#------------------------------------------------------------------------------ #$Date: 2020-01-03 03:50:34 +0200 (Fri, 03 Jan 2020) $ #$Revision: 246446 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/57/7125711.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_7125711 loop_ _publ_author_name 'Blanke, Meik' 'Balszuweit, Jan' 'Saccone, Marco' 'W\"olper, Christoph' 'Doblas Jim\'enez, David' 'Mezger, Markus' 'Voskuhl, Jens' 'Giese, Michael' _publ_section_title ; Photo-switching and -cyclisation of hydrogen bonded liquid crystals based on resveratrol ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC07721A _journal_year 2020 _chemical_formula_sum 'C77 H93 N3 O6' _chemical_formula_weight 1156.54 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2019-07-09 deposited with the CCDC. 2019-12-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.602(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 22.357(3) _cell_length_b 10.0540(15) _cell_length_c 28.899(4) _cell_measurement_reflns_used 9326 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 33.13 _cell_measurement_theta_min 2.47 _cell_volume 6493.3(16) _computing_cell_refinement 'BRUKER APEX2(v2009.5-1)' _computing_data_collection 'BRUKER APEX2(v2009.5-1)' _computing_data_reduction 'BRUKER APEX2(v2009.5-1)' _computing_molecular_graphics 'ORTEP/PLATON (Spek)' _computing_publication_material 'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'BRUKER APEX2(v2009.5-1)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 512 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'Bruker D8 KAPPA II (APEX II detector)' _diffrn_measurement_method 'Data collection strategy APEX 2/COSMO' _diffrn_radiation_monochromator 'Triumph Goebel mirror' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_unetI/netI 0.0375 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_number 210866 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.211 _diffrn_reflns_theta_min 1.167 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.183 _exptl_crystal_description tablet _exptl_crystal_F_000 2496 _exptl_crystal_size_max 0.491 _exptl_crystal_size_mid 0.188 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.619 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.058 _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 790 _refine_ls_number_reflns 24524 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0516 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+2.3663P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1231 _refine_ls_wR_factor_ref 0.1428 _reflns_Friedel_coverage 0.000 _reflns_number_gt 17323 _reflns_number_total 24524 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc07721a2.cif _cod_data_source_block jv_r_s_c8m _cod_depositor_comments ; The following automatic conversions were performed: data item '_atom_sites_solution_secondary' value 'diffmap' was changed to 'difmap'. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_cell_volume 6493.2(17) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7125711 _shelx_shelxl_version_number 2017/1 _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 0.965 _shelx_estimated_absorpt_t_max 0.989 _shelx_res_file ; TITL jv_r_s_c8m in P2(1)/n jv_r_s_c8m.res created by SHELXL-2017/1 at 09:38:53 on 14-Nov-2018 CELL 0.71073 22.3568 10.0540 28.8988 90.000 91.602 90.000 ZERR 4.00 0.0033 0.0015 0.0044 0.000 0.008 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 308 372 12 24 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.140 SIZE 0.150 0.188 0.491 L.S. 16 ACTA FMAP 2 PLAN 20 WGHT 0.065200 2.366300 FVAR 0.04293 RESI 1 O1 4 -0.889814 0.421076 0.114174 11.00000 0.01172 0.02180 = 0.02632 0.00494 -0.00676 0.00234 N1 3 -0.427480 0.217887 0.200471 11.00000 0.01144 0.01991 = 0.02115 0.00122 -0.00127 0.00052 C3 1 -0.550763 0.252328 0.180563 11.00000 0.01056 0.01582 = 0.01420 0.00041 -0.00010 0.00163 C4 1 -0.614729 0.264687 0.169148 11.00000 0.01090 0.01609 = 0.01827 -0.00068 -0.00081 0.00052 AFIX 43 H4 2 -0.637500 0.184938 0.167751 11.00000 -1.20000 AFIX 0 C5 1 -0.643975 0.378948 0.160486 11.00000 0.01184 0.01703 = 0.01627 -0.00049 -0.00156 0.00050 AFIX 43 H5 2 -0.621064 0.458526 0.161481 11.00000 -1.20000 AFIX 0 C6 1 -0.708021 0.391790 0.149648 11.00000 0.01187 0.01588 = 0.01499 -0.00103 -0.00217 0.00236 C9 1 -0.829942 0.419720 0.124906 11.00000 0.01171 0.01949 = 0.01639 -0.00048 -0.00353 0.00285 C10 1 -0.913782 0.535330 0.090403 11.00000 0.01400 0.02106 = 0.01768 0.00218 -0.00354 0.00514 AFIX 23 H10A 2 -0.892401 0.550650 0.061339 11.00000 -1.20000 H10B 2 -0.909459 0.615547 0.110080 11.00000 -1.20000 AFIX 0 C11 1 -0.979213 0.506583 0.079994 11.00000 0.01304 0.02165 = 0.01944 -0.00076 -0.00399 0.00433 AFIX 23 H11A 2 -0.999691 0.491096 0.109447 11.00000 -1.20000 H11B 2 -0.982601 0.424188 0.061347 11.00000 -1.20000 AFIX 0 C12 1 -1.010508 0.619632 0.053830 11.00000 0.01267 0.02243 = 0.01920 0.00035 -0.00229 0.00443 AFIX 23 H12A 2 -0.989461 0.636513 0.024719 11.00000 -1.20000 H12B 2 -1.007936 0.701540 0.072796 11.00000 -1.20000 AFIX 0 C13 1 -1.076261 0.589264 0.042353 11.00000 0.01411 0.02008 = 0.02005 -0.00074 -0.00369 0.00440 AFIX 23 