#------------------------------------------------------------------------------ #$Date: 2021-09-06 13:29:07 +0300 (Mon, 06 Sep 2021) $ #$Revision: 268671 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/32/7243244.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_7243244 loop_ _publ_author_name 'Bereczki, Laura' 'Zodge, Amit' 'K\>or\"osi, M\'arton' 'Holczbauer, Tam\'as' 'De, Sourav' 'Sz\'ekely, Edit' 'Bombicz, Petra' _publ_section_title ; A bug in enantiomer separation: double salt formation -- diastereomeric and double salt structures of 1-cyclohexylethylammonium 2- and 4-chloromandelate ; _journal_issue 31 _journal_name_full CrystEngComm _journal_page_first 5367 _journal_page_last 5376 _journal_paper_doi 10.1039/D1CE00145K _journal_volume 23 _journal_year 2021 _chemical_absolute_configuration rmad _chemical_formula_moiety 'C8 H18 N 1+, C8 H6 Cl O3 1-' _chemical_formula_sum 'C16 H24 Cl N O3' _chemical_formula_weight 313.81 _chemical_melting_point 426(1) _chemical_name_common ; (R)-(1-cyclohexylethyl)ammonium (S)-4-chloromandelate' ; _chemical_name_systematic ; (R)-(1-cyclohexylethyl)ammonium (S)-2-(4-chlorophenyl)-2-hydroxyacetate ; _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-01-29 deposited with the CCDC. 2021-07-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.843(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 10.4640(6) _cell_length_b 10.4673(7) _cell_length_c 29.8915(16) _cell_measurement_reflns_used 5466 _cell_measurement_temperature 113(2) _cell_measurement_theta_max 66.380 _cell_measurement_theta_min 6.910 _cell_volume 3250.7(3) _computing_cell_refinement ; RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015) ; _computing_data_collection ; RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015) ; _computing_data_reduction ; RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015) ; _computing_molecular_graphics ; Spek, A.L. (2003). J.Appl.Cryst. 36,7-13. ; _computing_publication_material ; C. F. Macrae, J. Appl. Cryst., 41, 466-470, 2008 ; _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution ; Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8. ; _diffrn_ambient_temperature 113(2) _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type RAXIS-RAPID _diffrn_measurement_method dtprofit.ref _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54187 _diffrn_reflns_av_unetI/netI 0.0803 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 6812 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 50.435 _diffrn_reflns_theta_max 50.435 _diffrn_reflns_theta_min 6.536 _diffrn_source 'Sealed Tube' _exptl_absorpt_coefficient_mu 2.161 _exptl_absorpt_correction_T_max 0.841 _exptl_absorpt_correction_T_min 0.373 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; NUMABS, Numerical Absorption correction Program (T.Higashi, 2003) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.282 _exptl_crystal_description prism _exptl_crystal_F_000 1344 _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.020 _exptl_transmission_factor_max 0.840704 _exptl_transmission_factor_min 0.372680 _refine_diff_density_max 0.496 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.108 _refine_ls_abs_structure_details ; Flack x determined using 2166 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.036(11) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 725 _refine_ls_number_reflns 6812 _refine_ls_number_restraints 607 _refine_ls_restrained_S_all 1.102 _refine_ls_R_factor_all 0.0974 _refine_ls_R_factor_gt 0.0908 _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^)+16.4355P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1842 _refine_ls_wR_factor_ref 0.1879 _reflns_Friedel_coverage 0.868 _reflns_Friedel_fraction_full 0.997 _reflns_Friedel_fraction_max 0.997 _reflns_number_gt 6308 _reflns_number_total 6812 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ce00145k2.cif _cod_data_source_block shelx_CCDC2 _cod_depositor_comments 'Adding full bibliography for 7243242--7243247.cif.' _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 7243244 _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 0.411 _shelx_estimated_absorpt_t_max 0.958 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL SIR2014 run in space group P 1 New:P21 CELL 1.54187 10.4640 10.4673 29.8915 90.000 96.843 90.000 ZERR 8.00 0.0006 0.0007 0.0016 0.000 0.003 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H CL N O UNIT 128 192 8 8 24 MERG 2 delu 0.001 c11a c12a c13a c14a c15a c16a delu 0.001 c11b c12b c13b c14b c15b c16b delu 0.001 c11c c12c c13c c14c c15c c16c delu 0.001 c11d c12d c13d c14d c15d c16d isor 0.001 c11a c12a c13a c14a c15a c16a isor 0.001 c11b c12b c13b c14b c15b c16b isor 0.001 c11c c12c c13c c14c c15c c16c isor 0.001 c11d c12d c13d c14d c15d c16d isor 0.002 o1a o2a o3a o1b o2b o3b o1c o2c o3c o1d o2d o3d delu 0.001 c1a c2a c3a c4a c5a c6a c7a c8a c9a c10a delu 0.001 c1b c2b c3b c4b c5b c6b c7b c8b c9b c10b delu 0.001 c1c c2c c3c c4c c5c c6c c7c c8c c9c c10c delu 0.001 c1d c2d c3d c4d c5d c6d c7d c8d c9d c10d isor 0.001 c1a c2a c3a c4a c5a c6a c7a c8a c9a c10a isor 0.001 c1b c2b c3b c4b c5b c6b c7b c8b c9b c10b isor 0.001 c1c c2c c3c c4c c5c c6c c7c c8c c9c c10c isor 0.001 c1d c2d c3d c4d c5d c6d c7d c8d c9d c10d isor 0.005 n1a n1b n1c n1d DFIX 0.95 0.005 O3A H3OA O3C H3OC O3D H3OD DFIX 0.95 0.005 O3B H3OB DFIX 1.9 0.02 O1D H3OC O2B H3OA SHEL 999 1 FMAP 2 1 53 PLAN 50 SIZE 0.020 0.100 0.500 ACTA BOND $H CONF L.S. 8 TEMP -160.00 WGHT 0.000000 16.032301 FVAR 13.69783 CL1A 3 0.423162 0.839844 0.315371 11.00000 0.08688 0.02814 = 0.04530 0.00738 -0.01295 -0.00725 O1A 5 0.635429 0.466714 0.493320 11.00000 0.02781 0.02979 = 0.03225 -0.00549 0.00433 0.00469 O2A 5 0.509601 0.317392 0.457055 11.00000 0.02257 0.02209 = 0.02706 -0.00447 0.00280 -0.00153 O3A 5 0.298753 0.432497 0.479442 11.00000 0.02293 0.02365 = 0.03268 -0.00012 0.00778 -0.00796 C1A 1 0.528538 0.423943 0.477065 11.00000 0.02656 0.02697 = 0.02625 -0.00017 0.00370 -0.00071 C2A 1 0.410230 0.510707 0.479681 11.00000 0.02790 0.02841 = 0.02880 -0.00079 0.00347 0.00045 AFIX 13 H2A 2 0.422635 0.561107 0.508290 11.00000 -1.40000 AFIX 66 C3A 1 0.405482 0.601182 0.439870 11.00000 0.02861 0.02825 = 0.02929 -0.00067 0.00332 0.00094 C4A 1 0.501189 0.692938 0.439023 11.00000 0.03078 0.03044 = 0.03117 0.00048 0.00315 -0.00100 AFIX 43 H4A 2 0.563833 0.704055 0.464457 11.00000 -1.50000 AFIX 65 C5A 1 0.505238 0.768428 0.400961 11.00000 0.03195 0.03098 = 0.03163 0.00071 0.00346 -0.00077 AFIX 43 H5A 2 0.570650 0.831139 0.400382 11.00000 -1.50000 AFIX 65 C6A 1 0.413580 0.752163 0.363746 11.00000 0.03116 0.03035 = 0.03084 0.00004 0.00389 0.00053 C7A 1 0.317872 0.660407 0.364593 11.00000 0.03093 0.03129 = 0.03048 0.00043 0.00322 0.00030 AFIX 43 H7A 2 0.255228 0.649291 0.339158 11.00000 -1.50000 AFIX 65 C8A 1 0.313822 0.584916 0.402654 11.00000 0.03019 0.03009 = 0.02988 -0.00011 0.00266 0.00013 AFIX 43 H8A 2 0.248410 0.522205 0.403233 11.00000 -1.50000 AFIX 0 CL1B 3 -0.101174 0.936891 0.304179 11.00000 0.08871 0.02957 = 0.04945 0.01135 -0.00907 -0.00608 O1B 5 -0.041151 0.713478 0.522682 11.00000 0.02724 0.02591 = 0.03503 -0.00780 0.00645 0.00218 O2B 5 0.116989 0.578977 0.510610 11.00000 0.02319 0.02600 = 0.02912 -0.00661 0.00023 -0.00587 O3B 5 -0.040107 0.449438 0.446083 11.00000 