#------------------------------------------------------------------------------ #$Date: 2020-10-06 09:57:52 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257279 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557907.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_1557907 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_page_last 7675 _journal_paper_doi 10.1039/D0SC01909G _journal_volume 11 _journal_year 2020 _chemical_absolute_configuration unk _chemical_formula_sum 'C29 H37 N3 O2' _chemical_formula_weight 459.61 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _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 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 16.4161(9) _cell_length_b 12.4001(8) _cell_length_c 25.3104(17) _cell_measurement_reflns_used 5269 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 29.6580 _cell_measurement_theta_min 2.9400 _cell_volume 5152.2(6) _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 0.999 _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 0.0930 _diffrn_reflns_av_unetI/netI 0.0616 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 35337 _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 2.481 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.40848 _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 1.185 _exptl_crystal_description platelet _exptl_crystal_F_000 1984 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.030 _refine_diff_density_max 0.203 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.044 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 315 _refine_ls_number_reflns 4538 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.017 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0484 _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^)+(0.0448P)^2^+1.5455P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0932 _refine_ls_wR_factor_ref 0.1093 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2985 _reflns_number_total 4538 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01909g2.cif _cod_data_source_block 2a _cod_depositor_comments ;Adding full bibliography for 1557900--1557907.cif. Adding full bibliography for 1557900--1557907.cif. ; _cod_database_code 1557907 _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 0.985 _shelx_estimated_absorpt_t_max 0.998 _shelx_res_file ; TITL okude4 okude4.res created by SHELXL-2016/6 at 18:31:39 on 20-Oct-2018 REM Yadorkari-X generated CELL 0.71073 16.4161 12.4001 25.3104 90.0000 90.0000 90.0000 ZERR 8.0 0.0009 0.0008 0.0017 0.0000 0.0000 0.0000 LATT 1 SYMM 1/2-X, -Y, 1/2+Z SYMM 1/2+X, 1/2-Y, -Z SYMM -X, 1/2+Y, 1/2-Z REM SPGR Pbca orthorhombic SFAC C H N O UNIT 232 296 24 16 SIZE 0.20 0.05 0.03 TEMP -150.0 L.S. 4 FMAP 2 PLAN -25 ACTA CONF WPDB -1 BOND $H MERG 2 OMIT -10.000000 50.000000 WGHT 0.044800 1.545500 FVAR 0.12629 O1 4 0.398196 0.021808 0.467210 11.00000 0.02871 0.02205 = 0.03104 -0.00089 0.00606 0.00455 C1 1 0.373726 0.114422 0.475964 11.00000 0.01722 0.02435 = 0.02202 -0.00152 -0.00129 0.00013 N1 3 0.400826 0.201530 0.448832 11.00000 0.01977 0.01869 = 0.02234 -0.00069 0.00444 0.00105 C2 1 0.458586 0.186891 0.404048 11.00000 0.01951 0.02640 = 0.02195 -0.00001 0.00557 -0.00049 AFIX 13 H30 2 0.463885 0.258800 0.386497 11.00000 -1.20000 AFIX 0 C3 1 0.425710 0.109496 0.362388 11.00000 0.02938 0.03386 = 0.02738 -0.00600 0.00602 -0.00262 AFIX 137 H1 2 0.421881 0.036826 0.377403 11.00000 -1.50000 H2 2 0.462558 0.108524 0.331929 11.00000 -1.50000 H3 2 0.371556 0.133388 0.351053 11.00000 -1.50000 AFIX 0 C4 1 0.543465 0.156673 0.423803 11.00000 0.02001 0.03371 = 0.03587 -0.00194 0.00426 -0.00049 AFIX 137 H4 2 0.564218 0.214050 0.446777 11.00000 -1.50000 H5 2 0.580142 0.147555 0.393581 11.00000 -1.50000 H6 2 0.540508 0.089022 0.443728 11.00000 -1.50000 AFIX 0 C5 1 0.372882 0.312395 0.460095 11.00000 0.02393 0.01990 = 0.02692 0.00052 0.00651 0.00148 AFIX 13 H31 2 0.340940 0.309816 0.493714 11.00000 -1.20000 AFIX 0 C6 1 0.315681 0.352634 0.416926 11.00000 0.03148 0.03048 = 0.04024 0.00443 0.00125 0.00796 AFIX 137 H7 2 0.346471 0.363492 0.384183 11.00000 -1.50000 H8 2 0.291120 0.421083 0.427920 11.00000 -1.50000 H9 2 0.272685 0.299193 0.410926 11.00000 -1.50000 AFIX 0 C7 1 0.444175 0.388891 0.468972 11.00000 0.03616 0.02466 = 0.03080 -0.00313 0.00930 -0.00430 AFIX 137 H10 2 0.477624 0.362378 0.498295 11.00000 -1.50000 H11 2 0.423444 0.460926 0.477511 11.00000 -1.50000 H12 2 0.477326 0.392586 0.436823 11.00000 -1.50000 AFIX 0 C8 1 0.314357 0.129735 0.520901 11.00000 0.02010 0.02210 = 0.02159 0.00053 -0.00033 -0.00145 C9 1 0.339974 0.180000 0.576720 11.00000 0.01613 0.02100 = 0.02466 0.00002 0.00101 