H13A 2 -1.078879 0.506226 0.023997 11.00000 -1.20000 H13B 2 -1.097504 0.574404 0.071507 11.00000 -1.20000 AFIX 0 C14 1 -1.107169 0.700803 0.015289 11.00000 0.01212 0.02095 = 0.02056 0.00147 -0.00241 0.00287 AFIX 23 H14A 2 -1.085747 0.714766 -0.013837 11.00000 -1.20000 H14B 2 -1.103610 0.783800 0.033594 11.00000 -1.20000 AFIX 0 C15 1 -1.173159 0.676666 0.003338 11.00000 0.01277 0.01757 = 0.02001 0.00017 -0.00302 0.00189 AFIX 23 H15A 2 -1.176993 0.598765 -0.017488 11.00000 -1.20000 H15B 2 -1.194542 0.656120 0.032013 11.00000 -1.20000 AFIX 0 C16 1 -1.202044 0.797325 -0.020157 11.00000 0.01296 0.02050 = 0.02493 0.00317 -0.00394 0.00106 AFIX 23 H16A 2 -1.198803 0.874154 0.001194 11.00000 -1.20000 H16B 2 -1.179339 0.819383 -0.048063 11.00000 -1.20000 AFIX 0 C17 1 -1.267526 0.778013 -0.034339 11.00000 0.01359 0.03018 = 0.02410 0.00190 -0.00455 0.00158 AFIX 137 H17A 2 -1.271194 0.703714 -0.056185 11.00000 -1.50000 H17B 2 -1.282871 0.859341 -0.049115 11.00000 -1.50000 H17C 2 -1.290687 0.758547 -0.006852 11.00000 -1.50000 AFIX 0 C1A 1 -0.463256 0.114792 0.189567 11.00000 0.01275 0.01662 = 0.02150 0.00105 -0.00016 0.00299 AFIX 43 H1A 2 -0.445883 0.028656 0.188485 11.00000 -1.20000 AFIX 0 C2A 1 -0.524023 0.126513 0.179795 11.00000 0.01197 0.01520 = 0.01978 0.00046 -0.00058 0.00053 AFIX 43 H2A 2 -0.547341 0.049859 0.172636 11.00000 -1.20000 AFIX 0 C7A 1 -0.749272 0.290398 0.158859 11.00000 0.01267 0.01626 = 0.01854 0.00185 -0.00263 0.00247 AFIX 43 H7A 2 -0.735678 0.210972 0.173526 11.00000 -1.20000 AFIX 0 C8A 1 -0.809143 0.304083 0.146996 11.00000 0.01284 0.01749 = 0.02044 0.00224 -0.00247 0.00025 AFIX 43 H8A 2 -0.836370 0.234741 0.153846 11.00000 -1.20000 AFIX 0 C1B 1 -0.453386 0.337923 0.202165 11.00000 0.01393 0.01829 = 0.02396 -0.00049 -0.00328 -0.00169 AFIX 43 H1B 2 -0.429057 0.412242 0.210316 11.00000 -1.20000 AFIX 0 C2B 1 -0.513713 0.359641 0.192680 11.00000 0.01399 0.01484 = 0.02229 -0.00089 -0.00285 0.00162 AFIX 43 H2B 2 -0.529804 0.446898 0.194399 11.00000 -1.20000 AFIX 0 C7B 1 -0.730075 0.507709 0.128785 11.00000 0.01465 0.01460 = 0.01880 0.00012 -0.00276 0.00082 AFIX 43 H7B 2 -0.703196 0.578584 0.122994 11.00000 -1.20000 AFIX 0 C8B 1 -0.790426 0.522656 0.116171 11.00000 0.01491 0.01609 = 0.01833 0.00175 -0.00303 0.00311 AFIX 43 H8B 2 -0.804291 0.602279 0.101788 11.00000 -1.20000 AFIX 0 RESI 2 O1 4 0.665143 0.699334 0.431330 11.00000 0.01334 0.02757 = 0.02420 0.00451 -0.00383 -0.00432 N1 3 0.210164 0.355801 0.397031 11.00000 0.01515 0.02021 = 0.02213 -0.00483 -0.00339 -0.00076 C3 1 0.332871 0.408627 0.414280 11.00000 0.01365 0.01467 = 0.01856 -0.00299 -0.00178 -0.00025 C4 1 0.396268 0.437467 0.423971 11.00000 0.01429 0.02039 = 0.01859 -0.00231 -0.00291 0.00074 AFIX 43 H4 2 0.416871 0.386455 0.447040 11.00000 -1.20000 AFIX 0 C5 1 0.426678 0.532232 0.401921 11.00000 0.01260 0.02029 = 0.02104 -0.00185 -0.00197 0.00135 AFIX 43 H5 2 0.404972 0.578529 0.378225 11.00000 -1.20000 AFIX 0 C6 1 0.488841 0.573507 0.409609 11.00000 0.01249 0.01776 = 0.01901 -0.00148 -0.00065 0.00112 C9 1 0.607498 0.662968 0.421872 11.00000 0.01278 0.02025 = 0.01900 -0.00168 -0.00122 -0.00034 C10 1 0.691034 0.798378 0.401935 11.00000 0.01581 0.02425 = 0.02909 0.00414 -0.00234 -0.00347 AFIX 23 H10A 2 0.667720 0.881953 0.403188 11.00000 -1.20000 H10B 2 0.690690 0.766811 0.369479 11.00000 -1.20000 AFIX 0 C11 1 0.754618 0.822250 0.419119 11.00000 0.01559 0.02390 = 0.03473 -0.00080 -0.00287 -0.00342 AFIX 23 H11A 2 0.753771 0.857407 0.451094 11.00000 -1.20000 H11B 2 0.772817 0.891215 0.399518 11.00000 -1.20000 AFIX 0 C12 1 0.794157 0.698609 0.418905 11.00000 0.01586 0.02341 = 0.02526 -0.00119 -0.00180 -0.00253 AFIX 23 H12A 2 0.780779 0.636221 0.443018 11.00000 -1.20000 H12B 2 0.789314 0.653611 0.388560 11.00000 -1.20000 AFIX 0 C13 1 0.860031 0.730866 0.427726 11.00000 0.01519 0.02422 = 0.03694 -0.00455 -0.00205 -0.00136 AFIX 23 H13A 2 0.873308 0.791947 0.403182 11.00000 -1.20000 H13B 2 0.864396 0.778336 0.457644 11.00000 -1.20000 AFIX 0 C14 1 0.900894 0.610179 0.428956 11.00000 0.01807 0.02312 = 0.02470 -0.00219 0.00019 -0.00149 AFIX 23 H14A 2 0.896419 0.561854 0.399212 11.00000 -1.20000 H14B 2 0.888304 0.549580 0.453870 11.00000 -1.20000 AFIX 0 C15 1 0.966719 0.646419 0.437188 11.00000 0.01754 0.02202 = 0.02657 -0.00463 -0.00043 0.00055 AFIX 23 H15A 2 0.978610 0.710152 0.413004 11.00000 -1.20000 H15B 2 0.971198 0.691877 0.467475 11.00000 -1.20000 AFIX 0 C16 1 1.009062 0.528147 0.436751 11.00000 0.02172 0.02381 = 0.02232 -0.00207 0.00152 0.00333 AFIX 23 H16A 2 1.005354 0.483368 0.406295 11.00000 -1.20000 H16B 2 0.997137 0.463675 0.460688 11.00000 -1.20000 AFIX 0 C17 1 1.074108 0.567760 0.445745 11.00000 0.01998 0.03792 = 0.02863 -0.00152 0.00079 0.00601 AFIX 137 H17A 2 1.086519 0.629816 0.421687 11.00000 -1.50000 H17B 2 1.099432 0.488244 0.445226 11.00000 -1.50000 H17C 2 1.078224 0.610710 0.476109 11.00000 -1.50000 AFIX 0 C1A 1 0.237693 0.320631 0.436957 11.00000 0.01678 0.02267 = 0.01884 -0.00262 0.00010 -0.00339 AFIX 43 H1A 2 0.214818 0.277045 0.459653 11.00000 -1.20000 AFIX 0 C2A 1 0.297859 0.344464 0.446947 11.00000 0.01609 0.02173 = 0.01789 -0.00073 -0.00279 -0.00184 AFIX 43 