#------------------------------------------------------------------------------ #$Date: 2020-05-14 02:50:20 +0300 (Thu, 14 May 2020) $ #$Revision: 252032 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/65/7126532.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_7126532 loop_ _publ_author_name 'Gao, Yuqi' 'Hou, Yi' 'Zhu, Liming' 'Chen, Junhan' 'Li, Ruoxin' 'Zhang, Shengyong' 'He, Yu-Peng' 'Xie, Weiqing' _publ_section_title ; Visible-Light Driven Synthesis of Polycyclic Benzo[d][1,3]oxazocine From 2-Aminochalcone via Tandem Aromatization/Dearomatization Process ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D0CC02416C _journal_year 2020 _chemical_formula_moiety 'C28 H23 N O2' _chemical_formula_sum 'C28 H23 N O2' _chemical_formula_weight 405.47 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-03-30 deposited with the CCDC. 2020-05-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.242(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.1842(6) _cell_length_b 20.0153(11) _cell_length_c 10.5231(6) _cell_measurement_reflns_used 2054 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 44.90 _cell_measurement_theta_min 4.42 _cell_volume 2136.1(2) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.963 _diffrn_measured_fraction_theta_max 0.943 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.1281 _diffrn_reflns_av_unetI/netI 0.1343 _diffrn_reflns_Laue_measured_fraction_full 0.963 _diffrn_reflns_Laue_measured_fraction_max 0.943 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 17833 _diffrn_reflns_point_group_measured_fraction_full 0.963 _diffrn_reflns_point_group_measured_fraction_max 0.943 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 73.078 _diffrn_reflns_theta_min 4.418 _exptl_absorpt_coefficient_mu 0.620 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.261 _exptl_crystal_description sheet _exptl_crystal_F_000 856 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.200 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.058 _refine_ls_extinction_coef 0.0059(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 285 _refine_ls_number_reflns 4023 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.948 _refine_ls_R_factor_all 0.2382 _refine_ls_R_factor_gt 0.0880 _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^)+(0.1483P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2222 _refine_ls_wR_factor_ref 0.3359 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1318 _reflns_number_total 4023 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cc02416c2.cif _cod_data_source_block 660 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7126532 _shelx_shelxl_version_number 2018/3 _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 0.876 _shelx_estimated_absorpt_t_max 0.952 _shelx_res_file ; TITL 660 in P2(1)/n 660.res created by SHELXL-2018/3 at 16:50:56 on 26-Mar-2020 CELL 1.54178 10.1842 20.0153 10.5231 90.000 95.242 90.000 ZERR 4.00 0.0006 0.0011 0.0006 0.000 0.004 0.000 LATT 1 SYMM -x+1/2, y+1/2, -z+1/2 SFAC C H N O UNIT 112 92 4 8 TEMP 20.000 ACTA L.S. 4 FMAP 2 PLAN 5 SIZE 0.08 0.16 0.22 HTAB BOND $H CONF WGHT 0.148300 EXTI 0.005895 FVAR 0.67587 O1 4 0.404082 0.729006 0.447394 11.00000 0.08009 0.07058 = 0.10950 0.01087 0.00501 -0.00559 O2 4 0.191961 0.529064 0.532942 11.00000 0.10524 0.08579 = 0.19241 0.01753 0.01553 -0.01342 N1 3 0.593273 0.737782 0.333293 11.00000 0.08087 0.06544 = 0.08439 -0.00746 0.00522 0.00920 C1 1 0.850430 0.630266 0.499531 11.00000 0.07717 0.06948 = 0.08880 0.00121 0.00254 -0.00735 AFIX 43 H1A 2 0.874950 0.613761 0.580861 11.00000 -1.20000 AFIX 0 C2 1 0.923415 0.613985 0.398807 11.00000 0.07586 0.07128 = 0.12345 0.00954 0.01135 -0.00018 AFIX 43 H2B 2 0.995298 0.585400 0.412582 11.00000 -1.20000 AFIX 0 C3 1 0.890638 0.639651 0.278810 11.00000 0.08766 0.08543 = 0.11565 0.00021 0.03178 -0.00459 AFIX 43 