#------------------------------------------------------------------------------ #$Date: 2024-12-06 18:39:13 +0200 (Fri, 06 Dec 2024) $ #$Revision: 296391 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/27/1572701.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_1572701 loop_ _publ_author_name 'Sun, Hui-Li' 'Zhang, Qiang-Sheng' 'Wang, Zhong-Hao' 'Huang, Yan-Ting' 'Pan, Mei' _publ_section_title ; Long-persistent luminescence by host-guest Förster resonance energy transfer. ; _journal_issue 42 _journal_name_full 'Chemical science' _journal_page_first 17600 _journal_page_last 17607 _journal_paper_doi 10.1039/d4sc04746j _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C22 H12 N2 O6, C3 H6 N O' _chemical_formula_sum 'C25 H18 N3 O7' _chemical_formula_weight 472.42 _chemical_name_systematic DPDA _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 mixed _atom_sites_solution_primary iterative _audit_creation_date 2023-12-06 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2023-12-06 deposited with the CCDC. 2024-09-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 8.5890(5) _cell_length_b 13.1840(8) _cell_length_c 39.0756(17) _cell_measurement_reflns_used 1629 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 40.6270 _cell_measurement_theta_min 2.2410 _cell_volume 4424.8(4) _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2013/2 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.344 _diffrn_measured_fraction_theta_max 0.959 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 46.00 72.00 0.50 5.00 -- 32.09-178.00 150.00 52 2 \w 81.00 106.00 0.50 5.00 -- 32.09-178.00 150.00 50 3 \w 31.00 57.00 0.50 5.00 -- 32.09 -82.00-164.00 52 4 \w -21.00 10.00 0.50 5.00 -- 32.09 -82.00-164.00 62 5 \w 18.00 105.00 0.50 5.00 -- 32.09 38.00 -60.00 174 6 \w -24.00 43.00 0.50 5.00 -- -32.41 19.00-120.00 134 7 \w -4.00 37.00 0.50 5.00 -- -32.41 82.00 -43.00 82 8 \w -54.00 -10.00 0.50 5.00 -- -32.41 82.00 -43.00 88 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0152945000 _diffrn_orient_matrix_UB_12 0.0237500000 _diffrn_orient_matrix_UB_13 0.0384448000 _diffrn_orient_matrix_UB_21 0.0869486000 _diffrn_orient_matrix_UB_22 0.0989920000 _diffrn_orient_matrix_UB_23 -0.0086216000 _diffrn_orient_matrix_UB_31 -0.1561989000 _diffrn_orient_matrix_UB_32 0.0573562000 _diffrn_orient_matrix_UB_33 -0.0010487000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_unetI/netI 0.0617 _diffrn_reflns_Laue_measured_fraction_full 0.344 _diffrn_reflns_Laue_measured_fraction_max 0.959 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 6322 _diffrn_reflns_point_group_measured_fraction_full 0.344 _diffrn_reflns_point_group_measured_fraction_max 0.959 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 41.083 _diffrn_reflns_theta_min 2.261 _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.887 _exptl_crystal_colour 'clear whiteish green' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier whiteish _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.418 _exptl_crystal_description needle _exptl_crystal_F_000 1960 _exptl_crystal_preparation 1 _exptl_crystal_recrystallization_method 1 _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.285 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.049 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 322 _refine_ls_number_reflns 1380 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0489 _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^)+(0.0938P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1236 _refine_ls_wR_factor_ref 0.1362 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1051 _reflns_number_total 1380 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc04746j10.cif _cod_data_source_block DPDA _cod_depositor_comments 'Adding full bibliography for 1572700--1572701.cif.' _cod_original_cell_volume 4424.9(4) _cod_database_code 1572701 _shelxl_version_number 2013-2 _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_max 0.991 _shelx_estimated_absorpt_t_min 0.991 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, {H33A,H33B,H33C} of C33, H16 of O16 At 1.5 times of: {H34A,H34B,H34C} of C34, H25 of O25 2.a Riding coordinates: C2(H2) 2.b Aromatic/amide H refined with riding coordinates: C23(H23), C9(H9), C22(H22), C13(H13), C12(H12), C5(H5), C19(H19), C20(H20), C10(H10) 