#------------------------------------------------------------------------------ #$Date: 2020-08-06 16:30:52 +0300 (Thu, 06 Aug 2020) $ #$Revision: 254934 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557905.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_1557905 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_absolute_configuration unk _chemical_formula_sum 'C32 H40 N2 O2' _chemical_formula_weight 484.66 _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 109.196(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.4974(4) _cell_length_b 24.3000(6) _cell_length_c 11.3737(4) _cell_measurement_reflns_used 13383 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 30.5180 _cell_measurement_theta_min 2.6020 _cell_volume 2739.97(17) _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 SIR-97 _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 0.0292 _diffrn_reflns_av_unetI/netI 0.0196 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 29817 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.998 _diffrn_reflns_theta_max 24.998 _diffrn_reflns_theta_min 2.441 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.79595 _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 1.175 _exptl_crystal_description block _exptl_crystal_F_000 1048 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.244 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.032 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 333 _refine_ls_number_reflns 4822 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0347 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+1.0182P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0817 _refine_ls_wR_factor_ref 0.0866 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4097 _reflns_number_total 4822 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01909g2.cif _cod_data_source_block 2k _cod_depositor_comments 'Adding full bibliography for 1557900--1557907.cif.' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1557905 _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 0.993 _shelx_estimated_absorpt_t_max 0.999 _shelx_res_file ; TITL qq qq.res created by SHELXL-2016/6 at 20:53:36 on 11-Jan-2019 REM Yadorkari-X generated CELL 0.71073 10.4974 24.3000 11.3737 90.0000 109.1960 90.0000 ZERR 4.0 0.0004 0.0006 0.0004 0.0000 0.0040 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 128 160 8 8 SIZE 0.10 0.05 0.01 TEMP -150.0 L.S. 10 FMAP 2 PLAN -25 ACTA CONF LIST 4 WPDB -1 BOND $H MERG 2 OMIT -10.000000 50.000000 WGHT 0.036200 1.018200 FVAR 0.43769 O1 4 0.156691 0.357818 0.360373 11.00000 0.02656 0.02444 = 0.01886 0.00070 0.00550 0.00435 C1 1 0.263340 0.343238 0.439589 11.00000 0.02443 0.02263 = 0.01486 0.00056 0.00961 0.00226 N1 3 0.355072 0.379838 0.507272 11.00000 0.02791 0.01902 = 0.02071 0.00067 0.00433 0.00081 C2 1 0.333150 0.439704 0.481675 11.00000 0.03697 0.01801 = 0.02689 -0.00058 0.00597 -0.00011 AFIX 13 H1 2 0.414774 0.458782 0.538180 11.00000 -1.20000 AFIX 0 C3 1 0.213357 0.461281 0.515234 11.00000 0.05377 0.02709 = 0.03218 -0.00438 0.01491 0.00893 AFIX 137 H2 2 0.130303 0.444111 0.461086 11.00000 -1.50000 H3 2 0.207193 0.501291 0.503961 11.00000 -1.50000 H4 2 0.225459 0.452332 0.602257 11.00000 -1.50000 AFIX 0 C4 1 0.325229 0.454457 0.349044 11.00000 0.04855 0.02272 = 0.03418 0.00571 0.01640 0.00056 AFIX 137 H5 2 0.405311 0.440373 0.332772 11.00000 -1.50000 H6 2 0.321135 0.494547 0.339133 11.00000 -1.50000 H7 2 0.244153 0.437927 0.290049 11.00000 -1.50000 AFIX 0 C5 1 0.477399 0.363322 0.609826 11.00000 0.02933 0.02359 = 0.02692 0.00302 -0.00001 -0.00118 AFIX 13 H8 2 0.471344 0.322700 0.621028 11.00000 -1.20000 AFIX 0 C6 1 0.483555 0.390370 0.732811 11.00000 0.04799 0.03162 = 0.02574 0.00007 -0.00259 -0.00617 AFIX 137 H9 2 0.493506 0.430263 0.726628 11.00000 -1.50000 H10 2 0.560855 0.375781 0.800005 11.00000 -1.50000 H11 2 0.400253 0.382420 0.750700 11.00000 -1.50000 AFIX 0 C7 1 0.603905 0.373702 0.575646 11.00000 0.02986 0.03823 = 0.05214 0.00745 0.00510 -0.00251 AFIX 137 H12 2 0.599639 0.352131 0.501643 11.00000 -1.50000 H13 2 0.683547 0.362732 0.645156 11.00000 -1.50000 H14 2 0.609961 0.412923 0.558137 11.00000 -1.50000 AFIX 0 C8 1 0.287470 0.282554 0.462101 11.00000 0.02134 