H3A 2 0.940158 0.628789 0.211733 11.00000 -1.20000 AFIX 0 C4 1 0.784136 0.681405 0.259404 11.00000 0.09024 0.07134 = 0.08762 0.00099 0.01733 0.00006 AFIX 43 H4A 2 0.763490 0.699273 0.178461 11.00000 -1.20000 AFIX 0 C5 1 0.706667 0.697895 0.354909 11.00000 0.07646 0.06694 = 0.07746 -0.00423 0.00648 -0.00094 C6 1 0.525521 0.765997 0.435985 11.00000 0.07665 0.06117 = 0.09299 -0.00417 0.00019 -0.00605 C7 1 0.611441 0.761793 0.562801 11.00000 0.08747 0.07659 = 0.07938 -0.00633 0.00529 0.00021 AFIX 23 H7A 2 0.688734 0.789942 0.560611 11.00000 -1.20000 H7B 2 0.562209 0.776450 0.632396 11.00000 -1.20000 AFIX 0 C8 1 0.652083 0.688686 0.580952 11.00000 0.08260 0.07804 = 0.07938 -0.00329 0.00128 -0.00135 AFIX 13 H8A 2 0.700637 0.682929 0.665016 11.00000 -1.20000 AFIX 0 C9 1 0.740492 0.671355 0.478383 11.00000 0.07641 0.06294 = 0.07972 -0.00323 0.00443 -0.00423 C10 1 0.531481 0.644274 0.570836 11.00000 0.09322 0.07179 = 0.06627 0.00421 0.02007 0.00790 C11 1 0.531519 0.581212 0.621180 11.00000 0.10958 0.07097 = 0.07046 0.00829 0.01552 0.01061 AFIX 43 H11A 2 0.609086 0.564768 0.663307 11.00000 -1.20000 AFIX 0 C12 1 0.419749 0.540719 0.611707 11.00000 0.11989 0.06478 = 0.08022 0.00473 0.02156 -0.00059 AFIX 43 H12A 2 0.421823 0.498005 0.646619 11.00000 -1.20000 AFIX 0 C13 1 0.304951 0.566424 0.548196 11.00000 0.09253 0.07312 = 0.10917 0.00496 0.02024 -0.00465 C14 1 0.302879 0.628606 0.496535 11.00000 0.08187 0.07171 = 0.11602 0.00367 0.00318 0.00234 AFIX 43 H14A 2 0.225528 0.645007 0.453918 11.00000 -1.20000 AFIX 0 C15 1 0.414488 0.667341 0.506972 11.00000 0.08555 0.07108 = 0.09064 0.00955 0.02122 0.00431 C16 1 0.539595 0.751395 0.201964 11.00000 0.11698 0.07587 = 0.08225 -0.00005 -0.00672 0.01085 AFIX 23 H16A 2 0.605676 0.775204 0.158919 11.00000 -1.20000 H16B 2 0.464023 0.780716 0.204331 11.00000 -1.20000 AFIX 0 C17 1 0.497598 0.690384 0.123879 11.00000 0.08546 0.06314 = 0.07567 -0.00108 0.00230 0.01158 C18 1 0.464238 0.631624 0.176805 11.00000 0.11678 0.07374 = 0.08158 -0.00210 0.00565 0.00246 AFIX 43 H18A 2 0.470657 0.627651 0.265208 11.00000 -1.20000 AFIX 0 C19 1 0.421302 0.577956 0.103248 11.00000 0.12474 0.08372 = 0.09899 -0.00985 -0.00605 -0.00592 AFIX 43 H19A 2 0.399035 0.538076 0.141233 11.00000 -1.20000 AFIX 0 C20 1 0.411731 0.583933 -0.026512 11.00000 0.11138 0.08468 = 0.11834 -0.02602 -0.00315 -0.00574 AFIX 43 H20A 2 0.383056 0.547612 -0.076735 11.00000 -1.20000 AFIX 0 C21 1 0.443263 0.641891 -0.083780 11.00000 0.11746 0.11639 = 0.07607 -0.03020 -0.00196 0.02460 AFIX 43 H21A 2 0.434994 0.645491 -0.172261 11.00000 -1.20000 AFIX 0 C22 1 0.487757 0.695383 -0.008825 11.00000 0.10280 0.08529 = 0.07295 0.00415 0.01835 0.01661 AFIX 43 H22A 2 0.511288 0.734964 -0.047098 11.00000 -1.20000 AFIX 0 C23 1 0.482244 0.837004 0.406174 11.00000 0.08483 0.06220 = 0.08798 -0.00192 0.00208 0.00218 C24 1 0.355923 0.858804 0.423238 11.00000 0.09234 0.07330 = 0.09525 0.00662 0.01180 0.00948 AFIX 43 H24A 2 0.293999 0.829280 0.450861 11.00000 -1.20000 AFIX 0 C25 1 0.322344 0.925703 0.398510 11.00000 0.10954 0.07909 = 0.09084 -0.00471 0.00427 0.02564 AFIX 43 H25A 2 0.237782 0.940032 0.411674 11.00000 -1.20000 AFIX 0 C26 1 0.408535 0.970443 0.356050 11.00000 0.12203 0.07867 = 0.12511 0.00135 -0.00177 0.01597 AFIX 43 H26A 2 0.383674 1.014416 0.338317 11.00000 -1.20000 AFIX 0 C27 1 0.534280 0.948350 0.340154 11.00000 0.12473 0.06275 = 0.13398 -0.00496 0.00523 -0.01547 AFIX 43 H27A 2 0.595894 0.978016 0.312427 11.00000 -1.20000 AFIX 0 C28 1 0.569939 0.882473 0.365000 11.00000 0.09206 0.06715 = 0.11860 -0.00866 0.00970 -0.00779 AFIX 43 H28A 2 0.655295 0.868756 0.353502 11.00000 -1.20000 AFIX 0 H2A 2 0.211974 0.498133 0.538549 11.00000 0.20112 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM 660 in P2(1)/n REM wR2 = 0.3359, GooF = S = 0.948, Restrained GooF = 0.948 for all data REM R1 = 0.0880 for 1318 Fo > 