#------------------------------------------------------------------------------ #$Date: 2020-08-06 16:30:52 +0300 (Thu, 06 Aug 2020) $ #$Revision: 254934 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557904.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_1557904 loop_ _publ_author_name 'Okude, Ryo' 'Mori, Genki' 'Yagi, Akiko' 'Itami, Kenichiro' _publ_section_title ; Programmable synthesis of multiply arylated cubanes through C--H metalation and arylation ; _journal_issue 29 _journal_name_full 'Chemical Science' _journal_page_first 7672 _journal_paper_doi 10.1039/D0SC01909G _journal_volume 11 _journal_year 2020 _chemical_formula_sum 'C31 H42 N2 O4' _chemical_formula_weight 506.66 _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 geom _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2020-03-30 deposited with the CCDC. 2020-04-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.9476(17) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.9747(2) _cell_length_b 12.3749(2) _cell_length_c 17.7595(3) _cell_measurement_reflns_used 19565 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 30.5650 _cell_measurement_theta_min 2.7050 _cell_volume 2789.71(8) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_molecular_graphics 'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)' _computing_publication_material 'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution SIR97 _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_unetI/netI 0.0141 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 29403 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 24.996 _diffrn_reflns_theta_max 24.996 _diffrn_reflns_theta_min 2.344 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.83277 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.206 _exptl_crystal_description block _exptl_crystal_F_000 1096 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.239 _refine_diff_density_min -0.220 _refine_diff_density_rms 0.036 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 343 _refine_ls_number_reflns 4911 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0343 _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^)+(0.0405P)^2^+1.1239P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.0887 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4475 _reflns_number_total 4911 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01909g2.cif _cod_data_source_block 2f _cod_depositor_comments 'Adding full bibliography for 1557900--1557907.cif.' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1557904 _shelx_shelxl_version_number 2016/6 _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 0.984 _shelx_estimated_absorpt_t_max 0.992 _shelx_res_file ; TITL okude2 okude.res created by SHELXL-2016/6 at 18:42:39 on 09-Oct-2018 REM Yadorkari-X generated CELL 0.71073 12.9747 12.3749 17.7595 90.0000 101.9476 90.0000 ZERR 4.0 0.0002 0.0002 0.0003 0.0000 0.0017 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z REM SPGR P21/n monoclinic SFAC C H N O UNIT 124 168 8 16 SIZE 0.20 0.20 0.10 TEMP -150.0 L.S. 10 FMAP 2 PLAN -25 ACTA CONF WPDB -1 BOND $H MERG 2 OMIT -10.000000 50.000000 WGHT 0.040500 1.123900 FVAR 1.76530 O1 4 0.867611 0.715705 0.491594 11.00000 0.03702 0.02351 = 0.06341 0.00569 -0.00627 -0.00687 C1 1 0.794127 0.657092 0.467344 11.00000 0.02757 0.02129 = 0.02279 0.00024 0.00712 0.00005 O2 4 0.702989 0.690930 0.424622 11.00000 0.03282 0.01540 = 0.03513 0.00196 -0.00014 0.00101 C2 1 0.688436 0.806654 0.412186 11.00000 0.03983 0.01403 = 0.03409 0.00261 0.00650 0.00135 AFIX 23 H1 2 0.708045 0.827861 0.363261 11.00000 -1.20000 H2 2 0.733437 0.847178 0.454708 11.00000 -1.20000 AFIX 0 C3 1 0.576156 0.831012 0.409222 11.00000 0.03998 0.02179 = 0.09070 0.00777 0.00552 0.00362 AFIX 137 H3 2 0.532331 0.789177 0.367751 11.00000 -1.50000 H4 2 0.563503 0.908325 0.399500 11.00000 -1.50000 H5 2 0.558181 0.811684 0.458452 11.00000 -1.50000 AFIX 0 C4 1 0.793254 0.538365 0.481877 11.00000 0.02568 0.01918 = 0.01821 -0.00023 0.00855 0.00128 C5 1 0.705438 0.474462 0.452399 11.00000 0.02274 0.02149 = 0.02193 0.00117 0.00256 0.00363 AFIX 43 H34 2 0.645178 0.505897 0.420338 11.00000 -1.20000 AFIX 0 C6 1 0.706053 0.365608 0.469783 11.00000 0.02061 0.02072 = 0.02252 -0.00158 0.00328 -0.00118 AFIX 43 H35 2 0.645807 0.322803 0.449828 11.00000 -1.20000 AFIX 0 C7 1 0.794321 0.317676 0.516414 11.00000 0.02164 0.01842 = 0.01552 -0.00061 0.00773 0.00176 C8 1 0.882298 0.381439 0.544313 11.00000 0.01977 0.02232 = 0.01735 0.00007 0.00453 0.00242 AFIX 43 H36 2 0.943376 0.349709 0.575156 11.00000 -1.20000 AFIX 0 C9 1 0.881564 0.491041 0.527449 11.00000 0.02128 0.02243 = 0.01953 -0.00310 0.00605 -0.00301 AFIX 43 H37 2 0.941851 0.533887 0.547216 11.00000 -1.20000 AFIX 0 C10 1 0.791151 0.201843 0.536540 11.00000 0.01811 0.01810 = 0.01583 -0.00067 0.00370 0.00055 C11 1 0.748803 0.106461 0.478168 11.00000 0.01844 0.01643 = 0.01795 -0.00001 0.00509 0.00032 C12 1 0.681321 0.062575 0.534903 11.00000 0.01981 0.02066 = 0.01739 0.00044 0.00483 -0.00177 AFIX 13 H38 2 0.606409 0.038177 0.519752 11.00000 -1.20000 AFIX 0 C13 1 0.721490 0.156283 0.592338 11.00000 0.01948 0.02054 = 0.01711 0.00014 0.00530 0.00124 AFIX 13 H39 2 0.676124 0.200994 0.619367 11.00000 -1.20000 AFIX 0 C14 1 0.816930 0.084626 0.633341 11.00000 0.01940 0.01749 = 0.01811 0.00077 0.00564 0.00017 C15 1 0.775636 -0.009809 0.575277 11.00000 0.02237 0.01829 = 0.01709 0.00086 0.00526 -0.00107 AFIX 13 H40 2 0.770269 -0.087438 0.589628 11.00000 -1.20000 AFIX 0 C16 1 0.844386 0.034500 0.519437 11.00000 0.02116 0.01748 = 0.01709 0.00144 0.00546 0.00187 AFIX 13 H41 2 0.889679 -0.010552 0.492568 11.00000 -1.20000 AFIX 0 C17 1 0.884750 