0.02061 = 0.01755 -0.00039 0.00651 0.00117 C9 1 0.196427 0.239972 0.369370 11.00000 0.02359 0.02226 = 0.01707 -0.00116 0.00505 0.00212 AFIX 13 H15 2 0.126563 0.249530 0.288128 11.00000 -1.20000 AFIX 0 C10 1 0.321241 0.202401 0.384234 11.00000 0.02563 0.02067 = 0.01866 -0.00116 0.00899 0.00143 AFIX 13 H16 2 0.343223 0.184562 0.314025 11.00000 -1.20000 AFIX 0 C11 1 0.413827 0.244353 0.478074 11.00000 0.02099 0.01966 = 0.02199 0.00006 0.00922 0.00070 AFIX 13 H17 2 0.504181 0.257185 0.477633 11.00000 -1.20000 AFIX 0 C12 1 0.386319 0.213376 0.588161 11.00000 0.02034 0.01833 = 0.01838 -0.00082 0.00627 -0.00016 AFIX 13 H18 2 0.456819 0.203363 0.668686 11.00000 -1.20000 AFIX 0 C13 1 0.293603 0.170991 0.493070 11.00000 0.01990 0.02097 = 0.01867 -0.00238 0.00725 -0.00020 C14 1 0.167669 0.209224 0.478261 11.00000 0.01999 0.01954 = 0.02092 -0.00227 0.00630 0.00035 AFIX 13 H19 2 0.077026 0.196352 0.477804 11.00000 -1.20000 AFIX 0 C15 1 0.261614 0.250995 0.575172 11.00000 0.02026 0.01847 = 0.01763 0.00035 0.00560 0.00029 C16 1 0.229161 0.278073 0.678716 11.00000 0.02065 0.01779 = 0.02040 -0.00177 0.00843 -0.00348 C17 1 0.294138 0.263698 0.800426 11.00000 0.02066 0.02025 = 0.02261 0.00003 0.00771 -0.00089 AFIX 43 H20 2 0.362762 0.236439 0.818611 11.00000 -1.20000 AFIX 0 C18 1 0.261501 0.288488 0.899837 11.00000 0.02153 0.02289 = 0.02101 -0.00124 0.00871 -0.00601 C19 1 0.325622 0.273220 1.025796 11.00000 0.02714 0.03313 = 0.02202 0.00175 0.00864 -0.00425 AFIX 43 H21 2 0.392364 0.245168 1.045635 11.00000 -1.20000 AFIX 0 C20 1 0.292169 0.298561 1.119059 11.00000 0.03401 0.04117 = 0.01945 -0.00140 0.01027 -0.01250 AFIX 43 H22 2 0.335806 0.287908 1.203096 11.00000 -1.20000 AFIX 0 C21 1 0.193824 0.340208 1.091626 11.00000 0.03960 0.03385 = 0.02607 -0.01077 0.02064 -0.01467 AFIX 43 H23 2 0.171957 0.357675 1.157244 11.00000 -1.20000 AFIX 0 C22 1 0.129420 0.355742 0.971069 11.00000 0.03059 0.02379 = 0.03116 -0.00635 0.01825 -0.00762 AFIX 43 H24 2 0.062801 0.383816 0.953519 11.00000 -1.20000 AFIX 0 C23 1 0.161229 0.330321 0.872197 11.00000 0.02401 0.01998 = 0.02483 -0.00336 0.01276 -0.00734 C24 1 0.095565 0.344725 0.745642 11.00000 0.02360 0.01936 = 0.02734 0.00008 0.01126 0.00082 AFIX 43 H25 2 0.027969 0.372435 0.725760 11.00000 -1.20000 AFIX 0 C25 1 0.127903 0.319456 0.652195 11.00000 0.02301 0.02138 = 0.02026 0.00026 0.00703 -0.00099 AFIX 43 H26 2 0.082147 0.329641 0.568221 11.00000 -1.20000 AFIX 0 C26 1 0.302733 0.109408 0.505148 11.00000 0.01702 0.02175 = 0.02265 -0.00293 0.00454 -0.00114 O2 4 0.337887 0.082556 0.429197 11.00000 0.03375 0.02271 = 0.03023 -0.00652 0.01553 0.00004 N2 3 0.273431 0.085631 0.600901 11.00000 0.02656 0.01788 = 0.02728 -0.00089 0.01210 -0.00067 C27 1 0.229588 0.117264 0.691557 11.00000 0.02832 0.02067 = 0.02812 -0.00094 0.01438 -0.00118 AFIX 13 H27 2 0.229814 0.156976 0.668571 11.00000 -1.20000 AFIX 0 C28 1 0.327146 0.111274 0.824095 11.00000 0.04203 0.02946 = 0.02779 0.00209 0.01513 -0.00073 AFIX 137 H28 2 0.327821 0.072940 0.851058 11.00000 -1.50000 H29 2 0.298232 0.135211 0.879924 11.00000 -1.50000 H30 2 0.418058 0.121824 0.826448 11.00000 -1.50000 AFIX 0 C29 1 0.085287 0.102777 0.681885 11.00000 0.03493 0.03706 = 0.04879 -0.00503 0.02422 -0.00423 AFIX 137 H31 2 0.025836 0.108140 0.595964 11.00000 -1.50000 H32 2 0.055917 0.126623 0.737573 11.00000 -1.50000 H33 2 0.081285 0.064250 0.705897 11.00000 -1.50000 AFIX 0 C30 1 0.289609 0.025252 0.620069 11.00000 0.03865 0.01782 = 0.03632 0.00139 0.01700 -0.00097 AFIX 13 H34 2 0.258216 0.016234 0.691846 11.00000 -1.20000 AFIX 0 C31 1 0.437556 0.008709 0.658896 11.00000 0.04333 0.02631 = 0.03933 0.00212 0.00775 0.00919 AFIX 137 H35 2 0.471752 0.015107 0.589593 11.00000 -1.50000 H36 2 0.446556 -0.030384 0.681291 11.00000 -1.50000 H37 2 0.489598 0.030754 0.730797 11.00000 -1.50000 AFIX 0 C32 1 0.200980 -0.007609 0.509449 11.00000 0.03877 0.02215 = 0.05877 -0.00670 0.01455 -0.00706 AFIX 137 H38 2 0.109194 0.007357 0.482697 11.00000 -1.50000 H39 2 0.199036 -0.046219 0.533692 11.00000 -1.50000 H40 2 0.237640 -0.005124 0.440732 11.00000 -1.50000 AFIX 0 HKLF 4 REM qq REM R1 = 0.0347 for 4097 Fo > 4sig(Fo) and 0.0432 for all 4822 data REM 333 parameters refined using 0 restraints END WGHT 0.0362 1.0181 REM