0.03118 0.01918 = 0.02653 0.00100 0.00080 0.00183 AFIX 3 H3OB 2 0.016463 0.420598 0.471949 11.00000 -1.30000 AFIX 0 C1B 1 0.005825 0.624238 0.500688 11.00000 0.02887 0.02867 = 0.02973 -0.00020 0.00434 -0.00006 C2B 1 -0.081701 0.569975 0.461181 11.00000 0.03069 0.03106 = 0.03114 -0.00100 0.00344 -0.00033 AFIX 13 H2B 2 -0.170570 0.560845 0.469919 11.00000 -1.40000 AFIX 66 C3B 1 -0.085101 0.663804 0.421179 11.00000 0.03087 0.03163 = 0.03115 -0.00053 0.00300 -0.00049 C4B 1 -0.138228 0.784587 0.424663 11.00000 0.03343 0.03245 = 0.03358 -0.00024 0.00380 0.00067 AFIX 43 H4B 2 -0.170583 0.809524 0.451728 11.00000 -1.50000 AFIX 65 C5B 1 -0.144017 0.868885 0.388547 11.00000 0.03466 0.03320 = 0.03458 0.00043 0.00429 0.00057 AFIX 43 H5B 2 -0.180327 0.951435 0.390929 11.00000 -1.50000 AFIX 65 C6B 1 -0.096678 0.832400 0.348948 11.00000 0.03340 0.03335 = 0.03384 0.00043 0.00360 0.00024 C7B 1 -0.043550 0.711617 0.345463 11.00000 0.03325 0.03308 = 0.03267 0.00051 0.00438 -0.00035 AFIX 43 H7B 2 -0.011196 0.686682 0.318398 11.00000 -1.50000 AFIX 65 C8B 1 -0.037760 0.627319 0.381578 11.00000 0.03278 0.03260 = 0.03197 -0.00013 0.00404 -0.00023 AFIX 43 H8B 2 -0.001450 0.544769 0.379197 11.00000 -1.50000 AFIX 0 CL1C 3 1.018871 0.019825 0.201422 11.00000 0.04880 0.02354 = 0.03965 0.00608 -0.00163 -0.00189 O1C 5 1.133286 0.394106 0.027095 11.00000 0.02323 0.02525 = 0.03451 -0.00817 0.00447 -0.00464 O2C 5 1.027960 0.568653 0.046190 11.00000 0.01798 0.01492 = 0.02560 -0.00295 0.00133 -0.00293 O3C 5 0.805963 0.444759 0.041722 11.00000 0.01770 0.02767 = 0.03074 0.00297 -0.00185 0.00321 C1C 1 1.036739 0.450985 0.037087 11.00000 0.02537 0.02540 = 0.02520 -0.00012 0.00271 0.00061 C2C 1 0.918845 0.368121 0.039715 11.00000 0.02587 0.02628 = 0.02651 -0.00049 0.00331 -0.00001 AFIX 13 H2C 2 0.905252 0.315018 0.011742 11.00000 -1.40000 AFIX 66 C3C 1 0.941325 0.277431 0.080294 11.00000 0.02610 0.02635 = 0.02684 -0.00018 0.00337 -0.00024 C4C 1 0.917733 0.320446 0.122534 11.00000 0.02641 0.02648 = 0.02682 -0.00023 0.00340 -0.00011 AFIX 43 H4C 2 0.885505 0.404296 0.125928 11.00000 -1.50000 AFIX 65 C5C 1 0.941295 0.240776 0.159806 11.00000 0.02774 0.02736 = 0.02715 0.00010 0.00329 0.00011 AFIX 43 H5C 2 0.925170 0.270175 0.188675 11.00000 -1.50000 AFIX 65 C6C 1 0.988449 0.118090 0.154841 11.00000 0.02711 0.02708 = 0.02747 0.00042 0.00300 -0.00012 C7C 1 1.012042 0.075074 0.112602 11.00000 0.02719 0.02684 = 0.02803 0.00010 0.00333 0.00004 AFIX 43 H7C 2 1.044270 -0.008776 0.109208 11.00000 -1.50000 AFIX 65 C8C 1 0.988480 0.154743 0.075328 11.00000 0.02678 0.02687 = 0.02711 -0.00041 0.00323 0.00045 AFIX 43 H8C 2 1.004605 0.125343 0.046460 11.00000 -1.50000 AFIX 0 CL1D 3 0.482610 0.049171 0.233527 11.00000 0.05126 0.02756 = 0.02954 0.00554 0.00394 -0.00048 O1D 5 0.628909 0.259135 0.016649 11.00000 0.01429 0.02564 = 0.03015 -0.00269 0.00202 -0.00457 O2D 5 0.449536 0.142958 0.002488 11.00000 0.02578 0.02390 = 0.02865 -0.00289 0.00361 -0.00278 O3D 5 0.503897 0.439121 0.060778 11.00000 0.02413 0.02455 = 0.02686 -0.00582 0.00149 0.00174 AFIX 3 H3OD 2 0.508807 0.448071 0.027728 11.00000 -1.30000 AFIX 0 C1D 1 0.514536 0.233364 0.021507 11.00000 0.02171 0.02136 = 0.02224 0.00031 0.00201 0.00020 C2D 1 0.445140 0.315681 0.053905 11.00000 0.02340 0.02362 = 0.02412 -0.00088 0.00327 0.00037 AFIX 13 H2D 2 0.352453 0.325643 0.041721 11.00000 -1.40000 AFIX 66 C3D 1 0.455805 0.250675 0.099507 11.00000 0.02412 0.02427 = 0.02392 -0.00089 0.00343 0.00048 C4D 1 0.575828 0.228938 0.123596 11.00000 0.02489 0.02553 = 0.02571 0.00006 0.00257 0.00032 AFIX 43 H4D 2 0.651561 0.256468 0.111779 11.00000 -1.50000 AFIX 65 C5D 1 0.585043 0.166921 0.164974 11.00000 0.02541 0.02538 = 0.02564 -0.00018 0.00234 -0.00007 AFIX 43 H5D 2 0.667074 0.152065 0.181438 11.00000 -1.50000 AFIX 65 C6D 1 0.474235 0.126641 0.182264 11.00000 0.02598 0.02580 = 0.02589 -0.00009 0.00275 -0.00024 C7D 1 0.354212 0.148377 0.158175 11.00000 0.02543 0.02494 = 0.02506 -0.00013 0.00335 -0.00024 AFIX 43 H7D 2 0.278480 0.120847 0.169992 11.00000 -1.50000 AFIX 65 C8D 1 0.344995 0.210394 0.116797 11.00000 0.02488 0.02466 = 0.02509 -0.00020 0.00344 -0.00036 AFIX 43 H8D 2 0.262964 0.225250 0.100334 11.00000 -1.50000 AFIX 0 N1A 4 0.286880 0.162665 0.447838 11.00000 0.02908 0.02677 = 0.02687 0.00648 0.00179 -0.00484 AFIX 137 H1A1 2 0.210699 0.198153 0.453103 11.00000 -1.50000 H1A2 2 0.348304 0.224493 0.448897 11.00000 -1.50000 H1A3 2 0.310747 0.102600 0.469220 11.00000 -1.50000 AFIX 0 C9A 1 0.271936 0.101553 0.402388 11.00000 0.02917 0.02890 = 0.02911 -0.00029 0.00352 0.00004 AFIX 13 H9A 2 0.357222 0.063387 0.398079 11.00000 -1.40000 AFIX 0 C10A 1 0.179453 -0.006255 0.402947 11.00000 0.03212 0.02978 = 0.03167 0.00029 0.00310 -0.00167 AFIX 137 H10A 2 0.210125 -0.065646 0.427220 11.00000 -1.40000 H10B 2 0.172511 -0.051120 0.373983 11.00000 -1.40000 H10C 2 0.094811 0.026999 0.408007 11.00000 -1.40000 AFIX 0 C11A 1 0.241926 0.200846 0.365507 11.00000 0.02580 0.02592 = 0.02662 -0.00013 0.00308 -0.00026 AFIX 13 H11A 2 0.304932 0.272037 0.372394 11.00000 -1.50000 AFIX 0 C12A 1 0.109990 0.258723 0.364151 11.00000 0.02571 0.02586 = 0.02586 -0.00048 0.00281 -0.00016 AFIX 23 H12A 2 0.101996 0.300199 0.393453 11.00000 -1.50000 H12B 2 0.044759 0.189940 0.359775 11.00000 -1.50000 AFIX 0 C13A 1 0.082232 0.357961 0.326247 11.00000 0.02664 0.02642 = 0.02657 0.00013 0.00297 0.00009 AFIX 23 H13A 2 -0.007721 0.388064 0.325375 11.00000 -1.50000 H13B 2 0.139706 0.432472 0.332776 11.00000 -1.50000 AFIX 0 C14A 1 0.102237 0.303194 0.280719 11.00000 0.02678 0.02672 = 0.02637 0.00027 0.00297 -0.00042 AFIX 23 H14A 2 0.091466 0.371600 0.257707 11.00000 -1.50000 H14B 2 0.036673 0.236639 0.272115 11.00000 -1.50000 AFIX 0 C15A 1 0.237080 0.244957 0.282078 11.00000 0.02735 0.02757 = 0.02712 0.00005 0.00380 0.00004 AFIX 23 H15A 2 0.245077 0.203101 0.252842 11.00000 -1.50000 H15B 2 0.301891 0.314166 0.286245 11.00000 -1.50000 AFIX 0 C16A 1 0.265574 0.147155 0.319886 11.00000 0.02658 0.02671 = 0.02722 -0.00042 0.00343 0.00040 AFIX 23 H16A 2 0.210406 0.071130 0.313056 11.00000 -1.50000 H16B 2 0.356435 0.119507 0.321264 11.00000 -1.50000 AFIX 0 N1B 4 0.755642 0.265811 0.432809 11.00000 0.02145 0.01583 = 0.02690 0.00319 0.00212 0.00951 AFIX 137 H1B1 2 0.812671 0.331787 0.434806 11.00000 -1.50000 H1B2 2 0.785573 0.203000 0.452355 11.00000 -1.50000 H1B3 2 0.678252 0.294015 0.439863 11.00000 -1.50000 AFIX 0 C9B 1 0.739920 0.214274 0.385828 11.00000 0.02208 0.02210 = 0.02191 -0.00001 0.00266 0.00052 AFIX 13 H9B 2 0.820078 0.166338 0.381349 11.00000 -1.40000 AFIX 0 C10B 1 0.629116 0.118375 0.383154 11.00000 0.02624 0.02578 = 0.02777 -0.00121 0.00314 -0.00306 AFIX 137 H10D 2 0.648513 0.052467 0.406251 11.00000 -1.40000 H10E 2 0.618178 0.078435 0.353290 11.00000 -1.40000 H10F 2 0.549616 0.162735 0.388206 11.00000 -1.40000 AFIX 0 C11B 1 0.722925 0.319935 0.351070 11.00000 0.03351 0.03371 = 0.03451 -0.00009 0.00430 -0.00067 AFIX 13 H11B 2 0.796389 0.380402 0.358477 11.00000 -1.50000 AFIX 0 C12B 1 0.600736 0.398294 0.350055 11.00000 0.03515 0.03547 = 0.03567 0.00006 0.00420 0.00092 AFIX 23 H12C 2 0.598281 0.439545 0.379744 11.00000 -1.50000 H12D 2 0.525235 0.340987 0.344547 11.00000 -1.50000 AFIX 0 C13B 1 0.592300 0.500895 0.313450 11.00000 0.03586 0.03585 = 0.03611 0.00048 0.00423 0.00077 AFIX 23 H13C 2 0.509948 