0.128705 0.576963 11.00000 0.01876 0.01835 = 0.01699 0.00152 0.00451 0.00007 AFIX 13 H42 2 0.959788 0.152612 0.592379 11.00000 -1.20000 AFIX 0 C18 1 0.702477 0.117199 0.393439 11.00000 0.02124 0.01314 = 0.01862 -0.00017 0.00445 0.00160 O3 4 0.608017 0.097366 0.370444 11.00000 0.02062 0.03117 = 0.02181 0.00275 0.00243 -0.00504 N1 3 0.766070 0.148212 0.345964 11.00000 0.01841 0.01853 = 0.01582 0.00062 0.00327 0.00097 C19 1 0.723939 0.153332 0.261680 11.00000 0.02437 0.02361 = 0.01483 0.00154 0.00413 -0.00131 AFIX 13 H6 2 0.783960 0.175198 0.237621 11.00000 -1.20000 AFIX 0 C20 1 0.687789 0.042976 0.228932 11.00000 0.05043 0.03118 = 0.02080 -0.00638 0.00772 -0.00748 AFIX 137 H7 2 0.746561 -0.008195 0.240834 11.00000 -1.50000 H8 2 0.663800 0.048496 0.172995 11.00000 -1.50000 H9 2 0.629699 0.017474 0.251853 11.00000 -1.50000 AFIX 0 C21 1 0.639733 0.239801 0.240266 11.00000 0.02750 0.03387 = 0.02553 0.00888 0.00140 0.00384 AFIX 137 H10 2 0.576837 0.218738 0.259191 11.00000 -1.50000 H11 2 0.621592 0.247689 0.184168 11.00000 -1.50000 H12 2 0.666490 0.308715 0.263636 11.00000 -1.50000 AFIX 0 C22 1 0.878794 0.174105 0.373251 11.00000 0.01745 0.02639 = 0.01845 0.00314 0.00393 0.00136 AFIX 13 H13 2 0.894035 0.170146 0.430731 11.00000 -1.20000 AFIX 0 C23 1 0.948672 0.091075 0.345063 11.00000 0.02714 0.04139 = 0.03107 0.00708 0.01018 0.01314 AFIX 137 H14 2 0.930646 0.018594 0.360454 11.00000 -1.50000 H15 2 1.022679 0.106466 0.367743 11.00000 -1.50000 H16 2 0.937687 0.094702 0.288839 11.00000 -1.50000 AFIX 0 C24 1 0.904526 0.288527 0.351477 11.00000 0.02590 0.03165 = 0.02400 0.00313 0.00526 -0.00702 AFIX 137 H17 2 0.896323 0.293564 0.295479 11.00000 -1.50000 H18 2 0.977319 0.306046 0.376234 11.00000 -1.50000 H19 2 0.856495 0.339601 0.368706 11.00000 -1.50000 AFIX 0 C25 1 0.861298 0.074306 0.718256 11.00000 0.02108 0.01533 = 0.01871 -0.00022 0.00456 0.00055 O4 4 0.953672 0.099095 0.743355 11.00000 0.02268 0.03132 = 0.02174 0.00171 0.00307 -0.00710 N2 3 0.797416 0.036163 0.763695 11.00000 0.01947 0.02559 = 0.01561 0.00221 0.00350 -0.00137 C26 1 0.840134 0.020379 0.847056 11.00000 0.02583 0.02982 = 0.01575 0.00387 0.00349 -0.00351 AFIX 13 H20 2 0.780763 -0.007263 0.869681 11.00000 -1.20000 AFIX 0 C27 1 0.876323 0.125996 0.888304 11.00000 0.05094 0.03792 = 0.01869 -0.00280 0.00702 -0.00962 AFIX 137 H21 2 0.934475 0.156381 0.867617 11.00000 -1.50000 H22 2 0.900209 0.112181 0.943500 11.00000 -1.50000 H23 2 0.817555 0.177337 0.880317 11.00000 -1.50000 AFIX 0 C28 1 0.924822 -0.066769 0.860360 11.00000 0.02884 0.03777 = 0.02664 0.01099 0.00162 0.00039 AFIX 137 H24 2 0.896256 -0.133503 0.834455 11.00000 -1.50000 H25 2 0.947508 -0.080238 0.915696 11.00000 -1.50000 H26 2 0.985205 -0.042654 0.839493 11.00000 -1.50000 AFIX 0 C29 1 0.686613 0.005674 0.733817 11.00000 0.01851 0.03671 = 0.01923 0.00414 0.00380 -0.00290 AFIX 13 H27 2 0.671539 0.019107 0.677068 11.00000 -1.20000 AFIX 0 C30 1 0.666692 -0.113767 0.745246 11.00000 0.03300 0.04102 = 0.03112 0.00145 0.00568 -0.01427 AFIX 137 H28 2 0.716903 -0.157005 0.723697 11.00000 -1.50000 H29 2 0.594709 -0.132117 0.719048 11.00000 -1.50000 H30 2 0.675631 -0.129118 0.800354 11.00000 -1.50000 AFIX 0 C31 1 0.612587 0.077887 0.767707 11.00000 0.02841 0.05610 = 0.03102 0.01063 0.01194 0.01117 AFIX 137 H31 2 0.625743 0.067767 0.823613 11.00000 -1.50000 H32 2 0.539414 0.058710 0.745189 11.00000 -1.50000 H33 2 0.625002 0.153620 0.756114 11.00000 -1.50000 AFIX 0 HKLF 4 REM okude2 REM R1 = 0.0343 for 4475 Fo > 4sig(Fo) and 0.0374 for all 4911 data REM 343 parameters refined using 0 restraints END WGHT 0.0405 1.1238 REM Highest difference peak 0.239, deepest hole -0.220, 1-sigma level 0.036 Q1 1 0.7999 0.0291 0.6145 11.00000 0.05 0.24 Q2 1 0.7665 0.1635 0.4981 11.00000 0.05 0.24 Q3 1 0.7709 0.1242 0.6259 11.00000 0.05 0.23 Q4 1 0.8621 0.1096 0.6165 11.00000 0.05 0.22 Q5 1 0.8805 0.0766 0.5473 11.00000 0.05 0.22 Q6 1 0.7981 0.0681 0.4865 11.00000 0.05 0.22 Q7 1 0.7024 0.0840 0.4967 11.00000 0.05 0.22 Q8 1 0.8325 0.0758 0.6747 11.00000 0.05 0.20 Q9 1 0.5226 0.7818 0.4120 11.00000 0.05 0.20 Q10 1 0.8181 -0.0021 0.5504 11.00000 0.05 0.19 Q11 1 0.8217 0.1617 0.3597 11.00000 0.05 0.19 Q12 1 0.7549 0.1901 0.5669 11.00000 0.05 0.19 Q13 1 0.6898 0.1125 0.5636 11.00000 0.05 0.18 Q14 1 0.8479 0.1766 0.5551 11.00000 0.05 0.18 Q15 1 0.8259 0.7186 0.5217 11.00000 0.05 0.18 Q16 1 0.7155 0.0092 0.5545 11.00000 0.05 0.17 Q17 1 0.7418 0.0205 0.7493 11.00000 0.05 0.17 Q18 1 0.8190 0.0274 0.8041 11.00000 0.05 0.16 Q19 1 0.7296 0.1133 0.4384 11.00000 0.05 0.16 Q20 1 0.8427 0.5161 0.4908 11.00000 0.05 0.16 Q21 1 0.9155 0.1361 0.3607 11.00000 0.05 0.16 Q22 1 0.7982 0.5871 0.4711 11.00000 0.05 0.15 Q23 1 0.8221 0.5194 0.5125 11.00000 0.05 0.15 Q24 1 0.7463 0.8545 0.4079 11.00000 0.05 0.14 Q25 1 0.7947 0.2563 0.5254 11.00000 0.05 0.14 ; _shelx_res_checksum 1084 _shelx_hkl_file ; 0 0 -2 12402.5 305.043 0 0 3 5.54286 2.72715 0 0 -3 7.20049 2.67523 0 0 3-0.59708 2.38827 0 0 3 2.92081 2.22929 0 0 -3 3.10140 2.16031 0 0 4 31377.8 737.191 0 0 4 30263.4 736.784 0 0 -4 31303.1 736.884 0 0 4 30539.4 737.257 0 0 -4 30087.4 737.453 0 0 -5 4.83687 3.96049 0 0 -5 4.91796 3.62071 0 0 5 1.45907 3.40267 0 0 5 3.84815 3.85709 0 0 5 2.49242 3.44756 0 0 -5 3.94188 3.10768 0 0 6 21461.3 535.139 0 0 6 22207.5 535.706 0 0 -6 21986.8 535.630 0 0 -6 20952.3 536.201 0 0 6 21191.0 535.823 0 0 -6 22315.4 535.309 0 0 -7-0.34609 3.69814 0 0 7 1.25549 3.65684 0 0 7 0.38350 4.29417 0 0 -7 4.86376 5.00019 0 0 -7 2.19543 4.48574 0 0 7 4.18307 4.21774 0 0 -8 70905.7 1735.21 0 0 -8 71314.9 1734.07 0 0 8 70867.1 1734.92 0 0 -8 69100.2 1733.60 0 0 8 69832.0 1733.52 0 0 8 72188.1 1734.25 0 0 -9 6.67494 6.01250 0 0 9 