H2A 2 0.315195 0.317359 0.475818 11.00000 -1.20000 AFIX 0 C7A 1 0.527245 0.516532 0.443414 11.00000 0.01451 0.01898 = 0.01882 0.00005 -0.00006 -0.00011 AFIX 43 H7A 2 0.513049 0.446629 0.462308 11.00000 -1.20000 AFIX 0 C8A 1 0.585434 0.560931 0.449524 11.00000 0.01524 0.02119 = 0.01813 0.00005 -0.00322 0.00076 AFIX 43 H8A 2 0.610693 0.521766 0.472730 11.00000 -1.20000 AFIX 0 C1B 1 0.243803 0.418111 0.366086 11.00000 0.01899 0.02023 = 0.02015 -0.00126 -0.00631 -0.00122 AFIX 43 H1B 2 0.225037 0.445197 0.337729 11.00000 -1.20000 AFIX 0 C2B 1 0.303892 0.445512 0.372696 11.00000 0.01818 0.01923 = 0.01753 -0.00079 -0.00252 -0.00292 AFIX 43 H2B 2 0.325424 0.489069 0.349209 11.00000 -1.20000 AFIX 0 C7B 1 0.511787 0.674736 0.382402 11.00000 0.01497 0.02271 = 0.02189 0.00250 -0.00333 0.00051 AFIX 43 H7B 2 0.486406 0.714862 0.359481 11.00000 -1.20000 AFIX 0 C8B 1 0.570560 0.719279 0.387565 11.00000 0.01512 0.02282 = 0.02341 0.00452 -0.00255 -0.00170 AFIX 43 H8B 2 0.585243 0.787047 0.367987 11.00000 -1.20000 AFIX 0 RESI 3 O1 4 0.751164 0.185799 0.371869 11.00000 0.01141 0.02893 = 0.03143 -0.00623 -0.00684 0.00090 N1 3 0.288142 0.121244 0.262722 11.00000 0.01116 0.02224 = 0.01618 -0.00053 -0.00046 0.00039 C3 1 0.411378 0.122589 0.286141 11.00000 0.01094 0.02258 = 0.01416 0.00120 -0.00060 -0.00065 C4 1 0.475478 0.116148 0.297965 11.00000 0.01192 0.02290 = 0.01833 0.00097 -0.00087 0.00053 AFIX 43 H4 2 0.495405 0.034536 0.292312 11.00000 -1.20000 AFIX 0 C5 1 0.508251 0.215548 0.316043 11.00000 0.01230 0.02279 = 0.01994 0.00073 -0.00108 0.00104 AFIX 43 H5 2 0.488416 0.297752 0.320855 11.00000 -1.20000 AFIX 0 C6 1 0.571983 0.209223 0.329109 11.00000 0.01274 0.02253 = 0.01668 0.00203 -0.00049 -0.00177 C9 1 0.692683 0.201414 0.358680 11.00000 0.01104 0.02341 = 0.01869 0.00303 -0.00198 -0.00144 C10 1 0.780422 0.287617 0.398873 11.00000 0.01396 0.02551 = 0.02163 -0.00057 -0.00356 -0.00162 AFIX 23 H10A 2 0.757341 0.308204 0.426723 11.00000 -1.20000 H10B 2 0.784519 0.369935 0.380432 11.00000 -1.20000 AFIX 0 C11 1 0.841387 0.232168 0.412491 11.00000 0.01269 0.03177 = 0.01980 0.00164 -0.00272 -0.00045 AFIX 23 H11A 2 0.836164 0.146477 0.428764 11.00000 -1.20000 H11B 2 0.861717 0.294442 0.434309 11.00000 -1.20000 AFIX 0 C12 1 0.880970 0.210225 0.370901 11.00000 0.01660 0.03411 = 0.02104 -0.00001 0.00029 -0.00152 AFIX 23 H12A 2 0.855787 0.177899 0.344513 11.00000 -1.20000 H12B 2 0.898495 0.296488 0.361834 11.00000 -1.20000 AFIX 0 C13 1 0.931437 0.110992 0.380252 11.00000 0.01790 0.02538 = 0.02763 -0.00417 0.00046 -0.00279 AFIX 23 H13A 2 0.913641 0.025087 0.389406 11.00000 -1.20000 H13B 2 0.952618 0.096085 0.351073 11.00000 -1.20000 AFIX 0 C14 1 0.977095 0.152622 0.417538 11.00000 0.01815 0.02374 = 0.02602 -0.00482 -0.00146 0.00199 AFIX 23 H14A 2 0.995215 0.238397 0.408618 11.00000 -1.20000 H14B 2 0.956373 0.166476 0.446981 11.00000 -1.20000 AFIX 0 C15 1 1.026391 0.050428 0.425121 11.00000 0.02254 0.02424 = 0.02972 -0.00427 -0.00137 0.00486 AFIX 23 H15A 2 1.007993 -0.035205 0.433864 11.00000 -1.20000 H15B 2 1.046766 0.036563 0.395527 11.00000 -1.20000 AFIX 0 C16 1 1.072591 0.088114 0.461820 11.00000 0.03000 0.03216 = 0.04005 -0.00708 -0.01119 0.01006 AFIX 23 H16A 2 1.052140 0.104602 0.491220 11.00000 -1.20000 H16B 2 1.091963 0.172240 0.452619 11.00000 -1.20000 AFIX 0 C17 1 1.120513 -0.016323 0.470112 11.00000 0.03169 0.04108 = 0.02799 0.00180 -0.00129 0.01551 AFIX 137 H17A 2 1.140744 -0.034214 0.441113 11.00000 -1.50000 H17B 2 1.102083 -0.098379 0.481197 11.00000 -1.50000 H17C 2 1.149725 0.016042 0.493391 11.00000 -1.50000 AFIX 0 C1A 1 0.320843 0.009722 0.262712 11.00000 0.01373 0.01969 = 0.01781 -0.00066 -0.00077 -0.00150 AFIX 43 H1A 2 0.301288 -0.071364 0.254795 11.00000 -1.20000 AFIX 0 C2A 1 0.381552 0.005733 0.273582 11.00000 0.01274 0.02075 = 0.01831 -0.00025 -0.00070 0.00217 AFIX 43 H2A 2 0.402719 -0.076087 0.272484 11.00000 -1.20000 AFIX 0 C7A 1 0.609399 0.103704 0.316295 11.00000 0.01552 0.02392 = 0.02170 -0.00225 -0.00246 -0.00241 AFIX 43 H7A 2 0.593552 0.034024 0.297438 11.00000 -1.20000 AFIX 0 C8A 1 0.668986 0.099807 0.330743 11.00000 0.01495 0.02320 = 0.02334 -0.00259 -0.00125 -0.00018 AFIX 43 H8A 2 0.693716 0.028096 0.321661 11.00000 -1.20000 AFIX 0 C1B 1 0.316923 0.234201 0.274150 11.00000 0.01455 0.01948 = 0.02196 -0.00147 -0.00170 0.00286 AFIX 43 H1B 2 0.294697 0.314740 0.274040 11.00000 -1.20000 AFIX 0 C2B 1 0.377319 0.239627 0.286101 11.00000 0.01528 0.01984 = 0.02281 -0.00129 -0.00268 -0.00238 AFIX 43 H2B 2 0.395518 0.322089 0.294210 11.00000 -1.20000 AFIX 0 C7B 1 0.597091 0.310846 0.355908 11.00000 0.01302 0.02215 = 0.01936 0.00211 0.00002 -0.00004 AFIX 43 H7B 2 0.572822 0.384215 0.364151 11.00000 -1.20000 AFIX 0 C8B 1 0.656840 0.308143 0.371020 11.00000 0.01322 0.02146 = 0.01885 0.00110 -0.00048 -0.00240 AFIX 43 H8B 2 0.672905 0.378345 0.389528 11.00000 -1.20000 AFIX 0 RESI 4 O1 4 -0.323423 0.086829 0.197504 11.00000 0.00786 0.02095 = 0.03128 -0.00304 -0.00382 -0.00007 H1 2 -0.351939 0.146423 0.202173 11.00000 0.06779 O2 4 0.097404 0.343114 0.357215 11.00000 0.01298 0.02638 = 0.02027 -0.00875 -0.00425 0.00244 H2A 2 0.134325 0.337482 0.369335 11.00000 