0.00041 C10 1 0.303500 0.076236 0.604294 11.00000 0.02200 0.02176 = 0.02353 0.00276 0.00188 -0.00082 AFIX 13 H13 2 0.330622 0.034231 0.633069 11.00000 -1.20000 AFIX 0 C11 1 0.277889 0.029869 0.549283 11.00000 0.02732 0.01898 = 0.02504 -0.00094 0.00459 -0.00352 AFIX 13 H14 2 0.285811 -0.046587 0.537814 11.00000 -1.20000 AFIX 0 C12 1 0.193416 0.087614 0.554243 11.00000 0.01892 0.02879 = 0.02621 -0.00260 0.00096 -0.00788 AFIX 13 H15 2 0.139618 0.053700 0.546032 11.00000 -1.20000 AFIX 0 C13 1 0.229305 0.188799 0.525546 11.00000 0.01605 0.02883 = 0.02201 0.00029 -0.00074 0.00047 AFIX 13 H16 2 0.201868 0.229835 0.496561 11.00000 -1.20000 AFIX 0 C14 1 0.255056 0.236544 0.580351 11.00000 0.01808 0.02071 = 0.02338 -0.00085 0.00135 -0.00002 AFIX 13 H17 2 0.246213 0.312956 0.591605 11.00000 -1.20000 AFIX 0 C15 1 0.218291 0.134721 0.609137 11.00000 0.01814 0.02375 = 0.02246 0.00136 -0.00106 -0.00306 C16 1 0.420118 0.229348 0.588951 11.00000 0.02025 0.02092 = 0.01969 0.00349 0.00076 -0.00047 C17 1 0.425890 0.332258 0.610668 11.00000 0.01686 0.02230 = 0.02386 0.00077 0.00166 0.00233 AFIX 43 H34 2 0.377614 0.372561 0.616873 11.00000 -1.20000 AFIX 0 C18 1 0.500799 0.377031 0.623411 11.00000 0.02512 0.02081 = 0.02256 0.00200 0.00029 -0.00236 AFIX 43 H35 2 0.503912 0.447348 0.638173 11.00000 -1.20000 AFIX 0 C19 1 0.571269 0.317657 0.614298 11.00000 0.01970 0.02327 = 0.02581 0.00399 -0.00072 -0.00370 C20 1 0.566914 0.215108 0.591543 11.00000 0.01699 0.02878 = 0.03113 0.00224 0.00388 0.00265 AFIX 43 H36 2 0.615338 0.175465 0.584821 11.00000 -1.20000 AFIX 0 C21 1 0.492037 0.171652 0.578876 11.00000 0.02158 0.02284 = 0.02697 -0.00094 0.00071 0.00307 AFIX 43 H37 2 0.489133 0.102136 0.563212 11.00000 -1.20000 AFIX 0 C22 1 0.649009 0.361745 0.629925 11.00000 0.02335 0.02994 = 0.03749 0.00650 -0.00090 0.00005 N2 3 0.709839 0.397511 0.643785 11.00000 0.02661 0.04264 = 0.06663 0.00886 -0.01181 -0.00469 C23 1 0.161223 0.137372 0.655581 11.00000 0.02130 0.02039 = 0.02454 0.00226 0.00299 -0.00119 O2 4 0.091127 0.102592 0.650055 11.00000 0.02254 0.03720 = 0.02996 -0.00500 0.00455 -0.01091 N3 3 0.188209 0.180426 0.701556 11.00000 0.01985 0.03044 = 0.01926 -0.00090 0.00105 -0.00261 C24 1 0.272454 0.220898 0.708432 11.00000 0.02219 0.04000 = 0.02754 -0.00542 -0.00125 -0.00537 AFIX 13 H32 2 0.301605 0.208311 0.674293 11.00000 -1.20000 AFIX 0 C25 1 0.317660 0.156615 0.750785 11.00000 0.03272 0.07228 = 0.04037 -0.00026 -0.00840 0.00064 AFIX 137 H18 2 0.291442 0.168036 0.785117 11.00000 -1.50000 H19 2 0.374418 0.180849 0.752528 11.00000 -1.50000 H20 2 0.316111 0.079733 0.741871 11.00000 -1.50000 AFIX 0 C26 1 0.274540 0.341666 0.718823 11.00000 0.04332 0.04549 = 0.04359 -0.01601 0.01022 -0.02051 AFIX 137 H21 2 0.244447 0.379328 0.690934 11.00000 -1.50000 H22 2 0.331186 0.366602 0.719112 11.00000 -1.50000 H23 2 0.249329 0.356889 0.753119 11.00000 -1.50000 AFIX 0 C27 1 0.132499 0.192026 0.747559 11.00000 0.02711 0.03148 = 0.01996 -0.00260 0.00437 -0.00040 AFIX 13 H33 2 0.165075 0.226275 0.776421 11.00000 -1.20000 AFIX 0 C28 1 0.103439 0.084313 0.768739 11.00000 0.04963 0.03858 = 0.03175 0.00470 0.01359 -0.00211 AFIX 137 H24 2 0.071005 0.047571 0.741672 11.00000 -1.50000 H25 2 0.069930 0.096076 0.800260 11.00000 -1.50000 H26 2 0.150599 0.039673 0.777973 11.00000 -1.50000 AFIX 0 C29 1 0.062773 0.268677 0.735497 11.00000 0.03300 0.03916 = 0.02920 -0.00366 0.00446 0.00631 AFIX 137 H27 2 0.084733 0.337542 0.722927 11.00000 -1.50000 H28 2 0.030747 0.280780 0.767631 11.00000 -1.50000 H29 2 0.027849 0.237166 0.708152 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM okude4 REM R1 = 0.0484 for 2985 Fo > 4sig(Fo) and 0.0940 for all 4538 data REM 315 parameters refined using 0 restraints END WGHT 0.0448 1.5456 REM Highest difference peak 0.203, deepest hole -0.304, 1-sigma level 0.044 Q1 1 0.1928 0.1007 0.5904 11.00000 0.05 0.20 Q2 1 0.1959 0.1220 0.6321 11.00000 0.05 0.19 Q3 1 0.1911 0.1387 0.5326 11.00000 0.05 0.17 Q4 1 0.0443 0.5198 0.0500 11.00000 0.05 0.16 Q5 1 0.2793 0.1675 0.5189 11.00000 0.05 0.15 Q6 1 0.2549 0.1054 0.6137 11.00000 0.05 0.15 Q7 1 0.3145 0.1185 0.4917 11.00000 0.05 0.15 Q8 1 0.3469 -0.0208 0.7493 11.00000 0.05 0.15 Q9 1 0.3456 -0.0374 0.4338 11.00000 0.05 0.15 Q10 1 0.5847 0.2180 0.3867 11.00000 0.05 0.15 Q11 1 0.2475 0.4192 0.6378 11.00000 0.05 0.15 Q12 1 0.3400 0.1372 0.5033 11.00000 0.05 0.14 Q13 1 0.1929 -0.0154 0.4914 11.00000 0.05 0.14 Q14 1 0.2274 0.0499 0.5478 11.00000 0.05 0.14 Q15 1 0.6594 0.1806 0.3700 11.00000 0.05 0.14 Q16 1 0.2852 0.3481 0.6269 11.00000 0.05 0.14 Q17 1 0.3455 0.1743 0.5423 11.00000 0.05 0.14 Q18 1 0.3537 -0.0494 0.4834 11.00000 0.05 0.14 Q19 1 0.3236 0.3333 