8.10095 5.21978 0 0 -9 4.02022 4.42420 0 0 9-0.49529 5.46851 0 0 -9 5.14932 5.48119 0 0 9 0.55108 4.68150 0 0 -10 26502.3 651.208 0 0 10 24787.1 650.959 0 0 10 26704.7 652.874 0 0 10 26731.8 651.872 0 0 -10 26775.5 651.581 0 0 -10 26626.3 653.244 0 0 -11 1.16665 6.34649 0 0 -11-2.80962 5.87852 0 0 -11 3.29374 5.11600 0 0 11-7.81309 6.84138 0 0 11 2.22950 5.88201 0 0 11-4.81367 5.45984 0 0 12 1083.90 37.2527 0 0 12 1094.73 36.2671 0 0 -12 1072.83 37.2370 0 0 -12 1164.00 35.9836 0 0 12 1158.23 36.0734 0 0 -12 1162.68 36.4685 0 0 -13-4.77317 7.26279 0 0 -13 6.63042 5.71305 0 0 13-4.15164 6.73732 0 0 13-3.91966 7.41617 0 0 14 661.777 27.4882 0 0 -14 683.563 25.5146 0 0 -14 624.098 26.0954 0 0 -15 6.72361 8.54538 0 0 15 4.86782 7.64358 0 0 -15-1.56458 6.95990 0 0 -16 2515.35 71.7607 0 0 16 2434.71 74.1743 0 0 -16 2352.78 73.7894 0 0 17 23.6701 10.5065 0 0 -17 8.06102 8.34985 0 0 -17-5.67690 9.78531 0 0 -18 5425.72 150.015 0 0 18 5466.70 149.902 0 0 -18 5375.03 146.142 0 0 -19 8.16504 10.0715 0 0 19-5.17563 11.6638 0 0 -19 15.5158 12.0020 0 0 -20 1106.29 41.1404 0 0 20 1042.40 43.4602 0 0 -20 1044.43 43.2038 0 0 -21 3.48923 11.8836 0 0 -21 14.5843 13.3723 0 0 21 10.3515 13.2157 0 0 22 152.575 19.4012 0 0 -22 135.263 19.5053 0 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377.161 24.4936 15 -2 4 409.898 26.9896 15 -2 4 411.068 24.2723 15 -2 5 616.469 32.9698 15 2 5 649.060 32.4509 15 -2 5 577.864 29.5470 -15 -2 -6 23.8668 13.7663 15 -2 6 34.3280 15.2415 15 2 6 18.6975 13.6853 15 -2 6 25.9672 12.3905 -15 -2 -7-4.45936 13.3406 15 -2 7-4.88737 14.4933 15 2 7-1.48735 13.9724 15 -2 7 6.45081 13.7003 -15 -2 -8 136.631 20.0804 15 -2 8 105.109 19.3911 15 2 8 97.2600 19.1015 15 -2 8 114.808 18.2611 15 -2 9 379.352 26.7525 15 3 -17 20.5641 17.0641 15 3 -16 582.096 32.5173 15 3 -15 1.42065 14.1691 15 -3 -15 14.4940 16.2865 15 3 -14 135.983 17.4224 15 -3 -14 90.8306 17.2690 15 3 -13 5.09198 13.0944 -15 -3 13 7.50479 12.7807 15 -3 -13 22.2334 14.2006 -15 -3 12 89.5126 14.7422 15 -3 -12 38.6357 14.4575 -15 -3 11 553.614 27.8378 15 -3 -11 486.153 28.5644 -15 -3 10 309.944 21.4689 15 -3 -10 299.969 21.8220 -15 -3 9 14.3588 11.8073 15 -3 -9-2.50377 12.4417 -15 -3 8-2.37645 11.2067 15 -3 -8 7.21976 12.1682 -15 -3 7 282.439 20.1190 -15 -3 6 22.5980 12.1559 15 -3 -6 7.92474 11.1765 -15 -3 5 158.710 16.0121 15 -3 -5 168.585 16.2108 -15 -3 4 5.93450 11.3272 15 -3 -4 9.58576 11.1705 15 -3 -3 8.27015 10.9778 15 3 -3-3.82342 10.1189 15 -3 -2 211.934 17.0365 15 -3 -2 198.756 15.9062 15 3 -2 205.458 19.0841 15 -3 -1 1111.85 42.3029 15 3 -1 1096.48 43.7128 15 -3 0 31.6461 12.1205 15 3 0 31.7829 12.3658 15 -3 1 719.716 33.3716 15 3 1 649.963 33.0762 15 -3 2 221.805 20.7201 15 3 2 239.922 20.5579 -15 -3 -3 134.992 16.2368 15 -3 3 152.265 18.3209 15 3 3 144.037 17.9012 -15 -3 -4 102.029 15.9865 15 -3 4 79.0989 16.9544 15 3 4 93.6190 16.1730 -15 -3 -5 114.166 16.7828 15 -3 5 134.698 18.7755 15 3 5 118.850 17.0700 -15 -3 -6 154.678 18.8228 15 -3 6 137.788 19.3635 15 3 6 168.807 20.4515 15 -3 6 167.345 17.9226 -15 -3 -7 205.588 21.5765 15 -3 7 262.162 23.8817 15 3 7 241.196 22.5907 15 -3 7 271.638 21.3614 15 -3 8 8.78436 15.9065 15 -3 8 13.2716 14.2266 15 -3 9 895.980 40.0667 15 4 -17 141.637 19.9134 -15 -4 15 19.5701 14.6614 15 -4 -15 4.95025 15.1934 -15 -4 14 86.3469 15.7677 15 -4 -14 75.1314 16.8787 15 -4 -13 10.7957 14.6050 -15 -4 12 33.2118 13.8684 15 -4 -12 37.1339 15.4002 -15 -4 11 701.450 33.2029 15 -4 -11 652.845 33.3371 -15 -4 10 940.616 38.7747 15 -4 -10 853.031 38.6712 -15 -4 9 61.9466 14.4262 15 -4 -9 42.1372 13.9112 -15 -4 8 6.40800 11.8026 15 -4 -8 19.2728 12.6359 -15 -4 7 533.469 28.4144 15 -4 -7 552.698 28.7704 -15 -4 6 118.807 15.4974 15 -4 -6 130.163 15.6049 15 -4 -5 219.376 18.7943 -15 -4 4 46.2657 13.6938 15 -4 -4 46.0516 11.8935 -15 -4 3 136.743 16.3622 15 -4 -3 94.7963 14.6240 15 -4 -3 89.5238 14.0755 15 -4 -2 131.133 15.0132 15 4 -2 63.5069 14.7576 15 -4 -1-4.92236 11.8772 15 -4 -1 1.08728 10.6506 15 4 -1 1.40084 12.6810 15 -4 0 727.062 31.3512 15 -4 0 729.782 34.3771 15 4 0 744.045 35.8492 15 -4 1 126.311 17.6379 15 4 1 100.345 15.8793 15 -4 2 28.3598 14.3463 15 4 2 10.1517 13.9519 15 -4 3 44.6402 14.1255 15 4 3 38.3002 14.6221 15 -4 4 21.8261 14.7706 15 4 4 21.0210 13.6602 -15 -4 -5 264.616 21.7724 15 4 5 230.766 21.9005 -15 -4 -6 361.227 25.4573 15 -4 6 456.062 30.2466 15 4 6 433.358 28.3624 -15 -4 -7 99.7199 18.2124 15 -4 7 111.054 19.8857 15 4 7 89.8458 17.7754 -15 -4 -8 17.2712 15.7191 -15 -5 16 173.348 20.4975 -15 -5 15-2.99060 14.4323 -15 -5 14 13.2030 15.3850 15 -5 -14 4.96980 14.8692 -15 -5 13 21.7263 13.6250 15 -5 -13 36.7286 15.8288 -15 -5 12 132.925 16.9825 15 -5 -12 97.7364 16.9009 -15 -5 11 167.109 18.1813 15 -5 -11 141.884 18.3181 -15 -5 10 13.8818 13.5988 15 -5 -10-2.86858 13.6868 -15 -5 9 66.2778 15.1850 15 -5 -9 56.2343 13.8522 -15 -5 8 216.038 20.1208 15 -5 -8 185.906 19.5324 15 -5 -7 585.314 30.3574 15 -5 -6 63.6305 15.1781 -15 -5 5 832.423 37.7877 15 -5 -5 830.097 36.2505 -15 -5 4 1452.13 53.8954 15 -5 -4 1461.96 52.4478 -15 -5 3 638.936 32.2600 15 -5 -3 605.672 30.0799 15 -5 -3 669.984 31.4285 15 -5 -2 173.408 17.2758 15 -5 -2 164.013 17.5841 15 -5 -1 100.654 15.1631 15 -5 -1 78.3407 14.8705 15 5 -1 93.4524 16.8511 15 -5 0 235.369 18.4233 15 -5 0 260.161 21.3881 15 5 0 235.319 22.5136 15 -5 1 106.440 14.6003 15 -5 1 97.3498 16.9039 15 5 1 89.9376 17.0958 15 -5 2 48.1070 14.9228 15 5 2 37.0381 15.2077 15 -5 3 417.124 28.4261 15 5 3 403.254 27.2677 15 -5 4 40.6968 15.8449 15 5 4 18.9961 14.4084 -15 -5 -6 194.253 20.1793 15 -5 6 236.998 24.0216 -15 -5 -7 170.579 20.6777 15 -5 7 135.821 20.7803 -15 -5 -8 203.647 21.8378 -15 -6 15 9.55307 14.8399 -15 -6 14 