Highest difference peak 0.244, deepest hole -0.222, 1-sigma level 0.032 Q1 1 0.3538 0.1840 0.5568 11.00000 0.05 0.24 Q2 1 0.2306 0.2678 0.4093 11.00000 0.05 0.23 Q3 1 0.3126 0.1789 0.4375 11.00000 0.05 0.22 Q4 1 0.3588 0.2728 0.4649 11.00000 0.05 0.22 Q5 1 0.2243 0.1816 0.4909 11.00000 0.05 0.22 Q6 1 0.2698 0.2753 0.5234 11.00000 0.05 0.22 Q7 1 0.2550 0.2200 0.3566 11.00000 0.05 0.21 Q8 1 0.1996 0.2324 0.5355 11.00000 0.05 0.21 Q9 1 0.3785 0.2223 0.4234 11.00000 0.05 0.20 Q10 1 0.2807 0.3091 0.4566 11.00000 0.05 0.19 Q11 1 0.3277 0.2318 0.6020 11.00000 0.05 0.18 Q12 1 0.1613 0.2269 0.4135 11.00000 0.05 0.18 Q13 1 0.2960 0.1441 0.5045 11.00000 0.05 0.18 Q14 1 0.1818 0.3006 0.8829 11.00000 0.05 0.15 Q15 1 0.2421 0.2629 0.6258 11.00000 0.05 0.14 Q16 1 0.2758 0.0576 0.6058 11.00000 0.05 0.14 Q17 1 0.3435 0.4087 0.4903 11.00000 0.05 0.14 Q18 1 0.4220 0.2263 0.5420 11.00000 0.05 0.14 Q19 1 0.2298 0.2583 0.7319 11.00000 0.05 0.13 Q20 1 0.2358 0.3185 0.8835 11.00000 0.05 0.13 Q21 1 0.2935 0.2861 0.7376 11.00000 0.05 0.13 Q22 1 0.1107 0.3288 0.8153 11.00000 0.05 0.13 Q23 1 0.4178 0.3708 0.5555 11.00000 0.05 0.13 Q24 1 0.2577 0.2661 0.8546 11.00000 0.05 0.13 Q25 1 0.1579 0.1120 0.6790 11.00000 0.05 0.12 ; _shelx_res_checksum 40001 _shelx_hkl_file ; 0 0 -2 5421.98 170.821 0 0 2 5390.25 170.830 0 0 3-0.44798 0.59098 0 0 -3-0.01147 0.72080 0 0 -4 82.2200 2.89886 0 0 4 84.9862 2.90019 0 0 5-0.43413 0.88422 0 0 -5-0.67996 0.81387 0 0 -6 439.834 14.4694 0 0 6 464.350 14.5450 0 0 7 0.19665 1.03329 0 0 -7 1.36165 1.00487 0 0 8 322.245 10.5007 0 0 -8 315.424 10.4011 0 0 9-0.29089 1.46333 0 0 10 109.250 3.97928 0 0 10 92.6683 4.16856 0 0 11-0.15911 1.72053 0 0 12 29.6718 2.28113 0 0 13 1.83758 2.12569 0 0 -14 2.64986 2.11307 0 1 -2 3.72035 0.61847 0 -1 -2 3.16816 0.47463 0 1 2 3.15034 0.43776 0 -1 2 2.42809 0.55146 0 -1 3 13.9353 0.82829 0 1 3 12.3923 0.78787 0 -1 -3 11.2002 0.81437 0 1 -3 14.4734 0.95018 0 -1 4 31.2320 1.30650 0 1 -4 30.0313 1.36032 0 -1 -4 29.5923 1.29289 0 1 4 26.4806 1.26642 0 -1 5 115.894 3.90936 0 1 5 109.456 3.89454 0 1 -5 116.881 3.87706 0 -1 -5 112.261 3.83545 0 -1 6 9.65732 1.03398 0 1 6 11.2481 1.04010 0 -1 -6 11.4894 1.02279 0 1 -6 10.6390 1.02390 0 -1 -7 42.2727 1.86141 0 1 -7 43.3921 1.92231 0 -1 7 43.4552 1.96938 0 1 7 47.7734 1.94976 0 -1 8 262.325 8.31231 0 1 -8 246.738 8.20043 0 -1 -8 249.582 8.16782 0 1 8 259.332 8.26903 0 -1 8 216.624 8.36517 0 -1 9 26.0894 1.78144 0 1 9 21.3666 1.70685 0 -1 9 20.6685 1.93972 0 -1 10 174.033 5.89334 0 1 10 177.395 5.84117 0 1 10 135.534 5.97381 0 1 11 47.5054 2.48240 0 -1 11 48.8341 2.59877 0 1 11 36.1156 2.71300 0 -1 12-1.07672 1.93787 0 1 12-2.24175 1.91925 0 -1 13 25.9147 2.57539 0 1 13 22.2768 2.45787 0 1 -14 43.8572 2.95437 0 -2 1 41.1328 1.26325 0 2 -1 40.6781 1.27157 0 -2 -1 41.5136 1.28821 0 2 2 204.429 6.48255 0 -2 -2 205.692 6.50138 0 -2 2 200.737 6.55813 0 -2 -2 199.569 6.49160 0 2 2 205.952 6.50404 0 -2 -3 10.7761 0.59267 0 2 -3 12.0951 0.87289 0 2 3 9.38606 0.51838 0 -2 -3 11.8643 0.77148 0 2 3 9.65932 0.70215 0 -2 3 11.2952 0.83071 0 -2 -4 140.143 4.56846 0 -2 -4 137.909 4.45801 0 2 4 139.798 4.59612 0 -2 4 135.497 4.64811 0 2 -4 140.769 4.64082 0 2 4 139.672 4.45322 0 -2 -5 756.583 23.3508 0 -2 5 771.646 23.4491 0 2 5 712.610 23.2259 0 2 5 756.819 23.3961 0 2 -5 760.664 23.4034 0 -2 -5 729.658 23.2321 0 -2 6 59.4156 2.12472 0 2 -6 50.1734 2.02029 0 2 6 47.5020 1.61427 0 -2 -6 51.0831 1.92351 0 2 6 56.2681 1.99244 0 -2 -6 49.4748 1.63274 0 -2 7 80.3313 3.43069 0 -2 7 93.5428 3.39053 0 2 7 96.4877 3.30671 0 2 -7 88.4412 3.31834 0 -2 -7 93.6023 3.23250 0 -2 8-1.63770 1.22717 0 2 -8-0.18684 1.16078 0 -2 -8 0.13489 1.02855 0 2 8-1.85266 1.06888 0 -2 9 67.6279 2.91415 0 2 9 66.7554 2.77500 0 -2 -9 64.5021 2.64571 0 -2 10 5.75771 1.68300 0 2 10 9.67013 1.59898 0 2 11 1.73477 1.62128 0 2 11-1.39769 1.90360 0 -2 11-0.95832 1.79736 0 2 12 24.2306 2.47942 0 2 12 33.4960 2.31982 0 -2 12 34.8312 2.52260 0 2 -13 8.47287 2.04830 0 -2 13 2.55413 2.25315 0 -2 14 14.9007 2.68829 0 -3 0-0.33360 0.38204 0 3 0-0.93063 0.35933 0 -3 -1 237.561 7.91842 0 -3 -1 260.179 7.88061 0 -3 1 251.127 7.90760 0 3 -1 246.416 7.90168 0 3 1 245.600 7.88202 0 3 1 239.850 7.91632 0 -3 2 139.413 4.45295 0 3 2 140.862 4.47989 0 