2.c Idealised Me refined as rotating group: C34(H34A,H34B,H34C), C33(H33A,H33B,H33C) 2.d Idealised tetrahedral OH refined as rotating group: O25(H25) ; _shelx_res_file ; TITL exp_7884-O-QIAN_autored in Pbca #61 REM reset to Pbca #61 CELL 1.54184 8.58903 13.18405 39.07565 90 90 90 ZERR 8 0.00046 0.00078 0.00166 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 200 144 24 56 L.S. 4 PLAN 1 SIZE 0.01 0.01 0.01 TEMP -173 CONF MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.093800 FVAR 0.58725 O17 4 0.221798 0.462252 0.434899 11.00000 0.04470 0.02718 = 0.01242 0.00034 0.00639 -0.00928 O15 4 0.082462 0.154234 0.678070 11.00000 0.06439 0.02348 = 0.04048 0.00411 0.00479 -0.00056 N28 3 0.501380 0.697867 0.548363 11.00000 0.04166 0.03110 = 0.03066 0.00183 -0.00145 0.00125 O7 4 0.246948 0.514764 0.575160 11.00000 0.04858 0.02492 = 0.01174 0.00199 0.00213 -0.01372 C11 1 0.092355 0.315363 0.650221 11.00000 0.02876 0.02672 = 0.01322 -0.00137 0.00468 0.00252 C8 1 0.192388 0.445309 0.598607 11.00000 0.04308 0.03214 = 0.01596 -0.00748 0.00552 0.00163 C23 1 0.239816 0.633848 0.413372 11.00000 0.04029 0.02928 = 0.02145 -0.00081 0.00202 0.00554 AFIX 43 H23 2 0.174100 0.657748 0.431187 11.00000 -1.20000 AFIX 0 C9 1 0.242400 0.345401 0.599169 11.00000 0.03003 0.03746 = 0.02468 -0.01234 0.00184 0.00147 AFIX 43 H9 2 0.312075 0.321313 0.582126 11.00000 -1.20000 AFIX 0 C22 1 0.294138 0.700649 0.388415 11.00000 0.03843 0.01714 = 0.02563 -0.00152 -0.00221 0.00627 AFIX 43 H22 2 0.269331 0.770747 0.389819 11.00000 -1.20000 AFIX 0 C13 1 0.094260 0.481424 0.623851 11.00000 0.03431 0.02570 = 0.02455 0.00305 -0.00230 -0.00181 AFIX 43 H13 2 0.061083 0.550160 0.623659 11.00000 -1.20000 AFIX 0 C12 1 0.044711 0.416010 0.649512 11.00000 0.03593 0.03614 = 0.01759 -0.00448 0.00490 -0.00070 AFIX 43 H12 2 -0.022931 0.440550 0.666874 11.00000 -1.20000 AFIX 0 C21 1 0.384478 0.664894 0.361499 11.00000 0.03308 0.01624 = 0.01488 -0.00622 -0.00278 0.00266 C5 1 0.323524 0.553338 0.484880 11.00000 0.02407 0.01667 = 0.02860 0.00619 0.00083 -0.00205 AFIX 43 H5 2 0.383637 0.598500 0.471304 11.00000 -1.20000 AFIX 0 C29 1 0.055318 0.335713 0.474682 11.00000 0.03762 0.03318 = 0.01354 0.01163 0.00410 0.01120 C3 1 0.148647 0.413617 0.490097 11.00000 0.02800 0.02551 = 0.01836 -0.01200 -0.01095 -0.00224 C2 1 0.148640 0.421571 0.525686 11.00000 0.04372 0.01031 = 0.03020 0.00152 -0.00436 0.01327 AFIX 3 H2 2 0.164790 0.362101 0.535246 11.00000 -1.20000 AFIX 0 C18 1 0.281673 0.533345 0.412104 11.00000 0.03034 0.02650 = 0.02271 0.00529 -0.00058 -0.00230 C1 1 0.240316 0.496154 0.540592 11.00000 0.03640 0.01988 = 0.00982 0.00058 0.00077 0.00474 C6 1 0.326530 0.560502 0.520283 11.00000 0.03835 0.01571 = 0.00899 0.00123 -0.00121 -0.00196 C19 1 0.375396 0.496992 0.386210 11.00000 0.04302 0.03009 = 0.02087 -0.00026 0.00098 0.00444 AFIX 43 H19 2 0.405585 0.427680 0.385836 11.00000 -1.20000 AFIX 0 C20 1 0.425274 0.562785 0.360655 11.00000 0.04112 0.02995 = 0.01324 -0.00771 -0.00129 -0.00484 AFIX 43 H20 2 0.487769 0.537800 0.342453 11.00000 -1.20000 AFIX 0 C4 1 0.232454 0.480039 0.469534 11.00000 0.03242 0.02240 = 0.01573 0.00434 0.00583 -0.00137 O26 4 0.430952 0.828397 0.338284 11.00000 0.06119 0.02183 = 0.02880 0.00263 -0.00125 0.00206 O30 4 0.086282 0.682540 0.740369 11.00000 0.05827 0.03152 = 0.03163 -0.00072 -0.00251 0.01424 O16 4 -0.039925 0.287126 0.701724 11.00000 0.06498 0.04450 = 0.02352 0.00512 0.01449 -0.00107 H16 2 -0.055901 0.255169 0.720771 11.00000 -1.20000 C34 1 0.221394 0.534484 0.782836 11.00000 0.05624 0.04438 = 0.03333 -0.00565 0.00342 0.00263 AFIX 137 H34A 2 0.318643 0.567108 0.789971 11.00000 -1.50000 H34B 2 0.218656 0.464786 0.791533 11.00000 -1.50000 H34C 2 0.132743 0.572486 0.792050 11.00000 -1.50000 AFIX 0 N32 3 0.212628 0.533098 0.745371 11.00000 0.04091 0.03185 = 0.01916 -0.01958 0.01119 0.00069 C31 1 0.148020 0.605635 0.726975 11.00000 0.03059 0.02434 = 0.06237 0.02918 -0.01439 0.00518 O25 4 0.488108 0.691857 0.306806 11.00000 0.07130 0.03553 = 0.02047 0.00347 0.01185 0.00349 AFIX 147 H25 2 0.510385 0.735967 0.292087 11.00000 -1.50000 AFIX 0 C27 1 0.421997 0.637084 0.536080 11.00000 0.03357 0.02808 = 0.01802 0.00772 0.00737 0.00586 C 1 0.046964 0.243665 0.677512 11.00000 0.03649 0.04570 = 0.01297 -0.00332 0.00382 -0.01184 C24 1 0.437151 0.737108 0.335085 11.00000 0.03813 0.02640 = 0.02524 0.00542 -0.00140 0.00413 C33 1 0.292131 0.448106 0.729103 11.00000 0.05721 0.04791 = 0.03653 -0.00572 0.00189 0.00262 AFIX 137 H33A 2 0.281361 0.453460 0.704200 11.00000 -1.20000 H33B 2 0.245731 0.384283 0.736930 11.00000 -1.20000 H33C 2 0.402738 0.449451 0.735244 11.00000 -1.20000 AFIX 0 C10 1 0.189887 0.280140 0.624933 11.00000 0.03613 0.02775 = 0.02260 0.00963 -0.00232 -0.00457 AFIX 43 H10 2 0.221731 0.211134 0.624972 11.00000 -1.20000 AFIX 0 N1 3 -0.019740 0.272177 0.462436 11.00000 0.04522 0.03227 = 0.02809 0.00101 -0.00105 0.00630 HKLF 4 REM exp_7884-O-QIAN_autored in Pbca #61 REM R1 = 0.0489 for 1051 Fo > 4sig(Fo) and 0.0702 for all 1380 data REM 322 parameters refined using 0 restraints END WGHT 0.0938 0.0000 REM Highest difference peak 0.285, deepest hole -0.324, 1-sigma level 0.049 Q1 1 0.1555 0.5998 0.6927 11.00000 0.05 0.29 ; _shelx_res_checksum 88800 _shelx_hkl_file ; 0 0 2 1343.17 103.467 6 0 0 -2 1415.19 103.511 6 0 0 -3 0.39638 9.07956 6 0 0 -4 179.148 19.2725 6 0 0 -5 11.6821 16.5848 6 0 0 -6 632.659 45.9436 6 0 0 6 504.597 40.5793 1 0 0 -7 2.88872 25.7982 6 0 0 7-6.24336 10.4649 1 0 0 -8 1693.63 125.913 6 0 0 8 1614.36 122.512 1 0 0 9 9.64638 11.4046 1 0 0 -9 3.03030 29.8086 6 0 0 -10 2871.83 197.617 6 0 0 10 2537.30 194.240 1 0 0 -11-7.53329 31.0938 6 0 0 -12 601.943 56.6162 6 0 0 -13 17.7632 32.9102 6 0 0 -14 7457.29 433.914 6 0 0 14 5615.70 429.867 2 0 0 -15-3.00917 35.3563 6 0 0 -16 4707.38 356.482 6 0 0 -17 53.9150 39.6379 6 0 0 -18 5524.78 418.302 6 0 0 -19 30.7783 39.2963 6 0 0 -20 1245.29 104.972 6 0 0 -21-27.7659 40.4782 6 0 0 -22 1838.66 152.274 6 0 0 22 2051.54 160.515 7 0 0 23-6.35805 59.7977 7 0 0 24-25.3956 60.2451 7 0 0 25 78.5648 59.4376 7 0 0 26 309.864 58.2715 7 0 0 27 31.1792 49.2710 7 0 0 28-9.58381 45.7424 7 0 0 29 15.6362 41.7262 7 0 0 30 76.1719 41.5006 7 0 0 31-20.8249 40.6529 7 0 0 32 4.31707 41.1057 7 0 -1 0-0.62602 5.89363 5 0 -1 1-0.30417 7.17083 5 0 -1 3-4.68153 11.6415 5 0 -1 4 5.50263 14.5706 6 0 -1 4 5.42327 14.4932 5 0 -1 -4 5.38419 13.2897 6 0 -1 5 1.92585 17.9160 5 0 -1 -5-5.23945 18.0862 6 0 -1 5 10.4340 19.6361 6 0 -1 -6 28.6342 22.4003 6 0 1 6 10.1898 15.9944 6 0 -1 6 20.3373 21.6546 5 0 -1 6 19.7027 24.8950 6 0 -1 -7 14.2385 22.1288 6 0 1 -7-0.99900 22.4090 5 0 -1 -8-15.8346 24.8907 6 0 1 -9 9.44859 29.7577 6 0 -1 -9 3.59446 26.7348 6 0 1 -10 17.7732 29.6078 6 0 -1 -10-28.4907 28.8393 6 0 1 -11-16.7018 30.9726 6 0 -1 -11-21.0895 31.4094 6 0 1 11-12.1905 20.3682 1 0 1 -12 15.8115 30.4078 6 0 1 12 23.6898 18.2254 1 0 -1 -12 14.6338 30.3492 6 0 1 13-9.44206 18.4782 1 0 1 -13-16.5007 31.2492 6 0 -1 -13 3.95005 33.5390 6 0 -1 -14-17.6451 36.7503 6 0 1 14 16.6341 18.6907 1 0 1 -14 23.3915 31.6681 6 0 -1 -15-35.7217 38.6722 6 0 1 15 6.51762 18.8926 1 0 -1 -16-49.6911 40.2280 6 0 1 16 14.7170 19.3579 1 0 -1 -17 42.8322 41.6026 6 0 -1 -18-4.23622 42.2233 6 0 -1 -19-18.1606 43.0668 6 0 1 19 2.27644 13.3644 2 0 1 20 9.60659 9.91304 2 0 -1 -20-26.1378 39.3514 6 0 -1 -21-1.28009 41.1100 6 0 -1 -22 22.0902 43.5349 6 0 -1 22 84.8508 58.5089 7 0 -1 -23 51.8502 44.2022 6 0 -1 23 35.7191 57.6212 7 0 -1 24-101.360 59.0154 7 0 -1 -24 4.75649 44.4785 6 0 -1 25-34.5937 53.5305 7 0 -1 -25-11.7069 44.2405 6 0 -1 26 36.0911 52.5828 7 0 -1 -26-52.8451 45.6993 6 0 -1 27-1.88136 48.5664 7 0 1 28-18.5670 42.8664 7 0 -1 28-62.0715 43.3461 7 0 1 29 30.7294 39.9786 7 0 -1 29 6.02026 40.8520 7 0 -1 30 34.9902 42.8236 7 0 1 30-43.0754 38.8782 7 0 1 31 20.4657 39.6942 7 0 -1 31 12.8271 39.7671 7 0 1 32-57.2702 43.1844 7 0 -1 32-93.0200 43.4404 7 0 -2 0 5852.85 440.966 5 0 2 0 5924.54 441.085 5 0 -2 1 933.671 68.1831 5 0 2 1 819.269 68.1862 5 0 2 -1 912.211 68.8918 5 0 -2 2 18059.6 1255.01 5 0 2 -2 16353.4 1254.94 5 0 2 2 16047.0 1254.88 5 0 2 -3 11650.5 892.599 5 0 -2 3 12162.7 892.536 5 0 2 -4 6610.56 501.108 5 0 -2 4 6748.53 501.097 5 0 -2 -6 22154.1 1658.48 6 0 -2 -7 13626.1 1018.83 6 0 2 -7 13589.1 1017.95 1 0 2 -8 9910.67 736.847 1 0 -2 -8 9621.69 738.087 6 0 -2 -9 3819.34 288.642 6 0 -2 -10 179.844 31.3776 6 0 -2 -11 2150.70 165.218 6 0 -2 -12 942.057 77.3980 6 0 2 12 905.823 74.7736 1 0 2 13 1968.02 149.829 1 0 -2 -13 1924.65 151.603 6 0 2 14 7155.11 541.610 1 0 -2 -14 7292.34 542.844 6 0 