0.04269 O3 4 0.174429 0.079882 0.232534 11.00000 0.00876 0.02111 = 0.02000 -0.00460 -0.00030 0.00195 H3A 2 0.210670 0.101704 0.245177 11.00000 0.04887 C1 1 -0.267392 0.128450 0.209441 11.00000 0.00922 0.01879 = 0.01852 0.00108 -0.00196 -0.00064 C2 1 -0.254650 0.251374 0.229598 11.00000 0.01063 0.01761 = 0.02659 -0.00272 -0.00140 0.00267 AFIX 43 H2 2 -0.285984 0.312915 0.234846 11.00000 -1.20000 AFIX 0 C3 1 -0.195757 0.283827 0.242052 11.00000 0.01181 0.01665 = 0.02489 -0.00410 -0.00193 0.00097 AFIX 43 H3 2 -0.187529 0.367340 0.256230 11.00000 -1.20000 AFIX 0 C4 1 -0.148465 0.196240 0.234154 11.00000 0.00939 0.01743 = 0.01643 -0.00178 -0.00131 -0.00032 C5 1 -0.162284 0.073624 0.213408 11.00000 0.01029 0.01819 = 0.02192 -0.00329 -0.00139 0.00154 AFIX 43 H5 2 -0.131014 0.012378 0.207612 11.00000 -1.20000 AFIX 0 C6 1 -0.220643 0.040185 0.201218 11.00000 0.01184 0.01686 = 0.02182 -0.00420 -0.00237 0.00035 AFIX 43 H6 2 -0.228978 -0.043432 0.187152 11.00000 -1.20000 AFIX 0 C7 1 -0.087399 0.230908 0.249548 11.00000 0.01094 0.01735 = 0.01821 -0.00176 -0.00229 -0.00148 AFIX 43 H7 2 -0.082803 0.306047 0.269260 11.00000 -1.20000 AFIX 0 C8 1 -0.037351 0.165923 0.238273 11.00000 0.01002 0.01910 = 0.01733 -0.00201 -0.00182 -0.00103 AFIX 43 H8 2 -0.041577 0.098098 0.215528 11.00000 -1.20000 AFIX 0 C9 1 0.023242 0.189147 0.257559 11.00000 0.01006 0.01409 = 0.01666 0.00128 -0.00162 -0.00060 C10 1 0.033561 0.261426 0.298289 11.00000 0.00977 0.01579 = 0.01758 -0.00023 -0.00044 0.00082 AFIX 43 H10 2 0.001072 0.302905 0.313116 11.00000 -1.20000 AFIX 0 C11 1 0.091368 0.272927 0.317269 11.00000 0.01196 0.01373 = 0.01531 -0.00046 -0.00168 -0.00034 C12 1 0.139745 0.213654 0.295608 11.00000 0.00974 0.01338 = 0.01636 0.00061 -0.00230 -0.00050 AFIX 43 H12 2 0.179127 0.222389 0.308455 11.00000 -1.20000 AFIX 0 C13 1 0.129508 0.141441 0.254857 11.00000 0.00937 0.01289 = 0.01664 0.00146 0.00006 0.00054 C14 1 0.071632 0.129121 0.235999 11.00000 0.01077 0.01614 = 0.01587 -0.00139 -0.00147 -0.00033 AFIX 43 H14 2 0.065012 0.079634 0.208323 11.00000 -1.20000 RESI 0 REM ##### AFIX 0 HKLF 4 REM jv_r_s_c8m in P2(1)/n REM R1 = 0.0516 for 17323 Fo > 4sig(Fo) and 0.0849 for all 24524 data REM 790 parameters refined using 0 restraints END WGHT 0.0652 2.3664 REM Highest difference peak 0.619, deepest hole -0.326, 1-sigma level 0.058 Q1 1 0.5915 0.2530 0.3439 11.00000 0.05 0.62 Q2 1 0.5797 0.1374 0.3243 11.00000 0.05 0.59 Q3 1 0.3971 0.0620 0.2810 11.00000 0.05 0.56 Q4 1 0.5118 0.1277 0.3079 11.00000 0.05 0.55 Q5 1 0.4741 0.1974 0.3093 11.00000 0.05 0.53 Q6 1 0.3515 0.0182 0.2698 11.00000 0.05 0.52 Q7 1 -0.7597 0.5102 0.1220 11.00000 0.05 0.50 Q8 1 -0.9476 0.5246 0.0875 11.00000 0.05 0.50 Q9 1 0.0612 0.2551 0.3100 11.00000 0.05 0.50 Q10 1 0.4044 0.1870 0.2915 11.00000 0.05 0.49 Q11 1 -0.4818 0.3420 0.1970 11.00000 0.05 0.49 Q12 1 0.0999 0.1307 0.2451 11.00000 0.05 0.49 Q13 1 -0.4919 0.1306 0.1844 11.00000 0.05 0.48 Q14 1 -0.7783 0.2980 0.1520 11.00000 0.05 0.48 Q15 1 0.4574 0.5537 0.4083 11.00000 0.05 0.47 Q16 1 -0.2238 0.2569 0.2393 11.00000 0.05 0.47 Q17 1 -0.7291 0.3428 0.1517 11.00000 0.05 0.47 Q18 1 0.5581 0.5283 0.4421 11.00000 0.05 0.46 Q19 1 0.3202 0.4248 0.3928 11.00000 0.05 0.46 Q20 1 -0.1175 0.2087 0.2406 11.00000 0.05 0.46 ; _shelx_res_checksum 16169 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 O1_1 O -0.88981(3) 0.42108(8) 0.11417(3) 0.02008(16) Uani 1 1 d . . N1_1 N -0.42748(4) 0.21789(10) 0.20047(3) 0.01753(18) Uani 1 1 d . . C3_1 C -0.55076(4) 0.25233(10) 0.18056(4) 0.01354(18) Uani 1 1 d . . C4_1 C -0.61473(4) 0.26469(11) 0.16915(4) 0.01511(19) Uani 1 1 d . . H4_1 H -0.637500 0.184938 0.167751 0.018 Uiso 1 1 calc R U C5_1 C -0.64397(4) 0.37895(11) 0.16049(4) 0.01508(19) Uani 1 1 d . . H5_1 H -0.621064 0.458526 0.161481 0.018 Uiso 1 1 calc R U C6_1 C -0.70802(4) 0.39179(10) 0.14965(4) 0.01429(18) Uani 1 1 d . . C9_1 C -0.82994(4) 0.41972(11) 0.12491(4) 0.01594(19) Uani 1 1 d . . C10_1 C -0.91378(5) 0.53533(11) 0.09040(4) 0.0177(2) Uani 1 1 d . . H10A_1 H -0.892401 0.550650 0.061339 0.021 Uiso 1 1 calc R U H10B_1 H -0.909459 0.615547 0.110080 0.021 Uiso 1 1 calc R U C11_1 C -0.97921(5) 0.50658(11) 0.07999(4) 0.0181(2) Uani 1 1 d . . H11A_1 H -0.999691 0.491096 0.109447 0.022 Uiso 1 1 calc R U H11B_1 H -0.982601 0.424188 0.061347 0.022 Uiso 1 1 calc R U C12_1 C -1.01051(5) 0.61963(12) 0.05383(4) 0.0182(2) Uani 1 1 d . . H12A_1 H -0.989461 0.636513 0.024719 0.022 Uiso 1 1 calc R U H12B_1 H -1.007936 0.701540 0.072796 0.022 Uiso 1 1 calc R U C13_1 C -1.07626(5) 0.58926(11) 0.04235(4) 0.0182(2) Uani 1 1 d . . H13A_1 H -1.078879 0.506226 0.023997 0.022 Uiso 1 1 calc R U H13B_1 H -1.097504 0.574404 0.071507 0.022 Uiso 1 1 calc R U C14_1 C -1.10717(5) 0.70080(11) 0.01529(4) 0.0179(2) Uani 1 1 d . . H14A_1 H -1.085747 0.714766 -0.013837 0.022 Uiso 1 1 calc R U H14B_1 H -1.103610 0.783800 0.033594 0.022 Uiso 1 1 calc R U C15_1 C -1.17316(5) 0.67667(11) 0.00334(4) 0.0168(2) Uani 1 1 d . . H15A_1 H -1.176993 0.598765 -0.017488 0.020 Uiso 1 1 calc R U H15B_1 H -1.194542 0.656120 0.032013 0.020 Uiso 1 1 calc R U C16_1 C -1.20204(5) 0.79732(12) -0.02016(4) 0.0195(2) Uani 1 1 d . . H16A_1 H -1.198803 0.874154 0.001194 0.023 Uiso 1 1 calc R U H16B_1 H -1.179339 0.819383 -0.048063 0.023 Uiso 1 1 calc R U C17_1 C -1.26753(5) 0.77801(13) -0.03434(4) 0.0227(2) Uani 1 1 d . . H17A_1 H -1.271194 0.703714 -0.056185 0.034 Uiso 1 1 calc R U H17B_1 H -1.282871 0.859341 -0.049115 0.034 Uiso 1 1 calc R U H17C_1 H -1.290687 0.758547 -0.006852 0.034 Uiso 1 1 calc R U C1A_1 C -0.46326(5) 0.11479(11) 0.18957(4) 0.0170(2) Uani 1 1 d . . H1A_1 H -0.445883 0.028656 0.188485 0.020 Uiso 1 1 calc R U C2A_1 C -0.52402(4) 0.12651(11) 0.17980(4) 0.01567(19) Uani 1 1 d . . H2A_1 H -0.547341 0.049859 0.172636 0.019 Uiso 1 1 calc R U C7A_1 C -0.74927(4) 0.29040(11) 0.15886(4) 0.01588(19) Uani 1 1 d . . H7A_1 H -0.735678 0.210972 0.173526 0.019 Uiso 1 1 calc R U C8A_1 C -0.80914(5) 0.30408(11) 0.14700(4) 0.0170(2) Uani 1 1 d . . H8A_1 H -0.836370 0.234741 0.153846 0.020 Uiso 1 1 calc R U C1B_1 C -0.45339(5) 0.33792(11) 0.20216(4) 0.0188(2) Uani 1 1 d . . H1B_1 H -0.429057 0.412242 0.210316 0.023 Uiso 1 1 calc R U C2B_1 C -0.51371(5) 0.35964(11) 0.19268(4) 0.0171(2) Uani 1 1 d . . H2B_1 H -0.529804 0.446898 0.194399 0.021 Uiso 1 1 calc R U C7B_1 C -0.73008(5) 0.50771(11) 0.12878(4) 0.01608(19) Uani 1 1 d . . H7B_1 H -0.703196 0.578584 0.122994 0.019 Uiso 1 1 calc R U C8B_1 C -0.79043(5) 0.52266(11) 0.11617(4) 0.01651(19) Uani 1 1 d . . H8B_1 H -0.804291 0.602279 0.101788 0.020 Uiso 1 1 calc R U O1_2 O 0.66514(3) 0.69933(9) 0.43133(3) 0.02178(17) Uani 1 1 d . . N1_2 N 0.21016(4) 0.35580(10) 0.39703(3) 0.01924(19) Uani 1 1 d . . C3_2 C 0.33287(5) 0.40863(11) 0.41428(4) 0.01567(19) Uani 1 1 d . . C4_2 C 0.39627(5) 0.43747(11) 0.42397(4) 0.0178(2) Uani 1 1 d . . H4_2 H 0.416871 0.386455 0.447040 0.021 Uiso 1 1 calc R U C5_2 C 0.42668(5) 0.53223(11) 0.40192(4) 0.0180(2) Uani 1 1 d . . H5_2 H 0.404972 0.578529 0.378225 0.022 Uiso 1 1 calc R U C6_2 C 0.48884(5) 0.57351(11) 0.40961(4) 0.01644(19) Uani 1 1 d . . C9_2 C 0.60750(5) 0.66297(11) 0.42187(4) 0.0174(2) Uani 1 1 d . . C10_2 C 0.69103(5) 0.79838(12) 0.40193(5) 0.0231(2) Uani 1 1 d . . H10A_2 H 0.667720 0.881953 0.403188 0.028 Uiso 1 1 calc R U H10B_2 H 0.690690 0.766811 0.369479 0.028 Uiso 1 1 calc R U C11_2 C 0.75462(5) 0.82225(13) 0.41912(5) 0.0248(2) Uani 1 1 d . . H11A_2 H 0.753771 0.857407 0.451094 0.030 Uiso 1 1 calc R U H11B_2 H 0.772817 0.891215 0.399518 0.030 Uiso 1 1 calc R U C12_2 C 0.79416(5) 0.69861(12) 0.41891(4) 0.0216(2) Uani 1 1 d . . H12A_2 H 0.780779 0.636221 0.443018 0.026 Uiso 1 1 calc R U H12B_2 H 0.789314 0.653611 0.388560 0.026 Uiso 1 1 calc R U C13_2 C 0.86003(5) 0.73087(13) 0.42773(5) 0.0255(2) Uani 1 1 d . . H13A_2 H 0.873308 0.791947 0.403182 0.031 Uiso 1 1 calc R U H13B_2 H 0.864396 0.778336 0.457644 0.031 Uiso 1 1 calc R U C14_2 C 0.90089(5) 0.61018(12) 0.42896(4) 0.0220(2) Uani 1 1 d . . H14A_2 H 0.896419 0.561854 0.399212 0.026 Uiso 1 1 calc R U H14B_2 H 0.888304 0.549580 0.453870 0.026 Uiso 1 1 calc R U C15_2 C 0.96672(5) 0.64642(12) 0.43719(4) 0.0221(2) Uani 1 1 d . . H15A_2 H 0.978610 0.710152 0.413004 0.026 Uiso 1 1 calc R U H15B_2 H 0.971198 0.691877 0.467475 0.026 Uiso 1 1 calc R U C16_2 C 1.00906(5) 0.52815(12) 0.43675(4) 0.0226(2) Uani 1 1 d . . H16A_2 H 1.005354 0.483368 0.406295 0.027 Uiso 1 1 calc R U H16B_2 H 0.997137 0.463675 0.460688 0.027 Uiso 1 1 calc R U C17_2 C 1.07411(5) 0.56776(15) 0.44574(5) 0.0288(3) Uani 1 1 d . . H17A_2 H 1.086519 0.629816 0.421687 0.043 Uiso 1 1 calc R U H17B_2 H 1.099432 0.488244 0.445226 0.043 Uiso 1 1 calc R U H17C_2 H 1.078224 0.610710 0.476109 0.043 Uiso 1 1 calc R U C1A_2 C 0.23769(5) 0.32063(12) 0.43696(4) 0.0194(2) Uani 1 1 d . . H1A_2 H 0.214818 0.277045 0.459653 0.023 Uiso 1 1 calc R U C2A_2 C 0.29786(5) 0.34446(12) 0.44695(4) 0.0186(2) Uani 1 1 d . . H2A_2 H 0.315195 0.317359 0.475818 0.022 Uiso 1 1 calc R U C7A_2 C 0.52724(5) 0.51653(11) 0.44341(4) 0.0174(2) Uani 1 1 d . . H7A_2 H 0.513049 0.446629 0.462308 0.021 Uiso 1 1 calc R U C8A_2 C 0.58543(5) 0.56093(11) 0.44952(4) 0.0183(2) Uani 1 1 d . . H8A_2 H 0.610693 0.521766 0.472730 0.022 Uiso 1 1 calc R U C1B_2 C 0.24380(5) 0.41811(12) 0.36609(4) 0.0199(2) Uani 1 1 d . . H1B_2 H 0.225037 0.445197 0.337729 0.024 Uiso 1 1 calc R U C2B_2 C 0.30389(5) 0.44551(11) 0.37270(4) 0.0184(2) Uani 1 1 d . . H2B_2 H 0.325424 0.489069 0.349209 0.022 Uiso 1 1 calc R U C7B_2 C 0.51179(5) 0.67474(12) 0.38240(4) 0.0199(2) Uani 1 1 d . . H7B_2 H 0.486406 0.714862 0.359481 0.024 Uiso 1 1 calc R U C8B_2 C 0.57056(5) 0.71928(12) 0.38757(4) 0.0205(2) Uani 1 1 d . . H8B_2 H 0.585243 0.787047 0.367987 0.025 Uiso 1 1 calc R U O1_3 O 0.75116(3) 0.18580(9) 0.37187(3) 0.02406(18) Uani 1 1 d . . N1_3 N 0.28814(4) 0.12124(10) 0.26272(3) 0.01654(17) Uani 1 1 d . . C3_3 C 0.41138(4) 0.12259(11) 0.28614(4) 0.01591(19) Uani 1 1 d . . C4_3 C 0.47548(5) 0.11615(12) 0.29796(4) 0.0177(2) Uani 1 1 d . . H4_3 H 0.495405 0.034536 0.292312 0.021 Uiso 1 1 calc R U C5_3 C 0.50825(5) 0.21555(12) 0.31604(4) 0.0184(2) Uani 1 1 d . . H5_3 H 0.488416 0.297752 0.320855 0.022 Uiso 1 1 calc R U C6_3 C 0.57198(5) 0.20922(11) 0.32911(4) 0.0173(2) Uani 1 1 d . . C9_3 C 0.69268(5) 0.20141(12) 0.35868(4) 0.0178(2) Uani 1 1 d . . C10_3 C 0.78042(5) 0.28762(12) 0.39887(4) 0.0204(2) Uani 1 1 d . . H10A_3 H 0.757341 0.308204 0.426723 0.025 Uiso 1 1 calc R U H10B_3 H 0.784519 0.369935 0.380432 0.025 Uiso 1 1 calc R U C11_3 C 0.84139(5) 0.23217(13) 0.41249(4) 0.0215(2) Uani 1 1 d . . H11A_3 H 0.836164 0.146477 0.428764 0.026 Uiso 1 1 calc R U H11B_3 H 0.861717 0.294442 0.434309 0.026 Uiso 1 1 calc R U C12_3 C 0.88097(5) 0.21022(14) 0.37090(4) 0.0239(2) Uani 1 1 d . . H12A_3 H 0.855787 0.177899 0.344513 0.029 Uiso 1 1 calc R U H12B_3 H 0.898495 0.296488 0.361834 0.029 Uiso 1 1 calc R U C13_3 C 0.93144(5) 0.11099(13) 0.38025(4) 0.0236(2) Uani 1 1 d . . H13A_3 H 0.913641 0.025087 0.389406 0.028 Uiso 1 1 calc R U H13B_3 H 0.952618 0.096085 0.351073 0.028 Uiso 1 1 calc R U C14_3 C 0.97710(5) 0.15262(12) 0.41754(4) 0.0227(2) Uani 1 1 d . . H14A_3 H 0.995215 0.238397 0.408618 0.027 Uiso 1 1 calc R U H14B_3 H 0.956373 0.166476 0.446981 0.027 Uiso 1 1 calc R U C15_3 C 1.02639(5) 0.05043(13) 0.42512(5) 0.0255(2) Uani 1 1 d . . H15A_3 H 1.007993 -0.035205 0.433864 0.031 Uiso 1 1 calc R U H15B_3 H 1.046766 0.036563 0.395527 0.031 Uiso 1 1 calc R U C16_3 C 1.07259(6) 0.08811(15) 0.46182(5) 0.0343(3) Uani 1 1 d . . H16A_3 H 1.052140 0.104602 0.491220 0.041 Uiso 1 1 calc R U H16B_3 H 1.091963 0.172240 0.452619 0.041 Uiso 1 1 calc R U C17_3 C 1.12051(6) -0.01632(16) 0.47011(5) 0.0336(3) Uani 1 1 d . . H17A_3 H 1.140744 -0.034214 0.441113 0.050 Uiso 1 1 calc R U H17B_3 H 1.102083 -0.098379 0.481197 0.050 Uiso 1 1 calc R U H17C_3 H 1.149725 0.016042 0.493391 0.050 Uiso 1 1 calc R U C1A_3 C 0.32084(5) 0.00972(11) 0.26271(4) 0.0171(2) Uani 1 1 d . . H1A_3 H 0.301288 -0.071364 0.254795 0.021 Uiso 1 1 calc R U C2A_3 C 0.38155(5) 0.00573(11) 0.27358(4) 0.0173(2) Uani 1 1 d . . H2A_3 H 0.402719 -0.076087 0.272484 0.021 Uiso 1 1 calc R U C7A_3 C 0.60940(5) 0.10370(12) 0.31630(4) 0.0204(2) Uani 1 1 d . . H7A_3 H 0.593552 0.034024 0.297438 0.025 Uiso 1 1 calc R U C8A_3 C 0.66899(5) 0.09981(12) 0.33074(4) 0.0205(2) Uani 1 1 d . . H8A_3 H 0.693716 0.028096 0.321661 0.025 Uiso 1 1 calc R U C1B_3 C 0.31692(5) 0.23420(12) 0.27415(4) 0.0187(2) Uani 1 1 d . . H1B_3 H 0.294697 0.314740 0.274040 0.022 Uiso 1 1 calc R U C2B_3 C 0.37732(5) 0.23963(12) 0.28610(4) 0.0194(2) Uani 1 1 d . . H2B_3 H 0.395518 0.322089 0.294210 0.023 Uiso 1 1 calc R U C7B_3 C 0.59709(5) 0.31085(12) 0.35591(4) 0.0182(2) Uani 1 1 d . . H7B_3 H 0.572822 0.384215 0.364151 0.022 Uiso 1 1 calc R U C8B_3 C 0.65684(5) 0.30814(12) 0.37102(4) 0.0179(2) Uani 1 1 d . . H8B_3 H 0.672905 0.378345 0.389528 0.021 Uiso 1 1 calc R U O1_4 O -0.32342(3) 0.08683(9) 0.19750(3) 0.02011(17) Uani 1 1 d . . H1_4 H -0.3519(10) 0.146(2) 0.2022(8) 0.068(7) Uiso 1 1 d . . O2_4 O 0.09740(4) 0.34311(9) 0.35722(3) 0.01996(16) Uani 1 1 d . . H2A_4 H 0.1343(8) 0.3375(18) 0.3693(6) 0.043(5) Uiso 1 1 d . . O3_4 O 0.17443(3) 0.07988(8) 0.23253(3) 0.01664(15) Uani 1 1 d . . H3A_4 H 0.2107(9) 0.102(2) 0.2452(7) 0.049(5) Uiso 1 1 d . . C1_4 C -0.26739(4) 0.12845(11) 0.20944(4) 0.01556(19) Uani 1 1 d . . C2_4 C -0.25465(5) 0.25137(11) 0.22960(4) 0.0183(2) Uani 1 1 d . . H2_4 H -0.285984 0.312915 0.234846 0.022 Uiso 1 1 calc R U C3_4 C -0.19576(5) 0.28383(11) 0.24205(4) 0.0178(2) Uani 1 1 d . . H3_4 H -0.187529 0.367340 0.256230 0.021 Uiso 1 1 calc R U C4_4 C -0.14847(4) 0.19624(11) 0.23415(4) 0.01445(18) Uani 1 1 d . . C5_4 C -0.16228(4) 0.07362(11) 0.21341(4) 0.0168(2) Uani 1 1 d . . H5_4 H -0.131014 0.012378 0.207612 0.020 Uiso 1 1 calc R U C6_4 C -0.22064(5) 0.04019(11) 0.20122(4) 0.0169(2) Uani 1 1 d . . H6_4 H -0.228978 -0.043432 0.187152 0.020 Uiso 1 1 calc R U C7_4 C -0.08740(4) 0.23091(11) 0.24955(4) 0.01555(19) Uani 1 1 d . . H7_4 H -0.082803 0.306047 0.269260 0.019 Uiso 1 1 calc R U C8_4 C -0.03735(4) 0.16592(11) 0.23827(4) 0.01553(19) Uani 1 1 d . . H8_4 H -0.041577 0.098098 0.215528 0.019 Uiso 1 1 calc R U C9_4 C 0.02324(4) 0.18915(10) 0.25756(4) 0.01364(18) Uani 1 1 d . . C10_4 C 0.03356(4) 0.26143(10) 0.29829(4) 0.01439(18) Uani 1 1 d . . H10_4 H 0.001072 0.302905 0.313116 0.017 Uiso 1 1 calc R U C11_4 C 0.09137(4) 0.27293(10) 0.31727(4) 0.01370(18) Uani 1 1 d . . C12_4 C 0.13974(4) 0.21365(10) 0.29561(4) 0.01321(18) Uani 1 1 d . . H12_4 H 0.179127 0.222389 0.308455 0.016 Uiso 1 1 calc R U C13_4 C 0.12951(4) 0.14144(10) 0.25486(4) 0.01298(18) Uani 1 1 d . . C14_4 C 0.07163(4) 0.12912(10) 0.23600(4) 0.01430(18) Uani 1 1 d . . H14_4 H 0.065012 0.079634 0.208323 0.017 Uiso 1 1 calc R U 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 O1_1 0.0117(3) 0.0218(4) 0.0263(4) 0.0049(3) -0.0068(3) 0.0023(3) N1_1 0.0114(4) 0.0199(4) 0.0212(5) 0.0012(4) -0.0013(3) 0.0005(3) C3_1 0.0106(4) 0.0158(4) 0.0142(4) 0.0004(4) -0.0001(3) 0.0016(3) C4_1 0.0109(4) 0.0161(5) 0.0183(5) -0.0007(4) -0.0008(3) 0.0005(3) C5_1 0.0118(4) 0.0170(5) 0.0163(5) -0.0005(4) -0.0016(3) 0.0005(3) C6_1 0.0119(4) 0.0159(4) 0.0150(5) -0.0010(4) -0.0022(3) 0.0024(3) C9_1 0.0117(4) 0.0195(5) 0.0164(5) -0.0005(4) -0.0035(3) 0.0029(4) C10_1 0.0140(4) 0.0211(5) 0.0177(5) 0.0022(4) -0.0035(4) 0.0051(4) C11_1 0.0130(4) 0.0217(5) 0.0194(5) -0.0008(4) -0.0040(4) 0.0043(4) C12_1 0.0127(4) 0.0224(5) 0.0192(5) 