3 2 136.712 4.46398 0 -3 -2 141.800 4.46209 0 -3 -2 140.481 4.48871 0 3 -2 139.438 4.45027 0 -3 2 127.089 4.54505 0 -3 3 341.961 12.1117 0 3 -3 382.511 11.9709 0 3 3 379.316 12.0387 0 -3 -3 385.670 12.0116 0 -3 -3 383.374 12.0323 0 3 -3 387.337 12.1025 0 3 3 375.585 12.0038 0 -3 3 371.592 11.9808 0 3 4 28.9833 1.01927 0 -3 -4 26.2091 1.02884 0 3 4 25.8962 1.16412 0 -3 -4 24.5868 1.17446 0 -3 4 27.1233 1.35095 0 3 -4 27.0969 1.36523 0 3 -5 7.52278 1.03193 0 3 5 6.56038 0.49034 0 -3 -5 7.21633 0.53587 0 -3 5 6.65562 1.06094 0 3 5 7.58528 0.83436 0 -3 -5 6.37259 0.81529 0 -3 6 0.44667 0.93866 0 -3 -6 0.40295 0.82665 0 3 6 1.08548 0.33189 0 -3 -6 0.69132 0.38618 0 3 -6 0.02581 0.97795 0 3 6 0.87523 0.80462 0 -3 -7 5.80186 0.95915 0 3 7 5.95896 0.96862 0 3 7 6.09096 0.35184 0 -3 7 6.32648 1.10427 0 -3 -7 5.87800 0.41486 0 3 -7 5.49432 1.15928 0 -3 8 70.9820 2.80479 0 3 8 65.6624 2.66095 0 -3 -8 66.6238 2.57818 0 -3 -9 180.519 6.13448 0 3 9 178.163 6.21295 0 -3 9 187.368 6.36922 0 3 10 206.009 7.03602 0 -3 10 204.406 7.17511 0 3 11 60.9490 2.81351 0 -3 11 60.0638 3.03055 0 3 -12 74.7489 3.57182 0 3 12 75.6611 3.79559 0 -3 12 86.2856 3.75282 0 3 12 88.0632 3.54234 0 3 -13 27.0351 2.39004 0 -3 13 33.1382 2.73920 0 3 13 28.5942 2.83950 0 3 -14 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14 -1 -5 8.81015 2.15894 14 1 -4 34.7022 2.63927 14 -1 -4 34.3185 2.61207 14 1 -4 32.4967 2.64656 14 -1 -4 32.7948 2.65352 14 1 -3 6.47051 2.18889 14 -1 -3 4.59636 1.92171 14 1 -3 9.78848 2.40943 14 1 -2 14.3414 2.24706 14 -1 -2 13.8508 2.09673 14 1 -2 14.4537 2.48106 14 -1 -2 11.5193 2.47025 14 -1 -1 9.00343 2.49244 14 2 -6 1.11658 2.09447 14 2 -5 34.9381 2.59800 14 -2 -5 34.8019 2.50040 14 2 -5 32.6993 2.69387 14 2 -4 5.27056 2.05401 14 -2 -4 9.06541 1.99774 14 2 -4 7.98188 2.27356 14 -2 -4 8.99545 2.16786 14 2 -3 0.07718 2.08424 14 -2 -3 3.71718 2.02958 14 2 -3 2.62404 2.24601 14 -2 -3 1.87315 2.09437 14 -2 -2 4.96263 2.10108 14 2 -2 2.50217 2.35557 14 -2 -2 3.65441 2.28859 14 -2 -1 3.00251 2.32337 14 3 -6 3.58827 2.22750 14 -3 -5 4.39369 1.95222 14 3 -4 0.69674 2.07336 14 -3 -4 1.74128 1.79813 14 3 -4 1.27497 2.11769 14 -3 -4 1.94012 2.04765 14 -3 -3 5.02655 2.07218 14 3 -3 5.15039 2.12471 14 -3 -3 3.97046 2.13784 14 -3 -2-0.21688 2.22878 14 -3 -1 3.75631 2.40447 14 4 -7 2.07885 2.19763 14 4 -5 10.5880 2.31740 14 4 -4-0.79247 2.22120 14 4 -3-0.59432 2.14789 14 -4 -3 2.09091 2.18374 14 4 -2 4.33211 2.30461 14 -4 -2 3.44647 2.32514 14 -4 -1 2.39104 2.44788 14 5 -7 7.57440 2.24171 14 5 -6 9.18041 2.29207 14 5 -5-1.94420 2.24477 14 5 -4-1.90356 2.29723 14 5 -3 6.24715 2.29433 14 -5 -3 8.60745 2.24734 14 -5 -2 8.06715 2.40669 14 -5 -1 22.4926 2.73023 14 6 -7 10.2532 2.33272 14 6 -6 18.0990 2.53029 14 6 -5 2.61624 2.28589 14 6 -4 1.34598 2.23021 14 -6 -2 1.57765 2.27398 14 -6 -1-3.12057 2.44172 14 7 -7 14.4115 2.48500 14 7 -6 3.75357 2.19787 14 7 -5 17.1003 2.39403 14 7 -4 6.12498 2.28147 14 7 -3-3.02322 2.39710 14 -7 -1 27.1450 2.87531 14 8 -8 36.2150 2.83708 14 8 -7 0.80354 2.33618 14 8 -6 4.79371 2.42256 14 8 -5 4.16587 2.30669 14 8 -4 2.53033 2.32881 14 -8 -1 1.81826 2.42200 14 9 -8 5.68645 2.36200 14 9 -7 22.7077 2.58703 14 9 -6 0.98143 2.23138 14 9 -5 0.60660 2.17466 14 10 -7 19.7999 2.47888 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 64107 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 0.15669(9) 0.35782(3) 0.36037(8) 0.0238(2) Uani 1 1 d . . . . . C1 C 0.26334(12) 0.34324(5) 0.43959(11) 0.0199(3) Uani 1 1 d . . . . . N1 N 0.35507(11) 0.37984(4) 0.50727(9) 0.0234(2) Uani 1 1 d . . . . . C2 C 0.33315(14) 0.43970(5) 0.48168(12) 0.0284(3) Uani 1 1 d . . . . . H1 H 0.414774 0.458782 0.538180 0.034 Uiso 1 1 calc R U . . . C3 C 0.21336(16) 0.46128(6) 0.51523(14) 0.0375(4) Uani 1 1 d . . . . . H2 H 0.130303 0.444111 0.461086 0.056 Uiso 1 1 calc R U . . . H3 H 0.207193 0.501291 0.503961 0.056 Uiso 1 1 calc R U . . . H4 H 0.225459 0.452332 0.602257 0.056 Uiso 1 1 calc R U . . . C4 C 0.32523(16) 0.45446(6) 0.34904(13) 0.0345(3) Uani 1 1 d . . . . . H5 H 0.405311 0.440373 0.332772 0.052 Uiso 1 1 calc R U . . . H6 H 0.321135 0.494547 0.339133 0.052 Uiso 1 1 calc R U . . . H7 H 0.244153 0.437927 0.290049 0.052 Uiso 1 1 calc R U . . . C5 C 0.47740(13) 