2 15 4447.94 335.351 1 0 -2 -15 4436.49 337.049 6 0 2 16 353.854 38.3881 1 0 -2 -16 414.395 49.1854 6 0 -2 -17 324.966 51.2256 6 0 2 17 408.844 39.7715 1 0 2 18 636.730 58.0402 1 0 -2 -18 804.367 69.7624 6 0 2 19 8531.63 644.427 1 0 -2 -19 8692.63 647.371 6 0 2 20 3608.13 306.081 7 0 -2 20 4069.91 305.029 7 0 -2 -20 4185.22 304.826 6 0 -2 -21 301.968 49.7236 6 0 2 21 243.698 62.6533 7 0 -2 21 285.219 56.0742 7 0 -2 22 789.426 77.2371 7 0 -2 -22 635.768 69.0616 6 0 2 22 608.045 78.2755 7 0 2 23 1888.10 155.577 7 0 -2 23 2060.66 155.019 7 0 -2 -23 1745.09 152.339 6 0 2 24 892.622 87.5620 7 0 -2 24 797.410 87.5675 7 0 -2 -24 974.412 84.8810 6 0 2 25 151.973 48.7709 7 0 -2 25 156.292 48.9167 7 0 -2 -25 181.576 49.5010 6 0 -2 26 247.200 51.4268 7 0 2 26 130.371 48.9934 7 0 -2 -26 130.813 48.5186 6 0 -2 -27 156.476 50.3373 6 0 2 27 63.5087 40.8177 7 0 -2 27 159.920 43.4789 7 0 -2 28 596.001 64.3042 7 0 -2 -28 526.960 67.8111 6 0 2 28 585.487 61.9960 7 0 -2 -29 191.251 50.7338 6 0 2 29 286.048 44.9955 7 0 -2 29 211.291 46.5431 7 0 -2 30 451.227 54.7584 7 0 2 30 345.131 51.7424 7 0 -2 31 61.1375 43.4829 7 0 2 31-10.1949 39.0358 7 0 -2 -32 270.540 42.3462 4 0 2 -32 162.240 41.8420 4 0 2 32 285.679 46.6957 7 0 -2 32 220.491 48.7687 7 0 -3 0 7.30421 16.3266 5 0 3 0 16.8044 18.6400 5 0 3 1-2.67798 18.3723 5 0 3 -1-17.2587 19.5325 5 0 -3 1 17.8378 15.9034 5 0 3 -2 10.2710 18.1986 5 0 -3 -2 4.75982 6.29883 4 0 -3 2 10.9647 17.9132 5 0 3 2 22.8301 18.1481 5 0 3 -3-15.3373 20.9907 5 0 -3 3-8.20212 9.18298 7 0 3 3-22.8186 18.1933 5 0 3 3-14.2866 9.92737 7 0 3 4-0.82065 14.3718 7 0 -3 4-16.2938 12.6365 7 0 3 -4-6.19410 21.8302 5 0 3 -5 8.39405 22.5922 5 0 3 -6 21.1543 23.9732 5 0 3 -7-3.53666 16.4996 1 0 3 -7 6.70198 25.7861 5 0 -3 -8-1.35942 24.6491 6 0 3 -8 34.0900 25.4331 5 0 3 -8-10.3753 15.5868 1 0 3 -9 45.5134 26.7212 5 0 -3 -9 6.90907 28.1945 6 0 3 -9 7.66269 14.8050 1 0 -3 -10 22.0477 27.2317 6 0 3 -10 27.0585 26.8608 5 0 3 -10-0.93112 13.4889 1 0 -3 -11-26.6169 29.7470 6 0 3 -11 33.4049 28.6069 5 0 3 -12-9.01767 7.81310 2 0 -3 -12-37.4841 31.8247 6 0 -3 -13 3.44189 31.0387 6 0 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315.219 44.2152 5 -2 2 -15 325.439 40.5059 4 2 2 -16 1004.26 94.6283 5 -2 2 16 1172.54 91.2903 2 -2 2 16 1132.26 93.6104 7 -2 -2 16 1109.75 93.3089 7 -2 2 -16 1176.64 92.4641 4 -2 -2 -16 1157.70 92.5523 4 2 2 -17 3088.51 252.219 5 -2 2 17 3252.78 251.057 2 -2 -2 17 3389.92 252.883 7 -2 2 17 3172.74 252.711 7 -2 -2 -17 3445.00 252.226 4 -2 2 -17 3471.03 252.386 4 2 2 -18 1895.55 153.476 5 -2 2 18 1981.64 151.412 2 -2 -2 18 1943.78 154.002 7 -2 2 18 1915.63 154.512 7 -2 2 -18 2017.95 153.623 4 -2 -2 -18 1994.54 153.659 4 -2 2 19 6.98072 21.7773 2 -2 -2 -19-20.3402 29.7421 4 -2 2 -19-6.32155 29.2597 4 -2 -2 19 32.2976 32.2072 7 -2 2 19-20.4724 33.8510 7 2 2 -19 55.4377 34.0308 5 -2 -2 20-40.3141 34.0845 7 -2 2 20 37.8215 34.1316 7 -2 -2 -20-4.02849 31.1823 4 -2 2 -20 9.39845 31.6105 4 -2 -2 -21 1248.07 113.072 6 -2 -2 21 1425.92 112.247 7 -2 2 21 1279.54 111.664 7 -2 2 -21 1376.46 110.714 4 -2 -2 -21 1436.09 110.675 4 -2 2 -22 303.051 40.9814 4 -2 -2 22 306.561 44.0121 7 -2 2 22 207.116 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25.9970 3 -2 -4 -4 221.772 27.9038 3 -2 4 5 1976.74 151.471 8 -2 4 -5 2012.90 152.209 2 2 4 5 1808.85 154.043 5 -2 -4 5 2163.72 151.366 8 2 -4 -5 1921.23 149.793 6 -2 4 -6 907.621 76.1230 2 2 4 6 849.609 80.6216 5 2 -4 -6 981.776 73.4150 6 -2 4 6 894.558 75.7764 8 -2 -4 6 985.275 75.3293 8 -2 4 7 124.932 25.0687 8 -2 4 -7 103.692 25.4287 2 -2 -4 7 152.938 23.3617 8 2 -4 -7 121.835 20.0766 6 -2 -4 8 74.7034 23.5218 8 -2 4 -8 58.4448 21.8361 2 -2 4 8 73.7569 24.9202 8 2 -4 -8 100.007 20.0725 6 -2 4 -9 6347.19 473.207 2 -2 -4 9 6354.71 473.298 8 -2 4 9 6509.93 473.981 8 -2 -4 -9 6420.66 474.400 6 2 -4 -9 6062.30 472.232 6 -2 4 -10 2088.08 156.730 2 -2 -4 -10 2163.31 159.800 6 2 -4 -10 1973.76 155.988 6 2 -4 -11 2645.64 201.727 6 -2 -4 -11 2770.32 204.842 6 -2 4 -11 2472.81 202.376 4 -2 -4 -11 2827.08 202.993 4 -2 4 -12-2.28603 22.3789 4 -2 -4 -12-20.6127 23.1872 4 -2 -4 -12 24.7675 35.9278 6 2 -4 -12-1.59282 24.4117 6 -2 4 -13 24.6728 22.3936 4 -2 -4 -13 80.9887 24.8447 4 -2 -4 13 21.5227 26.5663 7 -2 4 13 62.9589 31.5300 7 -2 -4 -13 57.6045 36.5801 6 2 -4 -13 