308.193 24.4290 15 -6 -13 85.7753 17.2593 -15 -6 12 51.8370 14.8510 15 -6 -12 75.2206 17.1179 -15 -6 11 74.9073 16.1454 15 -6 -11 63.8343 15.5099 -15 -6 10-16.3186 13.6008 15 -6 -10 9.17366 13.2980 -15 -6 9 82.4354 16.0378 15 -6 -9 75.9761 16.4180 -15 -6 8 41.1592 14.8364 15 -6 -8 26.2525 13.2281 -15 -6 7 832.067 37.9467 15 -6 -7 733.809 36.2733 15 -6 -6 54.2223 14.3121 -15 -6 5 14.5874 13.6595 15 -6 -5 29.7855 15.1263 -15 -6 4 129.565 17.4921 15 -6 -4 153.075 17.3555 15 -6 -3 10.5267 12.8951 15 -6 -3 21.3182 13.1992 15 -6 -2 28.4297 13.5729 15 -6 -2 35.0350 13.7872 15 -6 -1 82.4367 15.8905 15 6 -1 78.9037 17.2530 15 -6 0 166.347 16.8903 15 -6 0 167.187 19.4525 15 6 0 201.271 21.1988 15 -6 1 9.81386 11.9287 15 -6 1-12.0156 14.8729 15 6 1 3.22931 12.6764 15 -6 2 143.031 19.3450 15 6 2 165.320 20.2089 15 -6 3 221.799 22.8458 15 6 3 158.820 20.3446 15 -6 4-6.87432 16.0197 15 6 4-20.0894 16.6403 15 -6 5 7.16479 15.8655 15 -6 6-1.84526 16.1230 -15 -7 12 288.022 23.8807 15 -7 -12 265.859 24.0265 -15 -7 11 15.9025 15.1209 -15 -7 10 42.5419 16.2771 15 -7 -10 24.2217 14.8871 -15 -7 9 367.577 26.4850 15 -7 -9 360.980 26.9678 -15 -7 8 196.620 20.6262 15 -7 -8 163.384 20.0974 -15 -7 7 137.998 19.6161 15 -7 -7 132.877 18.4372 -15 -7 6 86.4672 16.9719 15 -7 -6 80.8269 15.9772 -15 -7 5 617.838 33.0442 15 -7 -5 588.732 31.8143 -15 -7 4 4.61635 13.8105 15 -7 -4 2.84942 14.2586 -15 -7 3 6.15605 13.8123 15 -7 -3-12.3571 15.6733 -15 -7 2 1.53311 13.8194 15 -7 -2 5.45734 12.6638 15 -7 -2 7.35135 13.8125 15 -7 -1 422.145 25.9023 15 -7 -1 465.968 28.6730 15 -7 0 403.605 24.8200 15 -7 0 387.424 26.9819 15 7 0 395.409 28.8448 15 -7 1 167.022 21.0423 15 7 1 128.635 20.1586 15 -7 2 90.6882 18.8797 -15 7 -2 72.1972 16.2909 15 7 2 89.9904 19.0488 15 -7 3 263.819 24.3835 15 -7 4 1219.31 52.1143 -15 -8 10 981.763 45.9897 15 -8 -10 1012.10 46.0701 -15 -8 9 47.9830 16.8867 -15 -8 8 1116.27 47.7168 15 -8 -8 1019.22 46.0438 -15 -8 7 85.2852 17.5257 15 -8 -7 74.5819 17.4255 15 -8 -6 212.875 21.1700 -15 -8 5 99.2008 18.0057 15 -8 -5 94.4999 16.9920 -15 -8 4 121.825 19.6862 15 -8 -4 117.756 17.5734 15 -8 -4 122.637 16.9467 -15 -8 3 43.8287 15.4735 15 -8 -3 51.2135 15.5816 -15 -8 2-13.0097 15.0939 15 -8 -2 5.72459 13.3910 15 -8 -2 13.5502 17.4188 -15 -8 1 28.8335 15.2357 15 -8 -1 18.1032 14.4725 15 -8 -1 17.7196 15.4983 15 -8 0 832.484 40.2927 15 8 0 801.117 41.3593 -15 8 -1 1105.81 45.5827 15 -8 1 1068.51 47.4353 -15 8 -2 63.2191 16.3516 15 -8 2 64.5062 17.4567 15 -8 3 177.333 22.6229 -15 8 -3 157.539 19.2402 15 -9 -6 26.0902 15.9276 15 -9 -5 9.62939 13.8956 15 -9 -4 97.0350 17.5295 15 -9 -4 121.073 18.0552 15 -9 -3 21.3126 14.6978 15 -9 -3 7.87974 14.8096 15 -9 -2 28.0806 14.2849 15 -9 -2 36.1605 16.3520 15 -9 -1 143.080 18.8113 15 -9 -1 179.144 23.8474 -15 9 -1 252.285 23.8357 15 -9 1 266.206 25.1765 15 -10 -4-1.65614 15.8638 15 -10 -3 160.053 21.3698 15 -10 -2 34.1984 16.7707 16 0 -16 38.8631 16.8987 16 0 -15 1.54510 15.6779 16 0 -14 7.33470 14.2126 16 0 -13 11.1454 13.9941 16 0 -12 1679.33 59.6970 16 0 -11-15.2762 13.6488 16 0 -3-1.06616 9.73354 16 0 -2 102.567 13.6533 16 0 -1-1.11416 10.5905 16 0 0 214.721 18.2910 16 0 1-3.52013 12.1072 16 0 2 219.161 19.1086 16 0 3 3.93489 12.4193 16 0 3 2.53336 13.5760 16 0 4 56.8046 14.0618 16 0 4 43.2020 13.3830 16 0 5-8.75177 13.9191 16 0 5-2.71487 13.8212 16 0 6-1.52987 14.4288 16 0 6-1.39879 13.8018 16 1 -16 8.01952 15.4803 16 -1 -16-11.3961 18.0755 16 -1 -15 13.9681 14.6477 16 1 -15 32.2189 16.6019 16 -1 -14 83.8932 17.3738 16 1 -14 61.2191 17.1711 16 -1 -13 58.9950 16.1915 16 1 -13 125.677 17.3414 16 -1 -12 674.996 34.3224 16 -1 -11 517.169 29.2734 16 -1 -9 429.958 25.3339 16 -1 -8 79.9644 14.0572 16 1 -5 6.82102 10.5959 16 1 -4 8.05795 11.0282 16 1 -3-1.16570 10.0915 16 1 -1 165.757 17.0077 16 1 0 230.783 19.4975 16 1 1 313.112 22.3191 16 -1 1 290.536 20.6124 16 -1 2 1.31304 11.4727 16 -1 2 1.15720 11.7020 16 -1 3 431.493 26.7177 16 1 3 393.817 25.4133 16 -1 4 33.1792 14.5530 16 1 4 32.8544 14.8202 16 -1 4 17.4859 13.1559 16 -1 5 25.6218 15.5100 16 1 5 16.9689 14.0140 16 -1 5 27.1095 14.4655 -16 -1 -6 66.3336 16.4308 16 -1 6 64.6368 17.4146 16 1 6 58.6953 16.5401 16 -1 6 50.9771 15.6648 -16 -1 -7 208.843 22.1210 16 -1 7 210.545 22.1172 16 -1 7 195.312 20.0944 16 2 -17 107.271 20.9738 16 -2 -15 102.492 18.6432 16 -2 -14 7.80353 14.7787 16 -2 -13 1373.28 53.5174 16 -2 -12 126.717 18.4120 16 -2 -11 718.952 34.8064 16 -2 -10 5.27536 13.0135 16 -2 -9 120.325 16.6831 -16 -2 8 97.3927 15.1406 16 -2 -8 70.3794 13.8156 -16 -2 7 199.687 18.3434 16 -2 -7 207.876 17.5231 -16 -2 6-4.60745 11.8463 16 2 -5 259.081 20.0321 16 2 -4 383.413 23.7341 16 2 -3 122.244 16.1006 16 2 -2-1.27936 11.6799 16 2 0 52.3478 14.1692 16 2 1 75.1197 15.6638 16 2 2 492.102 28.7563 16 -2 3 910.498 40.4495 16 -2 4 18.2243 15.3133 16 2 4 22.8512 14.5989 16 -2 5 84.4434 17.9725 16 2 5 93.0053 17.5211 16 -2 6 16.5638 15.6273 16 -2 7 307.998 26.5857 16 -3 -14 87.7063 18.5684 16 -3 -13 88.7638 17.1777 16 -3 -12 496.322 29.5720 16 -3 -11 252.717 21.9600 -16 -3 10 237.849 19.8357 16 -3 -10 223.921 20.2780 -16 -3 9 50.0702 13.0998 -16 -3 8 26.4229 12.4864 16 -3 -8 41.4991 13.6253 -16 -3 7 5.02469 12.7947 16 -3 -7 24.2185 12.4996 -16 -3 6 35.2379 12.8842 16 -3 -6 33.9849 13.3666 -16 -3 5 156.095 16.9341 16 -3 -5 146.347 16.3780 16 3 -4 246.976 20.6686 16 3 -3 104.185 15.8961 16 3 -2 272.454 21.2768 16 3 -1 55.5685 14.9508 16 3 1 86.5086 16.3675 16 -3 2 726.381 35.5336 16 -3 3 407.233 27.5484 16 -3 4 58.6129 16.6280 16 3 4 64.5437 15.6121 16 3 5 336.757 25.8649 16 -3 6 56.8303 18.1122 16 -4 -14 70.7844 17.5661 16 -4 -13 220.375 22.3737 -16 -4 12 310.384 23.1878 16 -4 -12 298.681 24.1541 -16 -4 11 