#------------------------------------------------------------------------------ #$Date: 2024-10-12 04:04:04 +0200 (Sat, 12 Oct 2024) $ #$Revision: 295461 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/32/2023284.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_2023284 loop_ _publ_author_name 'Shibata, Hiroki' 'Sakon, Aya' 'Takata, Noriyuki' 'Takiyama, Hiroshi' _publ_section_title ; Crystal structures of two different multi-component crystals consisting of 1-(3,4-dimethoxybenzyl)-6,7-dimethoxyisoquinoline and fumaric acid ; _journal_coeditor_code OX2007 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989024009794 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C20 H21 N O4, 0.5C4 H4 O4' _chemical_formula_moiety 'C20 H21 N O4, 0.5(C4 H4 O4)' _chemical_formula_sum 'C22 H23 N O6' _chemical_formula_weight 397.431 _chemical_name_systematic ; [1-(3,4-Dimethoxybenzyl)-6,7-dimethoxyisoquinoline--fumaric acid (1/0.5) ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _cell_angle_alpha 90 _cell_angle_beta 95.9308(12) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.05718(12) _cell_length_b 6.71363(11) _cell_length_c 32.8419(4) _cell_measurement_reflns_used 6957 _cell_measurement_temperature 99.99(11) _cell_measurement_theta_max 67.9440 _cell_measurement_theta_min 2.7010 _cell_volume 1986.31(5) _computing_cell_refinement ; CrysAlisPro 1.171.42.69a (Rigaku OD, 2022) ; _computing_data_collection ; CrysAlisPro 1.171.42.69a (Rigaku OD, 2022) ; _computing_data_reduction ; CrysAlisPro 1.171.42.69a (Rigaku OD, 2022) ; _computing_molecular_graphics ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_structure_refinement ; olex2.refine 1.5 (Bourhis et al., 2015) ; _computing_structure_solution ; SHELXT2018/2 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 99.99(11) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.9964 _diffrn_measured_fraction_theta_max 0.9917 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at home/near, HyPix3000' _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 0.0182 _diffrn_reflns_av_unetI/netI 0.0210 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_number 8710 _diffrn_reflns_theta_full 67.6840 _diffrn_reflns_theta_max 68.03 _diffrn_reflns_theta_min 2.71 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.803 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.90832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2022) ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_density_diffrn 1.329 _exptl_crystal_description block _exptl_crystal_F_000 843.079 _exptl_crystal_size_max 0.2200 _exptl_crystal_size_mid 0.112 _exptl_crystal_size_min 0.106 _refine_diff_density_max 0.2703 _refine_diff_density_min -0.2127 _refine_ls_extinction_coef 0.0012(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2019/2 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.0424 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_constraints 37 _refine_ls_number_parameters 268 _refine_ls_number_reflns 3589 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.0424 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0325 _refine_ls_shift/su_max -0.0003 _refine_ls_shift/su_mean 0.0000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.6045P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0852 _refine_ls_wR_factor_ref 0.0870 _reflns_number_gt 3325 _reflns_number_total 3589 _reflns_threshold_expression I>=2u(I) _iucr_refine_instructions_details ; TITL papa_fma_i_sl_004_1_auto_a.res in P2(1)/n REM Old TITL Papa_FMA_I_SL_004_1_auto in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.125, Rweak 0.009, Alpha 0.016 REM 0.659 for 335 systematic absences, Orientation as input REM Formula found by SHELXT: C33 N1 O18 CELL 1.54184 9.057179 6.713629 32.841901 90 95.9308 90 ZERR 4 0.000121 0.000105 0.00043 0 0.0012 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 88 92 4 24 L.S. 4 PLAN 5 SIZE 200 112 106 TEMP -173 CONF fmap 2 acta MORE -1 BOND $H EXTI 0.001224 WGHT 0.04294 0.60446 FVAR 0.550037 REM REM REM N1 3 0.51693 0.60177 0.44622 11.00000 0.01929 0.02118 0.02251 = -0.00052 0.00226 -0.00113 C2 1 0.60617 0.51334 0.42229 11.00000 0.01744 0.01938 0.01892 = 0.00188 -0.00016 -0.00106 C3 1 0.74048 0.60359 0.41307 11.00000 0.01780 0.01746 0.01880 = 0.00289 -0.00107 -0.00223 C4 1 0.83390 0.51426 0.38613 11.00000 0.01907 0.01838 0.02132 = 0.00031 0.00018 -0.00414 AFIX 43 H4 2 0.80587 0.39140 0.37322 11.00000 -1.20000 AFIX 0 C5 1 0.96396 0.60367 0.37863 11.00000 0.01958 0.02519 0.02072 = 0.00161 0.00243 -0.00357 C6 1 1.00943 0.78635 0.39912 11.00000 0.02256 0.02748 0.02092 = 0.00431 0.00019 -0.01139 C7 1 0.92008 0.87524 0.42489 11.00000 0.02713 0.01957 0.02088 = 0.00119 -0.00221 -0.00841 AFIX 43 H7 2 0.94998 0.99708 0.43796 11.00000 -1.20000 AFIX 0 C8 1 0.78282 0.78679 0.43229 11.00000 0.02273 0.01749 0.01892 = 0.00354 -0.00247 -0.00238 C9 1 0.68699 0.87280 0.45879 11.00000 0.02801 0.01781 0.02142 = -0.00141 -0.00121 -0.00161 AFIX 43 H9 2 0.71313 0.99387 0.47268 11.00000 -1.20000 AFIX 0 C10 1 0.55693 0.77991 0.46414 11.00000 0.02509 0.02108 0.02359 = -0.00189 0.00239 0.00105 AFIX 43 H10 2 0.49118 0.84156 0.48104 11.00000 -1.20000 AFIX 0 C11 1 0.56339 0.30741 0.40725 11.00000 0.01826 0.01900 0.02499 = 0.00035 0.00410 -0.00483 AFIX 23 H11a 2 0.47821 0.26165 0.42142 11.00000 -1.20000 H11b 2 0.64743 0.21623 0.41512 11.00000 -1.20000 AFIX 0 C12 1 0.52185 0.29044 0.36140 