0.547651 0.313106 11.00000 -1.50000 H13D 2 0.663303 0.562892 0.320480 11.00000 -1.50000 AFIX 0 C14B 1 0.600560 0.443325 0.267326 11.00000 0.03614 0.03636 = 0.03590 0.00030 0.00382 0.00040 AFIX 23 H14C 2 0.596133 0.511957 0.244405 11.00000 -1.50000 H14D 2 0.527108 0.384713 0.259374 11.00000 -1.50000 AFIX 0 C15B 1 0.726255 0.370558 0.267680 11.00000 0.03574 0.03559 = 0.03492 0.00022 0.00411 -0.00014 AFIX 23 H15C 2 0.799646 0.430297 0.273675 11.00000 -1.50000 H15D 2 0.730513 0.330691 0.237860 11.00000 -1.50000 AFIX 0 C16B 1 0.735348 0.266865 0.304212 11.00000 0.03470 0.03497 = 0.03466 -0.00021 0.00434 -0.00046 AFIX 23 H16C 2 0.666484 0.203095 0.296303 11.00000 -1.50000 H16D 2 0.819077 0.222459 0.304841 11.00000 -1.50000 AFIX 0 N1C 4 0.796364 0.726379 0.037415 11.00000 0.02035 0.01039 = 0.02524 0.00996 0.00158 -0.00139 AFIX 137 H1C1 2 0.721202 0.685341 0.028130 11.00000 -1.50000 H1C2 2 0.857363 0.668136 0.047789 11.00000 -1.50000 H1C3 2 0.822921 0.769994 0.013858 11.00000 -1.50000 AFIX 0 C9C 1 0.775940 0.818104 0.074434 11.00000 0.01952 0.01942 = 0.02011 -0.00005 0.00244 -0.00020 AFIX 13 H9C 2 0.858851 0.864563 0.082798 11.00000 -1.40000 AFIX 0 C10C 1 0.676974 0.915303 0.056442 11.00000 0.02116 0.02047 = 0.02110 -0.00034 0.00113 0.00075 AFIX 137 H10G 2 0.699380 0.949627 0.027884 11.00000 -1.40000 H10H 2 0.674980 0.984939 0.078262 11.00000 -1.40000 H10I 2 0.592105 0.874649 0.051459 11.00000 -1.40000 AFIX 0 C11C 1 0.745476 0.742594 0.116644 11.00000 0.02900 0.02934 = 0.02994 -0.00024 0.00314 -0.00015 AFIX 13 H11C 2 0.675464 0.679715 0.107225 11.00000 -1.50000 AFIX 0 C12C 1 0.697694 0.836311 0.151248 11.00000 0.03002 0.03024 = 0.03047 -0.00048 0.00346 0.00058 AFIX 23 H12E 2 0.762083 0.904919 0.158278 11.00000 -1.50000 H12F 2 0.616002 0.876321 0.138124 11.00000 -1.50000 AFIX 0 C13C 1 0.676603 0.765671 0.194456 11.00000 0.03100 0.03135 = 0.03059 -0.00012 0.00367 0.00066 AFIX 23 H13E 2 0.652155 0.828237 0.216775 11.00000 -1.50000 H13F 2 0.604106 0.705167 0.187814 11.00000 -1.50000 AFIX 0 C14C 1 0.792342 0.693837 0.214577 11.00000 0.03018 0.03045 = 0.03014 0.00006 0.00395 -0.00011 AFIX 23 H14E 2 0.770777 0.645602 0.241162 11.00000 -1.50000 H14F 2 0.861654 0.755123 0.224950 11.00000 -1.50000 AFIX 0 C15C 1 0.841276 0.600349 0.180707 11.00000 0.03036 0.03003 = 0.02970 0.00016 0.00334 0.00006 AFIX 23 H15E 2 0.922486 0.560351 0.194293 11.00000 -1.50000 H15F 2 0.777006 0.531785 0.173395 11.00000 -1.50000 AFIX 0 C16C 1 0.864007 0.669752 0.138323 11.00000 0.02923 0.02891 = 0.02943 -0.00023 0.00308 -0.00015 AFIX 23 H16E 2 0.890394 0.607184 0.116342 11.00000 -1.50000 H16F 2 0.935788 0.730853 0.145401 11.00000 -1.50000 AFIX 0 N1D 4 0.295684 0.636833 0.056967 11.00000 0.01865 0.02332 = 0.03866 0.00067 0.00508 0.00055 AFIX 137 H1D1 2 0.209951 0.619631 0.051788 11.00000 -1.50000 H1D2 2 0.339727 0.563135 0.063948 11.00000 -1.50000 H1D3 2 0.322450 0.671823 0.031813 11.00000 -1.50000 AFIX 0 C9D 1 0.320439 0.729564 0.095695 11.00000 0.02865 0.02867 = 0.02872 -0.00027 0.00354 -0.00024 AFIX 13 H9D 2 0.415362 0.735967 0.104718 11.00000 -1.40000 AFIX 0 C10D 1 0.270448 0.858358 0.078228 11.00000 0.03068 0.02927 = 0.02989 0.00084 0.00431 0.00008 AFIX 137 H10J 2 0.309856 0.880515 0.051113 11.00000 -1.40000 H10K 2 0.292441 0.923543 0.101403 11.00000 -1.40000 H10L 2 0.176733 0.854267 0.070878 11.00000 -1.40000 AFIX 0 C11D 1 0.256624 0.679602 0.135704 11.00000 0.02966 0.03026 = 0.03074 -0.00034 0.00355 -0.00024 AFIX 13 H11D 2 0.162721 0.669666 0.125319 11.00000 -1.50000 AFIX 0 C12D 1 0.268895 0.769823 0.175650 11.00000 0.03072 0.03082 = 0.03106 -0.00041 0.00360 -0.00021 AFIX 23 H12G 2 0.361379 0.787383 0.184588 11.00000 -1.50000 H12H 2 0.227208 0.851790 0.165966 11.00000 -1.50000 AFIX 0 C13D 1 0.212191 0.723276 0.215622 11.00000 0.03113 0.03153 = 0.03104 -0.00017 0.00383 0.00004 AFIX 23 H13G 2 0.117394 0.719245 0.208620 11.00000 -1.50000 H13H 2 0.232681 0.784084 0.240824 11.00000 -1.50000 AFIX 0 C14D 1 0.262722 0.593525 0.229698 11.00000 0.03216 0.03166 = 0.03164 0.00027 0.00387 -0.00002 AFIX 23 H14G 2 0.216207 0.561821 0.254446 11.00000 -1.50000 H14H 2 0.354920 0.600949 0.241496 11.00000 -1.50000 AFIX 0 C15D 1 0.248386 0.497138 0.191594 11.00000 0.03252 0.03139 = 0.03182 0.00033 0.00379 -0.00006 AFIX 23 H15G 2 0.155918 0.479282 0.182749 11.00000 -1.50000 H15H 2 0.290767 0.416139 0.202046 11.00000 -1.50000 AFIX 0 C16D 1 0.308652 0.547097 0.150592 11.00000 0.03107 0.03070 = 0.03115 -0.00006 0.00331 0.00018 AFIX 23 H16G 2 0.290178 0.486252 0.125291 11.00000 -1.50000 H16H 2 0.403231 0.552038 0.158183 11.00000 -1.50000 AFIX 0 H3OC 2 0.723323 0.405932 0.038190 11.00000 0.23646 H3OA 2 0.236352 0.498828 0.476609 11.00000 0.25094 HKLF 5 REM SIR2014 run in space group P 1 New:P21 REM R1 = 0.0908 for 6308 Fo > 4sig(Fo) and 0.0974 for all 6812 data REM 725 parameters refined using 607 restraints END WGHT 0.0000 16.0423 REM Highest difference peak 0.496, deepest hole -0.539, 1-sigma level 0.108 Q1 1 0.3233 0.3175 0.5002 11.00000 0.05 0.44 Q2 1 0.4212 0.8346 0.2994 11.00000 0.05 0.42 Q3 1 1.0351 -0.1022 0.2186 11.00000 0.05 0.41 Q4 1 0.5469 -0.0432 0.2190 11.00000 0.05 0.41 Q5 1 0.7071 0.3030 0.3420 11.00000 0.05 0.40 Q6 1 -0.0824 0.8498 0.3860 11.00000 0.05 0.39 Q7 1 0.5149 0.2566 0.2014 11.00000 0.05 0.38 Q8 1 0.8339 0.3468 0.0167 11.00000 0.05 0.38 Q9 1 1.1168 -0.0215 0.1010 11.00000 0.05 0.38 Q10 1 0.4476 0.3317 0.0413 11.00000 0.05 0.38 Q11 1 0.6103 0.0473 0.2566 11.00000 0.05 0.37 Q12 1 1.0322 0.0224 0.2376 11.00000 0.05 0.37 Q13 1 0.9413 0.2928 0.1005 11.00000 0.05 0.36 Q14 1 0.6249 0.0776 0.1781 11.00000 0.05 0.36 Q15 1 -0.0215 0.7406 0.5606 11.00000 0.05 0.36 Q16 1 0.9045 0.4228 0.1402 11.00000 0.05 0.36 Q17 1 0.8487 0.8172 0.1391 11.00000 0.05 0.35 Q18 1 0.4325 0.9004 0.1054 11.00000 0.05 0.35 Q19 1 0.9614 0.6183 0.1216 11.00000 0.05 0.35 Q20 1 0.0447 0.8365 0.3599 11.00000 0.05 0.35 Q21 1 0.5119 0.3313 0.3343 11.00000 0.05 0.35 Q22 1 0.0913 0.0334 0.3380 11.00000 0.05 0.35 Q23 1 -0.0283 0.1314 0.2555 11.00000 0.05 0.35 Q24 1 0.4765 0.5232 0.3607 11.00000 0.05 0.35 Q25 1 0.3334 0.1166 0.1824 11.00000 0.05 0.35 Q26 1 0.8344 0.8233 0.1053 11.00000 0.05 0.34 Q27 1 0.6117 0.5759 0.0596 11.00000 0.05 0.34 Q28 1 0.0293 0.0404 0.4418 11.00000 0.05 0.34 Q29 1 0.2657 0.5463 0.5229 11.00000 0.05 0.34 Q30 1 0.5337 0.7573 0.3790 11.00000 0.05 0.34 Q31 1 -0.0926 0.6515 0.3857 11.00000 0.05 0.34 Q32 1 -0.1782 0.8204 0.3595 11.00000 0.05 0.34 Q33 1 0.3261 0.8875 0.2160 11.00000 0.05 0.34 Q34 1 -0.1996 0.9262 0.3564 11.00000 0.05 0.33 Q35 1 1.0229 0.5614 0.0618 11.00000 0.05 0.33 Q36 1 0.8649 -0.0089 0.2342 11.00000 0.05 0.33 Q37 1 0.7565 0.7229 0.1340 11.00000 0.05 0.33 Q38 1 -0.2203 0.9144 0.3039 11.00000 0.05 0.33 Q39 1 0.4295 0.4047 0.3950 11.00000 0.05 0.33 Q40 1 0.8188 0.4128 0.2970 11.00000 0.05 0.33 Q41 1 1.0604 0.2094 0.0981 11.00000 0.05 0.33 Q42 1 0.2032 0.3541 0.4942 11.00000 0.05 0.32 Q43 1 0.0343 0.8233 0.4372 11.00000 0.05 0.32 Q44 1 0.9883 0.1136 0.1408 11.00000 0.05 0.32 Q45 1 1.0850 0.6705 0.0208 11.00000 0.05 0.32 Q46 1 0.9767 0.1327 0.2288 11.00000 0.05 0.32 Q47 1 1.1365 0.3821 0.0375 11.00000 0.05 0.32 Q48 1 0.6653 0.6766 0.1850 11.00000 0.05 0.32 Q49 1 0.6437 0.5902 0.3172 11.00000 0.05 0.32 Q50 1 0.7626 0.1440 0.1002 11.00000 0.05 0.32 ; _shelx_res_checksum 6765 _shelx_hkl_file ; 0 12 0 46461 6337 -2 0 -12 0 46461 6337 1 1 -12 0 33617 8184 1 2 -12 0 3779 4888 1 -3 12 2 36146 6990 -2 3 -12 0 36146 6990 1 1 -11 0 11793 6905 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10656 8837 1 -1 -1 33 9008 7019 1 0 1 33 27734 6507 -2 0 -1 33 27734 6507 1 1 -1 33 35378 8042 1 2 -1 33 22790 6678 1 -3 1 35 49473 8013 -2 3 -1 33 49473 8013 1 -6 0 33 15288 3812 1 -5 0 33 49035 8056 1 -4 0 33 30320 8525 1 3 0 31 29728 5282 -2 -3 0 33 29728 5282 1 -2 0 33 38874 10486 1 -1 0 33 21483 11395 1 0 0 33 9394 3992 -2 0 0 33 9394 3992 1 1 0 33 12079 4856 1 2 0 33 5067 5499 1 -3 0 35 24921 8013 -2 3 0 33 24921 8013 1 -5 1 33 11962 4348 1 -4 1 33 14436 6649 1 3 -1 31 11537 6848 -2 -3 1 33 11537 6848 1 -2 1 33 20232 9974 1 -1 1 33 3353 5967 1 0 -1 33 12275 4683 -2 0 1 33 12275 4683 1 1 1 33 38480 6969 1 2 1 33 29439 6564 1 -3 -1 35 45344 6372 -2 3 1 33 45344 6372 1 -5 2 33 4938 2759 1 -4 2 33 18357 7303 1 3 -2 31 23614 8212 -2 -3 2 33 23614 8212 1 -2 2 33 17306 7303 1 -1 2 33 24665 7672 1 0 -2 33 9178 9292 -2 0 2 33 9178 9292 1 1 2 33 11901 4731 1 2 2 33 15696 3872 1 -4 3 33 8866 5655 1 3 -3 31 -4120 5257 -2 -3 3 33 -4120 5257 1 -2 3 33 37254 9832 1 -1 3 33 12645 6621 1 0 -3 33 10685 8553 -2 0 3 33 10685 8553 1 1 3 33 25603 5712 1 2 3 33 33617 10201 1 3 -4 31 39953 11963 -2 -3 4 33 39953 11963 1 -2 4 33 13441 6394 1 -1 4 33 -4944 4944 1 0 -4 33 43733 12390 -2 0 4 33 43733 12390 1 1 4 33 1989 4518 1 -1 -3 34 19380 6308 1 0 3 34 11310 4177 -2 0 -3 34 11310 4177 1 -1 -2 34 7371 5143 1 0 2 34 77150 12475 -2 0 -2 34 77150 12475 1 1 -2 34 21398 5797 1 -4 -1 34 21483 7559 1 3 1 32 11367 5484 -2 -3 -1 34 11367 5484 1 -2 -1 34 11699 4350 1 -1 -1 34 4888 5712 1 1 -1 34 9946 4433 1 2 -1 34 11253 4575 1 -5 0 34 30832 8667 1 -4 0 34 42255 8610 1 3 0 32 16311 6280 -2 -3 0 34 16311 6280 1 -2 0 34 20176 7530 1 -1 0 34 43164 10258 1 0 0 34 8605 4081 -2 0 0 34 8605 4081 1 1 0 34 14817 4216 1 2 0 34 26370 5911 1 -4 1 34 23955 7076 1 3 -1 32 5769 5769 -2 -3 1 34 5769 5769 1 -2 1 34 28360 6621 1 -1 1 34 19693 6138 1 0 -1 34 35691 8269 -2 0 1 34 35691 8269 1 1 1 34 7665 5385 1 2 1 34 13649 3382 1 -4 2 34 15913 6138 1 3 -2 32 27564 7758 -2 -3 2 34 27564 7758 1 -2 2 34 22818 7530 1 -1 2 34 30917 7843 1 0 -2 34 59049 11651 -2 0 2 34 59049 11651 1 1 2 34 37083 9548 1 3 -3 32 17163 6280 -2 -3 3 34 17163 6280 1 -2 3 34 23983 7331 1 -1 3 34 20488 6479 1 0 -3 34 5570 5229 -2 0 3 34 5570 5229 1 3 0 33 23813 6195 -2 -3 0 35 23813 6195 1 -2 0 35 12396 5598 1 -1 0 35 41147 9974 1 3 -1 33 44187 8610 -2 -3 1 35 44187 8610 1 -2 1 35 18868 6166 1 -1 1 35 29184 7161 1 0 -1 35 12674 5200 -2 0 1 35 12674 5200 1 -2 2 35 30803 7417 1 -1 2 35 15885 5911 1 ; _shelx_hkl_checksum 14542 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 Cl1A Cl 0.4232(6) 0.8398(4) 0.31537(16) 0.0551(15) Uani 1 1 d . . . . . O1A O 0.6354(10) 0.4667(10) 0.4933(3) 0.030(3) Uani 1 1 d . U . . . O2A O 0.5096(10) 0.3174(9) 0.4571(3) 0.024(3) Uani 1 1 d . U . . . O3A O 0.2988(11) 0.4325(10) 0.4794(3) 0.026(3) Uani 1 1 d D U . . . C1A C 0.5285(17) 0.4239(16) 0.4771(5) 0.027(2) Uani 1 1 d . U . . . C2A C 0.4102(15) 0.5107(16) 0.4797(5) 0.0284(19) Uani 1 1 d . U . . . H2A H 0.4226 0.5611 0.5083 0.040 Uiso 1 1 calc R U . . . C3A C 0.4055(10) 0.6012(9) 0.4399(3) 0.0287(18) Uani 1 1 d G U . . . C4A C 0.5012(9) 0.6929(10) 0.4390(3) 0.0308(19) Uani 1 1 d G U . . . H4A H 0.5638 0.7041 0.4645 0.046 Uiso 1 1 calc R U . . . C5A C 0.5052(9) 0.7684(9) 0.4010(3) 0.0315(19) Uani 1 1 d G U . . . H5A H 0.5706 0.8311 0.4004 0.047 Uiso 1 1 calc R U . . . C6A C 0.4136(11) 0.7522(10) 0.3637(3) 0.031(2) Uani 1 1 d G U . . . C7A C 0.3179(9) 0.6604(10) 0.3646(3) 0.0309(19) Uani 1 1 d G U . . . H7A H 0.2552 0.6493 0.3392 0.046 Uiso 1 1 calc R U . . . C8A C 0.3138(9) 0.5849(9) 0.4027(3) 0.0301(19) Uani 1 1 d G U . . . H8A H 0.2484 0.5222 0.4032 0.045 Uiso 1 1 calc R U . . . Cl1B Cl -0.1012(6) 0.9369(5) 0.30418(16) 0.0573(16) Uani 1 1 d . . . . . O1B O -0.0412(10) 0.7135(10) 0.5227(3) 0.029(3) Uani 1 1 d . U . . . O2B O 0.1170(10) 0.5790(10) 0.5106(3) 0.026(3) Uani 1 1 d D U . . . O3B O -0.0401(10) 0.4494(10) 0.4461(3) 0.026(3) Uani 1 1 d D U . . . H3OB H 0.0165 0.4206 0.4719 0.034 Uiso 1 1 d DR U . . . C1B C 0.0058(17) 0.6242(16) 0.5007(6) 0.029(2) Uani 1 1 d . U . . . C2B C -0.0817(16) 0.5700(16) 0.4612(5) 0.0310(19) Uani 1 1 d . U . . . H2B H -0.1706 0.5608 0.4699 0.043 Uiso 1 1 calc R U . . . C3B C -0.0851(11) 0.6638(9) 0.4212(3) 0.0313(18) Uani 1 1 d G U . . . C4B C -0.1382(11) 0.7846(10) 0.4247(3) 0.0332(19) Uani 1 1 d G U . . . H4B H -0.1706 0.8095 0.4517 0.050 Uiso 1 1 calc R U . . . C5B C -0.1440(11) 0.8689(8) 0.3885(3) 0.0341(19) Uani 1 1 d G U . . . H5B H -0.1803 0.9514 0.3909 0.051 Uiso 1 1 calc R U . . . C6B C -0.0967(11) 0.8324(9) 0.3489(3) 0.0336(19) Uani 1 1 d G U . . . C7B C -0.0435(10) 0.7116(10) 0.3455(3) 0.0330(19) Uani 1 1 d G U . . . H7B H -0.0112 0.6867 0.3184 0.049 Uiso 1 1 calc R U . . . C8B C -0.0378(10) 0.6273(8) 0.3816(3) 0.0324(19) Uani 1 1 d G U . . . H8B H -0.0014 0.5448 0.3792 0.049 Uiso 1 1 calc R U . . . Cl1C Cl 1.0189(4) 0.0198(4) 0.20142(14) 0.0379(12) Uani 1 1 d . . . . . O1C O 1.1333(10) 0.3941(10) 0.0271(3) 0.028(3) Uani 1 1 d . U . . . O2C O 1.0280(9) 0.5687(9) 0.0462(3) 0.020(2) Uani 1 1 d . U . . . O3C O 0.8060(10) 0.4448(11) 0.0417(3) 0.026(3) Uani 1 1 d D U . . . C1C C 1.0367(16) 0.4510(16) 0.0371(5) 0.025(2) Uani 1 1 d . U . . . C2C C 0.9188(15) 0.3681(16) 0.0397(5) 0.0262(18) Uani 1 1 d . U . . . H2C H 0.9053 0.3150 0.0117 0.037 Uiso 1 1 calc R U . . . C3C C 0.9413(10) 0.2774(8) 0.0803(3) 0.0264(17) Uani 1 1 d G U . . . C4C C 0.9177(10) 0.3204(7) 0.1225(3) 0.0266(17) Uani 1 1 d G U . . . H4C H 0.8855 0.4043 0.1259 0.040 Uiso 1 1 calc R U . . . C5C C 0.9413(10) 0.2408(9) 0.1598(2) 0.0274(18) Uani 1 1 d G U . . . H5C H 0.9252 0.2702 0.1887 0.041 Uiso 1 1 calc R U . . . C6C C 0.9884(11) 0.1181(9) 0.1548(3) 0.0272(18) Uani 1 1 d G U . . . C7C C 1.0120(10) 0.0751(7) 0.1126(3) 0.0274(18) Uani 1 1 d G U . . . H7C H 1.0443 -0.0088 0.1092 0.041 Uiso 1 1 calc R U . . . C8C C 0.9885(10) 0.1547(9) 0.0753(2) 0.0269(17) Uani 1 1 d G U . . . H8C H 1.0046 0.1253 0.0465 0.040 Uiso 1 1 calc R U . . . Cl1D Cl 0.4826(4) 0.0492(4) 0.23353(13) 0.0362(11) Uani 1 1 d . . . . . O1D O 0.6289(9) 0.2591(10) 0.0166(3) 0.023(3) Uani 1 1 d D U . . . O2D O 0.4495(10) 0.1430(10) 0.0025(3) 0.026(3) Uani 1 1 d . U . . . O3D O 0.5039(10) 0.4391(10) 0.0608(3) 0.025(3) Uani 1 1 d D U . . . H3OD H 0.5088 0.4481 0.0277 0.033 Uiso 1 1 d DR U . . . C1D C 0.5145(15) 0.2334(15) 0.0215(5) 0.022(2) Uani 1 1 d . U . . . C2D C 0.4451(16) 0.3157(14) 0.0539(5) 0.0237(17) Uani 1 1 d . U . . . H2D H 0.3525 0.3256 0.0417 0.033 Uiso 1 1 calc R U . . . C3D C 0.4558(9) 0.2507(9) 0.0995(2) 0.0241(16) Uani 1 1 d G U . . . C4D C 0.5758(8) 0.2289(10) 0.1236(3) 0.0254(17) Uani 1 1 d G U . . . H4D H 0.6516 0.2565 0.1118 0.038 Uiso 1 1 calc R U . . . C5D C 0.5850(7) 0.1669(10) 0.1650(3) 0.0255(17) Uani 1 1 d G U . . . H5D H 0.6671 0.1521 0.1814 0.038 Uiso 1 1 calc R U . . . C6D C 0.4742(9) 0.1266(9) 0.1823(2) 0.0259(18) Uani 1 1 d G U . . . C7D C 0.3542(8) 0.1484(10) 0.1582(3) 0.0251(17) Uani 1 1 d G U . . . H7D H 0.2785 0.1208 0.1700 0.038 Uiso 1 1 calc R U . . . C8D C 0.3450(7) 0.2104(10) 0.1168(3) 0.0248(17) Uani 1 1 d G U . . . H8D H 0.2630 0.2252 0.1003 