66.8826 15.0592 16 -4 -11 57.8579 15.6809 -16 -4 10 82.7265 15.5640 16 -4 -10 79.4179 15.6463 -16 -4 9-6.74928 13.0286 16 -4 -9 13.7131 13.0856 -16 -4 8 34.9855 14.2634 16 -4 -8 25.2618 13.2331 16 -4 -7 84.5327 16.0185 -16 -4 6 356.001 23.7212 16 -4 -6 313.138 22.5756 -16 -4 5 10.8310 12.2099 16 -4 -5 22.2398 13.0036 -16 -4 4 88.3491 14.8864 16 -4 -4 56.5868 14.3977 16 4 -3 151.590 18.3006 16 4 -2 213.823 20.5534 16 4 -1 395.187 26.2437 16 -4 0 121.522 17.5361 16 4 0 163.056 19.0226 16 4 1 94.1739 17.0683 16 4 2 451.221 28.4026 16 -4 3 90.3999 18.7407 16 4 3 78.1760 16.9818 16 -4 4 459.386 30.6949 16 4 4 420.185 28.0169 16 -4 5 17.2834 15.3136 -16 -5 14 112.967 18.1715 16 -5 -13 16.6116 14.7184 -16 -5 12 66.2038 15.3354 16 -5 -12 81.4942 17.5287 -16 -5 11 376.690 25.6979 16 -5 -11 323.225 25.8706 -16 -5 10 1.45761 13.0828 16 -5 -10 13.4263 14.6143 -16 -5 9 141.549 18.9330 16 -5 -9 159.842 18.8872 -16 -5 8 35.9390 14.4757 16 -5 -8 51.3347 15.2727 -16 -5 7 40.3256 15.2990 16 -5 -7-2.77848 12.5826 -16 -5 6 300.879 23.2136 16 -5 -6 268.036 21.5208 -16 -5 5 144.001 18.3358 16 -5 -5 143.051 18.1819 -16 -5 4-1.43698 12.1470 16 -5 -4 16.8688 13.6515 16 -5 -3 425.163 25.9050 16 5 -2 68.1438 17.2756 16 5 -1 114.856 18.5541 16 -5 0 181.479 19.9017 16 5 0 219.347 22.4012 16 -5 1 150.896 19.7330 16 5 1 131.757 19.4672 16 -5 2 329.819 26.1000 16 5 2 397.963 27.9309 16 -5 3 568.192 34.4201 16 -5 4 8.71793 16.3810 16 -5 5 18.0816 17.4573 -16 -6 12 62.6621 16.4987 -16 -6 11 143.100 20.3474 16 -6 -11 106.677 17.9931 -16 -6 10 20.1768 14.4065 16 -6 -10-6.30891 14.6401 -16 -6 9 386.995 27.4780 16 -6 -9 398.733 27.2609 -16 -6 8-13.8125 14.7014 16 -6 -8 3.02846 14.3381 -16 -6 7 111.731 18.5445 16 -6 -7 87.6015 17.0749 -16 -6 6 52.2946 15.5415 16 -6 -6 40.5175 15.4081 -16 -6 5 88.7485 17.9233 16 -6 -5 89.3922 16.6405 -16 -6 3 1.51863 14.0382 16 -6 -3 4.08638 12.0105 16 6 -2 775.830 38.9867 16 6 -1 4.99103 14.4029 16 -6 0 321.638 25.1565 16 6 0 277.224 25.2993 16 -6 1 724.619 37.2811 16 6 1 698.705 37.8359 16 -6 2 8.33427 16.6829 16 -6 3 83.7403 19.4777 -16 -7 9 16.3899 15.2147 16 -7 -9 4.91694 14.9023 -16 -7 8-3.25886 14.1717 16 -7 -8 4.82441 14.4953 -16 -7 7 1.62098 14.4845 16 -7 -7-1.56764 14.3117 -16 -7 6 592.795 33.8038 16 -7 -6 513.041 31.1807 -16 -7 5 843.352 40.2998 16 -7 -5 826.375 39.6770 -16 -7 4 102.041 19.4120 16 -7 -4 92.5625 17.7228 16 -7 -3 7.22918 14.3693 16 -7 -2 120.737 18.0481 16 7 -2 142.331 20.6906 16 -7 -1 50.4420 15.5173 16 -7 0 824.814 40.2486 16 -7 1 329.988 27.6971 16 -7 2 19.3739 17.0057 16 -8 -6 419.460 29.1331 16 -8 -5 81.8739 18.4152 16 -8 -4 1340.24 53.3069 16 -8 -3-1.53288 15.5540 16 -8 -2 139.932 18.5017 16 -8 -1 34.4557 17.7957 16 -8 0 1.42659 14.7686 16 -8 0 12.1844 15.2095 17 0 4 29.1254 16.6747 17 0 5 2242.26 74.8600 17 1 -2 2.49263 11.2341 17 1 -1 490.606 27.7627 17 1 0 298.957 22.3172 17 1 1 31.7952 13.4193 17 1 2 9.50923 14.3376 17 1 3 11.2311 13.8547 17 1 4 2679.37 86.6295 17 -2 -13 38.4441 16.4576 17 -2 -12 296.530 24.9234 17 2 -5 7.77980 12.7491 17 2 -3-1.32620 11.6936 17 2 -2 43.1172 14.2582 17 2 -1 1.35830 13.1591 17 2 0 112.587 17.3556 17 2 1 258.567 21.9508 17 2 2 331.629 24.9016 17 2 3 29.3840 16.8744 17 -3 -13 80.3707 18.9853 17 -3 -12 7.61850 14.8723 17 -3 -11 75.2341 16.8926 17 -3 -10 5.69395 14.1468 17 3 -5 24.8966 14.0001 17 3 -3 106.822 16.9331 17 3 -2 87.7554 16.7771 17 3 -1 86.1772 17.1124 17 3 0 798.831 38.5575 17 3 1 365.178 26.5136 17 3 2 187.611 20.8553 17 -4 -12 302.837 25.1974 17 -4 -11 1.54064 14.2998 17 -4 -10 142.740 19.5911 -17 -4 9 29.7549 14.9610 17 -4 -9 11.3880 14.4037 -17 -4 8 203.359 19.7417 17 -4 -8 159.952 18.2353 -17 -4 7 33.8670 15.3295 -17 -4 6 1226.95 48.5127 17 4 -3 197.806 20.7856 17 4 -2 308.185 24.8321 17 4 -1 198.746 22.3941 17 4 0 7.87648 14.0776 17 4 1 266.214 23.9848 -17 -5 11 103.235 18.4972 -17 -5 10 24.1791 16.1017 17 -5 -10 7.74563 14.3250 -17 -5 9 9.04093 14.2147 17 -5 -9 16.5417 16.1199 -17 -5 8 16.6547 14.6258 17 -5 -8 33.7273 15.0428 -17 -5 7 42.1634 16.6817 17 -5 -7 7.20805 14.6893 -17 -5 6 3.01817 14.5107 17 -5 -6 7.02965 14.3148 -17 -5 5 2010.31 69.8621 17 5 -4 85.7947 17.0534 17 5 -3-19.2919 16.3749 17 5 -1 21.4214 15.7322 17 -6 -8 15.6932 15.4333 17 -6 -7-6.13449 14.0020 17 -6 -6 322.238 25.0174 17 -6 -5 765.115 37.4757 17 -7 -5 305.443 25.3165 17 -7 -4 33.4484 16.2656 18 3 -3-10.3956 14.1731 18 3 -2 178.318 21.2487 18 3 -1 60.6750 16.2753 18 4 -6 1317.47 52.6075 18 4 -5 92.5443 18.1212 18 4 -4 3.13177 15.5061 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 1162 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.86761(8) 0.71570(8) 0.49159(7) 0.0437(3) Uani 1 1 d . . . . . C1 C 0.79413(10) 0.65709(10) 0.46734(7) 0.0236(3) Uani 1 1 d . . . . . O2 O 0.70299(7) 0.69093(7) 0.42462(5) 0.0288(2) Uani 1 1 d . . . . . C2 C 0.68844(11) 0.80665(10) 0.41219(8) 0.0295(3) Uani 1 1 d . . . . . H1 H 0.708045 0.827861 0.363261 0.035 Uiso 1 1 calc R U . . . H2 H 0.733437 0.847178 0.454708 0.035 Uiso 1 1 calc R U . . . C3 C 0.57616(12) 0.83101(12) 0.40922(12) 0.0520(5) Uani 1 1 d . . . . . H3 H 0.532331 0.789177 0.367751 0.078 Uiso 1 1 calc R U . . . H4 H 0.563503 0.908325 0.399500 0.078 Uiso 1 1 calc R U . . . H5 H 0.558181 0.811684 0.458452 0.078 Uiso 1 1 calc R U . . . C4 C 0.79325(9) 0.53836(9) 0.48188(6) 0.0204(3) Uani 1 1 d . . . . . C5 C 0.70544(9) 0.47446(10) 0.45240(7) 0.0223(3) Uani 1 1 d . . . . . H34 H 0.645178 0.505897 0.420338 0.027 Uiso 1 1 calc R U . . . C6 C 0.70605(9) 0.36561(10) 0.46978(7) 0.0215(3) Uani 1 1 d . . . . . H35 H 0.645807 0.322803 0.449828 0.026 Uiso 1 1 calc R U . . . C7 C 0.79432(9) 0.31768(9) 0.51641(6) 0.0180(2) Uani 1 1 d . . . . . C8 C 0.88230(9) 0.38144(10) 0.54431(6) 