11.00000 0.01440 0.01847 0.02506 = -0.00140 0.00342 -0.00610 C13 1 0.58166 0.13608 0.33954 11.00000 0.01627 0.01776 0.02722 = 0.00088 0.00136 -0.00086 AFIX 43 H13 2 0.64718 0.04275 0.35364 11.00000 -1.20000 AFIX 0 C14 1 0.54649 0.11766 0.29756 11.00000 0.01803 0.01766 0.02712 = -0.00263 0.00449 0.00010 C15 1 0.44833 0.25584 0.27672 11.00000 0.01717 0.01944 0.02341 = -0.00071 0.00221 -0.00314 C16 1 0.38820 0.40628 0.29850 11.00000 0.01803 0.01952 0.02897 = 0.00007 0.00058 0.00112 AFIX 43 H16 2 0.32136 0.49876 0.28463 11.00000 -1.20000 AFIX 0 C17 1 0.42478 0.42374 0.34077 11.00000 0.01853 0.01920 0.02815 = -0.00458 0.00399 -0.00028 AFIX 43 H17 2 0.38266 0.52785 0.35539 11.00000 -1.20000 AFIX 0 O18 4 0.60006 -0.02676 0.27362 11.00000 0.03304 0.02553 0.02675 = -0.00442 0.00123 0.01199 C19 1 0.70127 -0.16789 0.29353 11.00000 0.04009 0.03127 0.03679 = -0.00507 0.00006 0.01887 AFIX 137 H19a 2 0.73348 -0.26094 0.27322 11.00000 -1.50000 H19b 2 0.78781 -0.09774 0.30701 11.00000 -1.50000 H19c 2 0.65194 -0.24179 0.31401 11.00000 -1.50000 AFIX 0 O20 4 0.41893 0.22626 0.23544 11.00000 0.02655 0.02249 0.02282 = -0.00122 0.00057 0.00408 C21 1 0.32565 0.37026 0.21353 11.00000 0.03702 0.02367 0.02586 = 0.00305 0.00003 0.00567 AFIX 137 H21a 2 0.31495 0.33717 0.18431 11.00000 -1.50000 H21b 2 0.22777 0.36964 0.22376 11.00000 -1.50000 H21c 2 0.37024 0.50276 0.21749 11.00000 -1.50000 AFIX 0 O22 4 1.05851 0.53419 0.35250 11.00000 0.02285 0.03333 0.03004 = -0.00586 0.00980 -0.00987 C23 1 1.00672 0.37103 0.32693 11.00000 0.02825 0.02864 0.03144 = -0.00560 0.01107 -0.00626 AFIX 137 H23a 2 1.08006 0.34025 0.30790 11.00000 -1.50000 H23b 2 0.99240 0.25412 0.34395 11.00000 -1.50000 H23c 2 0.91220 0.40688 0.31141 11.00000 -1.50000 AFIX 0 O24 4 1.14269 0.85526 0.39014 11.00000 0.02811 0.03978 0.03029 = -0.00497 0.00713 -0.02181 C25 1 1.20004 1.02963 0.41170 11.00000 0.03716 0.04310 0.03133 = -0.00279 0.00211 -0.02789 AFIX 137 H25a 2 1.29696 1.06373 0.40284 11.00000 -1.50000 H25b 2 1.13123 1.14101 0.40575 11.00000 -1.50000 H25c 2 1.21102 1.00306 0.44120 11.00000 -1.50000 AFIX 0 C30 1 0.18953 0.55150 0.48065 11.00000 0.02168 0.02000 0.01996 = 0.00098 0.00186 -0.00012 O31 4 0.26149 0.45088 0.45496 11.00000 0.02166 0.02569 0.03075 = -0.00635 0.00922 -0.00443 AFIX 147 H31 2 0.34425 0.50468 0.45310 11.00000 -1.50000 AFIX 0 O32 4 0.23373 0.70574 0.49758 11.00000 0.02525 0.02456 0.03259 = -0.00780 0.00710 -0.00631 C33 1 0.04511 0.45913 0.48787 11.00000 0.02233 0.01966 0.02178 = -0.00109 0.00140 -0.00194 AFIX 43 H33 2 0.01702 0.33727 0.47454 11.00000 -1.20000 AFIX 0 HKLF 4 END Q1 1 0.4375 0.541667 0.45 11 0.05 0.27 Q2 1 0.65625 0.583333 0.408333 11 0.05 0.25 Q3 1 0.59375 0.416667 0.416667 11 0.05 0.2 Q4 1 0.46875 0.375 0.283333 11 0.05 0.19 Q5 1 0.78125 0.666667 0.425 11 0.05 0.19 REM The information below was added by Olex2. REM REM R1 = 0.0325 for 3325 Fo > 4sig(Fo) and 0.0347 for all 3589 data REM 268 parameters refined using 0 restraints REM Highest difference peak 0.2703, deepest hole -0.2127 REM Mean Shift 0.0000, Max Shift -0.0003. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0347 REM R1_gt = 0.0325 REM wR_ref = 0.0870 REM GOOF = 1.0424 REM Shift_max = -0.0003 REM Shift_mean = 0.0000 REM Reflections_all = 3589 REM Reflections_gt = 3325 REM Parameters = 268 REM Hole = -0.2127 REM Peak = 0.2703 REM Flack = n/a ; _cod_data_source_file ox2007.cif _cod_data_source_block II _cod_database_code 2023284 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x+1/2,y+1/2,-z+1/2 3 -x,-y,-z 4 x-1/2,-y-1/2,z-1/2 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_occupancy N N1 0.51693(10) 0.60177(14) 0.44622(3) 0.0210(2) Uani 1.000000 C C2 0.60617(12) 0.51334(17) 0.42229(3) 0.0187(2) Uani 1.000000 C C3 0.74048(11) 0.60359(17) 0.41307(3) 0.0182(2) Uani 1.000000 C C4 0.83390(12) 0.51426(17) 0.38613(3) 0.0197(2) Uani 1.000000 H H4 0.80587(12) 0.39140(17) 0.37322(3) 0.0237(3) Uiso 1.000000 C C5 0.96396(12) 0.60367(18) 0.37863(3) 0.0218(2) Uani 1.000000 C C6 1.00943(13) 0.78635(18) 0.39912(3) 0.0238(3) Uani 1.000000 C C7 0.92008(13) 0.87524(17) 0.42489(3) 0.0229(3) Uani 1.000000 H H7 0.94998(13) 0.99708(17) 0.43796(3) 0.0274(3) Uiso 1.000000 C C8 0.78282(12) 0.78679(17) 0.43229(3) 0.0200(2) Uani 1.000000 C C9 0.68699(13) 0.87280(17) 0.45879(3) 0.0227(2) Uani 1.000000 H H9 0.71313(13) 0.99387(17) 0.47268(3) 0.0272(3) Uiso 1.000000 C C10 0.55693(13) 0.77991(18) 0.46414(3) 0.0233(3) Uani 1.000000 H H10 0.49118(13) 0.84156(18) 0.48104(3) 0.0279(3) Uiso 1.000000 C C11 0.56339(12) 0.30741(17) 0.40725(3) 0.0206(2) Uani 1.000000 H H11a 0.47821(12) 0.26165(17) 0.42142(3) 0.0247(3) Uiso 1.000000 H H11b 0.64743(12) 0.21623(17) 0.41512(3) 0.0247(3) Uiso 1.000000 C C12 0.52185(11) 0.29044(16) 0.36140(3) 0.0192(2) Uani 1.000000 C C13 0.58166(12) 0.13608(17) 0.33954(3) 0.0205(2) Uani 1.000000 H H13 0.64718(12) 0.04275(17) 0.35364(3) 0.0246(3) Uiso 1.000000 C C14 0.54649(12) 0.11766(17) 0.29756(3) 0.0208(2) Uani 1.000000 C C15 0.44833(11) 0.25584(17) 0.27672(3) 0.0200(2) Uani 1.000000 C C16 0.38820(12) 0.40628(17) 0.29850(4) 0.0223(2) Uani 1.000000 H H16 0.32136(12) 0.49876(17) 0.28463(4) 0.0268(3) Uiso 1.000000 C C17 0.42478(12) 0.42374(17) 0.34077(4) 0.0219(2) Uani 1.000000 H H17 0.38266(12) 0.52785(17) 0.35539(4) 0.0262(3) Uiso 1.000000 O O18 0.60006(10) -0.02676(13) 0.27362(3) 0.0286(2) Uani 1.000000 C C19 0.70127(16) -0.1679(2) 0.29353(4) 0.0363(3) Uani 1.000000 H