4sig(Fo) and 0.2382 for all 4023 data REM 285 parameters refined using 0 restraints END WGHT 0.1485 0.0000 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.200, deepest hole -0.264, 1-sigma level 0.058 Q1 1 0.8005 0.7997 0.4659 11.00000 0.05 0.20 Q2 1 0.4681 0.8421 0.3593 11.00000 0.05 0.20 Q3 1 0.7731 0.8171 0.4872 11.00000 0.05 0.20 Q4 1 0.6184 0.9461 0.4213 11.00000 0.05 0.20 Q5 1 0.9254 0.5678 0.3750 11.00000 0.05 0.20 ; _shelx_res_checksum 36699 _shelx_hkl_file ; 1 0 0 0.20 1.70 -1 0 0 -2.30 2.80 -1 0 0 2.20 1.90 1 0 0 -3.10 2.10 1 0 0 -0.60 1.70 2 0 0 6656.23 145.79 2 0 0 6326.47 131.39 -2 0 0 6719.03 152.18 2 0 0 6794.42 148.99 -3 0 0 2.00 6.20 3 0 0 -4.20 3.80 3 0 0 -1.50 4.50 3 0 0 -0.60 7.20 4 0 0 5.40 7.00 4 0 0 8.30 5.30 -4 0 0 -7.00 12.30 -4 0 0 18.70 11.00 5 0 0 -11.00 7.40 5 0 0 -3.50 6.20 5 0 0 -8.30 9.80 6 0 0 115.39 19.60 6 0 0 93.79 25.60 6 0 0 112.49 24.00 6 0 0 139.89 33.10 -7 0 0 5.30 5.70 -7 0 0 26.20 9.00 -7 0 0 -1.90 8.90 7 0 0 31.30 24.90 7 0 0 -12.40 16.50 -8 0 0 28.30 8.10 -8 0 0 18.80 8.30 -8 0 0 12.20 7.00 -9 0 0 3.70 7.40 -9 0 0 0.50 6.30 -9 0 0 5.40 5.00 -10 0 0 14.10 11.20 -10 0 0 41.70 9.40 -10 0 0 40.40 10.00 -11 0 0 7.10 5.70 -11 0 0 -1.10 2.80 -11 0 0 1.20 8.20 -12 0 0 4.10 4.60 -12 0 0 3.20 2.60 0 -1 0 -2.40 2.80 0 -1 0 0.60 1.30 0 1 0 0.20 1.00 -1 -1 0 254.97 22.90 -1 -1 0 240.68 17.50 1 -1 0 225.48 14.40 -1 1 0 232.48 14.90 -1 1 0 227.78 22.00 1 1 0 242.58 17.70 1 1 0 247.68 21.80 1 1 0 249.18 8.50 2 -1 0 966.10 43.30 -2 -1 0 1003.30 53.49 -2 -1 0 1008.80 45.20 2 1 0 1005.10 52.09 -2 1 0 992.20 45.10 -2 1 0 981.00 55.09 2 1 0 967.20 44.40 -2 1 0 971.40 51.79 3 -1 0 971.60 37.60 3 -1 0 970.10 53.29 -3 -1 0 1002.50 59.89 3 1 0 988.90 57.59 -3 1 0 955.90 61.59 3 1 0 1003.80 52.29 -3 1 0 952.80 58.19 3 1 0 888.11 54.19 4 -1 0 29.90 11.30 4 -1 0 23.40 10.50 -4 -1 0 21.20 15.30 4 -1 0 30.60 8.80 4 1 0 13.00 6.50 4 1 0 45.90 14.40 4 1 0 40.80 10.40 4 1 0 24.50 14.70 -4 1 0 27.30 11.70 -4 1 0 16.40 14.50 5 -1 0 -8.80 7.50 5 -1 0 -3.30 5.30 5 -1 0 -21.00 10.60 5 1 0 7.90 7.00 5 1 0 4.10 7.90 5 1 0 -11.00 8.60 5 1 0 6.60 10.60 6 -1 0 12.30 26.20 6 -1 0 43.30 20.50 7 -1 0 28.80 25.50 -7 -1 0 26.10 9.60 -7 -1 0 20.30 7.50 7 -1 0 3.40 23.20 7 1 0 24.90 24.80 -7 1 0 47.80 12.90 -7 1 0 21.30 8.30 -7 1 0 20.00 11.20 -8 -1 0 16.30 7.80 -8 -1 0 10.10 9.20 -8 1 0 10.50 7.80 -8 1 0 20.10 8.80 -8 1 0 17.10 10.60 -9 -1 0 5.20 4.10 -9 -1 0 -5.90 6.30 -9 -1 0 0.00 4.80 -9 1 0 15.60 7.70 -9 1 0 -5.60 5.40 -9 1 0 0.60 4.20 -10 -1 0 12.40 7.20 -10 -1 0 -2.60 4.20 -10 -1 0 7.30 7.40 -10 1 0 -4.30 5.70 -10 1 0 7.20 6.00 -10 1 0 -0.70 6.40 -11 -1 0 4.40 4.20 -11 -1 0 0.00 3.00 -11 -1 0 -4.00 5.00 -11 1 0 0.40 4.80 -11 1 0 5.40 3.40 -12 -1 0 0.60 1.90 -12 -1 0 0.40 3.10 -12 1 0 1.30 4.20 -12 1 0 1.60 3.60 0 -2 0 3333.27 71.69 0 -2 0 3155.58 69.49 0 -2 0 3366.26 77.89 0 2 0 3265.37 76.39 0 2 0 3547.94 71.49 0 2 0 3079.39 111.49 0 2 0 3578.24 71.79 -1 -2 0 550.04 43.60 -1 -2 0 527.55 31.70 -1 -2 0 555.34 18.30 -1 -2 0 516.85 23.40 1 -2 0 531.95 23.90 1 -2 0 547.15 27.80 1 -2 0 591.24 46.30 1 -2 0 560.24 19.00 1 2 0 554.04 17.50 1 2 0 517.45 42.60 1 2 0 564.24 23.80 1 2 0 537.75 31.80 -1 2 0 557.64 25.20 -1 2 0 544.45 17.30 -2 -2 0 823.32 46.60 -2 -2 0 770.12 56.29 2 -2 0 807.02 38.20 -2 2 0 630.64 42.60 2 2 0 778.42 54.49 -2 2 0 792.32 57.59 -2 2 0 761.22 52.99 2 2 0 744.03 36.70 2 2 0 816.22 45.90 3 -2 0 758.22 45.90 3 -2 0 809.42 47.10 -3 -2 0 795.32 62.69 -3 -2 0 773.22 51.59 -3 2 0 788.02 49.80 3 2 0 823.52 51.99 -3 2 0 769.82 62.89 3 2 0 810.32 61.89 -3 2 0 767.12 59.09 3 2 0 781.02 29.80 -4 -2 0 157.78 33.20 4 -2 0 165.18 23.40 4 -2 0 166.78 24.50 4 2 0 160.18 25.10 -4 2 0 199.98 35.90 -4 2 0 152.98 32.30 4 2 0 155.48 32.20 5 -2 0 294.07 38.10 5 -2 0 311.27 40.80 5 2 0 401.76 41.90 -5 2 0 336.77 45.30 -5 2 0 287.57 47.50 5 2 0 335.27 45.80 6 -2 0 -2.30 12.40 6 -2 0 -0.90 