0.0197(2) Uani 1 1 d . . . . . H36 H 0.943376 0.349709 0.575156 0.024 Uiso 1 1 calc R U . . . C9 C 0.88156(9) 0.49104(10) 0.52745(6) 0.0208(3) Uani 1 1 d . . . . . H37 H 0.941851 0.533887 0.547216 0.025 Uiso 1 1 calc R U . . . C10 C 0.79115(9) 0.20184(9) 0.53654(6) 0.0173(2) Uani 1 1 d . . . . . C11 C 0.74880(9) 0.10646(9) 0.47817(6) 0.0174(2) Uani 1 1 d . . . . . C12 C 0.68132(9) 0.06258(9) 0.53490(6) 0.0191(2) Uani 1 1 d . . . . . H38 H 0.606409 0.038177 0.519752 0.023 Uiso 1 1 calc R U . . . C13 C 0.72149(9) 0.15628(9) 0.59234(6) 0.0188(2) Uani 1 1 d . . . . . H39 H 0.676124 0.200994 0.619367 0.023 Uiso 1 1 calc R U . . . C14 C 0.81693(9) 0.08463(9) 0.63334(6) 0.0181(2) Uani 1 1 d . . . . . C15 C 0.77564(9) -0.00981(9) 0.57528(6) 0.0191(2) Uani 1 1 d . . . . . H40 H 0.770269 -0.087438 0.589628 0.023 Uiso 1 1 calc R U . . . C16 C 0.84439(9) 0.03450(9) 0.51944(6) 0.0184(2) Uani 1 1 d . . . . . H41 H 0.889679 -0.010552 0.492568 0.022 Uiso 1 1 calc R U . . . C17 C 0.88475(9) 0.12870(9) 0.57696(6) 0.0179(2) Uani 1 1 d . . . . . H42 H 0.959788 0.152612 0.592379 0.021 Uiso 1 1 calc R U . . . C18 C 0.70248(9) 0.11720(9) 0.39344(6) 0.0176(2) Uani 1 1 d . . . . . O3 O 0.60802(6) 0.09737(7) 0.37044(5) 0.0248(2) Uani 1 1 d . . . . . N1 N 0.76607(7) 0.14821(8) 0.34596(5) 0.0176(2) Uani 1 1 d . . . . . C19 C 0.72394(9) 0.15333(10) 0.26168(6) 0.0209(3) Uani 1 1 d . . . . . H6 H 0.783960 0.175198 0.237621 0.025 Uiso 1 1 calc R U . . . C20 C 0.68779(12) 0.04298(11) 0.22893(7) 0.0341(3) Uani 1 1 d . . . . . H7 H 0.746561 -0.008195 0.240834 0.051 Uiso 1 1 calc R U . . . H8 H 0.663800 0.048496 0.172995 0.051 Uiso 1 1 calc R U . . . H9 H 0.629699 0.017474 0.251853 0.051 Uiso 1 1 calc R U . . . C21 C 0.63973(10) 0.23980(11) 0.24027(7) 0.0296(3) Uani 1 1 d . . . . . H10 H 0.576837 0.218738 0.259191 0.044 Uiso 1 1 calc R U . . . H11 H 0.621592 0.247689 0.184168 0.044 Uiso 1 1 calc R U . . . H12 H 0.666490 0.308715 0.263636 0.044 Uiso 1 1 calc R U . . . C22 C 0.87879(9) 0.17410(10) 0.37325(7) 0.0207(3) Uani 1 1 d . . . . . H13 H 0.894035 0.170146 0.430731 0.025 Uiso 1 1 calc R U . . . C23 C 0.94867(10) 0.09108(12) 0.34506(8) 0.0326(3) Uani 1 1 d . . . . . H14 H 0.930646 0.018594 0.360454 0.049 Uiso 1 1 calc R U . . . H15 H 1.022679 0.106466 0.367743 0.049 Uiso 1 1 calc R U . . . H16 H 0.937687 0.094702 0.288839 0.049 Uiso 1 1 calc R U . . . C24 C 0.90453(10) 0.28853(11) 0.35148(7) 0.0272(3) Uani 1 1 d . . . . . H17 H 0.896323 0.293564 0.295479 0.041 Uiso 1 1 calc R U . . . H18 H 0.977319 0.306046 0.376234 0.041 Uiso 1 1 calc R U . . . H19 H 0.856495 0.339601 0.368706 0.041 Uiso 1 1 calc R U . . . C25 C 0.86130(9) 0.07431(9) 0.71826(6) 0.0183(2) Uani 1 1 d . . . . . O4 O 0.95367(6) 0.09909(7) 0.74336(5) 0.0255(2) Uani 1 1 d . . . . . N2 N 0.79742(7) 0.03616(8) 0.76370(5) 0.0202(2) Uani 1 1 d . . . . . C26 C 0.84013(10) 0.02038(10) 0.84706(6) 0.0239(3) Uani 1 1 d . . . . . H20 H 0.780763 -0.007263 0.869681 0.029 Uiso 1 1 calc R U . . . C27 C 0.87632(12) 0.12600(12) 0.88830(7) 0.0359(3) Uani 1 1 d . . . . . H21 H 0.934475 0.156381 0.867617 0.054 Uiso 1 1 calc R U . . . H22 H 0.900209 0.112181 0.943500 0.054 Uiso 1 1 calc R U . . . H23 H 0.817555 0.177337 0.880317 0.054 Uiso 1 1 calc R U . . . C28 C 0.92482(10) -0.06677(11) 0.86036(8) 0.0317(3) Uani 1 1 d . . . . . H24 H 0.896256 -0.133503 0.834455 0.048 Uiso 1 1 calc R U . . . H25 H 0.947508 -0.080238 0.915696 0.048 Uiso 1 1 calc R U . . . H26 H 0.985205 -0.042654 0.839493 0.048 Uiso 1 1 calc R U . . . C29 C 0.68661(9) 0.00567(11) 0.73382(7) 0.0248(3) Uani 1 1 d . . . . . H27 H 0.671539 0.019107 0.677068 0.030 Uiso 1 1 calc R U . . . C30 C 0.66669(11) -0.11377(12) 0.74525(8) 0.0352(3) Uani 1 1 d . . . . . H28 H 0.716903 -0.157005 0.723697 0.053 Uiso 1 1 calc R U . . . H29 H 0.594709 -0.132117 0.719048 0.053 Uiso 1 1 calc R U . . . H30 H 0.675631 -0.129118 0.800354 0.053 Uiso 1 1 calc R U . . . C31 C 0.61259(11) 0.07789(13) 0.76771(8) 0.0377(3) Uani 1 1 d . . . . . H31 H 0.625743 0.067767 0.823613 0.057 Uiso 1 1 calc R U . . . H32 H 0.539414 0.058710 0.745189 0.057 Uiso 1 1 calc R U . . . H33 H 0.625002 0.153620 0.756114 0.057 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 0.0370(6) 0.0235(5) 0.0634(7) 0.0057(5) -0.0063(5) -0.0069(4) C1 0.0276(6) 0.0213(6) 0.0228(6) 0.0002(5) 0.0071(5) 0.0000(5) O2 0.0328(5) 0.0154(4) 0.0351(5) 0.0020(4) -0.0001(4) 0.0010(4) C2 0.0398(7) 0.0140(6) 0.0341(7) 0.0026(5) 0.0065(6) 0.0013(5) C3 0.0400(9) 0.0218(7) 0.0907(13) 0.0078(8) 0.0055(9) 0.0036(6) C4 0.0257(6) 0.0192(6) 0.0182(5) -0.0002(5) 0.0085(5) 0.0013(5) C5 0.0227(6) 0.0215(6) 0.0219(6) 0.0012(5) 0.0026(5) 0.0036(5) C6 0.0206(6) 0.0207(6) 0.0225(6) -0.0016(5) 0.0033(5) -0.0012(5) C7 0.0216(6) 0.0184(6) 0.0155(5) -0.0006(4) 0.0077(4) 0.0018(5) C8 0.0198(6) 0.0223(6) 0.0174(5) 0.0001(5) 0.0045(4) 0.0024(5) C9 0.0213(6) 0.0224(6) 0.0195(6) -0.0031(5) 0.0061(5) -0.0030(5) C10 0.0181(5) 0.0181(6) 0.0158(5) -0.0007(4) 0.0037(4) 0.0006(4) C11 0.0184(6) 0.0164(5) 0.0179(5) 0.0000(4) 0.0051(5) 0.0003(4) C12 0.0198(6) 0.0207(6) 0.0174(5) 0.0004(5) 0.0048(4) -0.0018(5) C13 0.0195(6) 0.0205(6) 0.0171(5) 0.0001(5) 0.0053(4) 0.0012(5) C14 0.0194(6) 0.0175(6) 0.0181(6) 0.0008(4) 0.0056(4) 0.0002(4) C15 0.0224(6) 0.0183(6) 0.0171(5) 0.0009(4) 0.0053(5) -0.0011(5) C16 0.0212(6) 0.0175(6) 0.0171(5) 0.0014(4) 0.0055(4) 0.0019(5) C17 0.0188(6) 0.0183(6) 0.0170(5) 0.0015(4) 0.0045(4) 0.0001(5) C18 0.0212(6) 0.0131(5) 0.0186(6) -0.0002(4) 0.0045(5) 0.0016(4) O3 0.0206(4) 0.0312(5) 0.0218(4) 0.0028(4) 0.0024(3) -0.0050(4) N1 0.0184(5) 0.0185(5) 0.0158(5) 0.0006(4) 0.0033(4) 0.0010(4) C19 0.0244(6) 0.0236(6) 0.0148(5) 0.0015(5) 0.0041(5) -0.0013(5) C20 0.0504(9) 