62.4180 25.7351 6 -2 4 13 112.263 32.0769 2 -2 4 -14 66.2719 23.4509 4 -2 -4 -14 82.6760 24.8294 4 -2 4 14 111.724 33.2934 7 -2 -4 14 81.0203 28.0540 7 -2 -4 -14 64.7913 35.9369 6 2 4 -14 131.850 39.1608 5 2 -4 -14 104.677 27.1736 6 -2 4 14 81.3315 30.8748 2 -2 4 -15 224.682 33.0294 4 -2 -4 -15 265.927 34.2234 4 -2 -4 15 356.035 37.2111 7 2 4 -15 260.522 46.1150 5 -2 4 15 258.134 40.6014 7 -2 -4 -15 328.337 43.5936 6 -2 4 15 330.027 38.1045 2 2 -4 -15 329.982 37.1407 6 -2 4 -16 35.2685 23.3500 4 -2 -4 -16 1.97433 24.8863 4 -2 -4 16 4.42992 27.5136 7 -2 4 16 8.97380 32.2000 7 2 4 -16 78.2383 39.5861 5 -2 -4 -16 60.7072 34.6580 6 -2 4 16 26.5503 28.9081 2 2 -4 -16 45.5575 27.4640 6 -2 4 -17 205.389 30.8725 4 -2 -4 -17 208.704 30.7861 4 2 4 -17 228.415 43.4999 5 -2 -4 17 280.581 34.8134 7 -2 4 17 273.632 39.3516 7 -2 -4 -17 217.912 40.2338 6 -2 4 17 171.765 33.1299 2 2 -4 -17 178.525 32.6080 6 -2 4 -18 341.144 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711.699 59.7142 8 -3 -2 -5 689.015 58.2802 6 -3 -2 5 637.203 58.4828 8 3 -2 -6 45.1169 20.7593 5 3 2 -6 11.5493 32.4394 5 -3 -2 6 26.3505 26.9321 8 -3 -2 -6 16.2339 30.7285 6 -3 2 6 10.9029 29.3925 8 3 -2 -7 2073.04 152.131 5 3 2 -7 2129.52 155.613 5 -3 -2 7 1970.33 154.482 8 -3 2 7 1943.23 154.983 8 -3 -2 -7 1816.50 154.312 6 -3 2 -7 1996.28 153.188 6 -3 2 -8 108.574 28.5945 6 -3 -2 8 95.5638 28.3408 8 3 -2 -8 104.441 25.5400 5 3 2 -8 190.304 34.4348 5 -3 2 8 94.7181 29.0953 8 -3 -2 -8 117.042 31.4516 6 -3 2 -9 181.296 31.2309 6 3 -2 -9 171.589 26.3056 5 -3 2 9 155.850 30.7176 8 -3 -2 9 143.754 29.4865 8 3 2 -9 130.556 33.4174 5 -3 -2 -9 121.450 35.2557 6 -3 2 -10 42.7818 31.9103 6 -3 2 10 23.8363 28.9656 8 3 -2 -10 64.1035 23.5730 5 3 2 -10 55.2043 32.5487 5 -3 -2 10 26.8417 27.9790 8 -3 -2 -10 47.3037 34.5843 6 3 -2 -11 805.211 65.9781 5 3 2 -11 943.431 72.1596 5 -3 -2 11 745.648 68.6705 8 -3 2 11 722.806 69.0358 8 -3 -2 -11 927.932 72.1771 6 -3 2 -11 741.338 69.9065 6 -3 2 -12 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-13 85.4064 46.0844 3 6 3 13 43.6835 49.0478 5 -6 -3 -13 62.1741 46.9147 6 6 3 -14 315.518 52.5906 5 -6 3 14 278.962 51.0258 8 -6 -3 14 211.377 46.3701 8 -6 3 -14 251.819 49.2972 3 -6 -3 -14 239.527 51.3423 3 6 3 14 265.409 55.4637 5 -6 -3 -14 228.537 51.2135 6 6 3 15 737.287 76.8970 5 -6 -3 15 622.587 72.0163 8 6 3 -15 714.433 73.9052 5 -6 3 15 576.792 74.5759 8 -6 3 -15 624.678 71.9191 3 -6 -3 -15 606.632 75.2537 6 6 3 -16 399.858 60.6618 5 -6 3 -16 436.864 56.8091 3 -6 -3 -16 350.412 60.9112 6 6 4 0-15.8371 45.3791 5 6 4 -1 376.966 57.0770 5 6 4 1 386.030 57.5170 5 6 4 -2 59.1760 47.5531 5 6 4 2 47.4423 48.2319 5 -6 -4 -2-83.0845 33.9530 6 6 4 -3 829.537 81.1144 5 6 4 3 964.910 83.5283 5 -6 -4 -3 715.210 72.8496 6 6 4 -4 78.9768 46.6933 5 6 4 4 85.6640 50.4282 5 -6 -4 -4 86.4611 36.9563 6 6 4 -5 340.651 54.0116 5 6 4 5 334.927 57.6495 5 -6 -4 -5 223.152 43.0687 6 6 4 -6 91.0396 44.7453 5 6 4 6 46.9506 51.9750 5 -6 -4 -6 9.07456 37.9366 6 6 4 -7 41.8436 44.5322 5 -6 -4 -7-38.4955 47.5896 3 6 4 7 41.3650 53.2419 5 -6 -4 -7 83.4053 41.2915 6 -6 4 8-2.50201 43.8445 8 -6 -4 8-16.8438 36.8964 8 6 4 -8 20.3751 42.5422 5 -6 4 -8-6.34652 45.9108 3 -6 -4 -8 49.2701 47.6455 3 6 4 8 70.5983 54.1924 5 -6 -4 -8-28.0546 39.7785 6 -6 4 9 25.4262 44.7607 8 -6 -4 9-42.5400 37.3308 8 6 4 -9-31.0672 43.0769 5 -6 4 -9-31.4038 45.0703 3 -6 -4 -9 77.5159 46.4015 3 6 4 9 45.0909 52.8252 5 -6 -4 -9 34.2902 37.7284 6 -6 4 10 20.7433 44.8603 8 -6 -4 10 4.31980 35.8290 8 6 4 -10 49.9179 48.4768 5 -6 4 -10 77.7206 43.0686 3 -6 -4 -10 58.7203 44.1801 3 6 4 10 54.6459 54.1725 5 -6 -4 -10-21.1197 41.1912 6 -6 4 11 65.9262 43.2442 8 -6 -4 11 6.57321 36.3067 8 6 4 -11-15.0134 49.2806 5 -6 4 -11-53.0152 43.1982 3 -6 -4 -11-21.7749 46.1795 3 6 4 11 55.1149 53.2367 5 -6 -4 -11-40.8282 43.1486 6 -6 4 12 2.69750 46.1681 8 -6 -4 12-26.8718 39.5394 8 6 4 -12 10.6927 47.8709 5 -6 4 -12-16.3653 42.0216 3 -6 -4 -12-8.75809 44.0127 3 6 4 12-2.40920 52.3087 5 -6 -4 -12 53.0451 42.1388 6 6 4 -13 63.6645 47.9868 5 -6 4 13 58.1503 46.9585 8 -6 -4 13 85.1168 39.6733 8 -6 4 -13 62.0722 44.0972 3 -6 -4 -13 116.591 45.7575 3 6 4 13 113.510 54.2744 5 -6 -4 -13 33.0151 45.0457 6 -6 4 -14 275.336 50.0469 3 -6 -4 -14 372.782 53.3102 3 -6 -4 -14 236.848 53.0942 6 6 5 0 188.224 