0.36332(6) 0.60983(12) 0.0289(3) Uani 1 1 d . . . . . H8 H 0.471344 0.322700 0.621028 0.035 Uiso 1 1 calc R U . . . C6 C 0.48355(16) 0.39037(6) 0.73281(13) 0.0387(4) Uani 1 1 d . . . . . H9 H 0.493506 0.430263 0.726628 0.058 Uiso 1 1 calc R U . . . H10 H 0.560855 0.375781 0.800005 0.058 Uiso 1 1 calc R U . . . H11 H 0.400253 0.382420 0.750700 0.058 Uiso 1 1 calc R U . . . C7 C 0.60390(15) 0.37370(7) 0.57565(16) 0.0421(4) Uani 1 1 d . . . . . H12 H 0.599639 0.352131 0.501643 0.063 Uiso 1 1 calc R U . . . H13 H 0.683547 0.362732 0.645156 0.063 Uiso 1 1 calc R U . . . H14 H 0.609961 0.412923 0.558137 0.063 Uiso 1 1 calc R U . . . C8 C 0.28747(12) 0.28255(5) 0.46210(11) 0.0198(3) Uani 1 1 d . . . . . C9 C 0.19643(12) 0.23997(5) 0.36937(11) 0.0214(3) Uani 1 1 d . . . . . H15 H 0.126563 0.249530 0.288128 0.026 Uiso 1 1 calc R U . . . C10 C 0.32124(12) 0.20240(5) 0.38423(11) 0.0212(3) Uani 1 1 d . . . . . H16 H 0.343223 0.184562 0.314025 0.025 Uiso 1 1 calc R U . . . C11 C 0.41383(12) 0.24435(5) 0.47807(11) 0.0203(3) Uani 1 1 d . . . . . H17 H 0.504181 0.257185 0.477633 0.024 Uiso 1 1 calc R U . . . C12 C 0.38632(12) 0.21338(5) 0.58816(11) 0.0190(3) Uani 1 1 d . . . . . H18 H 0.456819 0.203363 0.668686 0.023 Uiso 1 1 calc R U . . . C13 C 0.29360(12) 0.17099(5) 0.49307(11) 0.0196(3) Uani 1 1 d . . . . . C14 C 0.16767(12) 0.20922(5) 0.47826(11) 0.0203(3) Uani 1 1 d . . . . . H19 H 0.077026 0.196352 0.477804 0.024 Uiso 1 1 calc R U . . . C15 C 0.26161(12) 0.25099(5) 0.57517(11) 0.0189(3) Uani 1 1 d . . . . . C16 C 0.22916(12) 0.27807(5) 0.67872(11) 0.0192(3) Uani 1 1 d . . . . . C17 C 0.29414(12) 0.26370(5) 0.80043(11) 0.0210(3) Uani 1 1 d . . . . . H20 H 0.362762 0.236439 0.818611 0.025 Uiso 1 1 calc R U . . . C18 C 0.26150(12) 0.28849(5) 0.89984(11) 0.0214(3) Uani 1 1 d . . . . . C19 C 0.32562(13) 0.27322(6) 1.02580(12) 0.0273(3) Uani 1 1 d . . . . . H21 H 0.392364 0.245168 1.045635 0.033 Uiso 1 1 calc R U . . . C20 C 0.29217(14) 0.29856(6) 1.11906(12) 0.0312(3) Uani 1 1 d . . . . . H22 H 0.335806 0.287908 1.203096 0.037 Uiso 1 1 calc R U . . . C21 C 0.19382(14) 0.34021(6) 1.09163(13) 0.0308(3) Uani 1 1 d . . . . . H23 H 0.171957 0.357675 1.157244 0.037 Uiso 1 1 calc R U . . . C22 C 0.12942(14) 0.35574(5) 0.97107(12) 0.0265(3) Uani 1 1 d . . . . . H24 H 0.062801 0.383816 0.953519 0.032 Uiso 1 1 calc R U . . . C23 C 0.16123(12) 0.33032(5) 0.87220(11) 0.0218(3) Uani 1 1 d . . . . . C24 C 0.09556(13) 0.34473(5) 0.74564(12) 0.0227(3) Uani 1 1 d . . . . . H25 H 0.027969 0.372435 0.725760 0.027 Uiso 1 1 calc R U . . . C25 C 0.12790(12) 0.31946(5) 0.65219(11) 0.0216(3) Uani 1 1 d . . . . . H26 H 0.082147 0.329641 0.568221 0.026 Uiso 1 1 calc R U . . . C26 C 0.30273(12) 0.10941(5) 0.50515(11) 0.0210(3) Uani 1 1 d . . . . . O2 O 0.33789(9) 0.08256(4) 0.42920(8) 0.0277(2) Uani 1 1 d . . . . . N2 N 0.27343(10) 0.08563(4) 0.60090(10) 0.0231(2) Uani 1 1 d . . . . . C27 C 0.22959(13) 0.11726(5) 0.69156(12) 0.0244(3) Uani 1 1 d . . . . . H27 H 0.229814 0.156976 0.668571 0.029 Uiso 1 1 calc R U . . . C28 C 0.32715(15) 0.11127(6) 0.82410(12) 0.0322(3) Uani 1 1 d . . . . . H28 H 0.327821 0.072940 0.851058 0.048 Uiso 1 1 calc R U . . . H29 H 0.298232 0.135211 0.879924 0.048 Uiso 1 1 calc R U . . . H30 H 0.418058 0.121824 0.826448 0.048 Uiso 1 1 calc R U . . . C29 C 0.08529(15) 0.10278(6) 0.68189(15) 0.0377(4) Uani 1 1 d . . . . . H31 H 0.025836 0.108140 0.595964 0.057 Uiso 1 1 calc R U . . . H32 H 0.055917 0.126623 0.737573 0.057 Uiso 1 1 calc R U . . . H33 H 0.081285 0.064250 0.705897 0.057 Uiso 1 1 calc R U . . . C30 C 0.28961(14) 0.02525(5) 0.62007(13) 0.0298(3) Uani 1 1 d . . . . . H34 H 0.258216 0.016234 0.691846 0.036 Uiso 1 1 calc R U . . . C31 C 0.43756(15) 0.00871(6) 0.65890(14) 0.0378(4) Uani 1 1 d . . . . . H35 H 0.471752 0.015107 0.589593 0.057 Uiso 1 1 calc R U . . . H36 H 0.446556 -0.030384 0.681291 0.057 Uiso 1 1 calc R U . . . H37 H 0.489598 0.030754 0.730797 0.057 Uiso 1 1 calc R U . . . C32 C 0.20098(15) -0.00761(6) 0.50945(16) 0.0403(4) Uani 1 1 d . . . . . H38 H 0.109194 0.007357 0.482697 0.060 Uiso 1 1 calc R U . . . H39 H 0.199036 -0.046219 0.533692 0.060 Uiso 1 1 calc R U . . . H40 H 0.237640 -0.005124 0.440732 0.060 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 