11.80 6 2 0 17.20 19.10 6 2 0 -19.90 11.10 -7 -2 0 1.00 5.00 7 -2 0 11.80 24.70 -7 -2 0 15.10 6.30 7 -2 0 14.50 25.20 7 -2 0 4.90 24.10 -7 -2 0 5.20 5.70 7 2 0 -6.10 24.50 -7 2 0 -0.80 5.90 -7 2 0 1.80 6.00 7 2 0 25.60 31.30 -8 -2 0 84.69 17.70 -8 -2 0 111.49 15.60 -8 -2 0 111.89 16.80 -8 2 0 104.49 14.90 -8 2 0 96.39 16.40 -8 2 0 62.79 14.10 -9 -2 0 76.69 13.80 -9 2 0 45.40 10.80 -9 2 0 34.60 9.30 -10 -2 0 1.10 3.70 -10 -2 0 4.70 5.90 -10 -2 0 1.90 4.50 -10 2 0 5.50 6.60 -10 2 0 7.80 6.10 -11 -2 0 -1.20 4.90 -11 -2 0 2.80 3.90 -11 -2 0 0.10 4.00 -11 2 0 1.50 2.60 -11 2 0 0.90 5.00 -12 -2 0 0.60 4.10 -12 -2 0 -1.60 2.00 -12 2 0 8.30 5.60 -12 2 0 3.00 2.60 0 -3 0 1.50 2.30 0 -3 0 0.60 3.30 0 -3 0 -2.20 5.30 0 -3 0 -0.80 2.30 0 3 0 -2.60 3.80 0 3 0 -0.60 1.50 0 3 0 5.70 7.10 0 3 0 -1.70 2.20 -1 -3 0 1261.87 41.80 -1 -3 0 1180.08 58.39 -1 -3 0 1295.87 38.60 1 -3 0 1284.77 42.80 1 -3 0 1261.07 41.20 -1 -3 0 1323.27 84.19 1 -3 0 1280.67 82.39 1 -3 0 1205.18 49.60 1 3 0 1309.17 43.30 1 3 0 1292.77 81.79 1 3 0 1236.68 56.39 -1 3 0 1258.17 44.30 -1 3 0 1259.77 83.19 -1 3 0 1244.48 38.50 2 -3 0 6035.20 147.09 -2 -3 0 5828.62 161.38 2 -3 0 6258.97 135.79 -2 -3 0 6096.99 201.88 2 3 0 6296.27 149.79 -2 3 0 5512.35 198.28 2 3 0 6099.89 200.58 2 3 0 6183.68 161.88 -2 3 0 6524.85 144.99 3 -3 0 260.97 28.60 -3 -3 0 227.58 31.30 3 -3 0 207.68 23.90 -3 -3 0 162.78 35.00 3 -3 0 240.88 30.40 3 3 0 286.37 41.40 3 3 0 233.18 30.60 -3 3 0 211.88 35.80 -3 3 0 200.48 26.10 -3 3 0 271.37 43.80 3 3 0 210.18 24.10 4 -3 0 56.49 17.50 -4 -3 0 30.40 22.90 4 -3 0 33.00 13.50 4 -3 0 46.10 17.80 -4 3 0 34.50 21.40 4 3 0 40.40 25.70 4 3 0 48.90 19.20 4 3 0 49.90 19.90 -4 3 0 61.59 25.10 4 3 0 37.50 14.80 5 -3 0 361.66 44.20 -5 -3 0 376.76 51.39 5 -3 0 348.77 41.20 5 3 0 380.46 57.39 5 3 0 342.17 46.50 -5 3 0 509.25 66.49 -5 3 0 388.16 58.19 5 3 0 331.77 42.10 6 -3 0 -27.10 12.90 6 3 0 3.80 18.10 6 3 0 34.10 18.70 7 -3 0 60.59 28.60 -7 -3 0 51.89 14.10 7 -3 0 21.20 24.60 -7 -3 0 22.70 8.30 -7 -3 0 21.70 7.80 -7 3 0 21.30 7.90 7 3 0 -27.10 25.40 7 3 0 -1.10 24.60 -7 3 0 26.70 11.70 -8 -3 0 -10.40 12.50 -8 -3 0 6.00 6.90 -8 -3 0 17.20 7.20 -8 3 0 7.60 5.20 -9 -3 0 -1.30 4.00 -9 -3 0 6.00 4.90 -9 -3 0 0.70 6.20 -9 3 0 0.50 3.80 -9 3 0 8.50 6.50 -10 -3 0 -1.00 4.60 -10 -3 0 4.00 4.30 -10 3 0 8.60 7.50 -10 3 0 8.50 4.30 -11 -3 0 8.60 4.70 -11 -3 0 0.60 4.10 -11 -3 0 8.80 5.20 -11 3 0 5.50 5.60 -12 -3 0 3.40 4.90 -12 -3 0 1.90 2.20 -12 3 0 4.10 2.80 -12 3 0 -1.60 3.10 0 -4 0 1392.66 50.89 0 -4 0 1403.66 99.39 0 4 0 1290.77 95.69 0 4 0 1382.36 53.39 0 4 0 1205.18 55.09 0 4 0 1396.76 53.19 1 -4 0 3235.48 97.49 1 -4 0 3013.90 80.79 -1 -4 0 3121.79 81.49 -1 -4 0 3215.38 109.29 1 -4 0 3078.69 151.38 -1 -4 0 3061.29 78.19 -1 -4 0 3150.28 153.98 1 -4 0 3136.79 91.79 1 -4 0 3234.28 86.19 -1 4 0 3058.99 80.09 1 4 0 3280.47 83.99 -1 4 0 3135.09 94.09 1 4 0 2942.91 101.69 -1 4 0 3058.19 98.79 1 4 0 3122.59 151.58 -1 4 0 3060.99 154.18 -2 -4 0 -3.30 6.80 2 -4 0 7.70 9.30 2 -4 0 -4.20 11.90 -2 -4 0 9.10 4.00 2 -4 0 3.50 4.00 -2 -4 0 -0.90 10.90 2 -4 0 11.40 6.40 2 -4 0 4.40 5.10 2 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43.10 -2 -6 -11 17.30 39.80 -2 -6 -11 3.40 6.40 2 -6 11 -1.50 8.80 -2 6 -11 0.90 21.90 3 -6 11 3.40 13.30 -3 -6 -11 2.60 3.40 -3 -6 -11 -25.90 16.80 -3 6 -11 12.20 32.40 -4 -6 -11 7.10 3.90 -4 -6 -11 -17.80 18.30 -4 6 -11 18.90 23.20 -6 7 11 -4.10 2.10 -5 -7 11 -1.30 17.10 5 7 -11 -7.30 5.00 -4 -7 11 -2.70 11.10 4 7 -11 4.40 4.90 -3 -7 11 10.50 11.80 3 7 -11 -7.70 6.10 -2 -7 11 18.20 11.50 2 7 -11 1.30 9.10 -2 7 11 -15.70 13.40 -1 -7 11 -6.00 7.30 0 -7 11 -6.40 7.30 1 -7 11 7.50 11.20 -1 7 -11 39.70 44.80 -2 -7 -11 25.20 37.20 -2 7 -11 12.00 32.80 -3 -7 -11 -23.30 21.10 -3 -7 -11 1.00 2.90 3 -7 11 -5.40 12.30 -3 7 -11 2.50 23.20 -4 -7 -11 0.80 2.60 -4 -7 -11 -14.70 25.20 -6 -8 11 -2.40 2.70 -6 8 11 0.60 2.20 -5 -8 11 3.90 17.80 5 8 -11 -12.60 7.30 -4 -8 11 -6.10 9.40 4 8 -11 4.90 5.90 -3 -8 11 22.60 15.70 3 8 -11 -9.80 5.60 -2 -8 11 4.30 9.10 -2 8 11 -3.00 15.00 2 8 -11 -2.50 8.20 -1 -8 11 17.80 12.30 0 -8 11 13.70 12.00 -1 -8 -11 5.20 4.50 1 -8 11 -3.90 10.10 -1 8 -11 -25.70 22.30 2 -8 11 -18.70 10.70 -2 -8 -11 4.80 4.20 -2 -8 -11 23.80 22.80 -2 8 -11 -14.50 18.20 -3 -8 -11 3.60 3.60 -3 -8 -11 9.60 24.10 3 -8 11 33.70 16.60 -3 8 -11 -9.90 18.60 -4 -8 -11 -6.00 9.60 -4 -8 -11 1.90 3.10 -4 8 -11 4.80 10.00 -5 -9 11 25.90 19.10 5 9 -11 8.60 6.80 -4 -9 11 -7.20 12.40 4 9 -11 2.60 7.70 -3 -9 11 17.30 11.10 3 9 -11 7.40 7.40 -2 -9 11 8.50 11.60 2 9 -11 6.20 7.60 0 -9 11 12.50 12.50 1 -9 11 5.50 10.10 -1 -9 -11 -0.20 2.50 -1 9 -11 17.70 26.10 -2 -9 -11 -1.90 19.20 2 -9 11 -19.10 10.20 -2 -9 -11 4.70 3.00 -2 9 -11 -5.20 20.00 -3 -9 -11 23.00 28.40 -3 -9 -11 3.30 3.10 -3 9 -11 -18.20 9.10 -4 -10 11 4.80 11.70 4 10 -11 4.60 5.80 -3 -10 11 4.60 11.50 3 10 -11 -6.20 5.00 -2 -10 11 10.90 10.00 2 10 -11 3.60 7.00 -1 -10 11 7.60 12.80 0 -10 11 7.80 12.60 1 -10 11 6.60 13.70 2 -10 11 5.00 17.00 -2 -10 -11 -0.40 2.90 -2 10 -11 2.00 26.80 -3 -10 -11 2.70 2.40 -3 10 -11 -15.00 13.20 -4 -11 11 -25.70 13.70 -3 -11 11 -10.20 9.00 -2 -11 11 9.70 11.90 -1 -11 11 13.50 12.20 0 -11 11 3.10 9.30 1 -11 11 11.50 11.10 -3 -12 11 -15.30 10.30 -2 -12 11 16.90 14.00 -1 -12 11 6.70 12.30 0 -12 11 -5.40 21.30 -2 -13 11 7.80 14.40 -1 -13 11 -2.60 13.10 -3 0 12 -0.20 12.60 -2 0 12 13.40 11.80 -1 0 12 -8.90 11.30 0 0 12 -3.10 8.30 1 0 12 -7.10 5.20 2 0 12 0.30 7.70 -3 0 -12 9.80 25.80 3 0 12 1.70 7.90 -4 -1 12 8.40 21.80 -2 -1 12 -1.40 9.20 -2 1 12 4.10 11.90 -1 -1 12 2.60 9.20 -1 1 12 12.80 11.90 0 -1 12 4.60 10.80 1 -1 12 -3.50 10.00 1 1 12 -0.90 5.70 2 -1 12 12.60 9.50 2 1 12 1.10 7.00 -3 -1 -12 13.90 19.10 3 -1 12 -4.80 8.30 3 1 12 6.30 7.40 -4 -2 12 -2.30 19.10 -3 -2 12 17.20 11.00 -3 2 12 -7.20 16.10 -2 -2 12 9.00 10.50 -2 2 12 16.10 8.80 -1 -2 12 -15.00 8.40 -1 2 12 -2.80 12.20 0 -2 12 -6.80 6.60 0 2 12 9.70 8.40 1 -2 12 -5.70 6.90 1 2 12 9.10 9.70 2 -2 12 7.90 8.40 2 2 12 -4.70 7.50 3 -2 12 -13.40 12.70 3 2 12 8.80 8.20 -3 2 -12 -7.10 19.80 -4 -3 12 -2.10 18.90 -3 -3 12 -1.60 12.30 -3 3 12 18.40 19.80 -2 -3 12 -10.90 9.00 -2 3 12 4.90 9.90 -1 -3 12 10.00 8.20 -1 3 12 -20.10 11.50 0 -3 12 3.20 10.00 0 3 12 5.90 10.60 1 -3 12 -2.90 9.10 1 3 12 13.10 9.50 2 -3 12 8.70 9.70 2 3 12 17.20 9.70 3 -3 12 10.20 9.60 3 3 12 11.20 9.40 -4 -4 12 17.60 16.60 -3 -4 12 -12.10 11.60 -2 -4 12 -6.30 11.40 -2 4 12 -2.80 14.40 -1 -4 12 6.50 11.20 0 4 12 16.00 10.10 1 4 12 -13.40 8.90 2 -4 12 1.40 9.20 2 4 12 4.20 9.60 3 4 12 -9.90 7.70 -4 -5 12 25.20 17.00 -3 -5 12 5.20 11.00 -2 -5 12 3.30 7.60 -2 5 12 -19.10 18.20 -1 -5 12 11.30 9.70 -1 5 12 7.30 10.00 0 -5 12 -7.20 8.50 0 5 12 8.60 9.20 1 -5 12 -1.60 7.50 1 5 12 -8.50 8.10 2 -5 12 14.30 10.80 2 5 12 -6.00 9.00 3 5 12 -6.00 7.90 -3 -6 12 22.00 13.50 -2 -6 12 -7.90 7.80 -1 -6 12 20.80 12.70 -1 6 12 -10.60 11.00 0 -6 12 0.80 8.90 0 6 12 6.50 12.20 1 -6 12 10.90 9.40 1 6 12 14.50 10.50 2 -6 12 17.60 12.80 2 6 12 -2.50 8.80 -3 -7 12 5.70 11.30 -2 -7 12 -14.30 8.50 -1 -7 12 -9.50 10.00 -1 7 12 7.40 15.50 0 -7 12 11.70 11.30 0 7 12 7.60 12.60 1 -7 12 1.60 9.90 1 7 12 -1.60 11.90 2 7 12 -14.80 8.10 -3 -8 12 -11.30 9.30 -1 -8 12 1.80 7.60 0 -8 12 18.00 11.10 1 -8 12 7.10 8.00 1 8 12 -6.30 16.80 -2 -9 12 24.90 15.10 -1 -9 12 -1.60 8.40 0 -9 12 4.50 10.