#------------------------------------------------------------------------------ #$Date: 2019-05-24 05:17:41 +0300 (Fri, 24 May 2019) $ #$Revision: 215468 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021645.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2021645 loop_ _publ_author_name 'Ren, Xiu-Hui' 'Li, Gang-Yuan' 'Du, Hua' 'Ma, Jian-Ping' 'Geng, Yan' 'Dong, Yu-bin' _publ_section_title ; Thermally activated delayed fluorescent (TADF) coordination polymer with the generation of singlet oxygen ; _journal_coeditor_code YP3184 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229619006119 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac 'C39 H26 N2 O4' _chemical_formula_moiety 'C39 H26 N2 O4' _chemical_formula_sum 'C39 H26 N2 O4' _chemical_formula_weight 586.62 _chemical_name_systematic ; 4,4'-{9,9'-Spirobi[10H-acridine]-10,10'-diyl}dibenzoic acid ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _cell_angle_alpha 65.029(7) _cell_angle_beta 75.294(7) _cell_angle_gamma 68.420(7) _cell_formula_units_Z 2 _cell_length_a 12.6717(10) _cell_length_b 13.0727(9) _cell_length_c 13.9254(11) _cell_measurement_reflns_used 3153 _cell_measurement_temperature 293.86(10) _cell_measurement_theta_max 70.5540 _cell_measurement_theta_min 7.0410 _cell_volume 1931.2(3) _computing_cell_refinement ; CrysAlis PRO (Rigaku OD, 2015) ; _computing_data_collection ; CrysAlis PRO (Rigaku OD, 2015) ; _computing_data_reduction ; CrysAlis PRO (Rigaku OD, 2015) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL97 (Sheldrick, 2008) ; _computing_structure_solution ; olex2.solve (Bourhis et al., 2015) ; _diffrn_ambient_temperature 293.86(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0793 _diffrn_measured_fraction_theta_full 0.9983 _diffrn_measured_fraction_theta_max 0.9767 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku SuperNova Dual Source diffractometer with an Eos detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_unetI/netI 0.0362 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 13193 _diffrn_reflns_theta_full 70.95 _diffrn_reflns_theta_max 70.94 _diffrn_reflns_theta_min 3.53 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.527 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.84811 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO (Rigaku OD, 2015) ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_density_diffrn 1.009 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 612 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.207 _refine_diff_density_min -0.193 _refine_ls_extinction_coef 0.0008(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL97 (Sheldrick, 2008) ; _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 409 _refine_ls_number_reflns 7278 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.096 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0569 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0968P)^2^+0.1740P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1852 _refine_ls_wR_factor_ref 0.1997 _reflns_number_gt 4599 _reflns_number_total 7278 _reflns_threshold_expression >2sigma(I) _cod_data_source_file yp3184sup1.cif _cod_data_source_block L _cod_database_code 2021645 _shelx_res_file ; TITL exp_2611 in P-1 #2 CELL 1.54184 12.67173 13.07272 13.92537 65.0292 75.294 68.4197 ZERR 2 0.00098 0.00093 0.00111 0.0073 0.0068 0.0069 LATT 1 SFAC C H O N UNIT 78 52 8 4 EQIV $1 2-X,1-Y,-Z L.S. 4 PLAN 20 HTAB O3 O4_$1 BOND $h htab 2 conf fmap 2 acta REM D:/% & 6('#& /20180404/2611-gengyan/olex2_exp_2611/exp_2611_sqd.hkl 4sig(Fo) and 0.0821 for all 7278 data REM 409 parameters refined using 0 restraints END WGHT 0.0959 0.1784 REM Highest difference peak 0.207, deepest hole -0.193, 1-sigma level 0.037 Q1 1 -0.1102 0.8988 1.1548 11.00000 0.05 0.21 Q2 1 0.4838 0.7396 0.6877 11.00000 0.05 0.19 Q3 1 0.4806 0.6444 0.7182 11.00000 0.05 0.18 Q4 1 -0.0108 0.9225 1.2045 11.00000 0.05 0.17 Q5 1 0.4920 0.6798 0.6243 11.00000 0.05 0.15 Q6 1 0.4976 0.6659 0.5482 11.00000 0.05 0.15 Q7 1 0.6186 0.5596 0.8472 11.00000 0.05 0.14 Q8 1 0.4336 0.7970 0.7341 11.00000 0.05 0.14 Q9 1 0.5003 0.6946 0.5302 11.00000 0.05 0.14 Q10 1 0.8777 0.5388 0.1916 11.00000 0.05 0.14 Q11 1 -0.0054 0.8752 1.4433 11.00000 0.05 0.14 Q12 1 0.6747 0.6411 0.6056 11.00000 0.05 0.14 Q13 1 0.8672 0.5846 0.8099 11.00000 0.05 0.14 Q14 1 0.4566 0.7835 0.7554 11.00000 0.05 0.13 Q15 1 0.8393 0.5737 0.2138 11.00000 0.05 0.12 Q16 1 0.6541 0.5764 0.6500 11.00000 0.05 0.12 Q17 1 0.0410 0.7619 1.2973 11.00000 0.05 0.12 Q18 1 0.8282 0.5800 0.6964 11.00000 0.05 0.12 Q19 1 0.2997 0.7641 0.6536 11.00000 0.05 0.12 Q20 1 0.8995 0.5736 0.4819 11.00000 0.05 0.12 REM The information below was added by Olex2. REM REM R1 = 0.0569 for 4599 Fo > 4sig(Fo) and 0.0821 for all 13193 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.21, deepest hole -0.19 REM Mean Shift 0, Max Shift 0. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0821 REM R1_gt = 0.0569 REM wR_ref = 0.1997 REM GOOF = 1.096 REM Shift_max = 0 REM Shift_mean = 0 REM Reflections_all = 13193 REM Reflections_gt = 4599 REM Parameters = n/a REM Hole = 0.21 REM Peak = -0.19 REM Flack = n/a ; loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity C C22 0.53570(17) 0.67838(18) 0.48653(15) 0.0406(4) Uani d . 1 1 N N1 0.65184(15) 0.62169(18) 0.49259(14) 0.0519(5) Uani d . 1 1 C C27 0.46400(17) 0.70674(17) 0.57183(15) 0.0383(4) Uani d . 1 1 C C1 0.50747(17) 0.67556(17) 0.67685(15) 0.0387(4) Uani d . 1 1 N N2 0.33683(17) 0.72755(17) 0.85048(15) 0.0564(5) Uani d . 1 1 C C9 0.37209(19) 0.61385(19) 0.84749(16) 0.0465(5) Uani d . 1 1 O O3 0.94039(18) 0.41989(18) 0.12965(16) 0.0796(6) Uani d . 1 1 H H3 0.9798 0.4149 0.0742 0.119 Uiso calc R 1 1 C C15 0.63745(18) 0.62050(18) 0.67021(16) 0.0432(5) Uani d . 1 1 C C20 0.70306(17) 0.59262(18) 0.58282(16) 0.0446(5) Uani d . 1 1 C C7 0.39304(19) 0.81187(19) 0.78121(16) 0.0477(5) Uani d . 