0.0312(7) 0.0208(6) -0.0064(5) 0.0077(6) -0.0075(6) C21 0.0275(7) 0.0339(7) 0.0255(6) 0.0089(5) 0.0014(5) 0.0038(6) C22 0.0175(6) 0.0264(6) 0.0185(6) 0.0031(5) 0.0039(4) 0.0014(5) C23 0.0271(7) 0.0414(8) 0.0311(7) 0.0071(6) 0.0102(6) 0.0131(6) C24 0.0259(6) 0.0316(7) 0.0240(6) 0.0031(5) 0.0053(5) -0.0070(5) C25 0.0211(6) 0.0153(5) 0.0187(6) -0.0002(4) 0.0046(5) 0.0005(4) O4 0.0227(4) 0.0313(5) 0.0217(4) 0.0017(4) 0.0031(3) -0.0071(4) N2 0.0195(5) 0.0256(5) 0.0156(5) 0.0022(4) 0.0035(4) -0.0014(4) C26 0.0258(6) 0.0298(7) 0.0157(6) 0.0039(5) 0.0035(5) -0.0035(5) C27 0.0509(9) 0.0379(8) 0.0187(6) -0.0028(6) 0.0070(6) -0.0096(7) C28 0.0288(7) 0.0378(8) 0.0266(7) 0.0110(6) 0.0016(5) 0.0004(6) C29 0.0185(6) 0.0367(7) 0.0192(6) 0.0041(5) 0.0038(5) -0.0029(5) C30 0.0330(7) 0.0410(8) 0.0311(7) 0.0015(6) 0.0057(6) -0.0143(6) C31 0.0284(7) 0.0561(10) 0.0310(7) 0.0106(7) 0.0119(6) 0.0112(7) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 123.88(11) . . ? O1 C1 C4 124.40(12) . . ? O2 C1 C4 111.72(10) . . ? C1 O2 C2 117.86(10) . . ? O2 C2 C3 107.58(11) . . ? O2 C2 H1 110.2 . . ? C3 C2 H1 110.2 . . ? O2 C2 H2 110.2 . . ? C3 C2 H2 110.2 . . ? H1 C2 H2 108.5 . . ? C2 C3 H3 109.5 . . ? C2 C3 H4 109.5 . . ? H3 C3 H4 109.5 . . ? C2 C3 H5 109.5 . . ? H3 C3 H5 109.5 . . ? H4 C3 H5 109.5 . . ? C9 C4 C5 119.38(11) . . ? C9 C4 C1 118.77(11) . . ? C5 C4 C1 121.84(11) . . ? C6 C5 C4 120.12(11) . . ? C6 C5 H34 119.9 . . ? C4 C5 H34 119.9 . . ? C5 C6 C7 120.79(11) . . ? C5 C6 H35 119.6 . . ? C7 C6 H35 119.6 . . ? C8 C7 C6 118.75(11) . . ? C8 C7 C10 121.66(10) . . ? C6 C7 C10 119.57(10) . . ? C9 C8 C7 120.56(11) . . ? C9 C8 H36 119.7 . . ? C7 C8 H36 119.7 . . ? C4 C9 C8 120.38(11) . . ? C4 C9 H37 119.8 . . ? C8 C9 H37 119.8 . . ? C7 C10 C17 127.83(10) . . ? C7 C10 C13 123.10(9) . . ? C17 C10 C13 89.79(8) . . ? C7 C10 C11 125.73(9) . . ? C17 C10 C11 90.02(8) . . ? C13 C10 C11 88.78(8) . . ? C18 C11 C12 120.92(9) . . ? C18 C11 C16 128.78(9) . . ? C12 C11 C16 89.76(8) . . ? C18 C11 C10 126.71(9) . . ? C12 C11 C10 90.10(8) . . ? C16 C11 C10 89.08(8) . . ? C13 C12 C11 90.42(8) . . ? C13 C12 C15 90.13(8) . . ? C11 C12 C15 90.29(8) . . ? C13 C12 H38 125.1 . . ? C11 C12 H38 125.1 . . ? C15 C12 H38 125.1 . . ? C12 C13 C14 90.46(8) . . ? C12 C13 C10 90.70(8) . . ? C14 C13 C10 89.64(8) . . ? C12 C13 H39 125.1 . . ? C14 C13 H39 125.1 . . ? C10 C13 H39 125.1 . . ? C25 C14 C17 121.53(9) . . ? C25 C14 C13 127.80(9) . . ? C17 C14 C13 90.02(8) . . ? C25 C14 C15 126.89(9) . . ? C17 C14 C15 89.99(8) . . ? C13 C14 C15 89.24(8) . . ? C16 C15 C12 90.19(8) . . ? C16 C15 C14 89.64(8) . . ? C12 C15 C14 90.17(8) . . ? C16 C15 H40 125.3 . . ? C12 C15 H40 125.3 . . ? C14 C15 H40 125.3 . . ? C15 C16 C17 90.28(8) . . ? C15 C16 C11 89.76(8) . . ? C17 C16 C11 90.43(8) . . ? C15 C16 H41 125.2 . . ? C17 C16 H41 125.2 . . ? C11 C16 H41 125.2 . . ? C14 C17 C10 90.54(8) . . ? C14 C17 C16 90.09(8) . . ? C10 C17 C16 90.48(8) . . ? C14 C17 H42 125.0 . . ? C10 C17 H42 125.0 . . ? C16 C17 H42 125.0 . . ? O3 C18 N1 122.88(10) . . ? O3 C18 C11 118.48(10) . . ? N1 C18 C11 118.64(10) . . ? C18 N1 C22 123.20(9) . . ? C18 N1 C19 119.74(9) . . ? C22 N1 C19 117.02(9) . . ? N1 C19 C20 111.56(10) . . ? N1 C19 C21 112.19(10) . . ? C20 C19 C21 112.82(11) . . ? N1 C19 H6 106.6 . . ? C20 C19 H6 106.6 . . ? C21 C19 H6 106.6 . . ? C19 C20 H7 109.5 . . ? C19 C20 H8 109.5 . . ? H7 C20 H8 109.5 . . ? C19 C20 H9 109.5 . . ? H7 C20 H9 109.5 . . ? H8 C20 H9 109.5 . . ? C19 C21 H10 109.5 . . ? C19 C21 H11 109.5 . . ? H10 C21 H11 109.5 . . ? C19 C21 H12 109.5 . . ? H10 C21 H12 109.5 . . ? H11 C21 H12 109.5 . . ? N1 C22 C23 111.24(10) . . ? N1 C22 C24 111.87(9) . . ? C23 C22 C24 111.55(10) . . ? N1 C22 H13 107.3 . . ? C23 C22 H13 107.3 . . ? C24 C22 H13 107.3 . . ? C22 C23 H14 109.5 . . ? C22 C23 H15 109.5 . . ? H14 C23 H15 109.5 . . ? C22 C23 H16 109.5 . . ? H14 C23 H16 109.5 . . ? H15 C23 H16 109.5 . . ? C22 C24 H17 109.5 . . ? C22 C24 H18 109.5 . . ? H17 C24 H18 109.5 . . ? C22 C24 H19 109.5 . . ? H17 C24 H19 109.5 . . ? H18 C24 H19 109.5 . . ? O4 C25 N2 122.81(10) . . ? O4 C25 C14 119.01(10) . . ? N2 C25 C14 118.17(10) . . ? C25 N2 C29 123.06(9) . . ? C25 N2 C26 119.48(9) . . ? C29 N2 C26 117.43(9) . . ? N2 C26 C28 110.91(10) . . ? N2 C26 C27 112.42(10) . . ? C28 C26 C27 113.09(11) . . ? N2 C26 H20 106.6 . . ? C28 C26 H20 106.6 . . ? C27 C26 H20 106.6 . . ? C26 C27 H21 109.5 . . ? C26 C27 H22 109.5 . . ? H21 C27 H22 109.5 . . ? C26 C27 H23 109.5 . . ? H21 C27 H23 109.5 . . ? H22 C27 H23 109.5 . . ? C26 C28 H24 109.5 . . ? C26 C28 H25 109.5 . . ? H24 C28 H25 109.5 . . ? C26 C28 H26 109.5 . . ? H24 C28 H26 109.5 . . ? H25 C28 H26 109.5 . . ? N2 C29 C30 112.36(10) . . ? N2 C29 C31 110.79(11) . . ? C30 C29 C31 112.25(11) . . ? N2 C29 H27 107.0 . . ? C30 C29 H27 107.0 . . ? C31 C29 H27 107.0 . . ? C29 C30 H28 109.5 . . ? C29 C30 H29 109.5 . . ? H28 C30 H29 109.5 . . ? C29 C30 H30 109.5 . . ? H28 C30 H30 109.5 . . ? H29 C30 H30 109.5 . . ? C29 C31 H31 109.5 . . ? C29 C31 H32 109.5 . . ? H31 C31 H32 109.5 . . ? C29 C31 H33 109.5 . . ? H31 C31 H33 109.5 . . ? H32 C31 H33 109.5 . . ? 