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 38507 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 0.4041(4) 0.7290(2) 0.4474(5) 0.0869(14) Uani 1 1 d . . . . . O2 O 0.1920(6) 0.5291(4) 0.5329(9) 0.128(3) Uani 1 1 d . . . . . N1 N 0.5933(5) 0.7378(2) 0.3333(6) 0.0770(15) Uani 1 1 d . . . . . C1 C 0.8504(6) 0.6303(3) 0.4995(7) 0.0788(18) Uani 1 1 d . . . . . H1A H 0.874950 0.613761 0.580861 0.095 Uiso 1 1 calc R U . . . C2 C 0.9234(6) 0.6140(3) 0.3988(8) 0.090(2) Uani 1 1 d . . . . . H2B H 0.995298 0.585400 0.412582 0.108 Uiso 1 1 calc R U . . . C3 C 0.8906(6) 0.6397(3) 0.2788(8) 0.095(2) Uani 1 1 d . . . . . H3A H 0.940158 0.628789 0.211733 0.114 Uiso 1 1 calc R U . . . C4 C 0.7841(6) 0.6814(3) 0.2594(7) 0.0825(19) Uani 1 1 d . . . . . H4A H 0.763490 0.699273 0.178461 0.099 Uiso 1 1 calc R U . . . C5 C 0.7067(6) 0.6979(3) 0.3549(6) 0.0737(17) Uani 1 1 d . . . . . C6 C 0.5255(6) 0.7660(3) 0.4360(7) 0.0774(18) Uani 1 1 d . . . . . C7 C 0.6114(6) 0.7618(3) 0.5628(6) 0.0813(18) Uani 1 1 d . . . . . H7A H 0.688734 0.789942 0.560611 0.098 Uiso 1 1 calc R U . . . H7B H 0.562209 0.776450 0.632396 0.098 Uiso 1 1 calc R U . . . C8 C 0.6521(6) 0.6887(3) 0.5810(7) 0.0804(18) Uani 1 1 d . . . . . H8A H 0.700637 0.682929 0.665016 0.096 Uiso 1 1 calc R U . . . C9 C 0.7405(6) 0.6714(3) 0.4784(6) 0.0732(17) Uani 1 1 d . . . . . C10 C 0.5315(6) 0.6443(3) 0.5708(6) 0.0763(17) Uani 1 1 d . . . . . C11 C 0.5315(7) 0.5812(3) 0.6212(6) 0.0832(19) Uani 1 1 d . . . . . H11A H 0.609086 0.564768 0.663307 0.100 Uiso 1 1 calc R U . . . C12 C 0.4197(7) 0.5407(3) 0.6117(7) 0.088(2) Uani 1 1 d . . . . . H12A H 0.421823 0.498005 0.646619 0.105 Uiso 1 1 calc R U . . . C13 C 0.3050(7) 0.5664(4) 0.5482(8) 0.091(2) Uani 1 1 d . . . . . C14 C 0.3029(6) 0.6286(3) 0.4965(7) 0.090(2) Uani 1 1 d . . . . . H14A H 0.225528 0.645007 0.453918 0.108 Uiso 1 1 calc R U . . . C15 C 0.4145(6) 0.6673(3) 0.5070(7) 0.0816(19) Uani 1 1 d . . . . . C16 C 0.5396(8) 0.7514(3) 0.2020(7) 0.093(2) Uani 1 1 d . . . . . H16A H 0.605676 0.775204 0.158919 0.111 Uiso 1 1 calc R U . . . H16B H 0.464023 0.780716 0.204331 0.111 Uiso 1 1 calc R U . . . C17 C 0.4976(6) 0.6904(3) 0.1239(7) 0.0751(17) Uani 1 1 d . . . . . C18 C 0.4642(7) 0.6316(3) 0.1768(7) 0.091(2) Uani 1 1 d . . . . . H18A H 0.470657 0.627651 0.265208 0.109 Uiso 1 1 calc R U . . . C19 C 0.4213(8) 0.5780(4) 0.1032(9) 0.103(2) Uani 1 1 d . . . . . H19A H 0.399035 0.538076 0.141233 0.124 Uiso 1 1 calc R U . . . C20 C 0.4117(8) 0.5839(4) -0.0265(9) 0.106(2) Uani 1 1 d . . . . . H20A H 0.383056 0.547612 -0.076735 0.127 Uiso 1 1 calc R U . . . C21 C 0.4433(8) 0.6419(4) -0.0838(8) 0.104(2) Uani 1 1 d . . . . . H21A H 0.434994 0.645491 -0.172261 0.125 Uiso 1 1 calc R U . . . C22 C 0.4878(7) 0.6954(4) -0.0088(7) 0.0864(19) Uani 1 1 d . . . . . H22A H 0.511288 0.734964 -0.047098 0.104 Uiso 1 1 calc R U . . . C23 C 0.4822(6) 0.8370(3) 0.4062(7) 0.0787(18) Uani 1 1 d . . . . . C24 C 0.3559(6) 0.8588(3) 0.4232(7) 0.087(2) Uani 1 1 d . . . . . H24A H 0.293999 0.829280 0.450861 0.104 Uiso 1 1 calc R U . . . C25 C 0.3223(8) 0.9257(4) 0.3985(7) 0.093(2) Uani 1 1 d . . . . . H25A H 0.237782 0.940032 0.411674 0.112 Uiso 1 1 calc R U . . . C26 C 0.4085(8) 0.9704(4) 0.3560(8) 0.109(3) Uani 1 1 d . . . . . H26A H 0.383674 1.014416 0.338317 0.131 Uiso 1 1 calc R U . . . C27 C 0.5343(8) 0.9483(4) 0.3402(8) 0.108(3) Uani 1 1 d . . . . . H27A H 0.595894 0.978016 0.312427 0.129 Uiso 1 1 calc R U . . . C28 C 0.5699(7) 0.8825(3) 0.3650(7) 0.093(2) Uani 1 1 d . . . . . H28A H 0.655295 0.868756 0.353502 0.111 Uiso 1 1 calc R U . . . H2A H 0.212(12) 0.498(6) 0.539(13) 0.20(6) Uiso 1 1 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 O1 0.080(2) 0.071(3) 0.109(4) 0.011(3) 0.005(2) -0.006(2) O2 0.105(4) 0.086(5) 0.192(8) 0.018(4) 0.016(4) -0.013(3) N1 0.081(3) 0.065(3) 0.084(4) -0.007(3) 0.005(3) 0.009(2) C1 0.077(4) 0.069(4) 0.089(5) 0.001(3) 0.003(4) -0.007(3) C2 0.076(4) 0.071(4) 0.123(7) 0.010(4) 0.011(4) 0.000(3) C3 0.088(4) 0.085(5) 0.116(7) 0.000(5) 0.032(4) -0.005(4) C4 0.090(4) 0.071(4) 0.088(5) 0.001(4) 0.017(4) 0.000(3) C5 0.076(3) 0.067(4) 0.077(5) -0.004(3) 0.006(3) -0.001(3) C6 0.077(3) 0.061(4) 0.093(5) -0.004(3) 0.000(3) -0.006(3) C7 0.087(4) 0.077(5) 0.079(5) -0.006(3) 0.005(4) 0.000(3) C8 0.083(4) 0.078(4) 0.079(5) -0.003(4) 