1 1 C C23 0.48805(19) 0.7091(2) 0.39345(17) 0.0497(5) Uani d . 1 1 H H23 0.5351 0.6909 0.3360 0.060 Uiso calc R 1 1 C C26 0.34906(18) 0.76437(19) 0.56126(16) 0.0459(5) Uani d . 1 1 H H26 0.3014 0.7838 0.6179 0.055 Uiso calc R 1 1 C C2 0.47551(18) 0.78941(18) 0.69887(15) 0.0413(4) Uani d . 1 1 O O4 0.95665(18) 0.60151(19) 0.05478(16) 0.0843(6) Uani d . 1 1 C C25 0.3024(2) 0.7942(2) 0.47000(18) 0.0535(6) Uani d . 1 1 H H25 0.2249 0.8329 0.4652 0.064 Uiso calc R 1 1 C C14 0.45200(18) 0.58593(18) 0.76623(15) 0.0418(5) Uani d . 1 1 C C13 0.4815(2) 0.47302(19) 0.76557(17) 0.0494(5) Uani d . 1 1 H H13 0.5339 0.4544 0.7107 0.059 Uiso calc R 1 1 C C28 0.72263(18) 0.5949(2) 0.40229(17) 0.0493(5) Uani d . 1 1 C C19 0.8203(2) 0.5349(2) 0.5862(2) 0.0615(6) Uani d . 1 1 H H19 0.8642 0.5150 0.5286 0.074 Uiso calc R 1 1 C C24 0.3736(2) 0.7652(2) 0.38586(18) 0.0527(5) Uani d . 1 1 H H24 0.3438 0.7839 0.3240 0.063 Uiso calc R 1 1 C C3 0.5279(2) 0.8758(2) 0.63173(18) 0.0532(5) Uani d . 1 1 H H3A 0.5817 0.8621 0.5756 0.064 Uiso calc R 1 1 C C31 0.85364(18) 0.5457(2) 0.22652(17) 0.0515(5) Uani d . 1 1 C C10 0.3252(2) 0.5263(2) 0.92660(18) 0.0584(6) Uani d . 1 1 H H10 0.2716 0.5444 0.9811 0.070 Uiso calc R 1 1 C C32 0.7999(2) 0.4666(2) 0.30380(19) 0.0581(6) Uani d . 1 1 H H32 0.8080 0.3961 0.2971 0.070 Uiso calc R 1 1 C C30 0.8421(2) 0.6502(2) 0.23725(18) 0.0549(6) Uani d . 1 1 H H30 0.8778 0.7041 0.1849 0.066 Uiso calc R 1 1 C C11 0.3568(2) 0.4155(2) 0.92503(19) 0.0626(6) Uani d . 1 1 H H11 0.3255 0.3586 0.9785 0.075 Uiso calc R 1 1 C C12 0.4357(2) 0.3875(2) 0.84348(19) 0.0575(6) Uani d . 1 1 H H12 0.4573 0.3122 0.8415 0.069 Uiso calc R 1 1 C C6 0.3661(2) 0.9199(2) 0.7938(2) 0.0638(7) Uani d . 1 1 H H6 0.3100 0.9364 0.8475 0.077 Uiso calc R 1 1 C C29 0.7778(2) 0.6742(2) 0.32570(18) 0.0542(6) Uani d . 1 1 H H29 0.7715 0.7433 0.3338 0.065 Uiso calc R 1 1 C C4 0.5026(2) 0.9808(2) 0.6457(2) 0.0636(7) Uani d . 1 1 H H4 0.5395 1.0368 0.6004 0.076 Uiso calc R 1 1 C C16 0.6916(2) 0.5923(2) 0.75704(18) 0.0572(6) Uani d . 1 1 H H16 0.6483 0.6112 0.8154 0.069 Uiso calc R 1 1 C C34 0.92137(19) 0.5231(2) 0.13005(19) 0.0559(6) Uani d . 1 1 C C37 0.2650(2) 0.7485(2) 0.94296(18) 0.0552(6) Uani d . 1 1 C C40 0.1335(2) 0.7950(2) 1.11868(19) 0.0604(6) Uani d . 1 1 O O1 -0.0419(2) 0.8608(3) 1.21770(19) 0.1048(8) Uani d . 1 1 O O2 0.1199(2) 0.8055(3) 1.28629(18) 0.1035(8) Uani d . 1 1 H H2 0.0760 0.8200 1.3365 0.155 Uiso calc R 1 1 C C38 0.1499(2) 0.8020(3) 0.9411(2) 0.0690(7) Uani d . 1 1 H H38 0.1160 0.8221 0.8811 0.083 Uiso calc R 1 1 C C42 0.3145(2) 0.7142(3) 1.0333(2) 0.0693(7) Uani d . 1 1 H H42 0.3922 0.6750 1.0351 0.083 Uiso calc R 1 1 C C33 0.7338(2) 0.4919(2) 0.3915(2) 0.0604(6) Uani d . 1 1 H H33 0.6970 0.4388 0.4431 0.073 Uiso calc R 1 1 C C5 0.4219(3) 1.0013(2) 0.7276(2) 0.0685(7) Uani d . 1 1 H H5 0.4048 1.0716 0.7383 0.082 Uiso calc R 1 1 C C39 0.0842(2) 0.8258(3) 1.0301(2) 0.0718(7) Uani d . 