0.0003(4) -0.0023(4) 0.0044(4) C13_1 0.0141(4) 0.0201(5) 0.0201(5) -0.0007(4) -0.0037(4) 0.0044(4) C14_1 0.0121(4) 0.0210(5) 0.0206(5) 0.0015(4) -0.0024(4) 0.0029(4) C15_1 0.0128(4) 0.0176(5) 0.0200(5) 0.0002(4) -0.0030(4) 0.0019(4) C16_1 0.0130(4) 0.0205(5) 0.0249(6) 0.0032(4) -0.0039(4) 0.0011(4) C17_1 0.0136(5) 0.0302(6) 0.0241(6) 0.0019(5) -0.0045(4) 0.0016(4) C1A_1 0.0127(4) 0.0166(5) 0.0215(5) 0.0011(4) -0.0002(4) 0.0030(4) C2A_1 0.0120(4) 0.0152(5) 0.0198(5) 0.0005(4) -0.0006(3) 0.0005(3) C7A_1 0.0127(4) 0.0163(5) 0.0185(5) 0.0019(4) -0.0026(3) 0.0025(3) C8A_1 0.0128(4) 0.0175(5) 0.0204(5) 0.0022(4) -0.0025(4) 0.0002(4) C1B_1 0.0139(4) 0.0183(5) 0.0240(5) -0.0005(4) -0.0033(4) -0.0017(4) C2B_1 0.0140(4) 0.0148(5) 0.0223(5) -0.0009(4) -0.0028(4) 0.0016(4) C7B_1 0.0146(4) 0.0146(5) 0.0188(5) 0.0001(4) -0.0028(4) 0.0008(4) C8B_1 0.0149(4) 0.0161(5) 0.0183(5) 0.0017(4) -0.0030(4) 0.0031(4) O1_2 0.0133(3) 0.0276(4) 0.0242(4) 0.0045(3) -0.0038(3) -0.0043(3) N1_2 0.0152(4) 0.0202(4) 0.0221(5) -0.0048(4) -0.0034(3) -0.0008(3) C3_2 0.0136(4) 0.0147(4) 0.0186(5) -0.0030(4) -0.0018(4) -0.0002(3) C4_2 0.0143(4) 0.0204(5) 0.0186(5) -0.0023(4) -0.0029(4) 0.0007(4) C5_2 0.0126(4) 0.0203(5) 0.0210(5) -0.0018(4) -0.0020(4) 0.0014(4) C6_2 0.0125(4) 0.0178(5) 0.0190(5) -0.0015(4) -0.0007(4) 0.0011(4) C9_2 0.0128(4) 0.0202(5) 0.0190(5) -0.0017(4) -0.0012(4) -0.0003(4) C10_2 0.0158(5) 0.0243(6) 0.0291(6) 0.0041(5) -0.0023(4) -0.0035(4) C11_2 0.0156(5) 0.0239(6) 0.0347(7) -0.0008(5) -0.0029(4) -0.0034(4) C12_2 0.0159(5) 0.0234(6) 0.0253(6) -0.0012(4) -0.0018(4) -0.0025(4) C13_2 0.0152(5) 0.0242(6) 0.0369(7) -0.0046(5) -0.0020(4) -0.0014(4) C14_2 0.0181(5) 0.0231(5) 0.0247(6) -0.0022(4) 0.0002(4) -0.0015(4) C15_2 0.0175(5) 0.0220(5) 0.0266(6) -0.0046(4) -0.0004(4) 0.0006(4) C16_2 0.0217(5) 0.0238(6) 0.0223(6) -0.0021(4) 0.0015(4) 0.0033(4) C17_2 0.0200(5) 0.0379(7) 0.0286(6) -0.0015(5) 0.0008(5) 0.0060(5) C1A_2 0.0168(5) 0.0227(5) 0.0188(5) -0.0026(4) 0.0001(4) -0.0034(4) C2A_2 0.0161(5) 0.0217(5) 0.0179(5) -0.0007(4) -0.0028(4) -0.0018(4) C7A_2 0.0145(4) 0.0190(5) 0.0188(5) 0.0001(4) -0.0001(4) -0.0001(4) C8A_2 0.0152(4) 0.0212(5) 0.0181(5) 0.0001(4) -0.0032(4) 0.0008(4) C1B_2 0.0190(5) 0.0202(5) 0.0202(5) -0.0013(4) -0.0063(4) -0.0012(4) C2B_2 0.0182(5) 0.0192(5) 0.0175(5) -0.0008(4) -0.0025(4) -0.0029(4) C7B_2 0.0150(5) 0.0227(5) 0.0219(5) 0.0025(4) -0.0033(4) 0.0005(4) C8B_2 0.0151(5) 0.0228(5) 0.0234(6) 0.0045(4) -0.0025(4) -0.0017(4) O1_3 0.0114(3) 0.0289(4) 0.0314(5) -0.0062(4) -0.0068(3) 0.0009(3) N1_3 0.0112(4) 0.0222(4) 0.0162(4) -0.0005(3) -0.0005(3) 0.0004(3) C3_3 0.0109(4) 0.0226(5) 0.0142(5) 0.0012(4) -0.0006(3) -0.0006(4) C4_3 0.0119(4) 0.0229(5) 0.0183(5) 0.0010(4) -0.0009(4) 0.0005(4) C5_3 0.0123(4) 0.0228(5) 0.0199(5) 0.0007(4) -0.0011(4) 0.0010(4) C6_3 0.0127(4) 0.0225(5) 0.0167(5) 0.0020(4) -0.0005(3) -0.0018(4) C9_3 0.0110(4) 0.0234(5) 0.0187(5) 0.0030(4) -0.0020(3) -0.0014(4) C10_3 0.0140(4) 0.0255(6) 0.0216(5) -0.0006(4) -0.0036(4) -0.0016(4) C11_3 0.0127(4) 0.0318(6) 0.0198(5) 0.0016(5) -0.0027(4) -0.0004(4) C12_3 0.0166(5) 0.0341(7) 0.0210(6) 0.0000(5) 0.0003(4) -0.0015(4) C13_3 0.0179(5) 0.0254(6) 0.0276(6) -0.0042(5) 0.0005(4) -0.0028(4) C14_3 0.0182(5) 0.0237(6) 0.0260(6) -0.0048(5) -0.0015(4) 0.0020(4) C15_3 0.0225(5) 0.0242(6) 0.0297(6) -0.0043(5) -0.0014(5) 0.0049(4) C16_3 0.0300(7) 0.0322(7) 0.0400(8) -0.0071(6) -0.0112(6) 0.0101(5) C17_3 0.0317(7) 0.0411(8) 0.0280(7) 0.0018(6) -0.0013(5) 0.0155(6) C1A_3 0.0137(4) 0.0197(5) 0.0178(5) -0.0007(4) -0.0008(4) -0.0015(4) C2A_3 0.0127(4) 0.0208(5) 0.0183(5) -0.0002(4) -0.0007(4) 0.0022(4) C7A_3 0.0155(5) 0.0239(5) 0.0217(5) -0.0022(4) -0.0025(4) -0.0024(4) C8A_3 0.0149(5) 0.0232(5) 0.0233(6) -0.0026(4) -0.0013(4) -0.0002(4) C1B_3 0.0145(4) 0.0195(5) 0.0220(5) -0.0015(4) -0.0017(4) 0.0029(4) C2B_3 0.0153(5) 0.0198(5) 0.0228(5) -0.0013(4) -0.0027(4) -0.0024(4) C7B_3 0.0130(4) 0.0222(5) 0.0194(5) 0.0021(4) 0.0000(4) 0.0000(4) C8B_3 0.0132(4) 0.0215(5) 0.0189(5) 0.0011(4) -0.0005(4) -0.0024(4) O1_4 0.0079(3) 0.0210(4) 0.0313(4) -0.0030(3) -0.0038(3) -0.0001(3) O2_4 0.0130(3) 0.0264(4) 0.0203(4) -0.0088(3) -0.0043(3) 0.0024(3) O3_4 0.0088(3) 0.0211(4) 0.0200(4) -0.0046(3) -0.0003(3) 0.0020(3) C1_4 0.0092(4) 0.0188(5) 0.0185(5) 0.0011(4) -0.0020(3) -0.0006(3) C2_4 0.0106(4) 0.0176(5) 0.0266(6) -0.0027(4) -0.0014(4) 0.0027(4) C3_4 0.0118(4) 0.0166(5) 0.0249(5) -0.0041(4) -0.0019(4) 0.0010(4) C4_4 0.0094(4) 0.0174(5) 0.0164(5) -0.0018(4) -0.0013(3) -0.0003(3) C5_4 0.0103(4) 0.0182(5) 0.0219(5) -0.0033(4) -0.0014(4) 0.0015(4) C6_4 0.0118(4) 0.0169(5) 0.0218(5) -0.0042(4) -0.0024(4) 0.0003(4) C7_4 0.0109(4) 0.0174(5) 0.0182(5) -0.0018(4) -0.0023(3) -0.0015(3) C8_4 0.0100(4) 0.0191(5) 0.0173(5) -0.0020(4) -0.0018(3) -0.0010(4) C9_4 0.0101(4) 0.0141(4) 0.0167(5) 0.0013(4) -0.0016(3) -0.0006(3) C10_4 0.0098(4) 0.0158(4) 0.0176(5) -0.0002(4) -0.0004(3) 0.0008(3) C11_4 0.0120(4) 0.0137(4) 0.0153(5) -0.0005(3) -0.0017(3) -0.0003(3) C12_4 0.0097(4) 0.0134(4) 0.0164(5) 0.0006(3) -0.0023(3) -0.0005(3) C13_4 0.0094(4) 0.0129(4) 0.0166(5) 0.0015(3) 0.0001(3) 0.0005(3) C14_4 0.0108(4) 0.0161(5) 