0.001(3) -0.001(3) C9 0.076(3) 0.063(4) 0.080(5) -0.003(3) 0.004(3) -0.004(3) C10 0.093(4) 0.072(4) 0.066(4) 0.004(3) 0.020(3) 0.008(3) C11 0.110(5) 0.071(5) 0.070(5) 0.008(4) 0.016(4) 0.011(3) C12 0.120(5) 0.065(4) 0.080(5) 0.005(3) 0.022(4) -0.001(4) C13 0.093(4) 0.073(5) 0.109(6) 0.005(4) 0.020(4) -0.005(4) C14 0.082(4) 0.072(5) 0.116(6) 0.004(4) 0.003(4) 0.002(3) C15 0.086(4) 0.071(4) 0.091(5) 0.010(4) 0.021(4) 0.004(3) C16 0.117(5) 0.076(5) 0.082(6) 0.000(4) -0.007(4) 0.011(4) C17 0.085(4) 0.063(4) 0.076(5) -0.001(3) 0.002(3) 0.012(3) C18 0.117(5) 0.074(5) 0.082(5) -0.002(4) 0.006(4) 0.002(4) C19 0.125(6) 0.084(6) 0.099(7) -0.010(5) -0.006(5) -0.006(4) C20 0.111(5) 0.085(6) 0.118(8) -0.026(5) -0.003(5) -0.006(4) C21 0.117(6) 0.116(7) 0.076(5) -0.030(5) -0.002(4) 0.025(5) C22 0.103(4) 0.085(5) 0.073(5) 0.004(4) 0.018(4) 0.017(4) C23 0.085(4) 0.062(4) 0.088(5) -0.002(3) 0.002(4) 0.002(3) C24 0.092(4) 0.073(5) 0.095(6) 0.007(4) 0.012(4) 0.009(3) C25 0.110(5) 0.079(5) 0.091(6) -0.005(4) 0.004(4) 0.026(4) C26 0.122(6) 0.079(6) 0.125(8) 0.001(5) -0.002(6) 0.016(5) C27 0.125(6) 0.063(5) 0.134(8) -0.005(5) 0.005(5) -0.015(4) C28 0.092(4) 0.067(5) 0.119(6) -0.009(4) 0.010(4) -0.008(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' 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 C15 O1 C6 117.4(5) . . ? C13 O2 H2A 105(10) . . ? C5 N1 C6 122.8(6) . . ? C5 N1 C16 119.3(6) . . ? C6 N1 C16 118.0(5) . . ? C2 C1 C9 119.7(7) . . ? C2 C1 H1A 120.1 . . ? C9 C1 H1A 120.1 . . ? C3 C2 C1 120.8(7) . . ? C3 C2 H2B 119.6 . . ? C1 C2 H2B 119.6 . . ? C4 C3 C2 119.1(7) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C3 C4 C5 122.5(7) . . ? C3 C4 H4A 118.7 . . ? C5 C4 H4A 118.7 . . ? C4 C5 N1 122.5(6) . . ? C4 C5 C9 118.2(6) . . ? N1 C5 C9 119.3(6) . . ? N1 C6 O1 109.2(5) . . ? N1 C6 C23 111.2(6) . . ? O1 C6 C23 105.2(5) . . ? N1 C6 C7 110.8(5) . . ? O1 C6 C7 108.8(5) . . ? C23 C6 C7 111.4(5) . . ? C8 C7 C6 106.8(5) . . ? C8 C7 H7A 110.4 . . ? C6 C7 H7A 110.4 . . ? C8 C7 H7B 110.4 . . ? C6 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? C9 C8 C10 110.4(5) . . ? C9 C8 C7 107.7(5) . . ? C10 C8 C7 110.2(5) . . ? C9 C8 H8A 109.5 . . ? C10 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? C1 C9 C5 119.6(6) . . ? C1 C9 C8 123.1(6) . . ? C5 C9 C8 117.3(5) . . ? C11 C10 C15 117.6(6) . . ? C11 C10 C8 122.9(6) . . ? C15 C10 C8 119.5(6) . . ? C10 C11 C12 122.5(7) . . ? C10 C11 H11A 118.8 . . ? C12 C11 H11A 118.8 . . ? C13 C12 C11 117.7(6) . . ? C13 C12 H12A 121.2 . . ? C11 C12 H12A 121.2 . . ? C14 C13 O2 118.1(7) . . ? C14 C13 C12 120.9(6) . . ? O2 C13 C12 121.0(7) . . ? C13 C14 C15 120.2(7) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C14 C15 O1 116.0(6) . . ? C14 C15 C10 121.2(6) . . ? O1 C15 C10 122.8(6) . . ? N1 C16 C17 115.2(6) . . ? N1 C16 H16A 108.5 . . ? C17 C16 H16A 108.5 . . ? N1 C16 H16B 108.5 . . ? C17 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? C18 C17 C22 118.4(6) . . ? C18 C17 C16 123.1(7) . . ? C22 C17 C16 118.5(6) . . ? C17 C18 C19 121.7(8) . . ? C17 C18 H18A 119.1 . . ? C19 C18 H18A 119.1 . . ? C20 C19 C18 119.1(8) . . ? C20 C19 H19A 120.5 . . ? C18 C19 H19A 120.5 . . ? C21 C20 C19 121.3(8) . . ? C21 C20 H20A 119.3 . . ? C19 C20 H20A 119.3 . . ? C20 C21 C22 119.1(8) . . ? C20 C21 H21A 120.4 . . ? C22 C21 H21A 120.4 . . ? C21 C22 C17 120.4(7) . . ? C21 C22 H22A 119.8 . . ? C17 C22 H22A 119.8 . . ? C28 C23 C24 118.1(6) . . ? C28 C23 C6 120.2(6) . . ? C24 C23 C6 121.7(6) . . ? C23 C24 C25 119.4(6) . . ? C23 C24 H24A 120.3 . . ? C25 C24 H24A 120.3 . . ? C26 C25 C24 122.5(7) . . ? C26 C25 H25A 118.7 . . ? C24 C25 H25A 118.7 . . ? C25 C26 C27 117.6(7) . . ? C25 C26 H26A 121.2 . . ? C27 C26 H26A 121.2 . . ? C26 C27 C28 120.8(7) . . ? C26 C27 H27A 119.6 . . ? C28 C27 H27A 119.6 . . ? C23 C28 C27 121.6(7) . . ? C23 C28 H28A 119.2 . . ? C27 C28 H28A 119.2 . . ? 