1 1 H H39 0.0060 0.8630 1.0292 0.086 Uiso calc R 1 1 C C17 0.8071(2) 0.5374(3) 0.7595(2) 0.0723(8) Uani d . 1 1 H H17 0.8417 0.5207 0.8181 0.087 Uiso calc R 1 1 C C41 0.2486(2) 0.7381(3) 1.1212(2) 0.0712(8) Uani d . 1 1 H H41 0.2821 0.7157 1.1820 0.085 Uiso calc R 1 1 C C18 0.8712(2) 0.5073(3) 0.6737(2) 0.0729(8) Uani d . 1 1 H H18 0.9490 0.4682 0.6752 0.087 Uiso calc R 1 1 C C43 0.0611(3) 0.8235(3) 1.2125(2) 0.0708(7) Uani d . 1 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C22 0.0393(11) 0.0459(11) 0.0368(10) -0.0105(9) -0.0003(8) -0.0197(9) N1 0.0432(10) 0.0695(12) 0.0438(10) -0.0056(9) -0.0009(8) -0.0333(9) C27 0.0435(11) 0.0391(10) 0.0333(9) -0.0133(9) 0.0006(8) -0.0162(8) C1 0.0412(11) 0.0439(11) 0.0319(9) -0.0131(9) 0.0021(8) -0.0179(8) N2 0.0663(13) 0.0571(12) 0.0463(10) -0.0238(10) 0.0177(9) -0.0284(9) C9 0.0507(12) 0.0519(13) 0.0370(10) -0.0163(10) 0.0024(9) -0.0198(9) O3 0.0809(14) 0.0932(14) 0.0723(13) -0.0251(11) 0.0247(10) -0.0569(11) C15 0.0455(11) 0.0464(11) 0.0385(10) -0.0137(9) -0.0023(8) -0.0176(9) C20 0.0399(11) 0.0477(12) 0.0432(11) -0.0077(9) -0.0031(9) -0.0196(9) C7 0.0533(13) 0.0498(12) 0.0413(11) -0.0161(10) 0.0025(9) -0.0217(9) C23 0.0541(13) 0.0592(14) 0.0391(11) -0.0133(11) -0.0013(9) -0.0263(10) C26 0.0430(11) 0.0512(12) 0.0421(11) -0.0107(10) -0.0003(9) -0.0213(9) C2 0.0471(11) 0.0443(11) 0.0359(10) -0.0160(9) -0.0003(8) -0.0185(8) O4 0.0943(15) 0.0992(15) 0.0657(12) -0.0410(12) 0.0334(11) -0.0496(12) C25 0.0468(12) 0.0559(14) 0.0564(13) -0.0082(10) -0.0103(10) -0.0228(11) C14 0.0466(11) 0.0484(12) 0.0338(10) -0.0191(9) -0.0015(8) -0.0156(9) C13 0.0563(13) 0.0507(12) 0.0422(11) -0.0153(10) -0.0006(9) -0.0211(10) C28 0.0425(11) 0.0632(14) 0.0426(11) -0.0089(10) 0.0042(9) -0.0307(10) C19 0.0437(12) 0.0769(17) 0.0554(14) -0.0052(12) -0.0025(10) -0.0290(13) C24 0.0564(14) 0.0601(14) 0.0439(12) -0.0145(11) -0.0132(10) -0.0192(10) C3 0.0597(14) 0.0579(14) 0.0469(12) -0.0256(11) 0.0057(10) -0.0234(10) C31 0.0403(11) 0.0700(15) 0.0475(12) -0.0103(10) 0.0029(9) -0.0342(11) C10 0.0673(15) 0.0665(15) 0.0408(12) -0.0301(13) 0.0118(10) -0.0205(11) C32 0.0599(15) 0.0623(15) 0.0580(14) -0.0174(12) 0.0118(11) -0.0386(12) C30 0.0527(13) 0.0643(15) 0.0487(12) -0.0199(11) 0.0076(10) -0.0271(11) C11 0.0809(18) 0.0594(15) 0.0471(13) -0.0351(13) -0.0001(12) -0.0113(11) C12 0.0728(16) 0.0491(13) 0.0524(13) -0.0222(12) -0.0068(12) -0.0170(11) C6 0.0734(17) 0.0624(15) 0.0577(14) -0.0188(13) 0.0101(12) -0.0351(12) C29 0.0552(13) 0.0572(14) 0.0548(13) -0.0131(11) 0.0043(10) -0.0340(11) C4 0.0776(18) 0.0572(15) 0.0621(15) -0.0324(13) 0.0017(13) -0.0226(12) C16 0.0524(13) 0.0767(16) 0.0428(12) -0.0199(12) -0.0049(10) -0.0220(11) C34 0.0430(12) 0.0755(17) 0.0540(14) -0.0114(12) 0.0037(10) -0.0388(13) C37 0.0600(14) 0.0596(14) 0.0451(12) -0.0199(11) 0.0133(10) -0.0273(11) C40 0.0633(16) 0.0671(16) 0.0524(14) -0.0214(13) 0.0144(11) -0.0336(12) O1 0.0699(14) 0.162(2) 0.1005(17) -0.0309(14) 