0.0266(5) 0.0244(5) 0.0189(5) 0.0007(4) 0.0055(4) 0.0044(4) C1 0.0244(7) 0.0226(6) 0.0149(6) 0.0006(5) 0.0096(5) 0.0023(5) N1 0.0279(6) 0.0190(5) 0.0207(5) 0.0007(4) 0.0043(4) 0.0008(4) C2 0.0370(8) 0.0180(6) 0.0269(7) -0.0006(5) 0.0060(6) -0.0001(6) C3 0.0538(10) 0.0271(7) 0.0322(8) -0.0044(6) 0.0149(7) 0.0089(7) C4 0.0485(9) 0.0227(7) 0.0342(8) 0.0057(6) 0.0164(7) 0.0006(6) C5 0.0293(7) 0.0236(7) 0.0269(7) 0.0030(5) 0.0000(6) -0.0012(5) C6 0.0480(9) 0.0316(8) 0.0257(8) 0.0001(6) -0.0026(7) -0.0062(7) C7 0.0299(8) 0.0382(8) 0.0521(10) 0.0074(7) 0.0051(7) -0.0025(7) C8 0.0213(6) 0.0206(6) 0.0175(6) -0.0004(5) 0.0065(5) 0.0012(5) C9 0.0236(6) 0.0223(6) 0.0171(6) -0.0012(5) 0.0050(5) 0.0021(5) C10 0.0256(7) 0.0207(6) 0.0187(6) -0.0012(5) 0.0090(5) 0.0014(5) C11 0.0210(6) 0.0197(6) 0.0220(6) 0.0001(5) 0.0092(5) 0.0007(5) C12 0.0203(6) 0.0183(6) 0.0184(6) -0.0008(5) 0.0063(5) -0.0002(5) C13 0.0199(6) 0.0210(6) 0.0187(6) -0.0024(5) 0.0073(5) -0.0002(5) C14 0.0200(6) 0.0195(6) 0.0209(6) -0.0023(5) 0.0063(5) 0.0003(5) C15 0.0203(6) 0.0185(6) 0.0176(6) 0.0003(5) 0.0056(5) 0.0003(5) C16 0.0207(6) 0.0178(6) 0.0204(6) -0.0018(5) 0.0084(5) -0.0035(5) C17 0.0207(6) 0.0203(6) 0.0226(6) 0.0000(5) 0.0077(5) -0.0009(5) C18 0.0215(6) 0.0229(6) 0.0210(6) -0.0012(5) 0.0087(5) -0.0060(5) C19 0.0271(7) 0.0331(7) 0.0220(7) 0.0017(6) 0.0086(5) -0.0043(6) C20 0.0340(8) 0.0412(8) 0.0195(7) -0.0014(6) 0.0103(6) -0.0125(6) C21 0.0396(8) 0.0339(8) 0.0261(7) -0.0108(6) 0.0206(6) -0.0147(6) C22 0.0306(7) 0.0238(7) 0.0312(7) -0.0063(5) 0.0183(6) -0.0076(5) C23 0.0240(6) 0.0200(6) 0.0248(7) -0.0034(5) 0.0128(5) -0.0073(5) C24 0.0236(6) 0.0194(6) 0.0273(7) 0.0001(5) 0.0113(5) 0.0008(5) C25 0.0230(6) 0.0214(6) 0.0203(6) 0.0003(5) 0.0070(5) -0.0010(5) C26 0.0170(6) 0.0217(6) 0.0227(6) -0.0029(5) 0.0045(5) -0.0011(5) O2 0.0338(5) 0.0227(5) 0.0302(5) -0.0065(4) 0.0155(4) 0.0000(4) N2 0.0266(6) 0.0179(5) 0.0273(6) -0.0009(4) 0.0121(5) -0.0007(4) C27 0.0283(7) 0.0207(6) 0.0281(7) -0.0009(5) 0.0144(6) -0.0012(5) C28 0.0420(8) 0.0295(7) 0.0278(7) 0.0021(6) 0.0151(6) -0.0007(6) C29 0.0349(8) 0.0371(8) 0.0488(9) -0.0050(7) 0.0242(7) -0.0042(6) C30 0.0387(8) 0.0178(6) 0.0363(8) 0.0014(6) 0.0170(6) -0.0010(6) C31 0.0433(9) 0.0263(7) 0.0393(9) 0.0021(6) 0.0078(7) 0.0092(6) C32 0.0388(9) 0.0222(7) 0.0588(10) -0.0067(7) 0.0145(7) -0.0071(6) 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 N1 122.14(11) . . ? O1 C1 C8 117.82(11) . . ? N1 C1 C8 120.01(10) . . ? C1 N1 C5 122.86(10) . . ? C1 N1 C2 119.83(10) . . ? C5 N1 C2 117.29(10) . . ? N1 C2 C3 112.05(11) . . ? N1 C2 C4 112.22(11) . . ? C3 C2 C4 112.70(12) . . ? N1 C2 H1 106.4 . . ? C3 C2 H1 106.4 . . ? C4 C2 H1 106.4 . . ? C2 C3 H2 109.5 . . ? C2 C3 H3 109.5 . . ? H2 C3 H3 109.5 . . ? C2 C3 H4 109.5 . . ? H2 C3 H4 109.5 . . ? H3 C3 H4 109.5 . . ? C2 C4 H5 109.5 . . ? C2 C4 H6 109.5 . . ? H5 C4 H6 109.5 . . ? C2 C4 H7 109.5 . . ? H5 C4 H7 109.5 . . ? H6 C4 H7 109.5 . . ? N1 C5 C7 110.97(11) . . ? N1 C5 C6 111.71(11) . . ? C7 C5 C6 112.63(12) . . ? N1 C5 H8 107.1 . . ? C7 C5 H8 107.1 . . ? C6 C5 H8 107.1 . . ? C5 C6 H9 109.5 . . ? C5 C6 H10 109.5 . . ? H9 C6 H10 109.5 . . ? C5 C6 H11 109.5 . . ? H9 C6 H11 109.5 . . ? H10 C6 H11 109.5 . . ? C5 C7 H12 109.5 . . ? C5 C7 H13 109.5 . . ? H12 C7 H13 109.5 . . ? C5 C7 H14 109.5 . . ? H12 C7 H14 109.5 . . ? H13 C7 H14 109.5 . . ? C1 C8 C9 120.25(10) . . ? C1 C8 C11 133.14(10) . . ? C9 C8 C11 89.57(9) . . ? C1 C8 C15 123.01(10) . . ? C9 C8 C15 89.85(9) . . ? C11 C8 C15 89.07(9) . . ? C14 C9 C10 90.49(9) . . ? C14 C9 C8 90.94(9) . . ? C10 C9 C8 90.51(9) . . ? C14 C9 H15 124.8 . . ? C10 C9 H15 124.8 . . ? C8 C9 H15 124.8 . . ? C9 C10 C13 90.21(9) . . ? C9 C10 C11 90.22(9) . . ? C13 C10 C11 90.77(9) . . ? C9 C10 H16 125.0 . . ? C13 C10 H16 125.0 . . ? C11 C10 H16 125.0 . . ? C10 C11 C12 89.76(9) . . ? C10 C11 C8 89.69(9) . . ? C12 C11 C8 90.33(9) . . ? C10 C11 H17 125.3 . . ? C12 C11 H17 125.3 . . ? C8 C11 H17 125.3 . . ? C15 C12 C11 90.70(9) . . ? C15 C12 C13 90.48(9) . . ? C11 C12 C13 90.00(9) . . ? C15 C12 H18 125.0 . . ? C11 C12 H18 125.0 . . ? C13 C12 H18 125.0 . . ? C26 C13 C10 122.45(10) . . ? C26 C13 C12 125.55(10) . . ? C10 C13 C12 89.47(9) . . ? C26 C13 C14 128.44(10) . . ? C10 C13 