0.037 Uiso 1 1 calc R U . . . N1A N 0.2869(13) 0.1627(12) 0.4478(4) 0.028(3) Uani 1 1 d . U . . . H1A1 H 0.2107 0.1982 0.4531 0.042 Uiso 1 1 calc R U . . . H1A2 H 0.3483 0.2245 0.4489 0.042 Uiso 1 1 calc R U . . . H1A3 H 0.3107 0.1026 0.4692 0.042 Uiso 1 1 calc R U . . . C9A C 0.2719(17) 0.1016(15) 0.4024(5) 0.029(3) Uani 1 1 d . U . . . H9A H 0.3572 0.0634 0.3981 0.041 Uiso 1 1 calc R U . . . C10A C 0.1795(16) -0.0063(15) 0.4029(5) 0.031(3) Uani 1 1 d . U . . . H10A H 0.2101 -0.0656 0.4272 0.044 Uiso 1 1 calc R U . . . H10B H 0.1725 -0.0511 0.3740 0.044 Uiso 1 1 calc R U . . . H10C H 0.0948 0.0270 0.4080 0.044 Uiso 1 1 calc R U . . . C11A C 0.2419(16) 0.2008(16) 0.3655(5) 0.0261(19) Uani 1 1 d . U . . . H11A H 0.3049 0.2720 0.3724 0.039 Uiso 1 1 calc R U . . . C12A C 0.1100(15) 0.2587(16) 0.3642(5) 0.0258(19) Uani 1 1 d . U . . . H12A H 0.1020 0.3002 0.3935 0.039 Uiso 1 1 calc R U . . . H12B H 0.0448 0.1899 0.3598 0.039 Uiso 1 1 calc R U . . . C13A C 0.0822(16) 0.3580(16) 0.3262(5) 0.027(2) Uani 1 1 d . U . . . H13A H -0.0077 0.3881 0.3254 0.040 Uiso 1 1 calc R U . . . H13B H 0.1397 0.4325 0.3328 0.040 Uiso 1 1 calc R U . . . C14A C 0.1022(15) 0.3032(15) 0.2807(5) 0.0266(19) Uani 1 1 d . U . . . H14A H 0.0915 0.3716 0.2577 0.040 Uiso 1 1 calc R U . . . H14B H 0.0367 0.2366 0.2721 0.040 Uiso 1 1 calc R U . . . C15A C 0.2371(16) 0.2450(16) 0.2821(5) 0.027(2) Uani 1 1 d . U . . . H15A H 0.2451 0.2031 0.2528 0.041 Uiso 1 1 calc R U . . . H15B H 0.3019 0.3142 0.2862 0.041 Uiso 1 1 calc R U . . . C16A C 0.2656(16) 0.1472(15) 0.3199(5) 0.027(2) Uani 1 1 d . U . . . H16A H 0.2104 0.0711 0.3131 0.040 Uiso 1 1 calc R U . . . H16B H 0.3564 0.1195 0.3213 0.040 Uiso 1 1 calc R U . . . N1B N 0.7556(12) 0.2658(11) 0.4328(4) 0.021(3) Uani 1 1 d . U . . . H1B1 H 0.8127 0.3318 0.4348 0.032 Uiso 1 1 calc R U . . . H1B2 H 0.7856 0.2030 0.4524 0.032 Uiso 1 1 calc R U . . . H1B3 H 0.6783 0.2940 0.4399 0.032 Uiso 1 1 calc R U . . . C9B C 0.7399(15) 0.2143(15) 0.3858(5) 0.022(3) Uani 1 1 d . U . . . H9B H 0.8201 0.1663 0.3813 0.031 Uiso 1 1 calc R U . . . C10B C 0.6291(15) 0.1184(15) 0.3832(5) 0.027(3) Uani 1 1 d . U . . . H10D H 0.6485 0.0525 0.4063 0.037 Uiso 1 1 calc R U . . . H10E H 0.6182 0.0784 0.3533 0.037 Uiso 1 1 calc R U . . . H10F H 0.5496 0.1627 0.3882 0.037 Uiso 1 1 calc R U . . . C11B C 0.7229(17) 0.3199(17) 0.3511(5) 0.034(2) Uani 1 1 d . U . . . H11B H 0.7964 0.3804 0.3585 0.051 Uiso 1 1 calc R U . . . C12B C 0.6007(17) 0.3983(16) 0.3501(6) 0.035(2) Uani 1 1 d . U . . . H12C H 0.5983 0.4395 0.3797 0.053 Uiso 1 1 calc R U . . . H12D H 0.5252 0.3410 0.3445 0.053 Uiso 1 1 calc R U . . . C13B C 0.5923(17) 0.5009(16) 0.3135(5) 0.036(2) Uani 1 1 d . U . . . H13C H 0.5099 0.5477 0.3131 0.054 Uiso 1 1 calc R U . . . H13D H 0.6633 0.5629 0.3205 0.054 Uiso 1 1 calc R U . . . C14B C 0.6006(17) 0.4433(17) 0.2673(6) 0.036(2) Uani 1 1 d . U . . . H14C H 0.5961 0.5120 0.2444 0.054 Uiso 1 1 calc R U . . . H14D H 0.5271 0.3847 0.2594 0.054 Uiso 1 1 calc R U . . . C15B C 0.7263(17) 0.3706(17) 0.2677(6) 0.035(2) Uani 1 1 d . U . . . H15C H 0.7996 0.4303 0.2737 0.053 Uiso 1 1 calc R U . . . H15D H 0.7305 0.3307 0.2379 0.053 Uiso 1 1 calc R U . . . C16B C 0.7353(18) 0.2669(17) 0.3042(5) 0.035(2) Uani 1 1 d . U . . . H16C H 0.6665 0.2031 0.2963 0.052 Uiso 1 1 calc R U . . . H16D H 0.8191 0.2225 0.3048 0.052 Uiso 1 1 calc R U . . . N1C N 0.7964(12) 0.7264(11) 0.0374(4) 0.019(3) Uani 1 1 d . U . . . H1C1 H 0.7212 0.6853 0.0281 0.028 Uiso 1 1 calc R U . . . H1C2 H 0.8574 0.6681 0.0478 0.028 Uiso 1 1 calc R U . . . H1C3 H 0.8229 0.7700 0.0139 0.028 Uiso 1 1 calc R U . . . C9C C 0.7759(15) 0.8181(14) 0.0744(5) 0.020(3) Uani 1 1 d . U . . . H9C H 0.8589 0.8646 0.0828 0.028 Uiso 1 1 calc R U . . . C10C C 0.6770(14) 0.9153(14) 0.0564(5) 0.021(3) Uani 1 1 d . U . . . H10G H 0.6994 0.9496 0.0279 0.029 Uiso 1 1 calc R U . . . H10H H 0.6750 0.9849 0.0783 0.029 Uiso 1 1 calc R U . . . H10I H 0.5921 0.8746 0.0515 0.029 Uiso 1 1 calc R U . . . C11C C 0.7455(16) 0.7426(16) 0.1166(5) 0.029(2) Uani 1 1 d . U . . . H11C H 0.6755 0.6797 0.1072 0.044 Uiso 1 1 calc R U . . . C12C C 0.6977(17) 0.8363(16) 0.1512(5) 0.030(2) Uani 1 1 d . U . . . H12E H 0.7621 0.9049 0.1583 0.045 Uiso 1 1 calc R U . . . H12F H 0.6160 0.8763 0.1381 0.045 Uiso 1 1 calc R U . . . C13C C 0.6766(17) 0.7657(16) 0.1945(5) 0.031(2) Uani 1 1 d . U . . . H13E H 0.6522 0.8282 0.2168 0.046 Uiso 1 1 calc R U . . . H13F H 0.6041 0.7052 0.1878 0.046 Uiso 1 1 calc R U . . . C14C C 0.7923(16) 0.6938(16) 0.2146(5) 0.030(2) Uani 1 1 d . U . . . H14E H 0.7708 0.6456 0.2412 0.045 Uiso 1 1 calc R U . . . H14F H 0.8617 0.7551 0.2250 0.045 Uiso 1 1 calc R U . . . C15C C 0.8413(17) 0.6003(16) 0.1807(5) 0.030(2) Uani 1 1 d . U . . . H15E H 0.9225 0.5604 0.1943 0.045 Uiso 1 1 calc R U . . . H15F H 0.7770 0.5318 0.1734 0.045 Uiso 1 1 calc R U . . . C16C C 0.8640(16) 0.6698(16) 0.1383(5) 0.029(2) Uani 1 1 d . U . . . H16E H 0.8904 0.6072 0.1163 0.044 Uiso 1 1 calc R U . . . H16F H 0.9358 0.7309 0.1454 0.044 Uiso 1 1 calc R U . . . N1D N 0.2957(12) 0.6368(12) 0.0570(4) 0.027(3) Uani 1 1 d . U . . . H1D1 H 0.2100 0.6196 0.0518 0.040 Uiso 1 1 calc R U . . . H1D2 H 0.3397 0.5631 0.0639 0.040 Uiso 1 1 calc R U . . . H1D3 H 0.3225 0.6718 0.0318 0.040 Uiso 1 1 calc R U . . . C9D C 0.3204(17) 0.7296(16) 0.0957(5) 0.029(3) Uani 1 1 d . U . . . H9D H 0.4154 0.7360 0.1047 0.040 Uiso 1 1 calc R U . . . C10D C 0.2704(16) 0.8584(15) 0.0782(5) 0.030(3) Uani 1 1 d . U . . . H10J H 0.3099 0.8805 0.0511 0.042 Uiso 1 1 calc R U . . . H10K H 0.2924 0.9235 0.1014 0.042 Uiso 1 1 calc R U . . . H10L H 0.1767 0.8543 0.0709 0.042 Uiso 1 1 calc R U . . . C11D C 0.2566(17) 0.6796(16) 0.1357(5) 0.030(2) Uani 1 1 d . U . . . H11D H 0.1627 0.6697 0.1253 0.045 Uiso 1 1 calc R U . . . C12D C 0.2689(17) 0.7698(16) 0.1756(5) 0.031(2) Uani 1 1 d . U . . . H12G H 0.3614 0.7874 0.1846 0.046 Uiso 1 1 calc R U . . . H12H H 0.2272 0.8518 0.1660 0.046 Uiso 1 1 calc R U . . . C13D C 0.2122(17) 0.7233(16) 0.2156(5) 0.031(2) Uani 1 1 d . U . . . H13G H 0.1174 0.7192 0.2086 0.047 Uiso 1 1 calc R U . . . H13H H 0.2327 0.7841 0.2408 0.047 Uiso 1 1 calc R U . . . C14D C 0.2627(17) 0.5935(15) 0.2297(5) 0.032(2) Uani 1 1 d . U . . . H14G H 0.2162 0.5618 0.2544 0.048 Uiso 1 1 calc R U . . . H14H H 0.3549 0.6009 0.2415 0.048 Uiso 1 1 calc R U . . . C15D C 0.2484(17) 0.4971(16) 0.1916(5) 0.032(2) Uani 1 1 d . U . . . H15G H 0.1559 0.4793 0.1827 0.048 Uiso 1 1 calc R U . . . H15H H 0.2908 0.4161 0.2020 0.048 Uiso 1 1 calc R U . . . C16D C 0.3087(16) 0.5471(16) 0.1506(5) 0.031(2) Uani 1 1 d . U . . . H16G H 0.2902 0.4863 0.1253 0.047 Uiso 1 1 calc R U . . . H16H H 0.4032 0.5520 0.1582 0.047 Uiso 1 1 calc R U . . . H3OC H 0.723(7) 0.406(15) 0.038(10) 0.24(18) Uiso 1 1 d D . . . . H3OA H 0.24(2) 0.499(18) 0.477(4) 0.3(2) Uiso 1 1 d D . . . . 