0.3405 11.00000 0.05 0.13 Q20 1 0.3554 -0.0380 0.5196 11.00000 0.05 0.13 Q21 1 0.1705 0.4024 0.6413 11.00000 0.05 0.13 Q22 1 0.2439 0.3936 0.7501 11.00000 0.05 0.13 Q23 1 0.3930 0.2580 0.4562 11.00000 0.05 0.13 Q24 1 0.5606 0.2573 0.4683 11.00000 0.05 0.13 Q25 1 0.0771 0.1438 0.8310 11.00000 0.05 0.13 ; _shelx_res_checksum 94660 _shelx_hkl_file ; 0 0 3-1.35023 0.39976 0 0 3-0.13227 0.40650 0 0 4 102.491 5.56723 0 0 4 107.153 5.56504 0 0 5-0.22347 0.73765 0 0 5 1.42901 0.81898 0 0 6 1854.41 96.3431 0 0 6 1819.34 96.3415 0 0 7 0.24169 0.83046 0 0 7-1.91458 1.08078 0 0 8 218.707 11.7541 0 0 8 224.772 11.7482 0 0 9-0.27346 1.12470 0 0 9 0.06641 1.00311 0 0 10 78.3960 4.21079 0 0 10 73.3221 4.16394 0 0 11 0.69742 1.12429 0 0 11 0.01752 1.19869 0 0 12 47.8052 2.83503 0 0 12 44.2819 2.79958 0 0 13-1.30707 1.17366 0 0 13 1.70364 1.36609 0 0 14 22.6272 1.82535 0 0 14 21.0720 1.84943 0 0 15 0.02417 1.37849 0 0 15-0.52124 1.31814 0 0 16 172.272 9.04215 0 0 16 163.737 9.05541 0 0 17-1.39385 1.48760 0 0 17 0.97324 1.46757 0 0 18 148.382 7.98031 0 0 18 144.367 8.00941 0 0 19-0.41860 1.65397 0 0 19-0.47635 1.63263 0 0 20 3.26077 1.75453 0 0 21-1.52692 1.86103 0 0 22 17.3980 2.21437 0 0 23-0.04690 1.96398 0 0 24 10.2377 2.21869 0 0 25 1.24584 2.08456 0 0 26 2.88107 2.21219 0 0 27 0.05685 2.22499 0 0 28-1.18753 2.44424 0 0 29-0.61924 2.48229 0 0 30 15.4815 2.80455 0 0 31-7.36668 2.80801 0 0 32 8.79019 2.87013 0 0 33 2.02407 2.87706 0 0 34-4.26013 3.09470 -1 0 -3 0.17963 0.43962 1 0 3 1.35236 0.43034 -1 0 3-0.15630 0.44845 -1 0 -3-0.53222 0.42498 -1 0 3 1.90083 0.42284 1 0 -4 5.28164 0.81792 -1 0 4 5.29516 0.71735 -1 0 4 4.30892 0.75415 1 0 4 4.07474 0.72122 -1 0 -4 5.46642 0.65850 -1 0 -5-0.13909 0.64410 1 0 5 0.27455 0.77522 -1 0 5-0.18080 0.74016 1 0 -5 1.58232 0.92880 -1 0 5 0.94051 0.76961 -1 0 -5 2.84057 0.91399 1 0 -6 242.814 12.0842 -1 0 6 239.031 12.0689 -1 0 -6 214.414 12.0625 1 0 6 243.687 12.0704 -1 0 6 196.786 12.0693 -1 0 -6 236.026 12.0552 1 0 -7-1.10619 1.08125 1 0 7-0.65621 1.01283 -1 0 -7-2.86890 0.95855 -1 0 7 1.34221 0.87958 -1 0 -7 0.65216 0.77680 -1 0 7-0.01089 1.06618 1 0 8 251.053 12.8418 -1 0 8 243.365 12.8410 -1 0 -8 214.656 12.8248 -1 0 -8 257.003 12.8306 -1 0 8 259.386 12.8353 1 0 -8 232.204 12.8530 -1 0 9 0.06781 0.98295 -1 0 -9-0.48034 0.88981 1 0 -9-0.53438 1.17701 -1 0 -9 2.60697 0.91597 -1 0 9-1.09374 1.16787 1 0 9 0.19199 1.03386 -1 0 10 34.9147 2.06022 -1 0 10 32.0533 2.08469 -1 0 10 34.3023 1.95860 -1 0 -10 28.0845 1.93392 -1 0 -10 26.7471 1.92237 1 0 10 30.4470 2.04110 -1 0 11 1.47262 1.43013 -1 0 11 0.35417 1.00437 -1 0 -11-0.58372 1.02826 -1 0 11-0.56758 1.27907 1 0 11 0.09111 1.23702 -1 0 12 11.5091 1.46523 1 0 12 10.8072 1.39189 -1 0 -12 8.21977 1.22867 -1 0 12 9.46954 1.27927 1 0 12 9.64670 1.31038 -1 0 12 8.84332 1.60316 1 0 13 0.47815 1.34204 1 0 13 0.60669 1.18514 -1 0 13 0.89387 1.39464 -1 0 13 0.10143 1.59839 -1 0 -13 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6.26362 1.82111 -4 -15 -6 1.97732 1.93879 -4 -15 7 0.61885 1.76381 -4 -15 -7-0.21860 1.91905 -4 -15 8 0.49046 1.72754 -4 -15 -8 0.04462 2.01106 -4 -15 9 3.79683 1.72808 -4 -15 -9 4.34729 2.04575 -4 -15 10 3.71903 1.70134 -4 -15 -10 2.08229 2.04676 -4 -15 -11-1.31834 2.13755 4 -15 11 2.97432 2.54056 -4 -15 11-2.36020 1.65145 -4 -15 -12-1.65383 2.17402 4 -15 12 3.20710 2.57943 -4 -15 12 0.95983 1.59085 -4 -15 -13-0.49622 2.24345 4 -15 13-2.09447 2.72210 -4 -15 13 0.22938 1.56007 -4 -15 -14-0.45123 2.29215 4 -15 14-1.08606 2.87155 -4 -15 14-1.44033 1.57595 -4 -15 -15-0.87157 2.40255 4 -15 15 4.50428 3.01740 -4 -15 15-0.49326 1.57583 -4 -15 15-1.89155 2.61531 -4 -15 -16-1.05697 2.49734 -4 -15 16 4.55490 1.59477 4 -15 16-0.54809 3.07740 -4 -15 16 3.42723 2.72415 -4 -15 -17-2.19755 2.60877 -4 -15 17 1.98162 1.57860 4 -15 17-3.26483 3.23066 -4 -15 17-2.76840 2.81058 -4 -15 -18 1.74241 2.69532 -4 -15 18 4.92229 1.56089 -4 -15 18-1.99423 2.84002 -5 -15 0 1.41473 1.83591 -5 -15 1 5.37577 1.86155 -5 -15 -1-2.01391 1.88982 -5 -15 2 2.21170 1.81925 -5 -15 -2-0.82148 1.85485 -5 -15 3 1.69583 1.80073 -5 -15 -3 1.49864 1.92213 -5 -15 4 8.14036 1.92189 -5 -15 -4 7.44332 1.98937 -5 -15 5 4.77156 1.87114 -5 -15 -5 7.56755 1.98762 -5 -15 6 2.42278 1.80724 -5 -15 -6 4.26874 1.97208 -5 -15 7-1.81342 1.83537 -5 -15 -7-1.25963 1.95762 -5 -15 8 2.62625 1.72443 -5 -15 -8-1.87438 1.99112 -5 -15 9 4.19295 1.73765 -5 -15 -9 5.68229 2.11114 -5 -15 10 2.49428 1.69295 -5 -15 -10 0.52174 2.08168 -5 -15 -11 2.52001 2.16085 5 -15 11 3.68175 2.62650 -5 -15 11 1.02764 1.61311 -5 -15 -12 3.44870 2.18835 5 -15 12 7.62640 2.77557 -5 -15 12 5.57888 1.65692 -5 -15 -13-1.47588 2.27686 5 -15 13-3.31648 2.88265 -5 -15 13-1.08265 1.61889 -5 -15 -14-1.34963 2.35812 5 -15 14-0.92270 2.97020 -5 -15 14-0.54009 1.58274 -5 -15 -15 2.46395 2.38943 5 -15 15-1.22713 3.07216 -5 -15 15 1.26689 1.58783 -5 -15 -16 0.80371 2.45582 5 -15 16-2.61347 3.19707 -5 -15 16 2.33363 1.61431 -5 -15 -17 3.42259 2.57256 -5 -15 17 3.00848 1.62589 -5 -15 17-2.41294 2.76208 -6 -15 0 3.90890 1.88224 -6 -15 1 0.80185 1.91959 -6 -15 -1 1.42045 1.89944 -6 -15 2 0.61632 1.86294 -6 -15 -2 0.58190 1.88630 -6 -15 3 4.64775 1.87382 -6 -15 -3 6.56469 2.03039 -6 -15 4 1.31242 1.85280 -6 -15 -4 2.49817 1.95102 -6 -15 5 2.67802 1.85404 -6 -15 -5 0.91632 1.95277 -6 -15 6 2.05521 1.83191 -6 -15 -6 1.15269 1.98216 -6 -15 7-0.51981 1.81929 -6 -15 -7 0.37044 2.00208 -6 -15 8 1.96717 1.79613 -6 -15 -8-1.69377 2.03075 -6 -15 9 1.18018 1.75999 -6 -15 -9 0.86296 2.10326 -6 -15 10 0.04123 1.67638 -6 -15 -10 1.36437 2.03809 6 -15 11 1.41395 2.80912 -6 -15 11-1.66059 1.68669 -6 -15 -11-0.34755 2.14727 -6 -15 -12 4.05853 2.19185 6 -15 12-1.21499 2.88415 -6 -15 12 4.80197 1.68063 -6 -15 -13-0.10389 2.28307 6 -15 13-3.38799 3.03377 -6 -15 13 0.83374 1.62002 -6 -15 -14 0.90298 2.31886 6 -15 14 0.06872 3.12648 -6 -15 14-1.18293 1.59996 -6 -15 -15 2.42791 2.40798 6 -15 15-1.55872 3.22851 -6 -15 15 0.47448 1.65838 6 -15 16-2.41296 3.29866 -7 -15 0-1.01906 1.89764 -7 -15 1 7.79128 1.98930 -7 -15 -1 5.82365 1.97823 -7 -15 2 5.84574 1.96644 -7 -15 -2 6.54956 1.99975 -7 -15 3 2.49945 1.89175 -7 -15 -3 2.58553 1.96742 -7 -15 4-2.08441 1.88938 -7 -15 -4-0.04750 1.98094 -7 -15 5 2.08935 1.90597 -7 -15 -5-0.14250 1.99684 -7 -15 6 3.97513 1.90283 -7 -15 -6 1.00762 2.02561 -7 -15 7-0.17993 1.87526 -7 -15 -7 3.94679 2.04643 -7 -15 8 1.05879 1.78480 -7 -15 -8-0.04864 2.07879 -7 -15 9-0.82603 1.78205 -7 -15 -9-1.28303 2.07869 -7 -15 10 1.02702 1.75834 -7 -15 -10 0.45187 2.12804 7 -15 11-0.06395 2.88596 -7 -15 11-0.45999 1.72258 -7 -15 -11 1.27599 2.17016 -7 -15 -12-1.45832 2.21855 7 -15 12 1.65526 3.01608 -7 -15 12 0.28792 1.67577 -7 -15 -13-3.33062 2.24508 7 -15 13-0.34278 3.09268 -7 -15 13-0.77685 1.67067 -7 -15 -14 2.45465 2.34990 7 -15 14 0.99074 3.24065 -7 -15 14 2.53453 1.69231 7 -15 15 0.94957 3.34575 -8 -15 0 25.2223 2.50808 -8 -15 1 2.54322 1.97935 -8 -15 -1 2.98351 2.02587 -8 -15 2 8.50440 2.06357 -8 -15 -2 8.17074 2.08848 -8 -15 3 3.06997 1.95721 -8 -15 -3 5.81917 2.04422 -8 -15 4 0.37661 1.93265 -8 -15 -4 2.51726 2.05346 -8 -15 5 2.63989 1.95606 -8 -15 -5 4.83303 2.09904 -8 -15 6 1.54503 1.91578 -8 -15 -6-0.14927 2.02152 -8 -15 7 2.09895 1.87405 -8 -15 -7-1.04679 2.06686 -8 -15 8 3.56993 1.90051 -8 -15 -8 1.55959 2.13814 -8 -15 9-1.49263 1.84394 -8 -15 -9-0.45874 2.12228 -8 -15 10 1.64455 1.81014 -8 -15 -10 4.35074 2.21405 -8 -15 11 1.04947 1.75916 -8 -15 -11 2.36654 2.25383 -8 -15 12 0.47338 1.73735 -8 -15 -12 3.10917 2.26955 8 -15 13 1.56198 3.27274 8 -15 14 0.07329 3.37720 -9 -15 0 0.30177 2.00635 -9 -15 1 7.77921 2.09616 -9 -15 -1 1.00373 2.05775 -9 -15 2-0.59456 2.02618 -9 -15 -2-0.45393 2.02149 -9 -15 3 5.85780 2.02488 -9 -15 -3 2.80313 2.09013 -9 -15 4 0.58839 1.99294 -9 -15 -4 1.18275 2.11359 -9 -15 5 0.58638 1.98504 -9 -15 -5 3.28547 2.12883 -9 -15 6 1.85250 1.96319 -9 -15 -6 4.39666 2.14420 -9 -15 7-0.63151 1.96988 -9 -15 -7 3.54429 2.13243 -9 -15 8 2.25449 1.94157 -9 -15 -8 6.11095 2.18581 -9 -15 9 3.91609 1.91580 -9 -15 -9 0.95245 2.21446 -9 15 -13 12.2052 3.64063 -10 -15 0-2.10350 2.06558 -10 -15 1 2.57105 2.10228 -10 -15 -1-1.41678 2.11996 -10 -15 2 1.70785 2.09111 -10 -15 -2 1.31749 2.09788 -10 -15 3 4.32054 2.10433 -10 -15 -3 4.68689 2.16695 -10 -15 4 2.86065 2.07901 -10 -15 -4 3.91793 2.23802 -10 -15 5 3.72557 2.09757 -10 -15 -5 1.45177 2.18559 -4 -16 0-1.42470 1.97146 -4 -16 1 2.89046 1.98238 -4 -16 -1 0.49395 2.02492 -4 -16 2 2.64043 1.95296 -4 -16 -2-1.88258 2.04439 -4 -16 3-0.49188 1.98777 -4 -16 -3 2.61376 2.01354 -4 -16 4 2.30417 1.97411 -4 -16 -4 4.83462 2.08926 -4 -16 5 0.70928 1.95916 -4 -16 -5 1.22152 2.05712 -4 -16 6 2.75597 1.97395 -4 -16 -6 1.69567 2.04116 -4 -16 7 2.67970 1.92749 -4 -16 -7-1.21136 2.07009 -4 -16 8 5.02649 1.96575 -4 -16 -8 3.49849 2.16455 -4 -16 9 1.71843 1.87997 -4 -16 -9 2.01869 2.15833 -4 -16 -10 5.61583 2.23327 -5 -16 0-3.65105 2.02424 -5 -16 1 1.41221 1.95953 -5 -16 -1-1.84139 2.00385 -5 -16 2 4.98927 2.00849 -5 -16 -2 3.93950 2.04809 -5 -16 3 7.03338 2.02789 -5 -16 -3 5.91317 2.09948 -5 -16 4-1.85050 1.93897 -5 -16 -4-2.51290 2.03701 -5 -16 5 2.70176 1.92015 -5 -16 -5 0.32591 2.07163 -5 -16 6 0.81145 1.94928 -5 -16 -6 1.22007 2.06715 -5 -16 7-0.04504 1.91046 -5 -16 -7 5.79865 2.17553 -5 -16 8 4.16597 1.97258 -5 -16 -8 7.57690 2.21040 -5 -16 9-0.04424 1.85954 -5 -16 -9 0.24496 2.17151 -5 -16 10 1.00164 1.87263 -5 -16 -10 4.19305 2.30627 -5 -16 -11 0.10124 2.28010 -5 -16 11 0.04279 1.82642 -5 -16 -12-0.36537 2.37624 -5 -16 12-0.62943 1.76915 -5 -16 -13 3.23889 2.43368 -5 -16 13 1.02182 1.68852 -6 -16 0 16.3034 2.25006 -6 -16 1 4.17704 2.03520 -6 -16 -1 1.88707 2.03791 -6 -16 2 4.70654 2.02832 -6 -16 -2 2.10906 2.07305 -6 -16 3-0.60443 1.96852 -6 -16 -3 0.09528 2.08249 -6 -16 4-0.23065 1.94284 -6 -16 -4-1.77297 2.05471 -6 -16 5 0.91849 1.93973 -6 -16 -5 1.20101 2.07907 -6 -16 6-0.04588 1.93213 -6 -16 -6 1.49042 2.09125 -6 -16 7 8.46159 2.02995 -6 -16 -7 7.74052 2.18716 -6 -16 8-0.49943 1.90828 -6 -16 -8-0.74195 2.18155 -6 -16 9 0.40310 1.87626 -6 -16 -9-1.60448 2.19969 -6 -16 10-0.70418 1.83160 -6 -16 -10-1.06935 2.23429 -6 -16 -11-0.97399 2.28022 -6 -16 11 2.24744 1.85079 -6 -16 12 3.73174 1.80818 -7 -16 0 3.61948 2.04730 -7 -16 1 2.80230 2.03551 -7 -16 -1 0.82639 2.04476 -7 -16 2-0.91937 2.02754 -7 -16 -2 1.66949 2.11656 -7 -16 3-1.09803 1.99438 -7 -16 -3 1.53418 2.11257 -7 -16 4 3.31216 1.99091 -7 -16 -4 0.09878 2.07377 -7 -16 5 0.61164 1.94295 -7 -16 -5-3.03447 2.17922 -7 -16 6 1.68875 1.94037 -7 -16 -6 2.28924 2.13675 -7 -16 7 0.60788 1.92848 -7 -16 -7 1.05280 2.16101 -7 -16 8-2.31581 1.98202 -7 -16 -8 0.05070 2.17466 -7 -16 9 2.19104 1.89216 -7 -16 -9-1.28573 2.24637 -8 -16 0 4.38681 2.12784 -8 -16 1-0.74820 2.07917 -8 -16 -1 2.25985 2.09296 -8 -16 2 1.24792 2.09148 -8 -16 -2 4.61683 2.14808 -8 -16 3 10.6276 2.21038 -8 -16 -3 13.0907 2.27890 -8 -16 4 0.73075 2.06441 -8 -16 -4 0.61161 2.15446 -8 -16 5-0.04837 1.99776 -8 -16 -5 0.87237 2.14112 -8 -16 6 2.74778 2.03658 -8 -16 -6 0.46161 2.19511 -6 -17 0-0.45123 2.15732 -6 -17 1 5.02399 2.21341 -6 -17 -1-0.65980 2.24982 -6 -17 2-2.23198 2.18717 -6 -17 -2-1.61073 2.22550 -6 -17 3-0.64716 2.14961 -6 -17 -3 3.23292 2.25398 -6 -17 -4 1.26233 2.21793 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 83027 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -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 0.39820(8) 0.02181(11) 0.46721(6) 0.0273(4) Uani 1 1 d . . . . . C1 C 0.37373(12) 0.11442(16) 0.47596(8) 0.0212(5) Uani 1 1 d . . . . . N1 N 0.40083(9) 0.20153(12) 0.44883(6) 0.0203(4) Uani 1 1 d . . . . . C2 C 0.45859(11) 0.18689(16) 0.40405(8) 0.0226(5) Uani 1 1 d . . . . . H30 H 0.463885 0.258800 0.386497 0.027 Uiso 1 1 calc R U . . . C3 C 0.42571(13) 0.10950(17) 0.36239(8) 0.0302(5) Uani 1 1 d . . . . . H1 H 0.421881 0.036826 0.377403 0.045 Uiso 1 1 calc R U . . . H2 H 0.462558 0.108524 0.331929 0.045 Uiso 1 1 calc R U . . . H3 H 0.371556 0.133388 0.351053 0.045 Uiso 1 1 calc R U . . . C4 C 0.54347(12) 0.15667(18) 0.42380(9) 0.0299(5) Uani 1 1 d . . . . . H4 H 0.564218 0.214050 0.446777 0.045 Uiso 1 1 calc R U . . . H5 H 0.580142 0.147555 0.393581 0.045 Uiso 1 1 calc R U . . . H6 H 0.540508 0.089022 0.443728 0.045 Uiso 1 1 calc R U . . . C5 C 0.37288(12) 0.31240(15) 0.46010(8) 0.0236(5) Uani 1 1 d . . . . . H31 H 0.340940 0.309816 0.493714 0.028 Uiso 1 1 calc R U . . . C6 C 0.31568(13) 0.35263(18) 0.41693(9) 0.0341(6) Uani 1 1 d . . . . . H7 H 0.346471 0.363492 0.384183 0.051 Uiso 1 1 calc R U . . . H8 H 0.291120 0.421083 0.427920 0.051 Uiso 1 1 calc R U . . . H9 H 0.272685 0.299193 0.410926 0.051 Uiso 1 1 calc R U . . . C7 C 0.44417(13) 0.38889(16) 0.46897(9) 0.0305(5) Uani 1 1 d . . . . . H10 H 0.477624 0.362378 0.498295 0.046 Uiso 1 1 calc R U . . . H11 H 0.423444 0.460926 0.477511 0.046 Uiso 1 1 calc R U . . . H12 H 0.477326 0.392586 0.436823 0.046 Uiso 1 1 calc R U . . . C8 C 0.31436(12) 0.12974(15) 0.52090(8) 0.0213(5) Uani 1 1 d . . . . . C9 C 0.33997(11) 0.18000(15) 0.57672(8) 0.0206(5) Uani 1 1 d . . . . . C10 C 0.30350(12) 0.07624(15) 0.60429(8) 0.0224(5) Uani 1 1 d . . . . . H13 H 0.330622 0.034231 0.633069 0.027 Uiso 1 1 calc R U . . . C11 C 0.27789(12) 0.02987(16) 0.54928(8) 0.0238(5) Uani 1 1 d . . . . . H14 H 0.285811 -0.046587 0.537814 0.029 Uiso 1 1 calc R U . . . C12 C 0.19342(12) 0.08761(16) 0.55424(8) 0.0246(5) Uani 1 1 d . . . . . H15 H 0.139618 0.053700 0.546032 0.030 Uiso 1 1 calc R U . . . C13 C 0.22930(11) 0.18880(16) 0.52555(8) 0.0223(5) Uani 1 1 d . . . . . H16 H 0.201868 0.229835 0.496561 0.027 Uiso 1 1 calc R U . . . C14 C 0.25506(11) 0.23654(16) 0.58035(8) 0.0207(5) Uani 1 1 d . . . . . H17 H 0.246213 0.312956 0.591605 0.025 Uiso 1 1 calc R U . . . C15 C 0.21829(12) 0.13472(15) 0.60914(8) 0.0214(5) Uani 1 1 d . . . . . C16 C 0.42012(11) 0.22935(15) 0.58895(8) 0.0203(5) Uani 1 1 d . . . . . C17 C 0.42589(12) 0.33226(16) 0.61067(8) 0.0210(5) Uani 1 1 d . . . . . H34 H 0.377614 0.372561 0.616873 0.025 Uiso 1 1 calc R U . . . C18 C 0.50080(12) 0.37703(16) 