C14 89.72(9) . . ? C12 C13 C14 89.72(9) . . ? C9 C14 C13 89.58(9) . . ? C9 C14 C15 90.39(9) . . ? C13 C14 C15 89.71(9) . . ? C9 C14 H19 125.3 . . ? C13 C14 H19 125.3 . . ? C15 C14 H19 125.3 . . ? C16 C15 C12 126.03(10) . . ? C16 C15 C14 125.77(10) . . ? C12 C15 C14 90.08(9) . . ? C16 C15 C8 124.83(10) . . ? C12 C15 C8 89.89(8) . . ? C14 C15 C8 88.80(8) . . ? C17 C16 C25 118.89(11) . . ? C17 C16 C15 121.36(11) . . ? C25 C16 C15 119.75(11) . . ? C16 C17 C18 121.71(11) . . ? C16 C17 H20 119.1 . . ? C18 C17 H20 119.1 . . ? C19 C18 C17 122.37(12) . . ? C19 C18 C23 118.78(11) . . ? C17 C18 C23 118.84(11) . . ? C20 C19 C18 120.54(13) . . ? C20 C19 H21 119.7 . . ? C18 C19 H21 119.7 . . ? C19 C20 C21 120.59(13) . . ? C19 C20 H22 119.7 . . ? C21 C20 H22 119.7 . . ? C22 C21 C20 120.41(12) . . ? C22 C21 H23 119.8 . . ? C20 C21 H23 119.8 . . ? C21 C22 C23 120.53(13) . . ? C21 C22 H24 119.7 . . ? C23 C22 H24 119.7 . . ? C22 C23 C24 122.33(12) . . ? C22 C23 C18 119.14(12) . . ? C24 C23 C18 118.52(11) . . ? C25 C24 C23 121.11(12) . . ? C25 C24 H25 119.4 . . ? C23 C24 H25 119.4 . . ? C24 C25 C16 120.90(11) . . ? C24 C25 H26 119.5 . . ? C16 C25 H26 119.5 . . ? O2 C26 N2 122.51(11) . . ? O2 C26 C13 119.21(11) . . ? N2 C26 C13 118.27(10) . . ? C26 N2 C27 123.02(10) . . ? C26 N2 C30 119.62(10) . . ? C27 N2 C30 117.32(10) . . ? N2 C27 C29 111.12(11) . . ? N2 C27 C28 112.24(11) . . ? C29 C27 C28 112.20(11) . . ? N2 C27 H27 107.0 . . ? C29 C27 H27 107.0 . . ? C28 C27 H27 107.0 . . ? C27 C28 H28 109.5 . . ? C27 C28 H29 109.5 . . ? H28 C28 H29 109.5 . . ? C27 C28 H30 109.5 . . ? H28 C28 H30 109.5 . . ? H29 C28 H30 109.5 . . ? C27 C29 H31 109.5 . . ? C27 C29 H32 109.5 . . ? H31 C29 H32 109.5 . . ? C27 C29 H33 109.5 . . ? H31 C29 H33 109.5 . . ? H32 C29 H33 109.5 . . ? N2 C30 C32 112.81(11) . . ? N2 C30 C31 111.10(11) . . ? C32 C30 C31 112.91(12) . . ? N2 C30 H34 106.5 . . ? C32 C30 H34 106.5 . . ? C31 C30 H34 106.5 . . ? C30 C31 H35 109.5 . . ? C30 C31 H36 109.5 . . ? H35 C31 H36 109.5 . . ? C30 C31 H37 109.5 . . ? H35 C31 H37 109.5 . . ? H36 C31 H37 109.5 . . ? C30 C32 H38 109.5 . . ? C30 C32 H39 109.5 . . ? H38 C32 H39 109.5 . . ? C30 C32 H40 109.5 . . ? H38 C32 H40 109.5 . . ? H39 C32 H40 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 1.2359(15) . ? C1 N1 1.3503(16) . ? C1 C8 1.5038(17) . ? N1 C5 1.4784(16) . ? N1 C2 1.4866(16) . ? C2 C3 1.522(2) . ? C2 C4 1.5260(19) . ? C2 H1 1.0000 . ? C3 H2 0.9800 . ? C3 H3 0.9800 . ? C3 H4 0.9800 . ? C4 H5 0.9800 . ? C4 H6 0.9800 . ? C4 H7 0.9800 . ? C5 C7 1.522(2) . ? C5 C6 1.528(2) . ? C5 H8 1.0000 . ? C6 H9 0.9800 . ? C6 H10 0.9800 . ? C6 H11 0.9800 . ? C7 H12 0.9800 . ? C7 H13 0.9800 . ? C7 H14 0.9800 . ? C8 C9 1.5600(17) . ? C8 C11 1.5798(16) . ? C8 C15 1.5954(16) . ? C9 C14 1.5586(17) . ? C9 C10 1.5598(17) . ? C9 H15 1.0000 . ? C10 C13 1.5605(17) . ? C10 C11 1.5623(17) . ? C10 H16 1.0000 . ? C11 C12 1.5670(16) . ? C11 H17 1.0000 . ? C12 C15 1.5633(16) . ? C12 C13 1.5766(16) . ? C12 H18 1.0000 . ? C13 C26 1.5029(17) . ? C13 C14 1.5788(16) . ? C14 C15 1.5821(16) . ? C14 H19 1.0000 . ? C15 C16 1.4832(16) . ? C16 C17 1.3721(17) . ? C16 C25 1.4217(17) . ? C17 C18 1.4189(17) . ? C17 H20 0.9500 . ? C18 C19 1.4174(18) . ? C18 C23 1.4222(18) . ? C19 C20 1.3684(19) . ? C19 H21 0.9500 . ? C20 C21 1.406(2) . ? C20 H22 0.9500 . ? C21 C22 1.368(2) . ? C21 H23 0.9500 . ? C22 C23 1.4158(17) . ? C22 H24 0.9500 . ? C23 C24 1.4202(18) . ? C24 C25 1.3635(17) . ? C24 H25 0.9500 . ? C25 H26 0.9500 . ? C26 O2 1.2320(15) . ? C26 N2 1.3545(16) . ? N2 C27 1.4758(16) . ? N2 C30 1.4848(16) . ? C27 C29 1.5235(19) . ? C27 C28 1.5255(19) . ? C27 H27 1.0000 . ? C28 H28 0.9800 . ? C28 H29 0.9800 . ? C28 H30 0.9800 . ? C29 H31 0.9800 . ? C29 H32 0.9800 . ? C29 H33 0.9800 . ? C30 C32 1.522(2) . ? C30 C31 1.522(2) . ? C30 H34 1.0000 . ? C31 H35 0.9800 . ? C31 H36 0.9800 . ? C31 H37 0.9800 . ? C32 H38 0.9800 . ? C32 H39 0.9800 . ? C32 H40 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 N1 C5 174.51(11) . . . . ? C8 C1 N1 C5 -3.68(17) . . . . ? O1 C1 N1 C2 -3.97(18) . . . . ? C8 C1 N1 C2 177.84(11) . . . . ? C1 N1 C2 C3 67.33(15) . . . . ? C5 N1 C2 C3 -111.24(13) . . . . ? C1 N1 C2 C4 -60.64(16) . . . . ? C5 N1 C2 C4 120.80(13) . . . . ? C1 N1 C5 C7 