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 Cl1A 0.087(4) 0.028(3) 0.045(3) 0.007(2) -0.013(3) -0.007(3) O1A 0.028(5) 0.030(5) 0.032(5) -0.005(4) 0.004(4) 0.005(4) O2A 0.023(5) 0.022(5) 0.027(5) -0.004(4) 0.003(4) -0.002(4) O3A 0.023(5) 0.024(5) 0.033(5) 0.000(4) 0.008(4) -0.008(4) C1A 0.027(3) 0.027(2) 0.026(3) -0.0002(14) 0.0037(14) -0.0007(15) C2A 0.028(2) 0.028(2) 0.029(2) -0.0008(13) 0.0035(14) 0.0004(13) C3A 0.029(2) 0.028(2) 0.029(2) -0.0007(13) 0.0033(12) 0.0009(12) C4A 0.031(2) 0.030(2) 0.031(2) 0.0005(13) 0.0031(13) -0.0010(13) C5A 0.032(2) 0.031(2) 0.032(2) 0.0007(13) 0.0035(13) -0.0008(14) C6A 0.031(2) 0.030(2) 0.031(2) 0.0000(14) 0.0039(13) 0.0005(14) C7A 0.031(2) 0.031(2) 0.030(2) 0.0004(13) 0.0032(13) 0.0003(13) C8A 0.030(2) 0.030(2) 0.030(2) -0.0001(13) 0.0027(12) 0.0001(14) Cl1B 0.089(4) 0.030(3) 0.049(3) 0.011(2) -0.009(3) -0.006(3) O1B 0.027(5) 0.026(5) 0.035(5) -0.008(4) 0.006(4) 0.002(4) O2B 0.023(5) 0.026(5) 0.029(4) -0.007(4) 0.000(4) -0.006(4) O3B 0.031(5) 0.019(4) 0.027(5) 0.001(4) 0.001(4) 0.002(4) C1B 0.029(3) 0.029(3) 0.030(2) -0.0002(14) 0.0043(14) -0.0001(15) C2B 0.031(2) 0.031(2) 0.031(2) -0.0010(13) 0.0034(13) -0.0003(15) C3B 0.031(2) 0.032(2) 0.0311(19) -0.0005(12) 0.0030(13) -0.0005(14) C4B 0.033(2) 0.032(2) 0.034(2) -0.0002(12) 0.0038(15) 0.0007(14) C5B 0.035(2) 0.033(2) 0.035(2) 0.0004(12) 0.0043(14) 0.0006(14) C6B 0.033(2) 0.033(2) 0.034(2) 0.0004(13) 0.0036(14) 0.0002(14) C7B 0.033(2) 0.033(2) 0.033(2) 0.0005(12) 0.0044(15) -0.0003(14) C8B 0.033(2) 0.033(2) 0.032(2) -0.0001(12) 0.0040(14) -0.0002(14) Cl1C 0.049(3) 0.024(2) 0.040(3) 0.006(2) -0.002(2) -0.002(2) O1C 0.023(5) 0.025(5) 0.035(5) -0.008(4) 0.004(4) -0.005(4) O2C 0.018(4) 0.015(5) 0.026(4) -0.003(4) 0.001(4) -0.003(4) O3C 0.018(5) 0.028(5) 0.031(5) 0.003(4) -0.002(4) 0.003(4) C1C 0.025(3) 0.025(3) 0.025(3) -0.0001(14) 0.0027(15) 0.0006(14) C2C 0.026(2) 0.026(2) 0.027(2) -0.0005(14) 0.0033(15) 0.0000(13) C3C 0.026(2) 0.0263(19) 0.0268(18) -0.0002(11) 0.0034(14) -0.0002(13) C4C 0.026(2) 0.026(2) 0.0268(18) -0.0002(11) 0.0034(15) -0.0001(15) C5C 0.028(2) 0.027(2) 0.0271(19) 0.0001(12) 0.0033(15) 0.0001(14) C6C 0.027(2) 0.027(2) 0.0275(19) 0.0004(13) 0.0030(15) -0.0001(14) C7C 0.027(2) 0.027(2) 0.028(2) 0.0001(11) 0.0033(14) 0.0000(15) C8C 0.027(2) 0.027(2) 0.0271(19) -0.0004(11) 0.0032(15) 0.0004(14) Cl1D 0.051(3) 0.028(2) 0.030(2) 0.006(2) 0.004(2) 0.000(2) O1D 0.014(4) 0.026(5) 0.030(5) -0.003(4) 0.002(4) -0.005(4) O2D 0.026(5) 0.024(5) 0.029(5) -0.003(4) 0.004(4) -0.003(4) O3D 0.024(5) 0.025(5) 0.027(5) -0.006(4) 0.001(4) 0.002(4) C1D 0.022(3) 0.021(3) 0.022(2) 0.0003(14) 0.0020(15) 0.0002(15) C2D 0.023(2) 0.024(2) 0.0241(19) -0.0009(12) 0.0033(12) 0.0004(14) C3D 0.0241(19) 0.024(2) 0.0239(18) -0.0009(13) 0.0034(11) 0.0005(14) C4D 0.0249(18) 0.026(2) 0.026(2) 0.0001(14) 0.0026(12) 0.0003(14) C5D 0.0254(19) 0.025(2) 0.026(2) -0.0002(14) 0.0023(13) -0.0001(14) C6D 0.026(2) 0.026(2) 0.026(2) -0.0001(14) 0.0028(12) -0.0002(14) C7D 0.0254(19) 0.025(2) 0.025(2) -0.0001(14) 0.0033(13) -0.0002(14) C8D 0.0249(19) 0.025(2) 0.025(2) -0.0002(14) 0.0034(13) -0.0004(14) N1A 0.029(7) 0.027(7) 0.027(7) 0.006(6) 0.002(6) -0.005(6) C9A 0.029(4) 0.029(4) 0.029(4) -0.0003(15) 0.0035(15) 0.0000(15) C10A 0.032(4) 0.030(4) 0.032(4) 0.000(3) 0.003(3) -0.002(3) C11A 0.026(2) 0.026(2) 0.027(2) -0.0001(13) 0.0031(14) -0.0003(14) C12A 0.026(2) 0.026(2) 0.026(2) -0.0005(13) 0.0028(14) -0.0002(14) C13A 0.027(2) 0.026(2) 0.027(2) 0.0001(12) 0.0030(14) 0.0001(14) C14A 0.027(2) 0.027(2) 0.026(2) 0.0003(13) 0.0030(14) -0.0004(14) C15A 0.027(2) 0.028(2) 0.027(2) 0.0000(13) 0.0038(14) 0.0000(14) C16A 0.027(2) 0.027(2) 0.027(2) -0.0004(12) 0.0034(14) 0.0004(14) N1B 0.021(7) 0.016(7) 0.027(7) 0.003(6) 0.002(6) 0.010(6) C9B 0.022(3) 0.022(3) 0.022(3) 0.0000(15) 0.0027(15) 0.0005(15) C10B 0.026(4) 0.026(4) 0.028(4) -0.001(3) 0.003(3) -0.003(3) C11B 0.034(2) 0.034(2) 0.035(2) -0.0001(13) 0.0043(15) -0.0007(14) C12B 0.035(2) 0.035(2) 0.036(2) 0.0001(13) 0.0042(15) 0.0009(14) C13B 0.036(3) 0.036(2) 0.036(2) 0.0005(11) 0.0042(14) 0.0008(14) C14B 0.036(2) 0.036(2) 0.036(2) 0.0003(13) 0.0038(15) 0.0004(14) C15B 0.036(2) 0.036(2) 0.035(2) 0.0002(13) 0.0041(15) -0.0001(14) C16B 0.035(3) 0.035(2) 0.035(2) -0.0002(12) 0.0043(14) -0.0005(14) N1C 0.020(7) 0.010(6) 0.025(7) 0.010(5) 0.002(6) -0.001(6) C9C 0.020(3) 0.019(3) 0.020(3) 0.0000(15) 0.0024(15) -0.0002(15) C10C 0.021(4) 0.020(4) 0.021(4) 0.000(3) 0.001(3) 0.001(3) C11C 0.029(2) 0.029(2) 0.030(2) -0.0002(13) 0.0031(13) -0.0002(14) C12C 0.030(2) 0.030(2) 0.030(2) -0.0005(12) 0.0035(14) 0.0006(14) C13C 0.031(2) 0.031(2) 0.031(2) -0.0001(14) 0.0037(14) 0.0007(13) C14C 0.030(2) 0.030(2) 0.030(2) 0.0001(13) 0.0039(13) -0.0001(14) C15C 0.030(2) 0.030(2) 0.030(2) 0.0002(12) 0.0033(14) 0.0001(14) C16C 0.029(2) 0.029(2) 0.029(2) -0.0002(13) 0.0031(14) -0.0002(13) N1D 0.019(7) 0.023(7) 0.039(7) 0.001(6) 0.005(6) 0.001(6) C9D 0.029(4) 0.029(3) 0.029(4) -0.0003(15) 0.0035(15) -0.0002(15) C10D 0.031(4) 0.029(4) 0.030(4) 0.001(3) 0.004(3) 0.000(3) C11D 0.030(3) 0.030(2) 0.031(2) -0.0003(11) 0.0035(15) -0.0002(14) C12D 0.031(3) 0.031(2) 0.031(2) -0.0004(11) 0.0036(14) -0.0002(15) C13D 0.031(3) 0.032(2) 0.031(2) -0.0002(13) 0.0038(14) 0.0000(14) C14D 0.032(3) 0.032(2) 0.032(2) 0.0003(11) 0.0039(15) 0.0000(14) C15D 0.033(3) 0.031(2) 0.032(2) 0.0003(11) 0.0038(14) -0.0001(15) C16D 0.031(3) 0.031(2) 0.031(2) -0.0001(13) 0.0033(14) 0.0002(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2A O3A H3OA 98(10) . . ? O1A C1A O2A 125.5(15) . . ? O1A C1A C2A 117.1(14) . . ? O2A C1A C2A 117.3(15) . . ? O3A C2A C3A 113.9(12) . . ? O3A C2A C1A 108.8(13) . . ? C3A C2A C1A 106.2(12) . . ? O3A C2A H2A 109.3 . . ? C3A C2A H2A 109.3 . . ? C1A C2A H2A 109.3 . . ? C4A C3A C8A 120.0 . . ? C4A C3A C2A 119.3(9) . . ? C8A C3A C2A 120.4(9) . . ? C3A C4A C5A 120.0 . . ? C3A C4A H4A 120.0 . . ? C5A C4A H4A 120.0 . . ? C6A C5A C4A 120.0 . . ? C6A C5A H5A 120.0 . . ? C4A C5A H5A 120.0 . . ? C7A C6A C5A 120.0 . . ? C7A C6A Cl1A 119.8(6) . . ? C5A C6A Cl1A 120.1(6) . . ? C6A C7A C8A 120.0 . . ? C6A C7A H7A 120.0 . . ? C8A C7A H7A 120.0 . . ? C7A C8A C3A 120.0 . . ? C7A C8A H8A 120.0 . . ? C3A C8A H8A 120.0 . . ? C2B O3B H3OB 101.8 . . ? O2B C1B O1B 123.9(15) . . ? O2B C1B C2B 119.9(15) . . ? O1B C1B C2B 116.2(15) . . ? O3B C2B C1B 113.5(14) . . ? O3B C2B C3B 107.3(11) . . ? C1B C2B C3B 108.7(13) . . ? O3B C2B H2B 109.1 . . ? C1B C2B H2B 109.1 . . ? C3B C2B H2B 109.1 . . ? C4B C3B C8B 120.0 . . ? C4B C3B C2B 119.5(9) . . ? C8B C3B C2B 120.5(9) . . ? C5B C4B C3B 120.0 . . ? C5B C4B H4B 120.0 . . ? C3B C4B H4B 120.0 . . ? C6B C5B C4B 120.0 . . ? C6B C5B H5B 120.0 . . ? C4B C5B H5B 120.0 . . ? C5B C6B C7B 120.0 . . ? C5B C6B Cl1B 120.5(6) . . ? C7B C6B Cl1B 119.5(6) . . ? C8B C7B C6B 120.0 . . ? C8B C7B H7B 120.0 . . ? C6B C7B H7B 120.0 . . ? C7B C8B C3B 120.0 . . ? C7B C8B H8B 120.0 . . ? C3B C8B H8B 120.0 . . ? C2C O3C H3OC 120(8) . . ? O1C C1C O2C 126.9(16) . . ? O1C C1C C2C 115.4(14) . . ? O2C C1C C2C 117.7(15) . . ? O3C C2C C1C 111.2(13) . . ? O3C C2C C3C 111.2(12) . . ? C1C C2C C3C 110.2(12) . . ? O3C C2C H2C 108.1 . . ? C1C C2C H2C 108.1 . . ? C3C C2C H2C 108.1 . . ? C4C C3C C8C 120.0 . . ? C4C C3C C2C 119.3(8) . . ? C8C C3C C2C 120.6(8) . . ? C5C C4C C3C 120.0 . . ? C5C C4C H4C 120.0 . . ? C3C C4C H4C 120.0 . . ? C6C C5C C4C 120.0 . . ? C6C C5C H5C 120.0 . . ? C4C C5C H5C 120.0 . . ? C5C C6C C7C 120.0 . . ? C5C C6C Cl1C 119.8(6) . . ? C7C C6C Cl1C 120.2(6) . . ? C8C C7C C6C 120.0 . . ? C8C C7C H7C 120.0 . . ? C6C C7C H7C 120.0 . . ? C7C C8C C3C 120.0 . . ? C7C C8C H8C 120.0 . . ? C3C C8C H8C 120.0 . . ? C2D O3D H3OD 90.8 . . ? O1D C1D O2D 125.5(15) . . ? O1D C1D C2D 118.7(14) . . ? O2D C1D C2D 115.7(14) . . ? O3D C2D C3D 106.9(11) . . ? O3D