0.62341(8) 0.0228(5) Uani 1 1 d . . . . . H35 H 0.503912 0.447348 0.638173 0.027 Uiso 1 1 calc R U . . . C19 C 0.57127(12) 0.31766(16) 0.61430(8) 0.0229(5) Uani 1 1 d . . . . . C20 C 0.56691(12) 0.21511(16) 0.59154(8) 0.0256(5) Uani 1 1 d . . . . . H36 H 0.615338 0.175465 0.584821 0.031 Uiso 1 1 calc R U . . . C21 C 0.49204(12) 0.17165(16) 0.57888(8) 0.0238(5) Uani 1 1 d . . . . . H37 H 0.489133 0.102136 0.563212 0.029 Uiso 1 1 calc R U . . . C22 C 0.64901(14) 0.36175(17) 0.62992(9) 0.0303(5) Uani 1 1 d . . . . . N2 N 0.70984(12) 0.39751(16) 0.64379(9) 0.0453(6) Uani 1 1 d . . . . . C23 C 0.16122(12) 0.13737(15) 0.65558(8) 0.0221(5) Uani 1 1 d . . . . . O2 O 0.09113(8) 0.10259(11) 0.65006(6) 0.0299(4) Uani 1 1 d . . . . . N3 N 0.18821(10) 0.18043(13) 0.70156(6) 0.0232(4) Uani 1 1 d . . . . . C24 C 0.27245(12) 0.22090(17) 0.70843(9) 0.0299(5) Uani 1 1 d . . . . . H32 H 0.301605 0.208311 0.674293 0.036 Uiso 1 1 calc R U . . . C25 C 0.31766(15) 0.1566(2) 0.75078(10) 0.0485(7) Uani 1 1 d . . . . . H18 H 0.291442 0.168036 0.785117 0.073 Uiso 1 1 calc R U . . . H19 H 0.374418 0.180849 0.752528 0.073 Uiso 1 1 calc R U . . . H20 H 0.316111 0.079733 0.741871 0.073 Uiso 1 1 calc R U . . . C26 C 0.27454(15) 0.34167(18) 0.71882(10) 0.0441(7) Uani 1 1 d . . . . . H21 H 0.244447 0.379328 0.690934 0.066 Uiso 1 1 calc R U . . . H22 H 0.331186 0.366602 0.719112 0.066 Uiso 1 1 calc R U . . . H23 H 0.249329 0.356889 0.753119 0.066 Uiso 1 1 calc R U . . . C27 C 0.13250(13) 0.19203(16) 0.74756(8) 0.0262(5) Uani 1 1 d . . . . . H33 H 0.165075 0.226275 0.776421 0.031 Uiso 1 1 calc R U . . . C28 C 0.10344(15) 0.08431(18) 0.76874(10) 0.0400(6) Uani 1 1 d . . . . . H24 H 0.071005 0.047571 0.741672 0.060 Uiso 1 1 calc R U . . . H25 H 0.069930 0.096076 0.800260 0.060 Uiso 1 1 calc R U . . . H26 H 0.150599 0.039673 0.777973 0.060 Uiso 1 1 calc R U . . . C29 C 0.06277(13) 0.26868(18) 0.73550(9) 0.0338(6) Uani 1 1 d . . . . . H27 H 0.084733 0.337542 0.722927 0.051 Uiso 1 1 calc R U . . . H28 H 0.030747 0.280780 0.767631 0.051 Uiso 1 1 calc R U . . . H29 H 0.027849 0.237166 0.708152 0.051 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 0.0287(8) 0.0220(8) 0.0310(9) -0.0009(7) 0.0061(7) 0.0045(7) C1 0.0172(10) 0.0243(12) 0.0220(12) -0.0015(10) -0.0013(9) 0.0001(10) N1 0.0198(9) 0.0187(9) 0.0223(10) -0.0007(8) 0.0044(7) 0.0010(8) C2 0.0195(11) 0.0264(11) 0.0220(12) 0.0000(10) 0.0056(9) -0.0005(9) C3 0.0294(12) 0.0339(13) 0.0274(13) -0.0060(11) 0.0060(10) -0.0026(11) C4 0.0200(11) 0.0337(13) 0.0359(13) -0.0019(11) 0.0043(10) -0.0005(10) C5 0.0239(11) 0.0199(11) 0.0269(12) 0.0005(10) 0.0065(9) 0.0015(10) C6 0.0315(13) 0.0305(13) 0.0402(15) 0.0044(11) 0.0013(11) 0.0080(11) C7 0.0362(13) 0.0247(12) 0.0308(13) -0.0031(10) 0.0093(11) -0.0043(11) C8 0.0201(11) 0.0221(11) 0.0216(11) 0.0005(9) -0.0003(9) -0.0015(9) C9 0.0161(10) 0.0210(11) 0.0247(11) 0.0000(9) 0.0010(9) 0.0004(9) C10 0.0220(11) 0.0218(11) 0.0235(12) 0.0028(9) 0.0019(9) -0.0008(9) C11 0.0273(12) 0.0190(11) 0.0250(12) -0.0009(10) 0.0046(9) -0.0035(10) C12 0.0189(11) 0.0288(12) 0.0262(12) -0.0026(10) 0.0010(9) -0.0079(10) C13 0.0160(11) 0.0288(12) 0.0220(11) 0.0003(10) -0.0007(9) 0.0005(9) C14 0.0181(10) 0.0207(11) 0.0234(11) -0.0008(9) 0.0014(9) 0.0000(9) C15 0.0181(10) 0.0238(11) 0.0225(12) 0.0014(9) -0.0011(9) -0.0031(9) C16 0.0202(11) 0.0209(11) 0.0197(12) 0.0035(9) 0.0008(9) -0.0005(9) C17 0.0169(11) 0.0223(11) 0.0239(12) 0.0008(10) 0.0017(9) 0.0023(9) C18 0.0251(12) 0.0208(11) 0.0226(12) 0.0020(9) 0.0003(9) -0.0024(10) C19 0.0197(11) 0.0233(11) 0.0258(12) 0.0040(10) -0.0007(9) -0.0037(10) C20 0.0170(11) 0.0288(12) 0.0311(13) 0.0022(10) 0.0039(9) 0.0026(10) C21 0.0216(12) 0.0228(11) 0.0270(12) -0.0009(10) 0.0007(9) 0.0031(10) C22 0.0233(13) 0.0299(13) 0.0375(14) 0.0065(11) -0.0009(11) 0.0001(11) N2 0.0266(11) 0.0426(12) 0.0666(15) 0.0089(11) -0.0118(11) -0.0047(10) C23 0.0213(12) 0.0204(11) 0.0245(13) 0.0023(10) 0.0030(9) -0.0012(9) O2 0.0225(8) 0.0372(9) 0.0300(9) -0.0050(7) 0.0046(7) -0.0109(7) N3 0.0198(9) 0.0304(10) 0.0193(10) -0.0009(8) 0.0010(7) -0.0026(8) C24 0.0222(12) 0.0400(13) 0.0275(13) -0.0054(11) -0.0012(10) -0.0054(11) C25 0.0327(14) 0.0723(18) 0.0404(16) -0.0003(14) -0.0084(12) 0.0006(14) C26 0.0433(15) 0.0455(15) 0.0436(16) -0.0160(13) 0.0102(12) -0.0205(13) C27 0.0271(12) 0.0315(12) 0.0200(12) -0.0026(10) 0.0044(9) -0.0004(10) C28 0.0496(16) 0.0386(14) 0.0318(14) 0.0047(12) 0.0136(12) -0.0021(12) C29 0.0330(13) 0.0392(13) 0.0292(13) -0.0037(11) 0.0045(11) 0.0063(11) 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 122.88(18) . . ? O1 C1 C8 117.48(18) . . ? N1 C1 C8 119.57(17) . . ? C1 N1 C5 122.83(16) . . ? C1 