H19a 0.7335(9) -0.2609(10) 0.27322(6) 0.0545(5) Uiso 1.000000 H H19b 0.7878(6) -0.0977(3) 0.3070(3) 0.0545(5) Uiso 1.000000 H H19c 0.6519(4) -0.2418(11) 0.3140(2) 0.0545(5) Uiso 1.000000 O O20 0.41893(9) 0.22626(12) 0.23544(2) 0.0241(2) Uani 1.000000 C C21 0.32565(14) 0.37026(19) 0.21353(4) 0.0291(3) Uani 1.000000 H H21a 0.3150(9) 0.3372(8) 0.18431(5) 0.0436(4) Uiso 1.000000 H H21b 0.2278(4) 0.3696(10) 0.2238(2) 0.0436(4) Uiso 1.000000 H H21c 0.3702(6) 0.5028(3) 0.2175(2) 0.0436(4) Uiso 1.000000 O O22 1.05851(9) 0.53419(14) 0.35250(3) 0.0282(2) Uani 1.000000 C C23 1.00672(13) 0.37103(19) 0.32693(4) 0.0289(3) Uani 1.000000 H H23a 1.0801(5) 0.3403(9) 0.3079(2) 0.0433(4) Uiso 1.000000 H H23b 0.9924(10) 0.2541(4) 0.34395(4) 0.0433(4) Uiso 1.000000 H H23c 0.9122(5) 0.4069(5) 0.3114(2) 0.0433(4) Uiso 1.000000 O O24 1.14269(9) 0.85526(14) 0.39014(3) 0.0324(2) Uani 1.000000 C C25 1.20004(16) 1.0296(2) 0.41170(4) 0.0373(3) Uani 1.000000 H H25a 1.2970(6) 1.0637(10) 0.4028(3) 0.0559(5) Uiso 1.000000 H H25b 1.1312(6) 1.1410(5) 0.4058(3) 0.0559(5) Uiso 1.000000 H H25c 1.2110(12) 1.0031(6) 0.44120(5) 0.0559(5) Uiso 1.000000 C C30 0.18953(12) 0.55150(17) 0.48065(3) 0.0206(2) Uani 1.000000 O O31 0.26149(9) 0.45088(13) 0.45496(3) 0.0256(2) Uani 1.000000 H H31 0.3443(7) 0.5047(14) 0.4531(4) 0.0384(3) Uiso 1.000000 O O32 0.23373(9) 0.70574(13) 0.49758(3) 0.0272(2) Uani 1.000000 C C33 0.04511(12) 0.45913(17) 0.48787(3) 0.0213(2) Uani 1.000000 H H33 0.01702(12) 0.33727(17) 0.47454(3) 0.0256(3) Uiso 1.000000 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 N1 0.0193(4) 0.0212(5) 0.0225(5) -0.0011(4) 0.0023(4) -0.0005(4) C2 0.0174(5) 0.0194(6) 0.0189(5) -0.0011(4) -0.0002(4) 0.0019(4) C3 0.0178(5) 0.0175(5) 0.0188(5) -0.0022(4) -0.0011(4) 0.0029(4) C4 0.0191(5) 0.0184(5) 0.0213(5) -0.0041(4) 0.0002(4) 0.0003(4) C5 0.0196(5) 0.0252(6) 0.0207(5) -0.0036(5) 0.0024(4) 0.0016(5) C6 0.0226(6) 0.0275(6) 0.0209(5) -0.0114(5) 0.0002(4) 0.0043(5) C7 0.0271(6) 0.0196(6) 0.0209(5) -0.0084(5) -0.0022(4) 0.0012(4) C8 0.0227(5) 0.0175(6) 0.0189(5) -0.0024(4) -0.0025(4) 0.0035(4) C9 0.0280(6) 0.0178(6) 0.0214(5) -0.0016(5) -0.0012(4) -0.0014(4) C10 0.0251(6) 0.0211(6) 0.0236(6) 0.0010(5) 0.0024(4) -0.0019(5) C11 0.0183(5) 0.0190(6) 0.0250(6) -0.0048(4) 0.0041(4) 0.0004(4) C12 0.0144(5) 0.0185(5) 0.0251(6) -0.0061(4) 0.0034(4) -0.0014(4) C13 0.0163(5) 0.0178(5) 0.0272(6) -0.0009(4) 0.0014(4) 0.0009(4) C14 0.0180(5) 0.0177(5) 0.0271(6) 0.0001(4) 0.0045(4) -0.0026(4) C15 0.0172(5) 0.0194(5) 0.0234(5) -0.0031(4) 0.0022(4) -0.0007(4) C16 0.0180(5) 0.0195(6) 0.0290(6) 0.0011(4) 0.0006(4) 0.0001(5) C17 0.0185(5) 0.0192(6) 0.0282(6) -0.0003(4) 0.0040(4) -0.0046(5) O18 0.0330(4) 0.0255(4) 0.0267(4) 