C2D C1D 111.6(13) . . ? C3D C2D C1D 108.9(12) . . ? O3D C2D H2D 109.8 . . ? C3D C2D H2D 109.8 . . ? C1D C2D H2D 109.8 . . ? C4D C3D C8D 120.0 . . ? C4D C3D C2D 120.3(9) . . ? C8D C3D C2D 119.7(9) . . ? C5D C4D C3D 120.0 . . ? C5D C4D H4D 120.0 . . ? C3D C4D H4D 120.0 . . ? C6D C5D C4D 120.0 . . ? C6D C5D H5D 120.0 . . ? C4D C5D H5D 120.0 . . ? C5D C6D C7D 120.0 . . ? C5D C6D Cl1D 121.1(6) . . ? C7D C6D Cl1D 118.9(6) . . ? C6D C7D C8D 120.0 . . ? C6D C7D H7D 120.0 . . ? C8D C7D H7D 120.0 . . ? C7D C8D C3D 120.0 . . ? C7D C8D H8D 120.0 . . ? C3D C8D H8D 120.0 . . ? C9A N1A H1A1 109.5 . . ? C9A N1A H1A2 109.5 . . ? H1A1 N1A H1A2 109.5 . . ? C9A N1A H1A3 109.5 . . ? H1A1 N1A H1A3 109.5 . . ? H1A2 N1A H1A3 109.5 . . ? C10A C9A N1A 108.2(13) . . ? C10A C9A C11A 116.6(14) . . ? N1A C9A C11A 110.9(13) . . ? C10A C9A H9A 106.9 . . ? N1A C9A H9A 106.9 . . ? C11A C9A H9A 106.9 . . ? C9A C10A H10A 109.5 . . ? C9A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C9A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C12A C11A C9A 113.9(14) . . ? C12A C11A C16A 111.8(13) . . ? C9A C11A C16A 110.8(13) . . ? C12A C11A H11A 106.6 . . ? C9A C11A H11A 106.6 . . ? C16A C11A H11A 106.6 . . ? C11A C12A C13A 112.6(13) . . ? C11A C12A H12A 109.1 . . ? C13A C12A H12A 109.1 . . ? C11A C12A H12B 109.1 . . ? C13A C12A H12B 109.1 . . ? H12A C12A H12B 107.8 . . ? C14A C13A C12A 111.8(13) . . ? C14A C13A H13A 109.2 . . ? C12A C13A H13A 109.2 . . ? C14A C13A H13B 109.2 . . ? C12A C13A H13B 109.2 . . ? H13A C13A H13B 107.9 . . ? C13A C14A C15A 110.6(13) . . ? C13A C14A H14A 109.5 . . ? C15A C14A H14A 109.5 . . ? C13A C14A H14B 109.5 . . ? C15A C14A H14B 109.5 . . ? H14A C14A H14B 108.1 . . ? C16A C15A C14A 112.6(13) . . ? C16A C15A H15A 109.1 . . ? C14A C15A H15A 109.1 . . ? C16A C15A H15B 109.1 . . ? C14A C15A H15B 109.1 . . ? H15A C15A H15B 107.8 . . ? C11A C16A C15A 112.2(13) . . ? C11A C16A H16A 109.2 . . ? C15A C16A H16A 109.2 . . ? C11A C16A H16B 109.2 . . ? C15A C16A H16B 109.2 . . ? H16A C16A H16B 107.9 . . ? C9B N1B H1B1 109.5 . . ? C9B N1B H1B2 109.5 . . ? H1B1 N1B H1B2 109.5 . . ? C9B N1B H1B3 109.5 . . ? H1B1 N1B H1B3 109.5 . . ? H1B2 N1B H1B3 109.5 . . ? N1B C9B C11B 111.8(13) . . ? N1B C9B C10B 106.5(12) . . ? C11B C9B C10B 114.7(13) . . ? N1B C9B H9B 107.9 . . ? C11B C9B H9B 107.9 . . ? C10B C9B H9B 107.9 . . ? C9B C10B H10D 109.5 . . ? C9B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C9B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C9B C11B C12B 116.0(14) . . ? C9B C11B C16B 110.4(14) . . ? C12B C11B C16B 110.0(14) . . ? C9B C11B H11B 106.6 . . ? C12B C11B H11B 106.6 . . ? C16B C11B H11B 106.6 . . ? C11B C12B C13B 111.8(14) . . ? C11B C12B H12C 109.3 . . ? C13B C12B H12C 109.3 . . ? C11B C12B H12D 109.3 . . ? C13B C12B H12D 109.3 . . ? H12C C12B H12D 107.9 . . ? C14B C13B C12B 111.5(14) . . ? C14B C13B H13C 109.3 . . ? C12B C13B H13C 109.3 . . ? C14B C13B H13D 109.3 . . ? C12B C13B H13D 109.3 . . ? H13C C13B H13D 108.0 . . ? C13B C14B C15B 109.6(14) . . ? C13B C14B H14C 109.7 . . ? C15B C14B H14C 109.7 . . ? C13B C14B H14D 109.7 . . ? C15B C14B H14D 109.7 . . ? H14C C14B H14D 108.2 . . ? C14B C15B C16B 109.9(15) . . ? C14B C15B H15C 109.7 . . ? C16B C15B H15C 109.7 . . ? C14B C15B H15D 109.7 . . ? C16B C15B H15D 109.7 . . ? H15C C15B H15D 108.2 . . ? C11B C16B C15B 113.0(14) . . ? C11B C16B H16C 109.0 . . ? C15B C16B H16C 109.0 . . ? C11B C16B H16D 109.0 . . ? C15B C16B H16D 109.0 . . ? H16C C16B H16D 107.8 . . ? C9C N1C H1C1 109.5 . . ? C9C N1C H1C2 109.5 . . ? H1C1 N1C H1C2 109.5 . . ? C9C N1C H1C3 109.5 . . ? H1C1 N1C H1C3 109.5 . . ? H1C2 N1C H1C3 109.5 . . ? N1C C9C C10C 108.8(12) . . ? N1C C9C C11C 109.5(12) . . ? C10C C9C C11C 115.8(13) . . ? N1C C9C H9C 107.5 . . ? C10C C9C H9C 107.5 . . ? C11C C9C H9C 107.5 . . ? C9C C10C H10G 109.5 . . ? C9C C10C H10H 109.5 . . ? H10G C10C H10H 109.5 . . ? C9C C10C H10I 109.5 . . ? H10G C10C H10I 109.5 . . ? H10H C10C H10I 109.5 . . ? C16C C11C C12C 110.0(13) . . ? C16C C11C C9C 111.3(13) . . ? C12C C11C C9C 109.5(13) . . ? C16C C11C H11C 108.7 . . ? C12C C11C H11C 108.7 . . ? C9C C11C H11C 108.7 . . ? C13C C12C C11C 110.4(14) . . ? C13C C12C H12E 109.6 . . ? C11C C12C H12E 109.6 . . ? C13C C12C H12F 109.6 . . ? C11C C12C H12F 109.6 . . ? H12E C12C H12F 108.1 . . ? C14C C13C C12C 113.2(14) . . ? C14C C13C H13E 108.9 . . ? C12C C13C H13E 108.9 . . ? C14C C13C H13F 108.9 . . ? C12C C13C H13F 108.9 . . ? H13E C13C H13F 107.8 . . ? C13C C14C C15C 111.9(13) . . ? C13C C14C H14E 109.2 . . ? C15C C14C H14E 109.2 . . ? C13C C14C H14F 109.2 . . ? C15C C14C H14F 109.2 . . ? H14E C14C H14F 107.9 . . ? C16C C15C C14C 110.2(14) . . ? C16C C15C H15E 109.6 . . ? C14C C15C H15E 109.6 . . ? C16C C15C H15F 109.6 . . ? C14C C15C H15F 109.6 . . ? H15E C15C H15F 108.1 . . ? C15C C16C C11C 113.3(14) . . ? C15C C16C H16E 108.9 . . ? C11C C16C H16E 108.9 . . ? C15C C16C H16F 108.9 . . ? C11C C16C H16F 108.9 . . ? H16E C16C H16F 107.7 . . ? C9D N1D H1D1 109.5 . . ? C9D N1D H1D2 109.5 . . ? H1D1 N1D H1D2 109.5 . . ? C9D N1D H1D3 109.5 . . ? H1D1 N1D H1D3 109.5 . . ? H1D2 N1D H1D3 109.5 . . ? N1D C9D C10D 106.7(12) . . ? N1D C9D C11D 109.2(13) . . ? C10D C9D C11D 114.1(14) . . ? N1D C9D H9D 108.9 . . ? C10D C9D H9D 108.9 . . ? C11D C9D H9D 108.9 . . ? C9D C10D H10J 109.5 . . ? C9D C10D H10K 109.5 . . ? H10J C10D H10K 109.5 . . ? C9D C10D H10L 109.5 . . ? H10J C10D H10L 109.5 . . ? H10K C10D H10L 109.5 . . ? C12D C11D C9D 113.5(14) . . ? C12D C11D C16D 109.9(13) . . ? C9D C11D C16D 111.3(14) . . ? C12D C11D H11D 107.3 . . ? C9D C11D H11D 107.3 . . ? C16D C11D H11D 107.3 . . ? C13D C12D C11D 115.3(14) . . ? C13D C12D H12G 108.5 . . ? C11D C12D H12G 108.5 . . ? C13D C12D H12H 108.5 . . ? C11D C12D H12H 108.5 . . ? H12G C12D H12H 107.5 . . ? C12D C13D C14D 111.3(15) . . ? C12D C13D H13G 109.4 . . ? C14D C13D H13G 109.4 . . ? C12D C13D H13H 109.4 . . ? C14D C13D H13H 109.4 . . ? H13G C13D H13H 108.0 . . ? C13D C14D C15D 113.1(14) . . ? C13D C14D H14G 109.0 . . ? C15D C14D H14G 109.0 . . ? C13D C14D H14H 109.0 . . ? C15D C14D H14H 109.0 . . ? H14G C14D H14H 107.8 . . ? C14D C15D C16D 111.1(14) . . ? C14D C15D H15G 109.4 . . ? C16D C15D H15G 109.4 . . ? C14D C15D H15H 109.4 . . ? C16D C15D H15H 109.4 . . ? H15G C15D H15H 108.0 . . ? C15D C16D C11D 111.9(14) . . ? C15D C16D H16G 109.2 . . ? C11D C16D H16G 109.2 . . ? C15D C16D H16H 109.2 . . ? C11D C16D H16H 109.2 . . ? H16G C16D H16H 107.9 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1A C6A 1.726(8) . ? O1A C1A 1.248(19) . ? O2A C1A 1.270(18) . ? O3A C2A 1.424(18) . ? O3A H3OA 0.950(8) . ? C1A C2A 1.54(2) . ? C2A C3A 1.517(17) . ? C2A H2A 1.0000 . ? C3A C4A 1.3900 . ? C3A C8A 1.3900 . ? C4A C5A 1.3900 . ? C4A H4A 0.9500 . ? C5A C6A 1.3900 . ? C5A H5A 0.9500 . ? C6A C7A 1.3900 . ? C7A C8A 1.3900 . ? C7A H7A 0.9500 . ? C8A H8A 0.9500 . ? Cl1B C6B 1.725(8) . ? O1B C1B 1.274(19) . ? O2B C1B 1.26(2) . ? O3B C2B 1.425(19) . ? O3B H3OB 0.9645 . ? C1B C2B 1.52(2) . ? C2B C3B 1.544(17) . ? C2B H2B 1.0000 . ? C3B C4B 1.3900 . ? C3B C8B 1.3900 . ? C4B C5B 1.3900 . ? C4B H4B 0.9500 . ? C5B C6B 1.3900 . ? C5B H5B 0.9500 . ? C6B C7B 1.3900 . ? C7B C8B 1.3900 . ? C7B H7B 0.9500 . ? C8B H8B 0.9500 . ? Cl1C C6C 1.730(8) . ? O1C C1C 1.239(19) . ? O2C C1C 1.267(18) . ? O3C C2C 1.435(19) . ? O3C H3OC 0.950(8) . ? C1C C2C 1.52(2) . ? C2C C3C 1.536(17) . ? C2C H2C 1.0000 . ? C3C C4C 1.3900 . ? C3C C8C 1.3900 . ? C4C C5C 1.3900 . ? C4C H4C 0.9500 . ? C5C C6C 1.3900 . ? C5C H5C 0.9500 . ? C6C C7C 1.3900 . ? C7C C8C 1.3900 . ? C7C H7C 0.9500 . ? C8C H8C 0.9500 . ? Cl1D C6D 1.727(7) . ? O1D C1D 1.252(18) . ? O2D C1D 1.261(17) . ? O3D C2D 1.435(18) . ? O3D H3OD 0.9997 . ? C1D C2D 1.54(2) . ? C2D C3D 1.516(16) . ? C2D H2D 1.0000 . ? C3D C4D 1.3900 . ? C3D C8D 1.3900 . ? C4D C5D 1.3900 . ? C4D H4D 0.9500 . ? C5D C6D 1.3900 . ? C5D H5D 0.9500 . ? C6D C7D 1.3900 . ? C7D C8D 1.3900 . ? C7D H7D 0.9500 . ? C8D H8D 0.9500 . ? N1A C9A 1.493(19) . ? N1A H1A1 0.9100 . ? N1A H1A2 0.9100 . ? N1A H1A3 0.9100 . ? C9A C10A 1.49(2) . ? C9A C11A 1.52(2) . ? C9A H9A 1.0000 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C11A C12A 1.50(2) . ? C11A C16A 1.52(2) . ? C11A H11A 1.0000 . ? C12A C13A 1.54(2) . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C13A C14A 1.51(2) . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C14A C15A 1.53(2) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A C16A 1.53(2) . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C16A H16A 0.9900 . ? C16A H16B 0.9900 . ? N1B C9B 1.495(18) . ? N1B H1B1 0.9100 . ? N1B H1B2 0.9100 . ? N1B H1B3 0.9100 . ? C9B C11B 1.51(2) . ? C9B C10B 1.53(2) . ? C9B H9B 1.0000 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11B C12B 1.52(2) . ? C11B C16B 1.53(2) . ? C11B H11B 1.0000 . ? C12B C13B 1.53(2) . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? C13B C14B 1.52(2) . ? C13B H13C 0.9900 . ? C13B H13D 0.9900 . ? C14B C15B 1.52(2) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B C16B 1.53(2) . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16B H16C 0.9900 . ? C16B H16D 0.9900 . ? N1C C9C 1.499(18) . ? N1C H1C1 0.9100 . ? N1C H1C2 0.9100 . ? N1C H1C3 0.9100 . ? C9C C10C 1.50(2) . ? C9C C11C 1.55(2) . ? C9C H9C 1.0000 . ? C10C H10G 0.9800 . ? C10C H10H 0.9800 . ? C10C H10I 0.9800 . ? C11C C16C 1.53(2) . ? C11C C12C 1.55(2) . ? C11C H11C 1.0000 . ? C12C C13C 1.53(2) . ? C12C H12E 0.9900 . ? C12C H12F 0.9900 . ? C13C C14C 1.49(2) . ? C13C H13E 0.9900 . ? C13C H13F 0.9900 . ? C14C C15C 1.54(2) . ? C14C H14E 0.9900 . ? C14C H14F 0.9900 . ? C15C C16C 1.50(2) . ? C15C H15E 0.9900 . ? C15C H15F 0.9900 . ? C16C H16E 0.9900 . ? C16C H16F 0.9900 . ? N1D C9D 1.509(19) . ? N1D H1D1 0.9100 . ? N1D H1D2 0.9100 . ? N1D H1D3 0.9100 . ? C9D C10D 1.52(2) . ? C9D C11D 1.53(2) . ? C9D H9D 1.0000 . ? C10D H10J 0.9800 . ? C10D H10K 0.9800 . ? C10D H10L 0.9800 . ? C11D C12D 1.52(2) . ? C11D C16D 1.54(2) . ? C11D H11D 1.0000 . ? C12D C13D 1.48(2) . ? C12D H12G 0.9900 . ? C12D H12H 0.9900 . ? C13D C14D 1.50(2) . ? C13D H13G 0.9900 . ? C13D H13H 0.9900 . ? C14D C15D 1.52(2) . ? C14D H14G 0.9900 . ? C14D H14H 0.9900 . ? C15D C16D 1.54(2) . ? C15D H15G 0.9900 . ? C15D H15H 0.9900 . ? C16D H16G 0.9900 . ? C16D H16H 0.9900 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1A C1A C2A O3A -153.9(14) . . . . ? O2A C1A C2A O3A 28.8(19) . . . . ? O1A C1A C2A C3A 83.2(16) . . . . ? O2A C1A C2A C3A -94.2(16) . . . . ? O3A C2A C3A C4A 172.3(9) . . . . ? C1A C2A C3A C4A -67.9(13) . . . . ? O3A C2A C3A C8A -13.8(16) . . . . ? C1A C2A C3A C8A 105.9(12) . . . . ? C8A C3A C4A C5A 0.0 . . . . ? C2A C3A C4A C5A 173.9(11) . . . . ? C3A C4A C5A C6A 0.0 . . . . ? C4A C5A C6A C7A 0.0 . . . . ? C4A C5A C6A Cl1A -176.6(9) . . . . ? C5A C6A C7A C8A 0.0 . . . . ? Cl1A C6A C7A C8A 176.6(9) . . . . ? C6A C7A C8A C3A 0.0 . . . . ? C4A C3A C8A C7A 0.0 . . . . ? C2A C3A C8A C7A -173.8(12) . . . . ? O2B C1B C2B O3B 15(2) . . . . ? O1B C1B C2B O3B -163.1(13) . . . . ? O2B C1B C2B C3B -103.9(16) . . . . ? O1B C1B C2B C3B 77.5(17) . . . . ? O3B C2B C3B C4B 171.8(9) . . . . ? C1B C2B C3B C4B -65.1(15) . . . . ? O3B C2B C3B C8B -7.0(15) . . . . ? C1B C2B C3B C8B 116.2(12) . . . . ? C8B C3B C4B C5B 0.0 . . . . ? C2B C3B C4B C5B -178.8(12) . . . . ? C3B C4B C5B C6B 0.0 . . . . ? C4B C5B C6B C7B 0.0 . . . . ? C4B C5B C6B Cl1B -179.1(9) . . . . ? C5B C6B C7B C8B 0.0 . . . . ? Cl1B C6B C7B C8B 179.1(9) . . . . ? C6B C7B C8B C3B 0.0 . . . . ? C4B C3B C8B C7B 0.0 . . . . ? C2B C3B C8B C7B 178.8(12) . . . . ? O1C C1C C2C O3C -167.5(13) . . . . ? O2C C1C C2C O3C 14.1(19) . . . . ? O1C C1C C2C C3C 68.8(17) . . . . ? O2C C1C C2C C3C -109.6(15) . . . . ? O3C C2C C3C C4C -38.9(15) . . . . ? C1C C2C C3C C4C 84.8(13) . . . . ? O3C C2C C3C C8C 143.0(10) . . . . ? C1C C2C C3C C8C -93.2(13) . . . . ? C8C C3C C4C C5C 0.0 . . . . ? C2C C3C C4C C5C -178.1(11) . . . . ? C3C C4C C5C C6C 0.0 . . . . ? C4C C5C C6C C7C 0.0 . . . . ? C4C C5C C6C Cl1C 179.5(8) . . . . ? C5C C6C C7C C8C 0.0 . . . . ? Cl1C C6C C7C C8C -179.5(8) . . . . ? C6C C7C C8C C3C 0.0 . . . . ? C4C C3C C8C C7C 0.0 . . . . ? C2C C3C C8C C7C 178.0(11) . . . . ? O1D C1D C2D O3D 22.5(19) . . . . ? O2D C1D C2D O3D -158.5(12) . . . . ? O1D C1D C2D C3D -95.3(16) . . . . ? O2D C1D C2D C3D 83.7(15) . . . . ? O3D C2D C3D C4D -59.5(13) . . . . ? C1D C2D C3D C4D 61.2(14) . . . . ? O3D C2D C3D C8D 121.8(10) . . . . ? C1D C2D C3D C8D -117.5(11) . . . . ? C8D C3D C4D C5D 0.0 . . . . ? C2D C3D C4D C5D -178.7(10) . . . . ? C3D C4D C5D C6D 0.0 . . . . ? C4D C5D C6D C7D 0.0 . . . . ? C4D C5D C6D Cl1D 179.9(8) . . . . ? C5D C6D C7D C8D 0.0 . . . . ? Cl1D C6D C7D C8D -179.9(8) . . . . ? C6D C7D C8D C3D 0.0 . . . . ? C4D C3D C8D C7D 0.0 . . . . ? C2D C3D C8D C7D 178.7(10) . . . . ? C10A C9A C11A C12A 54.8(19) . . . . ? N1A C9A C11A C12A -69.7(18) . . . . ? C10A C9A C11A C16A -72.3(19) . . . . ? N1A C9A C11A C16A 163.2(13) . . . . ? C9A C11A C12A C13A -179.5(13) . . . . ? C16A C11A C12A C13A -53.0(18) . . . . ? C11A C12A C13A C14A 54.6(19) . . . . ? C12A C13A C14A C15A -54.0(18) . . . . ? C13A C14A C15A C16A 53.8(18) . . . . ? C12A C11A C16A C15A 52.2(19) . . . . ? C9A C11A C16A C15A -179.6(14) . . . . ? C14A C15A C16A C11A -53.0(19) . . . . ? N1B C9B C11B C12B -65.8(18) . . . . ? C10B C9B C11B C12B 55.6(19) . . . . ? N1B C9B C11B C16B 168.2(13) . . . . ? C10B C9B C11B C16B -70.4(18) . . . . ? C9B C11B C12B C13B -179.2(14) . . . . ? C16B C11B C12B C13B -53.1(19) . . . . ? C11B C12B C13B C14B 56.9(19) . . . . ? C12B C13B C14B C15B -58.6(19) . . . . ? C13B C14B C15B C16B 57.6(19) . . . . ? C9B C11B C16B C15B -176.9(14) . . . . ? C12B C11B C16B C15B 54(2) . . . . ? C14B C15B C16B C11B -57(2) . . . . ? N1C C9C C11C C16C 69.5(16) . . . . ? C10C C9C C11C C16C -167.0(13) . . . . ? N1C C9C C11C C12C -168.7(13) . . . . ? C10C C9C C11C C12C -45.3(19) . . . . ? C16C C11C C12C C13C -53.3(18) . . . . ? C9C C11C C12C C13C -175.8(13) . . . . ? C11C C12C C13C C14C 54.7(19) . . . . ? C12C C13C C14C C15C -55.1(19) . . . . ? C13C C14C C15C C16C 54.1(19) . . . . ? C14C C15C C16C C11C -55.3(19) . . . . ? C12C C11C C16C C15C 55.6(19) . . . . ? C9C C11C C16C C15C 177.1(14) . . . . ? N1D C9D C11D C12D -176.6(14) . . . . ? C10D C9D C11D C12D -57.3(19) . . . . ? N1D C9D C11D C16D 58.9(17) . . . . ? C10D C9D C11D C16D 178.1(13) . . . . ? C9D C11D C12D C13D -178.1(15) . . . . ? C16D C11D C12D C13D -53(2) . . . . ? C11D C12D C13D C14D 53(2) . . . . ? C12D C13D C14D C15D -53(2) . . . . ? C13D C14D C15D C16D 54(2) . . . . ? C14D C15D C16D C11D -53.3(18) . . . . ? C12D C11D C16D C15D 51.8(18) . . . . ? C9D C11D C16D C15D 178.4(14) . . . . ?