0.0290(12) -0.0896(17) O2 0.0859(15) 0.156(2) 0.0783(15) -0.0162(15) 0.0114(12) -0.0807(16) C38 0.0582(16) 0.092(2) 0.0551(15) -0.0154(14) 0.0010(12) -0.0356(14) C42 0.0551(15) 0.092(2) 0.0585(15) -0.0068(14) 0.0045(12) -0.0447(15) C33 0.0639(15) 0.0640(15) 0.0558(14) -0.0224(12) 0.0117(11) -0.0319(12) C5 0.0866(19) 0.0527(15) 0.0735(17) -0.0216(14) -0.0025(14) -0.0329(13) C39 0.0541(15) 0.086(2) 0.0682(17) -0.0118(14) 0.0093(13) -0.0385(15) C17 0.0613(16) 0.095(2) 0.0553(15) -0.0190(15) -0.0188(12) -0.0197(14) C41 0.0684(17) 0.090(2) 0.0545(15) -0.0095(15) 0.0016(12) -0.0429(14) C18 0.0443(14) 0.091(2) 0.0727(17) -0.0075(13) -0.0134(12) -0.0269(15) C43 0.0710(18) 0.0831(19) 0.0630(16) -0.0261(15) 0.0185(13) -0.0434(15) 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' O O 0.0492 0.0322 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 C22 C27 120.94(17) N1 C22 C23 120.41(17) C27 C22 C23 118.65(19) C22 N1 C20 122.09(16) C22 N1 C28 118.98(17) C20 N1 C28 118.90(17) C22 C27 C1 122.51(18) C26 C27 C22 118.63(17) C26 C27 C1 118.86(17) C27 C1 C2 108.34(16) C15 C1 C27 111.04(15) C15 C1 C2 109.17(16) C15 C1 C14 108.60(16) C14 C1 C27 108.74(15) C14 C1 C2 110.95(15) C9 N2 C7 121.08(17) C9 N2 C37 119.08(18) C7 N2 C37 117.60(18) N2 C9 C10 120.03(19) C14 C9 N2 121.06(19) C14 C9 C10 118.9(2) C34 O3 H3 109.5 C20 C15 C1 122.88(17) C16 C15 C1 118.51(18) C16 C15 C20 118.6(2) C15 C20 N1 120.28(18) C15 C20 C19 119.3(2) C19 C20 N1 120.45(19) C2 C7 N2 120.49(19) C2 C7 C6 119.2(2) C6 C7 N2 120.4(2) C22 C23 H23 119.4 C24 C23 C22 121.28(19) C24 C23 H23 119.4 C27 C26 H26 118.7 C25 C26 C27 122.65(19) C25 C26 H26 118.7 C7 C2 C1 122.71(18) C3 C2 C1 118.77(18) C3 C2 C7 118.47(19) C26 C25 H25 120.7 C26 C25 C24 118.5(2) C24 C25 H25 120.7 C9 C14 C1 122.51(18) C13 C14 C1 118.85(18) C13 C14 C9 118.64(19) C14 C13 H13 118.9 C12 C13 C14 122.2(2) C12 C13 H13 118.9 C29 C28 N1 120.0(2) C33 C28 N1 119.9(2) C33 C28 C29 120.1(2) C20 C19 H19 119.6 C18 C19 C20 120.8(2) C18 C19 H19 119.6 C23 C24 C25 120.23(19) C23 C24 H24 119.9 C25 C24 H24 119.9 C2 C3 H3A 118.9 C4 C3 C2 122.1(2) C4 C3 H3A 118.9 C32 C31 C30 119.8(2) C32 C31 C34 121.2(2) C30 C31 C34 119.0(2) C9 C10 H10 119.3 C11 C10 C9 121.3(2) C11 C10 H10 119.3 C31 C32 H32 120.0 C31 C32 C33 120.0(2) C33 C32 H32 120.0 C31 C30 H30 120.0 C29 C30 C31 120.0(2) C29 C30 H30 120.0 C10 C11 H11 120.0 C10 C11 C12 120.0(2) C12 C11 H11 120.0 C13 C12 C11 119.0(2) C13 C12 H12 120.5 C11 C12 H12 120.5 C7 C6 H6 119.8 C5 C6 C7 120.5(2) C5 C6 H6 119.8 C28 C29 H29 120.1 C30 C29 C28 119.8(2) C30 C29 H29 120.1 C3 C4 H4 120.6 C5 C4 C3 118.8(2) C5 C4 H4 120.6 C15 C16 H16 118.9 C17 C16 C15 122.1(2) C17 C16 H16 118.9 O3 C34 C31 116.4(2) O4 C34 O3 123.2(2) O4 C34 C31 120.4(2) C38 C37 N2 120.8(2) C38 C37 C42 120.4(2) C42 C37 N2 118.8(2) C39 C40 C41 120.0(2) C39 C40 C43 119.4(2) C41 C40 C43 120.6(2) C43 O2 H2 109.5 C37 C38 H38 120.4 C37 C38 C39 119.1(2) C39 C38 H38 120.4 C37 C42 H42 120.0 C37 C42 C41 120.0(2) C41 C42 