N1 C2 119.85(16) . . ? C5 N1 C2 117.27(15) . . ? N1 C2 C3 112.20(16) . . ? N1 C2 C4 111.21(16) . . ? C3 C2 C4 113.27(17) . . ? N1 C2 H30 106.6 . . ? C3 C2 H30 106.6 . . ? C4 C2 H30 106.6 . . ? C2 C3 H1 109.5 . . ? C2 C3 H2 109.5 . . ? H1 C3 H2 109.5 . . ? C2 C3 H3 109.5 . . ? H1 C3 H3 109.5 . . ? H2 C3 H3 109.5 . . ? C2 C4 H4 109.5 . . ? C2 C4 H5 109.5 . . ? H4 C4 H5 109.5 . . ? C2 C4 H6 109.5 . . ? H4 C4 H6 109.5 . . ? H5 C4 H6 109.5 . . ? N1 C5 C7 111.68(16) . . ? N1 C5 C6 110.95(17) . . ? C7 C5 C6 112.03(17) . . ? N1 C5 H31 107.3 . . ? C7 C5 H31 107.3 . . ? C6 C5 H31 107.3 . . ? C5 C6 H7 109.5 . . ? C5 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C5 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C5 C7 H10 109.5 . . ? C5 C7 H11 109.5 . . ? H10 C7 H11 109.5 . . ? C5 C7 H12 109.5 . . ? H10 C7 H12 109.5 . . ? H11 C7 H12 109.5 . . ? C1 C8 C11 119.83(17) . . ? C1 C8 C13 133.18(17) . . ? C11 C8 C13 89.69(15) . . ? C1 C8 C9 122.98(16) . . ? C11 C8 C9 90.20(14) . . ? C13 C8 C9 89.20(14) . . ? C16 C9 C14 126.41(16) . . ? C16 C9 C10 125.39(17) . . ? C14 C9 C10 90.08(14) . . ? C16 C9 C8 125.30(16) . . ? C14 C9 C8 89.56(14) . . ? C10 C9 C8 88.47(14) . . ? C11 C10 C15 89.99(15) . . ? C11 C10 C9 90.46(15) . . ? C15 C10 C9 89.77(14) . . ? C11 C10 H13 125.2 . . ? C15 C10 H13 125.2 . . ? C9 C10 H13 125.2 . . ? C8 C11 C10 90.86(14) . . ? C8 C11 C12 90.79(15) . . ? C10 C11 C12 89.92(15) . . ? C8 C11 H14 124.9 . . ? C10 C11 H14 124.9 . . ? C12 C11 H14 124.9 . . ? C15 C12 C13 90.84(14) . . ? C15 C12 C11 90.62(15) . . ? C13 C12 C11 89.77(14) . . ? C15 C12 H15 125.0 . . ? C13 C12 H15 125.0 . . ? C11 C12 H15 125.0 . . ? C12 C13 C14 89.63(15) . . ? C12 C13 C8 89.75(15) . . ? C14 C13 C8 90.15(14) . . ? C12 C13 H16 125.4 . . ? C14 C13 H16 125.4 . . ? C8 C13 H16 125.4 . . ? C9 C14 C13 91.09(14) . . ? C9 C14 C15 90.53(14) . . ? C13 C14 C15 90.19(14) . . ? C9 C14 H17 124.8 . . ? C13 C14 H17 124.8 . . ? C15 C14 H17 124.8 . . ? C23 C15 C12 122.74(16) . . ? C23 C15 C14 125.58(17) . . ? C12 C15 C14 89.34(14) . . ? C23 C15 C10 128.48(17) . . ? C12 C15 C10 89.47(14) . . ? C14 C15 C10 89.59(14) . . ? C17 C16 C21 118.78(18) . . ? C17 C16 C9 121.37(17) . . ? C21 C16 C9 119.85(17) . . ? C18 C17 C16 121.25(19) . . ? C18 C17 H34 119.4 . . ? C16 C17 H34 119.4 . . ? C17 C18 C19 119.14(19) . . ? C17 C18 H35 120.4 . . ? C19 C18 H35 120.4 . . ? C18 C19 C20 120.50(18) . . ? C18 C19 C22 119.31(18) . . ? C20 C19 C22 120.17(19) . . ? C21 C20 C19 119.77(19) . . ? C21 C20 H36 120.1 . . ? C19 C20 H36 120.1 . . ? C20 C21 C16 120.53(19) . . ? C20 C21 H37 119.7 . . ? C16 C21 H37 119.7 . . ? N2 C22 C19 178.0(3) . . ? O2 C23 N3 122.60(18) . . ? O2 C23 C15 118.93(18) . . ? N3 C23 C15 118.45(17) . . ? C23 N3 C24 122.66(17) . . ? C23 N3 C27 120.62(16) . . ? C24 N3 C27 116.69(16) . . ? N3 C24 C26 112.02(18) . . ? N3 C24 C25 111.04(18) . . ? C26 C24 C25 112.42(19) . . ? N3 C24 H32 107.0 . . ? C26 C24 H32 107.0 . . ? C25 C24 H32 107.0 . . ? C24 C25 H18 109.5 . . ? C24 C25 H19 109.5 . . ? H18 C25 H19 109.5 . . ? C24 C25 H20 109.5 . . ? H18 C25 H20 109.5 . . ? H19 C25 H20 109.5 . . ? C24 C26 H21 109.5 . . ? C24 C26 H22 109.5 . . ? H21 C26 H22 109.5 . . ? C24 C26 H23 109.5 . . ? H21 C26 H23 109.5 . . ? H22 C26 H23 109.5 . . ? N3 C27 C28 112.64(17) . . ? N3 C27 C29 111.50(17) . . ? C28 C27 C29 112.66(18) . . ? N3 C27 H33 106.5 . . ? C28 C27 H33 106.5 . . ? C29 C27 H33 106.5 . . ? C27 C28 H24 109.5 . . ? C27 C28 H25 109.5 . . ? H24 C28 H25 109.5 . . ? C27 C28 H26 109.5 . . ? H24 C28 H26 109.5 . . ? H25 C28 H26 109.5 . . ? C27 C29 H27 109.5 . . ? C27 C29 H28 109.5 . . ? H27 C29 H28 109.5 . . ? C27 C29 H29 109.5 . . ? H27 C29 H29 109.5 . . ? H28 C29 H29 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 1.237(2) . ? C1 N1 1.355(2) . ? C1 C8 1.510(3) . ? N1 C5 1.477(2) . ? N1 C2 1.489(2) . ? C2 C3 1.525(3) . ? C2 C4 1.527(3) . ? C2 H30 1.0000 . ? C3 H1 0.9800 . ? C3 H2 0.9800 . ? C3 H3 0.9800 . ? C4 H4 0.9800 . ? C4 H5 0.9800 . ? C4 H6 0.9800 . ? C5 C7 1.523(3) . ? C5 C6 1.525(3) . ? C5 H31 1.0000 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C7 H10 0.9800 . ? C7 H11 0.9800 . ? C7 H12 0.9800 . ? C8 C11 1.552(3) . ? C8 C13 1.581(3) . ? C8 C9 1.600(3) . ? C9 C16 1.484(3) . ? C9 C14 1.563(3) . ? C9 C10 1.581(3) . ? C10 C11 1.564(3) . ? C10 C15 1.580(3) . ? C10 H13 1.0000 . ? C11 C12 1.566(3) . ? C11 H14 1.0000 . ? C12 C15 1.562(3) . ? C12 C13 1.565(3) . ? C12 H15 1.0000 . ? C13 C14 1.566(3) . ? C13 H16 1.0000 . ? C14 C15 1.578(3) . ? C14 H17 1.0000 . ? C15 C23 1.504(3) . ? C16 C17 1.393(3) . ? C16 C21 1.404(3) . ? C17 C18 1.387(3) . ? C17 H34 0.9500 . ? C18 C19 1.391(3) . ? C18 H35 0.9500 . ? C19 C20 1.398(3) . ? C19 