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 O1 C1 1.2044(15) . ? C1 O2 1.3334(15) . ? C1 C4 1.4922(17) . ? O2 C2 1.4553(14) . ? C2 C3 1.478(2) . ? C2 H1 0.9900 . ? C2 H2 0.9900 . ? C3 H3 0.9800 . ? C3 H4 0.9800 . ? C3 H5 0.9800 . ? C4 C9 1.3881(17) . ? C4 C5 1.3967(17) . ? C5 C6 1.3816(17) . ? C5 H34 0.9500 . ? C6 C7 1.3988(16) . ? C6 H35 0.9500 . ? C7 C8 1.3917(16) . ? C7 C10 1.4799(16) . ? C8 C9 1.3886(17) . ? C8 H36 0.9500 . ? C9 H37 0.9500 . ? C10 C17 1.5647(15) . ? C10 C13 1.5772(15) . ? C10 C11 1.5918(15) . ? C11 C18 1.5062(15) . ? C11 C12 1.5627(15) . ? C11 C16 1.5785(15) . ? C12 C13 1.5610(16) . ? C12 C15 1.5655(16) . ? C12 H38 1.0000 . ? C13 C14 1.5737(15) . ? C13 H39 1.0000 . ? C14 C25 1.5042(15) . ? C14 C17 1.5618(15) . ? C14 C15 1.5771(16) . ? C15 C16 1.5640(15) . ? C15 H40 1.0000 . ? C16 C17 1.5670(16) . ? C16 H41 1.0000 . ? C17 H42 1.0000 . ? C18 O3 1.2336(14) . ? C18 N1 1.3517(15) . ? N1 C22 1.4775(14) . ? N1 C19 1.4848(14) . ? C19 C20 1.5200(17) . ? C19 C21 1.5203(17) . ? C19 H6 1.0000 . ? C20 H7 0.9800 . ? C20 H8 0.9800 . ? C20 H9 0.9800 . ? C21 H10 0.9800 . ? C21 H11 0.9800 . ? C21 H12 0.9800 . ? C22 C23 1.5219(17) . ? C22 C24 1.5230(17) . ? C22 H13 1.0000 . ? C23 H14 0.9800 . ? C23 H15 0.9800 . ? C23 H16 0.9800 . ? C24 H17 0.9800 . ? C24 H18 0.9800 . ? C24 H19 0.9800 . ? C25 O4 1.2280(14) . ? C25 N2 1.3557(15) . ? N2 C29 1.4747(14) . ? N2 C26 1.4823(14) . ? C26 C28 1.5228(18) . ? C26 C27 1.5241(18) . ? C26 H20 1.0000 . ? C27 H21 0.9800 . ? C27 H22 0.9800 . ? C27 H23 0.9800 . ? C28 H24 0.9800 . ? C28 H25 0.9800 . ? C28 H26 0.9800 . ? C29 C30 1.5213(19) . ? C29 C31 1.5240(19) . ? C29 H27 1.0000 . ? C30 H28 0.9800 . ? C30 H29 0.9800 . ? C30 H30 0.9800 . ? C31 H31 0.9800 . ? C31 H32 0.9800 . ? C31 H33 0.9800 . ? 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 O1 C1 O2 C2 -5.47(18) . . . . ? C4 C1 O2 C2 173.99(10) . . . . ? C1 O2 C2 C3 -145.52(13) . . . . ? O1 C1 C4 C9 1.26(18) . . . . ? O2 C1 C4 C9 -178.19(10) . . . . ? O1 C1 C4 C5 179.79(12) . . . . ? O2 C1 C4 C5 0.34(16) . . . . ? C9 C4 C5 C6 1.22(17) . . . . ? C1 C4 C5 C6 -177.29(11) . . . . ? C4 C5 C6 C7 -0.48(17) . . . . ? C5 C6 C7 C8 -0.79(17) . . . . ? C5 C6 C7 C10 177.62(10) . . . . ? C6 C7 C8 C9 1.32(16) . . . . ? C10 C7 C8 C9 -177.05(10) . . . . ? C5 C4 C9 C8 -0.69(17) . . . . ? C1 C4 C9 C8 177.87(10) . . . . ? C7 C8 C9 C4 -0.59(17) . . . . ? C8 C7 C10 C17 -11.50(17) . . . . ? C6 C7 C10 C17 170.14(10) . . . . ? C8 C7 C10 C13 108.55(13) . . . . ? C6 C7 C10 C13 -69.82(14) . . . . ? C8 C7 C10 C11 -135.50(11) . . . . ? C6 C7 C10 C11 46.14(15) . . . . ? C7 C10 C11 C18 -1.61(17) . . . . ? C17 C10 C11 C18 -140.71(11) . . . . ? C13 C10 C11 C18 129.51(11) . . . . ? C7 C10 C11 C12 -131.57(11) . . . . ? C17 C10 C11 C12 89.34(8) . . . . ? C13 C10 C11 C12 -0.45(8) . . . . ? C7 C10 C11 C16 138.67(11) . . . . ? C17 C10 C11 C16 -0.42(8) . . . . ? C13 C10 C11 C16 -90.21(8) . . . . ? C18 C11 C12 C13 -133.79(10) . . . . ? C16 C11 C12 C13 89.53(8) . . . . ? C10 C11 C12 C13 0.45(8) . . . . ? C18 C11 C12 C15 136.08(10) . . . . ? C16 C11 C12 C15 -0.60(8) . . . . ? C10 C11 C12 C15 -89.67(8) . . . . ? C11 C12 C13 C14 -90.11(8) . . . . ? C15 C12 C13 C14 0.18(8) . . . . ? C11 C12 C13 C10 -0.46(8) . . . . ? C15 C12 C13 C10 89.83(8) . . . . ? C7 C10 C13 C12 133.56(11) . . . . ? C17 C10 C13 C12 -89.57(8) . . . . ? C11 C10 C13 C12 0.45(8) . . . . ? C7 C10 C13 C14 -135.98(11) . . . . ? C17 C10 C13 C14 0.88(8) . . . . ? C11 C10 C13 C14 90.91(8) . . . . ? C12 C13 C14 C25 -138.73(11) . . . . ? C10 C13 C14 C25 130.57(11) . . . . ? C12 C13 C14 C17 89.81(8) . . . . ? C10 C13 C14 C17 -0.89(8) . . . . ? C12 C13 C14 C15 -0.18(8) . . . . ? C10 C13 C14 C15 -90.88(8) . . . . ? C13 C12 C15 C16 -89.82(8) . . . . ? C11 C12 C15 C16 0.60(8) . . . . ? C13 C12 C15 C14 -0.18(8) . . . . ? C11 C12 C15 C14 90.24(8) . . . . ? C25 C14 C15 C16 -130.48(11) . . . . ? C17 C14 C15 C16 0.35(8) . . . . ? C13 C14 C15 C16 90.37(8) . . . . ? C25 C14 C15 C12 139.33(11) . . . . ? C17 C14 C15 C12 -89.84(8) . . . . ? C13 C14 C15 C12 0.18(8) . . . . ? C12 C15 C16 C17 89.83(8) . . . . ? C14 C15 C16 C17 -0.35(8) . . . . ? C12 C15 C16 C11 -0.60(8) . . . . ? C14 C15 C16 C11 -90.77(8) . . . . ? C18 C11 C16 C15 -130.37(12) . . . . ? C12 C11 C16 C15 0.60(8) . . . . ? C10 C11 C16 C15 90.70(8) . . . . ? C18 C11 C16 C17 139.34(11) . . . . ? C12 C11 C16 C17 -89.68(8) . . . . ? C10 C11 C16 C17 0.42(8) . . . . ? C25 C14 C17 C10 -135.10(10) . . . . ? C13 C14 C17 C10 0.89(8) . . . . ? C15 C14 C17 C10 90.13(8) . . . . ? C25 C14 C17 C16 134.42(10) . . . . ? C13 C14 C17 C16 -89.58(8) . . . . ? C15 C14 C17 C16 -0.35(8) . . . . ? C7 C10 C17 C14 132.63(11) . . . . ? C13 C10 C17 C14 -0.89(8) . . . . ? C11 C10 C17 C14 -89.67(8) . . . . ? C7 C10 C17 C16 -137.28(11) . . . . ? C13 C10 C17 C16 89.20(8) . . . . ? C11 C10 C17 C16 0.42(8) . . . . ? C15 C16 C17 C14 0.35(8) . . . . ? C11 C16 C17 C14 90.11(8) . . . . ? C15 C16 C17 C10 -90.19(8) . . . . ? C11 C16 C17 C10 -0.43(8) . . . . ? C12 C11 C18 O3 4.73(16) . . . . ? C16 C11 C18 O3 123.08(12) . . . . ? C10 C11 C18 O3 -111.95(12) . . . . ? C12 C11 C18 N1 -175.34(10) . . . . ? C16 C11 C18 N1 -56.99(16) . . . . ? C10 C11 C18 N1 67.98(14) . . . . ? O3 C18 N1 C22 178.80(10) . . . . ? C11 C18 N1 C22 -1.13(16) . . . . ? O3 C18 N1 C19 -3.58(16) . . . . ? C11 C18 N1 C19 176.49(9) . . . . ? C18 N1 C19 C20 -62.04(14) . . . . ? C22 N1 C19 C20 115.72(12) . . . . ? C18 N1 C19 C21 65.66(13) . . . . ? C22 N1 C19 C21 -116.58(11) . . . . ? C18 N1 C22 C23 112.40(12) . . . . ? C19 N1 C22 C23 -65.27(13) . . . . ? C18 N1 C22 C24 -122.10(11) . . . . ? C19 N1 C22 C24 60.23(13) . . . . ? C17 C14 C25 O4 -1.53(16) . . . . ? C13 C14 C25 O4 -119.98(13) . . . . ? C15 C14 C25 O4 115.88(13) . . . . ? C17 C14 C25 N2 179.50(10) . . . . ? C13 C14 C25 N2 61.04(15) . . . . ? C15 C14 C25 N2 -63.10(15) . . . . ? O4 C25 N2 C29 -179.64(11) . . . . ? C14 C25 N2 C29 -0.70(16) . . . . ? O4 C25 N2 C26 -1.67(17) . . . . ? C14 C25 N2 C26 177.26(10) . . . . ? C25 N2 C26 C28 -64.73(14) . . . . ? C29 N2 C26 C28 113.35(12) . . . . ? C25 N2 C26 C27 62.98(14) . . . . ? C29 N2 C26 C27 -118.94(12) . . . . ? C25 N2 C29 C30 117.00(12) . . . . ? C26 N2 C29 C30 -61.01(14) . . . . ? C25 N2 C29 C31 -116.55(12) . . . . ? C26 N2 C29 C31 65.45(14) . . . . ?