50.9454 5 -6 -5 0 107.006 34.1189 6 6 5 -1-41.5024 48.7124 5 6 5 1-35.2433 52.0798 5 -6 -5 1 10.4099 32.3086 6 -6 -5 -1 16.1173 33.8790 6 6 5 -2 188.023 54.4819 5 6 5 2 212.831 53.1701 5 -6 -5 -2 160.587 38.5079 6 6 5 -3 25.7983 48.6943 5 6 5 3-2.27411 52.6897 5 -6 -5 -3 68.8397 35.9082 6 6 5 -4 1642.94 126.818 5 6 5 4 1589.33 127.705 5 -6 -5 -4 1276.26 116.988 6 6 5 5 472.868 61.2256 5 -6 -5 -5 314.160 45.2290 6 6 5 -6 28.5180 44.8330 5 6 5 6-9.66024 52.5517 5 -6 -5 -6-46.3141 39.7825 6 6 5 -7 101.824 44.4967 5 6 5 7 164.680 57.0349 5 -6 -5 -7 187.678 41.5031 6 6 5 -8 54.1408 45.4346 5 6 5 8 74.7999 57.2697 5 -6 -5 -8 39.8492 41.2389 6 6 5 -9 21.3246 47.6693 5 6 5 9-2.52469 54.0734 5 -6 -5 -9-1.71715 42.3587 6 6 5 -10 15.6236 48.8131 5 -6 -5 -10 46.2939 47.6676 3 6 5 10 69.3339 56.9189 5 -6 -5 -10-1.69309 40.7462 6 -6 5 11 81.7822 46.9127 8 -6 5 -11 87.5008 45.4490 3 -6 -5 -11-45.5148 47.9234 3 -6 -5 -11 18.5342 39.2764 6 -6 5 -12 169.239 46.5494 3 6 6 0 4846.47 296.121 5 -6 -6 0 3295.31 287.626 6 6 6 -1 188.025 53.8918 5 6 6 1 184.111 53.2533 5 -6 -6 1 137.268 37.1672 6 -6 -6 -1 60.7499 36.0255 6 6 6 -2 584.642 68.4337 5 6 6 2 611.290 68.7750 5 -6 -6 2 411.086 50.1913 6 -6 -6 -2 367.808 52.2776 6 -6 -6 -3 13.5876 36.2023 6 -6 -6 -4 136.988 39.9033 6 -6 -6 -5 108.575 38.2028 6 7 1 2-17.2373 39.8026 5 7 1 3-52.6147 40.6851 5 7 1 4 192.481 44.9737 5 7 1 5 392.014 54.4809 5 7 1 6 26.2193 42.6324 5 7 1 7-9.57653 43.4204 5 7 1 8-17.6416 43.5048 5 7 2 0 3.80990 43.6530 5 7 2 -1 1.89843 43.2486 5 7 2 1 1.91256 43.8463 5 7 2 -2-67.9152 44.6305 5 7 2 2 5.76711 43.2595 5 7 2 -3 83.6506 44.1193 5 7 2 3 74.2482 45.0032 5 7 2 -4 164.069 45.3006 5 7 2 4 184.332 49.7233 5 7 2 -5 92.0125 40.4235 5 7 2 5 145.390 47.8373 5 7 2 6-37.2986 46.1849 5 0 0 0 0.00 0.00 0 TITL exp_7884-O-QIAN_autored in Pbca REM Pbca (#61 in standard setting) CELL 1.54184 8.589033 13.184049 39.075646 90.0000 90.0000 90.0000 ZERR 19.00 0.000460 0.000776 0.001662 0.0000 0.0000 0.0000 LATT 1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N O UNIT 209.00 190.00 19.00 19.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0 TEMP -173 TREF HKLF 4 END ; _shelx_hkl_checksum 23334 _olex2_exptl_crystal_mounting_method 1 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.447 _oxdiff_exptl_absorpt_empirical_full_min 0.713 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 O17 O 0.2218(4) 0.4623(3) 0.43490(13) 0.0281(12) Uani 1 1 d . . . . . O15 O 0.0825(5) 0.1542(4) 0.67807(10) 0.0428(14) Uani 1 1 d . . . . . N28 N 0.5014(6) 0.6979(4) 0.54836(13) 0.0345(17) Uani 1 1 d . . . . . O7 O 0.2469(4) 0.5148(3) 0.57516(14) 0.0284(12) Uani 1 1 d . . . . . C11 C 0.0924(8) 0.3154(6) 0.65022(19) 0.0229(17) Uani 1 1 d . . . . . C8 C 0.1924(9) 0.4453(7) 0.59861(19) 0.0304(17) Uani 1 1 d . . . . . C23 C 0.2398(7) 0.6338(7) 0.41337(17) 0.0303(18) Uani 1 1 d . . . . . H23 H 0.1741 0.6577 0.4312 0.036 Uiso 1 1 calc R U . . . C9 C 0.2424(7) 0.3454(7) 0.59917(18) 0.0307(17) Uani 1 1 d . . . . . H9 H 0.3121 0.3213 0.5821 0.037 Uiso 1 1 calc R U . . . C22 C 0.2941(8) 0.7006(5) 0.3884(2) 0.0271(18) Uani 1 1 d . . . . . H22 H 0.2693 0.7707 0.3898 0.032 Uiso 1 1 calc R U . . . C13 C 0.0943(8) 0.4814(5) 0.6239(2) 0.0282(18) Uani 1 1 d . . . . . H13 H 0.0611 0.5502 0.6237 0.034 Uiso 1 1 calc R U . . . C12 C 0.0447(7) 0.4160(7) 0.64951(17) 0.0299(17) Uani 1 1 d . . . . . H12 H -0.0229 0.4406 0.6669 0.036 Uiso 1 1 calc R U . . . C21 C 0.3845(8) 0.6649(6) 0.36150(18) 0.0214(17) Uani 1 1 d . . . . . C5 C 0.3235(7) 0.5533(5) 0.4849(2) 0.0231(16) Uani 1 1 d . . . . . H5 H 0.3836 0.5985 0.4713 0.028 Uiso 1 1 calc R U . . . C29 C 0.0553(9) 0.3357(6) 0.47468(17) 0.028(2) Uani 1 1 d . . . . . C3 C 0.1486(8) 0.4136(5) 0.4901(2) 0.0240(17) Uani 1 1 d . . . . . C2 C 0.1486(7) 0.4216(5) 0.5257(2) 0.0281(17) Uani 1 1 d . . . . . H2 H 0.1648 0.3621 0.5352 0.034 Uiso 1 1 d R U . . . C18 C 0.2817(8) 0.5333(7) 0.4121(2) 0.0265(17) Uani 1 1 d . . . . . C1 C 0.2403(9) 0.4962(6) 0.5406(2) 0.0220(16) Uani 1 1 d . . . . . C6 C 0.3265(8) 0.5605(5) 0.5203(2) 0.0210(16) Uani 1 1 d . . . . . C19 C 0.3754(8) 0.4970(5) 0.3862(2) 0.0313(18) Uani 1 1 d . . . . . H19 H 0.4056 0.4277 0.3858 0.038 Uiso 1 1 calc R U . . . C20 C 0.4253(7) 0.5628(7) 0.36065(16) 0.0281(17) Uani 1 1 d . . . . . H20 H 0.4878 0.5378 