H42 120.0 C28 C33 C32 120.3(2) C28 C33 H33 119.9 C32 C33 H33 119.9 C6 C5 C4 121.0(2) C6 C5 H5 119.5 C4 C5 H5 119.5 C40 C39 C38 120.6(2) C40 C39 H39 119.7 C38 C39 H39 119.7 C16 C17 H17 120.5 C16 C17 C18 119.0(2) C18 C17 H17 120.5 C40 C41 C42 119.9(2) C40 C41 H41 120.1 C42 C41 H41 120.1 C19 C18 C17 120.2(2) C19 C18 H18 119.9 C17 C18 H18 119.9 O1 C43 C40 122.1(3) O1 C43 O2 124.1(2) O2 C43 C40 113.8(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C22 N1 1.389(3) C22 C27 1.396(3) C22 C23 1.409(3) N1 C20 1.405(3) N1 C28 1.441(2) C27 C1 1.533(3) C27 C26 1.385(3) C1 C15 1.532(3) C1 C2 1.534(3) C1 C14 1.532(3) N2 C9 1.402(3) N2 C7 1.409(3) N2 C37 1.443(3) C9 C14 1.391(3) C9 C10 1.407(3) O3 H3 0.8200 O3 C34 1.282(3) C15 C20 1.394(3) C15 C16 1.388(3) C20 C19 1.400(3) C7 C2 1.394(3) C7 C6 1.402(3) C23 H23 0.9300 C23 C24 1.372(3) C26 H26 0.9300 C26 C25 1.382(3) C2 C3 1.391(3) O4 C34 1.242(3) C25 H25 0.9300 C25 C24 1.385(3) C14 C13 1.386(3) C13 H13 0.9300 C13 C12 1.377(3) C28 C29 1.386(3) C28 C33 1.370(3) C19 H19 0.9300 C19 C18 1.374(4) C24 H24 0.9300 C3 H3A 0.9300 C3 C4 1.376(3) C31 C32 1.378(3) C31 C30 1.387(3) C31 C34 1.481(3) C10 H10 0.9300 C10 C11 1.361(3) C32 H32 0.9300 C32 C33 1.385(3) C30 H30 0.9300 C30 C29 1.382(3) C11 H11 0.9300 C11 C12 1.389(3) C12 H12 0.9300 C6 H6 0.9300 C6 C5 1.369(4) C29 H29 0.9300 C4 H4 0.9300 C4 C5 1.373(4) C16 H16 0.9300 C16 C17 1.376(4) C37 C38 1.368(3) C37 C42 1.376(3) C40 C39 1.363(4) C40 C41 1.374(4) C40 C43 1.496(3) O1 C43 1.208(4) O2 H2 0.8200 O2 C43 1.312(4) C38 H38 0.9300 C38 C39 1.393(3) C42 H42 0.9300 C42 C41 1.380(3) C33 H33 0.9300 C5 H5 0.9300 C39 H39 0.9300 C17 H17 0.9300 C17 C18 1.382(4) C41 H41 0.9300 C18 H18 0.9300 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O3 H3 O4 2_765 0.82 1.84 2.648(2) 168.4 C4 H4 Cg1 2_656 0.93 2.90 3.7568(3) 154 C33 H33 Cg1 2_666 0.93 2.85 3.7156(3) 156 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 C22 N1 C20 C15 0.0(3) C22 N1 C20 C19 179.7(2) C22 N1 C28 C29 92.4(3) C22 N1 C28 C33 -86.6(3) C22 C27 C1 C15 4.6(3) C22 C27 C1 C2 124.5(2) C22 C27 C1 C14 -114.8(2) C22 C27 C26 C25 0.4(3) C22 C23 C24 C25 0.7(4) N1 C22 C27 C1 -1.2(3) N1 C22 C27 C26 179.33(19) N1 C22 C23 C24 -179.9(2) N1 C20 C19 C18 179.3(2) N1 C28 C29 C30 -177.6(2) N1 C28 C33 C32 178.7(2) C27 C22 N1 C20 -1.4(3) C27 C22 N1 C28 -179.57(19) C27 C22 C23 C24 -0.3(3) C27 C1 C15 C20 -6.1(3) C27 C1 C15 C16 176.87(19) C27 C1 C2 C7 110.3(2) C27 C1 C2 C3 -67.4(2) C27 C1 C14 C9 -111.3(2) C27 C1 C14 C13 67.9(2) C27 C26 C25 C24 0.0(3) C1 C27 C26 C25 -179.0(2) C1 C15 C20 N1 4.1(3) C1 C15 C20 C19 -175.6(2) C1 C15 C16 C17 176.8(2) C1 C2 C3 C4 179.2(2) C1 C14 C13 C12 179.6(2) N2 C9 C14 C1 1.0(3) N2 C9 C14 C13 -178.3(2) N2 C9 C10 C11 179.2(2) N2 C7 C2 C1 1.7(3) N2 C7 C2 C3 179.3(2) N2 C7 C6 C5 179.0(2) N2 C37 C38 C39 -177.0(2) N2 C37 C42 C41 177.1(2) C9 N2 C7 C2 8.3(3) C9 N2 C7 C6 -172.2(2) C9 N2 C37 C38 -101.3(3) C9 N2 C37 C42 78.9(3) C9 C14 C13 C12 -1.1(3) C9 C10 