0.0159(5) -0.0014(4) -0.0015(3) -0.0003(3) 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_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C9_1 O1_1 C10_1 117.86(9) C1B_1 N1_1 C1A_1 116.68(9) C2B_1 C3_1 C2A_1 116.80(9) C2B_1 C3_1 C4_1 123.98(9) C2A_1 C3_1 C4_1 119.22(9) C5_1 C4_1 C3_1 125.63(10) C4_1 C5_1 C6_1 125.76(10) C7B_1 C6_1 C7A_1 117.50(9) C7B_1 C6_1 C5_1 119.87(10) C7A_1 C6_1 C5_1 122.62(9) O1_1 C9_1 C8B_1 125.16(10) O1_1 C9_1 C8A_1 115.02(10) C8B_1 C9_1 C8A_1 119.81(9) O1_1 C10_1 C11_1 106.76(9) C10_1 C11_1 C12_1 112.58(9) C11_1 C12_1 C13_1 112.58(9) C14_1 C13_1 C12_1 112.60(9) C13_1 C14_1 C15_1 114.93(9) C16_1 C15_1 C14_1 111.66(9) C17_1 C16_1 C15_1 114.25(10) N1_1 C1A_1 C2A_1 123.87(10) C1A_1 C2A_1 C3_1 119.39(10) C8A_1 C7A_1 C6_1 121.20(10) C7A_1 C8A_1 C9_1 120.26(10) N1_1 C1B_1 C2B_1 123.63(10) C1B_1 C2B_1 C3_1 119.61(10) C6_1 C7B_1 C8B_1 122.00(10) C9_1 C8B_1 C7B_1 119.18(10) C9_2 O1_2 C10_2 117.48(9) C1B_2 N1_2 C1A_2 116.44(9) C2B_2 C3_2 C2A_2 116.54(10) C2B_2 C3_2 C4_2 122.25(10) C2A_2 C3_2 C4_2 121.19(10) C5_2 C4_2 C3_2 123.35(10) C4_2 C5_2 C6_2 128.45(10) C7B_2 C6_2 C7A_2 117.58(10) C7B_2 C6_2 C5_2 119.04(10) C7A_2 C6_2 C5_2 123.38(10) O1_2 C9_2 C8B_2 124.99(10) O1_2 C9_2 C8A_2 115.45(9) C8B_2 C9_2 C8A_2 119.56(10) O1_2 C10_2 C11_2 107.80(10) C10_2 C11_2 C12_2 114.14(10) C13_2 C12_2 C11_2 112.56(10) C14_2 C13_2 C12_2 114.34(10) C13_2 C14_2 C15_2 112.90(10) C16_2 C15_2 C14_2 114.17(10) C15_2 C16_2 C17_2 112.70(11) N1_2 C1A_2 C2A_2 123.53(11) C1A_2 C2A_2 C3_2 119.72(10) C8A_2 C7A_2 C6_2 120.80(10) C7A_2 C8A_2 C9_2 120.64(10) N1_2 C1B_2 C2B_2 124.30(10) C1B_2 C2B_2 C3_2 119.46(10) C8B_2 C7B_2 C6_2 122.41(10) C7B_2 C8B_2 C9_2 118.99(11) C9_3 O1_3 C10_3 119.35(9) C1A_3 N1_3 C1B_3 116.79(9) C2A_3 C3_3 C2B_3 116.84(9) C2A_3 C3_3 C4_3 118.75(10) C2B_3 C3_3 C4_3 124.41(10) C5_3 C4_3 C3_3 125.44(11) C4_3 C5_3 C6_3 125.92(11) C7B_3 C6_3 C7A_3 117.82(10) C7B_3 C6_3 C5_3 119.08(10) C7A_3 C6_3 C5_3 123.09(10) O1_3 C9_3 C8B_3 124.95(10) O1_3 C9_3 C8A_3 115.05(10) C8B_3 C9_3 C8A_3 120.01(10) O1_3 C10_3 C11_3 105.79(10) C10_3 C11_3 C12_3 112.67(10) C13_3 C12_3 C11_3 113.39(10) C14_3 C13_3 C12_3 115.08(10) C15_3 C14_3 C13_3 112.70(10) C16_3 C15_3 C14_3 114.31(11) C15_3 C16_3 C17_3 113.87(12) N1_3 C1A_3 C2A_3 123.78(10) C1A_3 C2A_3 C3_3 119.55(10) C8A_3 C7A_3 C6_3 121.05(11) C7A_3 C8A_3 C9_3 119.96(11) N1_3 C1B_3 C2B_3 123.50(10) C1B_3 C2B_3 C3_3 119.53(10) C6_3 C7B_3 C8B_3 121.90(11) C9_3 C8B_3 C7B_3 119.23(10) O1_4 C1_4 C2_4 123.85(10) O1_4 C1_4 C6_4 116.81(10) C2_4 C1_4 C6_4 119.33(9) C1_4 C2_4 C3_4 119.77(10) C2_4 C3_4 C4_4 121.54(10) C3_4 C4_4 C5_4 117.69(9) C3_4 C4_4 C7_4 120.15(9) C5_4 C4_4 C7_4 122.09(9) C6_4 C5_4 C4_4 121.18(10) C5_4 C6_4 C1_4 120.48(10) C8_4 C7_4 C4_4 125.84(10) C7_4 C8_4 C9_4 126.59(10) C10_4 C9_4 C14_4 119.19(9) C10_4 C9_4 C8_4 122.08(9) C14_4 C9_4 C8_4 118.58(9) C11_4 C10_4 C9_4 120.26(9) O2_4 C11_4 C10_4 116.54(9) O2_4 C11_4 C12_4 122.89(9) C10_4 C11_4 C12_4 120.57(9) C13_4 C12_4 C11_4 119.24(9) O3_4 C13_4 C14_4 117.65(9) O3_4 C13_4 C12_4 122.10(9) C14_4 C13_4 C12_4 120.24(9) C13_4 C14_4 C9_4 120.50(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1_1 C9_1 1.3656(12) O1_1 C10_1 1.4346(13) N1_1 C1B_1 1.3401(15) N1_1 C1A_1 1.3414(14) C3_1 C2B_1 1.3988(15) C3_1 C2A_1 1.3995(14) C3_1 C4_1 1.4639(14) C4_1 C5_1 1.3419(15) C5_1 C6_1 1.4629(14) C6_1 C7B_1 1.3958(14) C6_1 C7A_1 1.4051(15) C9_1 C8B_1 1.3884(15) C9_1 C8A_1 1.3996(15) C10_1 C11_1 1.5131(15) C11_1 C12_1 1.5243(15) C12_1 C13_1 1.5287(15) C13_1 C14_1 1.5220(15) C14_1 C15_1 1.5252(14) C15_1 C16_1 1.5248(15) C16_1 C17_1 1.5216(15) C1A_1 C2A_1 1.3849(14) C7A_1 C8A_1 1.3793(14) C1B_1 C2B_1 1.3861(14) C7B_1 C8B_1 1.3959(14) O1_2 C9_2 1.3600(13) O1_2 C10_2 1.4407(15) N1_2 C1B_2 1.3399(16) N1_2 C1A_2 1.3399(15) C3_2 C2B_2 1.3992(15) C3_2 C2A_2 1.4005(16) C3_2 C4_2 1.4660(14) C4_2 C5_2 1.3417(16) C5_2 C6_2 1.4614(15) C6_2 C7B_2 1.3928(16) C6_2 C7A_2 1.4046(15) C9_2 C8B_2 1.3927(15) C9_2 C8A_2 1.3987(16) C10_2 C11_2 1.5118(16) C11_2 C12_2 1.5255(17) C12_2 C13_2 1.5225(16) C13_2 C14_2 1.5187(17) C14_2 C15_2 1.5282(16) C15_2 C16_2 1.5202(17) C16_2 C17_2 1.5231(17) C1A_2 C2A_2 1.3887(15) C7A_2 C8A_2 1.3820(15) C1B_2 C2B_2 1.3794(15) C7B_2 C8B_2 1.3923(15) O1_3 C9_3 1.3607(12) O1_3 C10_3 1.4340(14) N1_3 C1A_3 1.3385(14) N1_3 C1B_3 1.3420(15) C3_3 C2A_3 1.3940(15) C3_3 C2B_3 1.4016(16) C3_3 C4_3 1.4654(14) C4_3 C5_3 1.3368(16) C5_3 C6_3 1.4652(14) C6_3 C7B_3 1.3909(16) C6_3 C7A_3 1.4070(16) C9_3 C8B_3 1.3917(16) C9_3 C8A_3 1.3972(16) C10_3 C11_3 1.5144(15) C11_3 C12_3 1.5283(17) C12_3 C13_3 1.5246(17) C13_3 C14_3 1.5221(17) C14_3 C15_3 1.5182(17) C15_3 C16_3 1.5080(18) C16_3 C17_3 1.5144(18) C1A_3 C2A_3 1.3851(14) C7A_3 C8A_3 1.3854(15) C1B_3 C2B_3 1.3854(15) C7B_3 C8B_3 1.3940(14) O1_4 C1_4 1.3562(12) O2_4 C11_4 1.3565(13) O3_4 C13_4 1.3580(12) C1_4 C2_4 1.3923(15) C1_4 C6_4 1.3965(15) C2_4 C3_4 1.3939(14) C3_4 C4_4 1.3996(14) C4_4 C5_4 1.4015(15) C4_4 C7_4 1.4660(14) C5_4 C6_4 1.3834(14) C7_4 C8_4 1.3437(15) C8_4 C9_4 1.4690(14) C9_4 C10_4 1.3970(15) C9_4 C14_4 1.4002(14) C10_4 C11_4 1.3946(13) C11_4 C12_4 1.3981(14) C12_4 C13_4 1.3969(14) C13_4 C14_4 1.3954(13)