0.3425 0.034 Uiso 1 1 calc R U . . . C4 C 0.2325(8) 0.4800(6) 0.4695(2) 0.0235(16) Uani 1 1 d . . . . . O26 O 0.4310(5) 0.8284(4) 0.33828(9) 0.0373(13) Uani 1 1 d . . . . . O30 O 0.0863(5) 0.6825(4) 0.74037(9) 0.0405(13) Uani 1 1 d . . . . . O16 O -0.0399(6) 0.2871(3) 0.70172(13) 0.0443(14) Uani 1 1 d . . . . . H16 H -0.056(7) 0.255(4) 0.7208(16) 0.053 Uiso 1 1 d . U . . . C34 C 0.2214(7) 0.5345(4) 0.78284(16) 0.0446(19) Uani 1 1 d . . . . . H34A H 0.3186 0.5671 0.7900 0.067 Uiso 1 1 calc R U . . . H34B H 0.2187 0.4648 0.7915 0.067 Uiso 1 1 calc R U . . . H34C H 0.1327 0.5725 0.7921 0.067 Uiso 1 1 calc R U . . . N32 N 0.2126(6) 0.5331(4) 0.74537(12) 0.0306(14) Uani 1 1 d . . . . . C31 C 0.1480(8) 0.6056(6) 0.72698(18) 0.039(2) Uani 1 1 d . . . . . O25 O 0.4881(5) 0.6919(3) 0.30681(11) 0.0424(13) Uani 1 1 d . . . . . H25 H 0.5104 0.7360 0.2921 0.064 Uiso 1 1 calc R U . . . C27 C 0.4220(8) 0.6371(6) 0.53608(17) 0.027(2) Uani 1 1 d . . . . . C C 0.0470(8) 0.2437(6) 0.67751(17) 0.0317(19) Uani 1 1 d . . . . . C24 C 0.4372(7) 0.7371(6) 0.33509(18) 0.0299(18) Uani 1 1 d . . . . . C33 C 0.2921(7) 0.4481(5) 0.72910(15) 0.047(2) Uani 1 1 d . . . . . H33A H 0.2814 0.4535 0.7042 0.057 Uiso 1 1 calc R U . . . H33B H 0.2457 0.3843 0.7369 0.057 Uiso 1 1 calc R U . . . H33C H 0.4027 0.4495 0.7352 0.057 Uiso 1 1 calc R U . . . C10 C 0.1899(8) 0.2801(5) 0.6249(2) 0.0288(18) Uani 1 1 d . . . . . H10 H 0.2217 0.2111 0.6250 0.035 Uiso 1 1 calc R U . . . N1 N -0.0197(7) 0.2722(4) 0.46244(13) 0.0352(17) Uani 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 O17 0.045(3) 0.027(3) 0.012(3) 0.000(3) 0.006(2) -0.009(2) O15 0.064(4) 0.023(3) 0.040(3) 0.004(3) 0.005(2) -0.001(3) N28 0.042(4) 0.031(4) 0.031(4) 0.002(3) -0.001(3) 0.001(3) O7 0.049(3) 0.025(3) 0.012(3) 0.002(3) 0.002(2) -0.014(2) C11 0.029(5) 0.027(7) 0.013(5) -0.001(5) 0.005(4) 0.003(4) C8 0.043(5) 0.032(7) 0.016(6) -0.007(5) 0.006(4) 0.002(5) C23 0.040(5) 0.029(6) 0.021(5) -0.001(5) 0.002(4) 0.006(5) C9 0.030(4) 0.037(6) 0.025(6) -0.012(5) 0.002(4) 0.001(5) C22 0.038(5) 0.017(5) 0.026(4) -0.002(5) -0.002(4) 0.006(4) C13 0.034(5) 0.026(5) 0.025(5) 0.003(6) -0.002(4) -0.002(4) C12 0.036(5) 0.036(6) 0.018(5) -0.004(5) 0.005(4) -0.001(5) C21 0.033(5) 0.016(7) 0.015(6) -0.006(5) -0.003(4) 0.003(4) C5 0.024(5) 0.017(5) 0.029(7) 0.006(4) 0.001(4) -0.002(4) C29 0.038(5) 0.033(6) 0.014(5) 0.012(4) 0.004(4) 0.011(5) C3 0.028(5) 0.026(6) 0.018(7) -0.012(5) -0.011(5) -0.002(4) C2 0.044(5) 0.010(5) 0.030(7) 0.002(4) -0.004(4) 0.013(4) C18 0.030(5) 0.026(7) 0.023(6) 0.005(5) -0.001(4) -0.002(4) C1 0.036(5) 0.020(5) 0.010(6) 0.001(6) 0.001(5) 0.005(4) C6 0.038(5) 0.016(5) 0.009(7) 0.001(5) -0.001(5) -0.002(4) C19 0.043(5) 0.030(5) 0.021(4) 0.000(6) 0.001(4) 0.004(4) C20 0.041(5) 0.030(6) 0.013(5) -0.008(5) -0.001(4) -0.005(5) C4 0.032(5) 0.022(5) 0.016(6) 0.004(6) 0.006(5) -0.001(4) O26 0.061(3) 0.022(3) 0.029(3) 0.003(3) -0.001(2) 0.002(3) O30 0.058(3) 0.032(3) 0.032(3) -0.001(2) -0.003(2) 0.014(3) O16 0.065(3) 0.045(4) 0.024(3) 0.005(2) 0.014(3) -0.001(3) C34 0.056(5) 0.044(5) 0.033(5) -0.006(3) 0.003(4) 0.003(4) N32 0.041(3) 0.032(4) 0.019(4) -0.020(3) 0.011(3) 0.001(3) C31 0.031(5) 0.024(5) 0.062(6) 0.029(5) -0.014(4) 0.005(4) O25 0.071(4) 0.036(3) 0.020(3) 0.003(2) 0.012(3) 0.003(3) C27 0.034(6) 0.028(6) 0.018(5) 0.008(4) 0.007(4) 0.006(4) C 0.036(5) 0.046(7) 0.013(5) -0.003(6) 0.004(4) -0.012(5) C24 0.038(5) 0.026(6) 0.025(5) 0.005(6) -0.001(4) 0.004(5) C33 0.057(5) 0.048(5) 0.037(4) -0.006(4) 0.002(4) 0.003(4) C10 0.036(5) 0.028(5) 0.023(4) 0.010(5) -0.002(4) -0.005(5) N1 0.045(4) 0.032(4) 0.028(4) 0.001(3) -0.001(3) 0.006(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 C4 O17 C18 119.3(5) . . ? C1 O7 C8 121.4(5) . . ? C12 C11 C 123.2(8) . . ? C10 C11 C12 119.2(6) . . ? C10 C11 C 117.6(8) . . ? O7 C8 C9 122.5(8) . . ? O7 C8 C13 116.9(8) . . ? C13 C8 C9 120.3(7) . . ? C22 C23 H23 120.1 . . ? C18 C23 H23 120.1 . . ? C18 C23 C22 119.8(6) . . ? C8 C9 H9 120.1 . . ? C8 C9 C10 119.7(6) . . ? C10 C9 H9 120.1 . . ? C23 C22 H22 119.9 . . ? C21 C22 C23 120.1(6) . . ? C21 C22 H22 119.9 . . ? C8 C13 H13 120.4 . . ? C8 C13 C12 119.2(6) . . ? C12 C13 H13 120.4 . . ? C11 C12 C13 121.1(6) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C22 C21 C20 119.1(6) . . ? C22 C21 C24 