C11 C12 -0.8(4) C15 C1 C2 C7 -128.7(2) C15 C1 C2 C3 53.7(2) C15 C1 C14 C9 127.7(2) C15 C1 C14 C13 -53.0(2) C15 C20 C19 C18 -1.0(4) C15 C16 C17 C18 -1.2(4) C20 N1 C28 C29 -85.8(3) C20 N1 C28 C33 95.2(3) C20 C15 C16 C17 -0.4(4) C20 C19 C18 C17 -0.7(5) C7 N2 C9 C14 -9.7(3) C7 N2 C9 C10 171.3(2) C7 N2 C37 C38 95.5(3) C7 N2 C37 C42 -84.3(3) C7 C2 C3 C4 1.5(3) C7 C6 C5 C4 2.0(4) C23 C22 N1 C20 178.2(2) C23 C22 N1 C28 0.0(3) C23 C22 C27 C1 179.15(18) C23 C22 C27 C26 -0.3(3) C26 C27 C1 C15 -175.95(17) C26 C27 C1 C2 -56.1(2) C26 C27 C1 C14 64.6(2) C26 C25 C24 C23 -0.6(3) C2 C1 C15 C20 -125.5(2) C2 C1 C15 C16 57.5(2) C2 C1 C14 C9 7.7(3) C2 C1 C14 C13 -173.01(18) C2 C7 C6 C5 -1.5(4) C2 C3 C4 C5 -1.0(4) C14 C1 C15 C20 113.4(2) C14 C1 C15 C16 -63.6(2) C14 C1 C2 C7 -9.0(3) C14 C1 C2 C3 173.32(19) C14 C9 C10 C11 0.2(4) C14 C13 C12 C11 0.5(4) C28 N1 C20 C15 178.1(2) C28 N1 C20 C19 -2.2(3) C3 C4 C5 C6 -0.8(4) C31 C32 C33 C28 -0.7(4) C31 C30 C29 C28 -1.5(4) C10 C9 C14 C1 180.0(2) C10 C9 C14 C13 0.7(3) C10 C11 C12 C13 0.5(4) C32 C31 C30 C29 0.6(4) C32 C31 C34 O3 -9.5(3) C32 C31 C34 O4 170.5(2) C30 C31 C32 C33 0.5(4) C30 C31 C34 O3 172.2(2) C30 C31 C34 O4 -7.8(3) C6 C7 C2 C1 -177.9(2) C6 C7 C2 C3 -0.2(3) C29 C28 C33 C32 -0.2(4) C16 C15 C20 N1 -178.8(2) C16 C15 C20 C19 1.5(3) C16 C17 C18 C19 1.7(5) C34 C31 C32 C33 -177.8(2) C34 C31 C30 C29 178.9(2) C37 N2 C9 C14 -172.3(2) C37 N2 C9 C10 8.8(3) C37 N2 C7 C2 171.1(2) C37 N2 C7 C6 -9.3(3) C37 C38 C39 C40 -0.8(4) C37 C42 C41 C40 0.7(5) C38 C37 C42 C41 -2.7(4) C42 C37 C38 C39 2.8(4) C33 C28 C29 C30 1.3(4) C39 C40 C41 C42 1.2(4) C39 C40 C43 O1 8.7(4) C39 C40 C43 O2 -170.6(3) C41 C40 C39 C38 -1.2(4) C41 C40 C43 O1 -171.2(3) C41 C40 C43 O2 9.5(4) C43 C40 C39 C38 179.0(3) C43 C40 C41 C42 -178.9(3) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.069 0.000 0.431 617 158 ' ' loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 0 -1 26672 1925 0 0 -2 1529754 548 0 0 -3 1530 4321 0 0 -4 794 917 0 0 -4 449 1031 0 0 -5 10527 2105 0 0 -5 11732 2897 0 0 -6 165001 6774 0 0 -6 166581 6712 0 0 -7 65208 1179 0 0 -7 56605 1028 0 0 -8 2941 1102 0 0 -9 721 2138 0 0 -10 6728 2440 0 0 -10 11101 3050 0 0 10 6101 2476 0 0 11 542986 13206 0 0 -11 545949 13758 0 0 12 53 966 0 0 -12 53 1625 0 0 -13 39587 4136 0 0 13 39659 3779 0 0 -14 5043 1532 0 0 -15 739 881 0 1 -14 14069 2040 0 -1 14 13225 1802 0 -1 13 104030 5423 0 1 -13 112748 5925 0 1 -12 84069 6002 0 -1 12 90078 5925 0 -1 11 9056 2737 0 1 -10 72526 4265 0 -1 10 64947 4108 0 1 -9 53762 2935 0 1 -8 1024 1654 0 1 -8 875 1717 0 1 -7 4635 3412 0 1 -7 4633 3432 0 1 -6 14303 902 0 1 -6 14298 896 0 1 -5 181 1403 0 1 -5 234 1462 0 1 -4 10662 480 0 1 -4 14472 629 0 1 -3 56102 1121 0 1 -3 58807 1321 0 1 -3 57354 596 0 1 -2 75785 3746 0 1 -1 52727 1281 0 1 0 11732110 4066 0 -1 -1 43868 1342 0 1 2 95299 3675 0 1 3 70357 1122 0 -1 -4 269307 3582 0 -1 -5 334806 8978 0 -1 -5 339354 7584 0 -1 -6 375229 6522 0 -1 -6 365863 5253 0 -1 -6 361969 