C22 1.444(3) . ? C20 C21 1.380(3) . ? C20 H36 0.9500 . ? C21 H37 0.9500 . ? C22 N2 1.148(3) . ? C23 O2 1.237(2) . ? C23 N3 1.355(2) . ? N3 C24 1.481(3) . ? N3 C27 1.488(3) . ? C24 C26 1.521(3) . ? C24 C25 1.528(3) . ? C24 H32 1.0000 . ? C25 H18 0.9800 . ? C25 H19 0.9800 . ? C25 H20 0.9800 . ? C26 H21 0.9800 . ? C26 H22 0.9800 . ? C26 H23 0.9800 . ? C27 C28 1.516(3) . ? C27 C29 1.519(3) . ? C27 H33 1.0000 . ? C28 H24 0.9800 . ? C28 H25 0.9800 . ? C28 H26 0.9800 . ? C29 H27 0.9800 . ? C29 H28 0.9800 . ? C29 H29 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 -178.64(18) . . . . ? C8 C1 N1 C5 -1.9(3) . . . . ? O1 C1 N1 C2 4.1(3) . . . . ? C8 C1 N1 C2 -179.25(17) . . . . ? C1 N1 C2 C3 55.4(2) . . . . ? C5 N1 C2 C3 -122.02(19) . . . . ? C1 N1 C2 C4 -72.6(2) . . . . ? C5 N1 C2 C4 109.96(19) . . . . ? C1 N1 C5 C7 127.34(19) . . . . ? C2 N1 C5 C7 -55.3(2) . . . . ? C1 N1 C5 C6 -106.9(2) . . . . ? C2 N1 C5 C6 70.5(2) . . . . ? O1 C1 C8 C11 -7.9(3) . . . . ? N1 C1 C8 C11 175.24(17) . . . . ? O1 C1 C8 C13 -129.9(2) . . . . ? N1 C1 C8 C13 53.3(3) . . . . ? O1 C1 C8 C9 104.3(2) . . . . ? N1 C1 C8 C9 -72.6(2) . . . . ? C1 C8 C9 C16 8.0(3) . . . . ? C11 C8 C9 C16 134.56(19) . . . . ? C13 C8 C9 C16 -135.76(19) . . . . ? C1 C8 C9 C14 144.23(18) . . . . ? C11 C8 C9 C14 -89.24(14) . . . . ? C13 C8 C9 C14 0.45(14) . . . . ? C1 C8 C9 C10 -125.68(18) . . . . ? C11 C8 C9 C10 0.85(14) . . . . ? C13 C8 C9 C10 90.54(14) . . . . ? C16 C9 C10 C11 -134.48(19) . . . . ? C14 C9 C10 C11 88.71(15) . . . . ? C8 C9 C10 C11 -0.84(14) . . . . ? C16 C9 C10 C15 135.53(19) . . . . ? C14 C9 C10 C15 -1.28(15) . . . . ? C8 C9 C10 C15 -90.83(14) . . . . ? C1 C8 C11 C10 128.15(18) . . . . ? C13 C8 C11 C10 -90.06(14) . . . . ? C9 C8 C11 C10 -0.86(14) . . . . ? C1 C8 C11 C12 -141.91(18) . . . . ? C13 C8 C11 C12 -0.12(15) . . . . ? C9 C8 C11 C12 89.07(14) . . . . ? C15 C10 C11 C8 90.64(15) . . . . ? C9 C10 C11 C8 0.87(14) . . . . ? C15 C10 C11 C12 -0.15(14) . . . . ? C9 C10 C11 C12 -89.92(14) . . . . ? C8 C11 C12 C15 -90.71(15) . . . . ? C10 C11 C12 C15 0.15(15) . . . . ? C8 C11 C12 C13 0.13(15) . . . . ? C10 C11 C12 C13 90.99(14) . . . . ? C15 C12 C13 C14 0.34(14) . . . . ? C11 C12 C13 C14 -90.28(14) . . . . ? C15 C12 C13 C8 90.49(14) . . . . ? C11 C12 C13 C8 -0.12(15) . . . . ? C1 C8 C13 C12 132.7(2) . . . . ? C11 C8 C13 C12 0.12(15) . . . . ? C9 C8 C13 C12 -90.08(14) . . . . ? C1 C8 C13 C14 -137.6(2) . . . . ? C11 C8 C13 C14 89.76(14) . . . . ? C9 C8 C13 C14 -0.45(14) . . . . ? C16 C9 C14 C13 135.0(2) . . . . ? C10 C9 C14 C13 -88.92(15) . . . . ? C8 C9 C14 C13 -0.45(14) . . . . ? C16 C9 C14 C15 -134.8(2) . . . . ? C10 C9 C14 C15 1.28(15) . . . . ? C8 C9 C14 C15 89.74(14) . . . . ? C12 C13 C14 C9 90.20(14) . . . . ? C8 C13 C14 C9 0.46(15) . . . . ? C12 C13 C14 C15 -0.34(14) . . . . ? C8 C13 C14 C15 -90.08(14) . . . . ? C13 C12 C15 C23 132.86(18) . . . . ? C11 C12 C15 C23 -137.36(18) . . . . ? C13 C12 C15 C14 -0.34(14) . . . . ? C11 C12 C15 C14 89.44(14) . . . . ? C13 C12 C15 C10 -89.93(14) . . . . ? C11 C12 C15 C10 -0.15(14) . . . . ? C9 C14 C15 C23 138.18(19) . . . . ? C13 C14 C15 C23 -130.73(19) . . . . ? C9 C14 C15 C12 -90.76(14) . . . . ? C13 C14 C15 C12 0.34(14) . . . . ? C9 C14 C15 C10 -1.28(15) . . . . ? C13 C14 C15 C10 89.81(14) . . . . ? C11 C10 C15 C23 133.3(2) . . . . ? C9 C10 C15 C23 -136.3(2) . . . . ? C11 C10 C15 C12 0.15(14) . . . . ? C9 C10 C15 C12 90.61(14) . . . . ? C11 C10 C15 C14 -89.19(14) . . . . ? C9 C10 C15 C14 1.27(15) . . . . ? C14 C9 C16 C17 6.6(3) . . . . ? C10 C9 C16 C17 -115.1(2) . . . . ? C8 C9 C16 C17 127.3(2) . . . . ? C14 C9 C16 C21 -173.75(19) . . . . ? C10 C9 C16 C21 64.5(3) . . . . ? C8 C9 C16 C21 -53.1(3) . . . . ? C21 C16 C17 C18 -1.4(3) . . . . ? C9 C16 C17 C18 178.21(18) . . . . ? C16 C17 C18 C19 -0.1(3) . . . . ? C17 C18 C19 C20 1.4(3) . . . . ? C17 C18 C19 C22 -176.93(19) . . . . ? C18 C19 C20 C21 -1.1(3) . . . . ? C22 C19 C20 C21 177.14(19) . . . . ? C19 C20 C21 C16 -0.4(3) . . . . ? C17 C16 C21 C20 1.7(3) . . . . ? C9 C16 C21 C20 -177.99(19) . . . . ? C12 C15 C23 O2 -1.3(3) . . . . ? C14 C15 C23 O2 115.0(2) . . . . ? C10 C15 C23 O2 -121.1(2) . . . . ? C12 C15 C23 N3 -179.64(17) . . . . ? C14 C15 C23 N3 -63.3(3) . . . . ? C10 C15 C23 N3 60.6(3) . . . . ? O2 C23 N3 C24 179.23(18) . . . . ? C15 C23 N3 C24 -2.5(3) . . . . ? O2 C23 N3 C27 -2.6(3) . . . . ? C15 C23 N3 C27 175.71(17) . . . . ? C23 N3 C24 C26 116.0(2) . . . . ? C27 N3 C24 C26 -62.3(2) . . . . ? C23 N3 C24 C25 -117.4(2) . . . . ? C27 N3 C24 C25 64.3(2) . . . . ? C23 N3 C27 C28 64.5(2) . . . . ? C24 N3 C27 C28 -117.3(2) . . . . ? C23 N3 C27 C29 -63.3(2) . . . . ? C24 N3 C27 C29 114.9(2) . . . . ?