118.8(7) . . ? C20 C21 C24 122.0(8) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C4 C5 C6 119.4(6) . . ? N1 C29 C3 179.4(8) . . ? C2 C3 C29 118.2(9) . . ? C4 C3 C29 119.8(8) . . ? C4 C3 C2 122.0(6) . . ? C3 C2 H2 110.9 . . ? C1 C2 C3 118.1(6) . . ? C1 C2 H2 111.3 . . ? C23 C18 O17 122.0(8) . . ? C23 C18 C19 121.0(6) . . ? C19 C18 O17 116.8(8) . . ? O7 C1 C2 124.2(8) . . ? O7 C1 C6 115.7(8) . . ? C6 C1 C2 120.0(6) . . ? C5 C6 C27 119.1(8) . . ? C1 C6 C5 121.5(6) . . ? C1 C6 C27 119.4(8) . . ? C18 C19 H19 120.3 . . ? C18 C19 C20 119.3(6) . . ? C20 C19 H19 120.3 . . ? C21 C20 H20 119.7 . . ? C19 C20 C21 120.6(6) . . ? C19 C20 H20 119.7 . . ? O17 C4 C5 125.7(8) . . ? O17 C4 C3 115.3(8) . . ? C5 C4 C3 118.9(6) . . ? C O16 H16 119(4) . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N32 C34 H34A 109.5 . . ? N32 C34 H34B 109.5 . . ? N32 C34 H34C 109.5 . . ? C31 N32 C34 123.8(5) . . ? C31 N32 C33 121.1(6) . . ? C33 N32 C34 114.9(5) . . ? O30 C31 N32 122.3(6) . . ? C24 O25 H25 109.5 . . ? N28 C27 C6 178.5(7) . . ? O15 C C11 124.5(7) . . ? O15 C O16 122.9(6) . . ? O16 C C11 112.6(7) . . ? O26 C24 C21 123.8(6) . . ? O26 C24 O25 123.1(6) . . ? O25 C24 C21 113.1(6) . . ? N32 C33 H33A 109.5 . . ? N32 C33 H33B 109.5 . . ? N32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C11 C10 C9 120.4(6) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? 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 O17 C18 1.392(7) . ? O17 C4 1.377(7) . ? O15 C 1.218(7) . ? N28 C27 1.156(8) . ? O7 C8 1.378(7) . ? O7 C1 1.374(7) . ? C11 C12 1.389(7) . ? C11 C 1.477(9) . ? C11 C10 1.376(7) . ? C8 C9 1.386(8) . ? C8 C13 1.382(8) . ? C23 H23 0.9500 . ? C23 C22 1.394(7) . ? C23 C18 1.374(7) . ? C9 H9 0.9500 . ? C9 C10 1.399(8) . ? C22 H22 0.9500 . ? C22 C21 1.389(7) . ? C13 H13 0.9500 . ? C13 C12 1.389(7) . ? C12 H12 0.9500 . ? C21 C20 1.391(7) . ? C21 C24 1.475(8) . ? C5 H5 0.9500 . ? C5 C6 1.387(7) . ? C5 C4 1.380(8) . ? C29 C3 1.435(10) . ? C29 N1 1.160(8) . ? C3 C2 1.395(7) . ? C3 C4 1.389(8) . ? C2 H2 0.8795 . ? C2 C1 1.388(8) . ? C18 C19 1.379(8) . ? C1 C6 1.378(8) . ? C6 C27 1.440(9) . ? C19 H19 0.9500 . ? C19 C20 1.390(8) . ? C20 H20 0.9500 . ? O26 C24 1.211(7) . ? O30 C31 1.258(7) . ? O16 H16 0.87(6) . ? O16 C 1.334(8) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C34 N32 1.466(7) . ? N32 C31 1.319(7) . ? N32 C33 1.458(7) . ? O25 H25 0.8400 . ? O25 C24 1.330(7) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C10 H10 0.9500 . ? 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 O17 C18 C19 C20 173.4(5) . . . . ? O7 C8 C9 C10 176.1(5) . . . . ? O7 C8 C13 C12 -175.5(5) . . . . ? O7 C1 C6 C5 -176.6(5) . . . . ? O7 C1 C6 C27 3.4(8) . . . . ? C8 O7 C1 C2 16.1(8) . . . . ? C8 O7 C1 C6 -167.0(5) . . . . ? C8 C9 C10 C11 -1.8(8) . . . . ? C8 C13 C12 C11 0.1(8) . . . . ? C23 C22 C21 C20 -2.8(8) . . . . ? C23 C22 C21 C24 178.6(5) . . . . ? C23 C18 C19 C20 -1.4(8) . . . . ? C9 C8 C13 C12 -0.9(8) . . . . ? C22 C23 C18 O17 -175.3(5) . . . . ? C22 C23 C18 C19 -0.8(8) . . . . ? C22 C21 C20 C19 0.5(8) . . . . ? C22 C21 C24 O26 13.8(9) . . . . ? C22 C21 C24 O25 -164.3(5) . . . . ? C13 C8 C9 C10 1.7(8) . . . . ? C12 C11 C O15 177.2(5) . . . . ? C12 C11 C O16 -2.0(8) . . . . ? C12 C11 C10 C9 1.1(8) . . . . ? C29 C3 C2 C1 179.3(5) . . . . ? C29 C3 C4 O17 -2.1(7) . . . . ? C29 C3 C4 C5 -178.9(5) . . . . ? C3 C2 C1 O7 177.6(5) . . . . ? C3 C2 C1 C6 0.8(8) . . . . ? C2 C3 C4 O17 179.6(5) . . . . ? C2 C3 C4 C5 2.8(8) . . . . ? C2 C1 C6 C5 0.5(8) . . . . ? C2 C1 C6 C27 -179.6(5) . . . . ? C18 O17 C4 C5 -13.1(8) . . . . ? C18 O17 C4 C3 170.3(5) . . . . ? C18 C23 C22 C21 2.9(8) . . . . ? C18 C19 C20 C21 1.5(8) . . . . ? C1 O7 C8 C9 54.2(7) . . . . ? C1 O7 C8 C13 -131.3(5) . . . . ? C6 C5 C4 O17 -177.9(5) . . . . ? C6 C5 C4 C3 -1.5(8) . . . . ? C20 C21 C24 O26 -164.8(5) . . . . ? C20 C21 C24 O25 17.1(8) . . . . ? C4 O17 C18 C23 -53.3(7) . . . . ? C4 O17 C18 C19 132.0(5) . . . . ? C4 C5 C6 C1 -0.1(8) . . . . ? C4 C5 C6 C27 179.9(5) . . . . ? C4 C3 C2 C1 -2.4(8) . . . . ? C34 N32 C31 O30 -0.8(9) . . . . ? C C11 C12 C13 178.0(5) . . . . ? C C11 C10 C9 -177.3(5) . . . . ? C24 C21 C20 C19 179.1(5) . . . . ? C33 N32 C31 O30 -176.0(5) . . . . ? C10 C11 C12 C13 -0.2(8) . . . . ? C10 C11 C O15 -4.5(9) . . . . ? C10 C11 C O16 176.3(5) . . . . ?