6297 0 -1 -7 49272 1342 0 -1 -7 50903 957 0 -1 -8 12705 2978 0 -1 -9 70078 5187 0 -1 -10 3262 1586 0 -1 -11 1187508 19241 0 -1 -11 1247541 21800 0 -1 -11 1238286 20913 0 -1 -12 157310 7547 0 -1 -13 892 1675 0 -1 -14 419 1289 0 -1 -15 590 1083 0 -2 14 886 714 0 2 -14 0 702 0 2 -13 20 1143 0 -2 13 850 1271 0 -2 12 7584 2218 0 2 -12 10617 2250 0 -2 11 12298 2836 0 -2 10 87248 6033 0 2 -10 86189 5757 0 -2 9 4066 1783 0 2 -9 4131 1678 0 2 -8 12068 2250 0 2 -8 9890 2101 0 2 -7 22014 2243 0 2 -7 20732 2095 0 2 -6 6379 1508 0 2 -6 9376 1692 0 2 -5 52986 2545 0 2 -5 50989 2522 0 2 -4 55001 2760 0 2 -4 56378 2416 0 2 -4 61157 2812 0 2 -3 286766 6824 0 2 -3 283420 5806 0 2 -3 292338 4782 0 2 -2 717328 2730 0 2 -2 687650 2186 0 2 -1 200948 1455 0 2 0 104705 613 0 -2 -1 255467 2480 0 2 1 249945 2370 0 2 2 1587036 13291 0 -2 -2 1601459 12803 0 2 3 286949 3358 0 -2 -4 92777 6161 0 2 4 81895 4552 0 2 5 8841 2604 0 -2 -5 8728 3997 0 2 5 7383 3872 0 -2 -6 1470992 17160 0 -2 -6 1444554 15690 0 -2 -7 150727 4580 0 -2 -7 151884 4025 0 -2 -8 148958 5554 0 -2 -8 150596 4715 0 -2 -9 5538 1461 0 -2 -10 99043 6903 0 -2 -11 3935 2581 0 -2 -11 3751 2235 0 -2 -11 3466 2409 0 -2 -12 106128 6949 0 -2 -12 121873 8065 0 -2 -13 14220 2448 0 -2 -14 5489 2163 0 -2 -15 739 1221 0 -2 -16 82 826 0 -3 13 2 972 0 3 -13 2 982 0 3 -12 53379 4141 0 -3 12 51579 4234 0 -3 11 16637 2738 0 -3 10 1559 1399 0 -3 9 1721 1550 0 3 -9 1721 937 0 -3 9 1721 1210 0 3 -8 1496 891 0 -3 8 3645 1212 0 3 -8 2138 861 0 3 -7 20896 3529 0 3 -7 19598 3553 0 3 -6 168497 7207 0 3 -6 167961 7021 0 3 -5 365476 9661 0 3 -5 351384 10042 0 3 -4 109028 2271 0 3 -4 106447 2337 0 3 -3 16126 962 0 -3 3 17308 1097 0 3 -3 17218 1250 0 3 -3 16398 1135 0 -3 2 1614 2673 0 -3 2 1915 2302 0 3 -2 2289 2315 0 3 -2 2092 2061 0 3 -2 2920 2141 0 3 -1 101466 4694 0 3 -1 103385 2167 0 3 0 689072 10284 0 3 1 1761380 8992 0 3 1 1713030 9073 0 -3 -2 1193048 1963 0 -3 -2 1209793 2096 0 -3 -3 16059 4865 0 3 3 14839 4885 0 -3 -3 15128 4741 0 -3 -4 25410 6486 0 3 4 27934 6038 0 -3 -4 22862 6306 0 3 4 24047 5824 0 3 5 162053 6012 0 -3 -5 163810 7279 0 3 5 164136 6953 0 -3 -5 158244 6869 0 -3 -6 1161086 10158 0 -3 -6 1184120 10281 0 -3 -7 341200 7602 0 -3 -7 336157 7165 0 -3 -8 11236 2076 0 -3 -8 9268 2151 0 -3 -9 243594 8874 0 -3 -9 248268 7950 0 -3 -10 153297 5284 0 -3 -11 93310 6687 0 -3 -11 101203 7330 0 -3 -11 97499 6568 0 -3 -12 89100 6824 0 -3 -12 87704 6377 0 -3 -12 86407 6145 0 -3 -13 112457 7345 0 -3 -14 1590 1659 0 -3 -15 6748 1691 0 -3 -16 280 815 0 -4 13 755 830 0 4 -12 1554 1016 0 -4 12 2274 1382 0 -4 11 2473 1475 0 -4 10 729 1409 0 -4 9 453 1865 0 -4 8 6417 1333 0 -4 8 7320 1248 0 -4 7 92161 4105 0 -4 6 50464 2887 0 4 -5 54457 4954 0 -4 5 61398 5697 0 4 -4 118888 2876 0 -4 4 113797 3213 0 4 -3 141400 3737 0 -4 3 143066 4278 0 -4 3 143416 3595 0 -4 2 82766 5387 0 4 -2 77695 4615 0 -4 2 79978 4732 0 4 -2 87407 4763 0 4 -1 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