15 179.6(3) C10 C9 C14 C13 -1.7(6) C8 C9 C14 C13 176.3(3) C12 C13 C14 C9 1.1(6) C15 C13 C14 C9 -178.3(3) C16 C17 C18 C19 -61.9(4) N3 C17 C18 C19 174.1(3) C22 C17 C18 C19 57.5(4) C17 C18 C19 C20 -57.0(4) C18 C19 C20 C21 54.2(4) C19 C20 C21 C22 -54.6(4) C20 C21 C22 C17 56.7(4) C16 C17 C22 C21 62.1(4) N3 C17 C22 C21 -173.4(3) C18 C17 C22 C21 -57.1(4) N3 C23 C24 C29 -174.9(4) N3 C23 C24 C25 7.5(6) C29 C24 C25 C26 -1.0(6) C23 C24 C25 C26 176.6(4) C24 C25 C26 C27 0.3(6) C25 C26 C27 C28 1.7(6) C25 C26 C27 C30 179.6(3) C26 C27 C28 C29 -3.1(7) C30 C27 C28 C29 178.9(4) C25 C24 C29 C28 -0.4(7) C23 C24 C29 C28 -178.1(4) C27 C28 C29 C24 2.5(7) C28 C27 C30 N4 174.2(4) C26 C27 C30 N4 -3.7(6) C37 C31 C32 C33 -69.1(4) N4 C31 C32 C33 168.3(3) C36 C31 C32 C33 52.8(4) C31 C32 C33 C34 -54.9(4) C32 C33 C34 C35 56.4(4) C33 C34 C35 C36 -57.7(4) C37 C31 C36 C35 69.4(3) N4 C31 C36 C35 -168.2(3) C32 C31 C36 C35 -53.5(3) C34 C35 C36 C31 57.1(4) C44 C39 C40 C41 -2.1(5) C38 C39 C40 C41 173.3(3) C39 C40 C41 C42 0.0(5) C39 C40 C41 C45 -178.6(3) C40 C41 C42 C43 2.4(5) C45 C41 C42 C43 -179.1(3) C41 C42 C43 C44 -2.6(5) C40 C39 C44 C43 2.0(5) C38 C39 C44 C43 -173.4(3) C42 C43 C44 C39 0.4(5) N2 C47 C48 C49 173.7(3) C46 C47 C48 C49 -64.2(4) C52 C47 C48 C49 57.1(4) C47 C48 C49 C50 -56.7(4) C48 C49 C50 C51 53.6(4) C49 C50 C51 C52 -52.5(4) N2 C47 C52 C51 -172.4(3) C46 C47 C52 C51 63.3(4) C48 C47 C52 C51 -55.9(4) C50 C51 C52 C47 54.5(4) N2 C53 C54 C59 177.5(4) N2 C53 C54 C55 2.2(6) C59 C54 C55 C56 -1.6(6) C53 C54 C55 C56 173.8(3) C54 C55 C56 C57 -0.1(6) C55 C56 C57 C58 1.9(6) C55 C56 C57 C60 -177.1(3) C56 C57 C58 C59 -2.0(6) C60 C57 C58 C59 177.0(4) C55 C54 C59 C58 1.4(6) C53 C54 C59 C58 -174.0(4) C57 C58 C59 C54 0.4(6) C58 C57 C60 N1 173.4(4) C56 C57 C60 N1 -7.6(5) C57 C60 N1 C1 -178.1(3) C7 C1 N1 C60 -25.0(5) C6 C1 N1 C60 -144.9(3) C2 C1 N1 C60 98.0(4) C54 C53 N2 C47 -179.9(3) C46 C47 N2 C53 34.5(5) C48 C47 N2 C53 153.4(3) C52 C47 N2 C53 -88.9(4) C24 C23 N3 C17 178.6(3) C16 C17 N3 C23 32.9(5) C18 C17 N3 C23 154.2(4) C22 C17 N3 C23 -89.0(4) C27 C30 N4 C31 -174.3(3) C37 C31 N4 C30 -30.8(5) C36 C31 N4 C30 -151.5(3) C32 C31 N4 C30 91.1(4) C6S C1S C2S C3S -4.0(17) C7S C1S C2S C3S -177.1(12) C1S C2S C3S C4S 6.8(17) C2S C3S C4S C5S -5.7(18) C3S C4S C5S C6S 1.8(18) C4S C5S C6S C1S 1.0(18) C2S C1S C6S C5S 0.2(18) C7S C1S C6S C5S 173.2(12) C2S C1S C7S C8S -149.1(14) C6S C1S C7S C8S 38(2) C1S C7S C8S C9S 12(2) C7S C8S C9S C14S -140.9(15) C7S C8S C9S C10S 39(2) C14S C9S C10S C11S -5(2) C8S C9S C10S C11S 175.5(13) C9S C10S C11S C12S 2(2) C10S C11S C12S C13S 5.7(19) C11S C12S C13S C14S -11.1(19) C12S C13S C14S C9S 9(2) C10S C9S C14S C13S -2(2) C8S C9S C14S C13S 178.2(14) C6' C1' C2' C3' -2(3) C7' C1' C2' C3' -174.0(15) C1' C2' C3' C4' 3(2) C2' C3' C4' C5' -10(2) C3' C4' C5' C6' 16(2) C4' C5' C6' C1' -15(3) C2' C1' C6' C5' 9(3) C7' C1' C6' C5' -178.2(16) C2' C1' C7' C8' -29(3) C6' C1' C7' C8' 158.8(16) C1' C7' C8' C9' -11(3) C7' C8' C9' C10' 127.0(15) C7' C8' C9' C14' -44(2) C14' C9' C10' C11' 0.0 C8' C9' C10' C11' -171.4(11) C9' C10' C11' C12' 0.0 C10' C11' C12' C13' 0.0 C11' C12' C13' C14' 0.0 C12' C13' C14' C9' 0.0 C10' C9' C14' C13' 0.0 C8' C9' C14' C13' 170.9(11)