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 C15 1.384(7) . ? O1 C6 1.456(7) . ? O2 C13 1.369(9) . ? O2 H2A 0.65(11) . ? N1 C5 1.405(7) . ? N1 C6 1.449(8) . ? N1 C16 1.465(8) . ? C1 C2 1.388(9) . ? C1 C9 1.391(8) . ? C1 H1A 0.9300 . ? C2 C3 1.376(9) . ? C2 H2B 0.9300 . ? C3 C4 1.370(8) . ? C3 H3A 0.9300 . ? C4 C5 1.373(8) . ? C4 H4A 0.9300 . ? C5 C9 1.417(8) . ? C6 C23 1.512(8) . ? C6 C7 1.530(8) . ? C7 C8 1.528(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.508(8) . ? C8 C10 1.512(8) . ? C8 H8A 0.9800 . ? C10 C11 1.369(8) . ? C10 C15 1.392(8) . ? C11 C12 1.393(9) . ? C11 H11A 0.9300 . ? C12 C13 1.391(9) . ? C12 H12A 0.9300 . ? C13 C14 1.358(9) . ? C14 C15 1.372(8) . ? C14 H14A 0.9300 . ? C16 C17 1.512(9) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.358(9) . ? C17 C22 1.394(9) . ? C18 C19 1.372(9) . ? C18 H18A 0.9300 . ? C19 C20 1.365(10) . ? C19 H19A 0.9300 . ? C20 C21 1.359(10) . ? C20 H20A 0.9300 . ? C21 C22 1.381(9) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C28 1.373(8) . ? C23 C24 1.386(8) . ? C24 C25 1.400(8) . ? C24 H24A 0.9300 . ? C25 C26 1.358(10) . ? C25 H25A 0.9300 . ? C26 C27 1.379(10) . ? C26 H26A 0.9300 . ? C27 C28 1.386(9) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? 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 C9 C1 C2 C3 2.0(10) . . . . ? C1 C2 C3 C4 -0.4(10) . . . . ? C2 C3 C4 C5 -1.2(10) . . . . ? C3 C4 C5 N1 -176.4(6) . . . . ? C3 C4 C5 C9 1.1(10) . . . . ? C6 N1 C5 C4 -167.8(6) . . . . ? C16 N1 C5 C4 12.7(9) . . . . ? C6 N1 C5 C9 14.6(9) . . . . ? C16 N1 C5 C9 -164.9(6) . . . . ? C5 N1 C6 O1 -105.4(6) . . . . ? C16 N1 C6 O1 74.1(7) . . . . ? C5 N1 C6 C23 139.0(6) . . . . ? C16 N1 C6 C23 -41.5(7) . . . . ? C5 N1 C6 C7 14.5(8) . . . . ? C16 N1 C6 C7 -166.0(5) . . . . ? C15 O1 C6 N1 77.4(7) . . . . ? C15 O1 C6 C23 -163.2(5) . . . . ? C15 O1 C6 C7 -43.8(7) . . . . ? N1 C6 C7 C8 -54.1(6) . . . . ? O1 C6 C7 C8 66.0(6) . . . . ? C23 C6 C7 C8 -178.5(5) . . . . ? C6 C7 C8 C9 66.2(6) . . . . ? C6 C7 C8 C10 -54.3(7) . . . . ? C2 C1 C9 C5 -2.0(9) . . . . ? C2 C1 C9 C8 176.9(6) . . . . ? C4 C5 C9 C1 0.5(9) . . . . ? N1 C5 C9 C1 178.1(5) . . . . ? C4 C5 C9 C8 -178.5(5) . . . . ? N1 C5 C9 C8 -0.8(8) . . . . ? C10 C8 C9 C1 -98.1(7) . . . . ? C7 C8 C9 C1 141.6(6) . . . . ? C10 C8 C9 C5 80.9(7) . . . . ? C7 C8 C9 C5 -39.5(7) . . . . ? C9 C8 C10 C11 82.4(8) . . . . ? C7 C8 C10 C11 -158.8(6) . . . . ? C9 C8 C10 C15 -97.0(7) . . . . ? C7 C8 C10 C15 21.8(9) . . . . ? C15 C10 C11 C12 -0.7(10) . . . . ? C8 C10 C11 C12 179.8(6) . . . . ? C10 C11 C12 C13 0.0(10) . . . . ? C11 C12 C13 C14 0.5(11) . . . . ? C11 C12 C13 O2 178.7(7) . . . . ? O2 C13 C14 C15 -178.6(7) . . . . ? C12 C13 C14 C15 -0.4(12) . . . . ? C13 C14 C15 O1 177.8(7) . . . . ? C13 C14 C15 C10 -0.4(11) . . . . ? C6 O1 C15 C14 -168.9(6) . . . . ? C6 O1 C15 C10 9.3(9) . . . . ? C11 C10 C15 C14 0.9(10) . . . . ? C8 C10 C15 C14 -179.6(6) . . . . ? C11 C10 C15 O1 -177.1(6) . . . . ? C8 C10 C15 O1 2.4(10) . . . . ? C5 N1 C16 C17 60.3(8) . . . . ? C6 N1 C16 C17 -119.2(6) . . . . ? N1 C16 C17 C18 23.7(9) . . . . ? N1 C16 C17 C22 -158.9(6) . . . . ? C22 C17 C18 C19 -0.2(10) . . . . ? C16 C17 C18 C19 177.3(7) . . . . ? C17 C18 C19 C20 -0.1(12) . . . . ? C18 C19 C20 C21 -0.3(13) . . . . ? C19 C20 C21 C22 1.0(12) . . . . ? C20 C21 C22 C17 -1.3(10) . . . . ? C18 C17 C22 C21 0.9(10) . . . . ? C16 C17 C22 C21 -176.7(6) . . . . ? N1 C6 C23 C28 -49.2(8) . . . . ? O1 C6 C23 C28 -167.3(6) . . . . ? C7 C6 C23 C28 75.0(8) . . . . ? N1 C6 C23 C24 133.0(6) . . . . ? O1 C6 C23 C24 14.9(9) . . . . ? C7 C6 C23 C24 -102.9(7) . . . . ? C28 C23 C24 C25 -0.1(11) . . . . ? C6 C23 C24 C25 177.7(6) . . . . ? C23 C24 C25 C26 1.1(12) . . . . ? C24 C25 C26 C27 -1.5(13) . . . . ? C25 C26 C27 C28 1.0(13) . . . . ? C24 C23 C28 C27 -0.4(11) . . . . ? C6 C23 C28 C27 -178.3(7) . . . . ? C26 C27 C28 C23 -0.1(13) . . . . ?