111.52(14) . . . . ? C2 N1 C5 C7 -69.96(15) . . . . ? C1 N1 C5 C6 -121.89(13) . . . . ? C2 N1 C5 C6 56.63(15) . . . . ? O1 C1 C8 C9 12.91(16) . . . . ? N1 C1 C8 C9 -168.83(11) . . . . ? O1 C1 C8 C11 135.24(13) . . . . ? N1 C1 C8 C11 -46.50(18) . . . . ? O1 C1 C8 C15 -99.14(13) . . . . ? N1 C1 C8 C15 79.13(15) . . . . ? C1 C8 C9 C14 -127.96(11) . . . . ? C11 C8 C9 C14 90.10(9) . . . . ? C15 C8 C9 C14 1.03(9) . . . . ? C1 C8 C9 C10 141.54(11) . . . . ? C11 C8 C9 C10 -0.40(9) . . . . ? C15 C8 C9 C10 -89.47(9) . . . . ? C14 C9 C10 C13 0.23(9) . . . . ? C8 C9 C10 C13 91.17(9) . . . . ? C14 C9 C10 C11 -90.54(9) . . . . ? C8 C9 C10 C11 0.40(9) . . . . ? C9 C10 C11 C12 89.94(9) . . . . ? C13 C10 C11 C12 -0.28(9) . . . . ? C9 C10 C11 C8 -0.40(9) . . . . ? C13 C10 C11 C8 -90.61(9) . . . . ? C1 C8 C11 C10 -132.73(13) . . . . ? C9 C8 C11 C10 0.40(9) . . . . ? C15 C8 C11 C10 90.25(9) . . . . ? C1 C8 C11 C12 137.52(13) . . . . ? C9 C8 C11 C12 -89.36(9) . . . . ? C15 C8 C11 C12 0.50(9) . . . . ? C10 C11 C12 C15 -90.20(9) . . . . ? C8 C11 C12 C15 -0.51(9) . . . . ? C10 C11 C12 C13 0.27(9) . . . . ? C8 C11 C12 C13 89.97(9) . . . . ? C9 C10 C13 C26 136.97(11) . . . . ? C11 C10 C13 C26 -132.81(11) . . . . ? C9 C10 C13 C12 -89.95(9) . . . . ? C11 C10 C13 C12 0.27(9) . . . . ? C9 C10 C13 C14 -0.22(9) . . . . ? C11 C10 C13 C14 90.00(9) . . . . ? C15 C12 C13 C26 -138.81(12) . . . . ? C11 C12 C13 C26 130.49(12) . . . . ? C15 C12 C13 C10 90.43(9) . . . . ? C11 C12 C13 C10 -0.27(9) . . . . ? C15 C12 C13 C14 0.70(9) . . . . ? C11 C12 C13 C14 -89.99(9) . . . . ? C10 C9 C14 C13 -0.22(9) . . . . ? C8 C9 C14 C13 -90.74(9) . . . . ? C10 C9 C14 C15 89.48(9) . . . . ? C8 C9 C14 C15 -1.04(9) . . . . ? C26 C13 C14 C9 -132.71(12) . . . . ? C10 C13 C14 C9 0.22(9) . . . . ? C12 C13 C14 C9 89.70(9) . . . . ? C26 C13 C14 C15 136.89(12) . . . . ? C10 C13 C14 C15 -90.17(9) . . . . ? C12 C13 C14 C15 -0.70(9) . . . . ? C11 C12 C15 C16 -134.32(11) . . . . ? C13 C12 C15 C16 135.67(12) . . . . ? C11 C12 C15 C14 89.31(9) . . . . ? C13 C12 C15 C14 -0.70(9) . . . . ? C11 C12 C15 C8 0.51(9) . . . . ? C13 C12 C15 C8 -89.50(8) . . . . ? C9 C14 C15 C16 134.57(12) . . . . ? C13 C14 C15 C16 -135.85(12) . . . . ? C9 C14 C15 C12 -88.88(9) . . . . ? C13 C14 C15 C12 0.70(9) . . . . ? C9 C14 C15 C8 1.01(9) . . . . ? C13 C14 C15 C8 90.59(9) . . . . ? C1 C8 C15 C16 -8.45(17) . . . . ? C9 C8 C15 C16 -135.26(11) . . . . ? C11 C8 C15 C16 135.17(11) . . . . ? C1 C8 C15 C12 -144.12(11) . . . . ? C9 C8 C15 C12 89.07(9) . . . . ? C11 C8 C15 C12 -0.50(9) . . . . ? C1 C8 C15 C14 125.80(11) . . . . ? C9 C8 C15 C14 -1.01(9) . . . . ? C11 C8 C15 C14 -90.59(9) . . . . ? C12 C15 C16 C17 -12.84(18) . . . . ? C14 C15 C16 C17 108.92(14) . . . . ? C8 C15 C16 C17 -133.06(12) . . . . ? C12 C15 C16 C25 167.77(11) . . . . ? C14 C15 C16 C25 -70.48(16) . . . . ? C8 C15 C16 C25 47.55(16) . . . . ? C25 C16 C17 C18 0.89(18) . . . . ? C15 C16 C17 C18 -178.51(11) . . . . ? C16 C17 C18 C19 178.58(12) . . . . ? C16 C17 C18 C23 -1.68(18) . . . . ? C17 C18 C19 C20 179.32(12) . . . . ? C23 C18 C19 C20 -0.42(18) . . . . ? C18 C19 C20 C21 -0.1(2) . . . . ? C19 C20 C21 C22 0.5(2) . . . . ? C20 C21 C22 C23 -0.30(19) . . . . ? C21 C22 C23 C24 179.18(12) . . . . ? C21 C22 C23 C18 -0.22(18) . . . . ? C19 C18 C23 C22 0.57(17) . . . . ? C17 C18 C23 C22 -179.18(11) . . . . ? C19 C18 C23 C24 -178.85(11) . . . . ? C17 C18 C23 C24 1.40(17) . . . . ? C22 C23 C24 C25 -179.80(12) . . . . ? C18 C23 C24 C25 -0.40(18) . . . . ? C23 C24 C25 C16 -0.40(18) . . . . ? C17 C16 C25 C24 0.16(18) . . . . ? C15 C16 C25 C24 179.57(11) . . . . ? C10 C13 C26 O2 2.63(17) . . . . ? C12 C13 C26 O2 -113.54(13) . . . . ? C14 C13 C26 O2 122.45(13) . . . . ? C10 C13 C26 N2 -178.24(10) . . . . ? C12 C13 C26 N2 65.59(16) . . . . ? C14 C13 C26 N2 -58.42(17) . . . . ? O2 C26 N2 C27 -179.21(11) . . . . ? C13 C26 N2 C27 1.69(17) . . . . ? O2 C26 N2 C30 2.86(18) . . . . ? C13 C26 N2 C30 -176.24(11) . . . . ? C26 N2 C27 C29 114.75(13) . . . . ? C30 N2 C27 C29 -67.28(15) . . . . ? C26 N2 C27 C28 -118.71(13) . . . . ? C30 N2 C27 C28 59.26(14) . . . . ? C26 N2 C30 C32 -60.56(16) . . . . ? C27 N2 C30 C32 121.39(13) . . . . ? C26 N2 C30 C31 67.39(15) . . . . ? C27 N2 C30 C31 -110.66(13) . . . . ?