0.0120(4) 0.0012(3) -0.0044(3) C19 0.0401(7) 0.0313(7) 0.0368(7) 0.0189(6) 0.0001(6) -0.0051(6) O20 0.0265(4) 0.0225(4) 0.0228(4) 0.0041(3) 0.0006(3) -0.0012(3) C21 0.0370(7) 0.0237(6) 0.0259(6) 0.0057(5) 0.0000(5) 0.0030(5) O22 0.0229(4) 0.0333(5) 0.0300(4) -0.0099(4) 0.0098(3) -0.0059(4) C23 0.0282(6) 0.0286(7) 0.0314(6) -0.0063(5) 0.0111(5) -0.0056(5) O24 0.0281(4) 0.0398(5) 0.0303(4) -0.0218(4) 0.0071(3) -0.0050(4) C25 0.0372(7) 0.0431(8) 0.0313(6) -0.0279(6) 0.0021(5) -0.0028(6) C30 0.0217(5) 0.0200(6) 0.0200(5) -0.0001(4) 0.0019(4) 0.0010(4) O31 0.0217(4) 0.0257(4) 0.0307(4) -0.0044(3) 0.0092(3) -0.0064(3) O32 0.0252(4) 0.0246(5) 0.0326(4) -0.0063(3) 0.0071(3) -0.0078(4) C33 0.0223(5) 0.0197(6) 0.0218(5) -0.0019(4) 0.0014(4) -0.0011(4) loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870 51.65120 0.21560 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' 0.01920 0.00962 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' H 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236 57.79970 0.00304 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' 0.00000 0.00000 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' N 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750 0.58260 -11.52900 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' 0.03256 0.01839 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' O 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390 32.90890 0.25080 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' 0.05239 0.03377 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l 0 0 -2 0 0 2 0 0 -2 0 0 -3 0 0 -3 0 0 3 0 0 -4 0 0 -4 0 0 4 0 0 -5 0 0 -5 0 0 5 0 0 -6 0 0 6 0 0 -6 0 0 -7 0 0 -7 0 0 7 0 0 -8 0 0 8 0 0 -8 0 0 -9 0 0 -9 0 0 9 0 0 10 0 0 -10 0 0 -10 0 0 -11 0 0 11 0 0 -11 0 0 -12 0 0 12 0 0 -12 0 0 -13 0 0 -13 0 0 13 0 0 14 0 0 -14 0 0 -14 0 0 -15 0 0 15 0 0 -16 0 0 16 0 0 -17 0 0 17 0 0 18 0 0 -18 0 0 19 0 0 -19 0 0 -20 0 0 20 0 0 -21 0 0 21 0 0 -22 0 0 -22 0 0 22 0 0 -23 0 0 -23 0 0 -24 0 0 -24 0 0 -25 0 0 -25 0 0 -26 0 0 -27 0 0 28 0 0 -28 0 0 -29 0 0 29 0 0 -30 0 0 30 0 0 31 0 0 -31 0 0 32 0 0 33 0 0 34 0 0 35 0 0 36 0 0 37 0 0 -37 0 0 38 0 0 -38 0 0 39 0 0 -39 0 1 0 0 1 -1 0 -1 -1 0 1 1 0 1 2 0 1 2 0 -1 -2 0 1 2 0 1 3 0 1 3 0 1 3 0 1 -3 0 -1 -3 0 -1 3 0 1 4 0 -1 4 0 1 4 0 -1 -4 0 1 4 0 1 -4 0 -1 -4 0 -1 -5 0 1 5 0 1 5 0 -1 -5 0 1 5 0 -1 5 0 -1 -6 0 1 6 0 1 6 0 -1 6 0 -1 -6 0 1 -6 0 1 7 0 -1 -7 0 -1 -7 0 -1 7 0 1 -7 0 -1 -8 0 1 -8 0 1 8 0 1 -8 0 -1 -9 0 1 -9 0 1 -9 0 1 9 0 1 -10 0 1 10 0 1 -10 0 -1 -10 0 -1 11 0 -1 -11 0 1 -11 0 1 -11 0 1 -12 0 -1 -12 0 1 -12 0 -1 12 0 1 -13 0 -1 -13 0 -1 13 0 1 -13 0 -1 14 0 1 -14 0 1 -14 0 -1 -14 0 1 -15 0 -1 -15 0 1 -15 0 -1 15 0 -1 -16 0 1 -16 0 1 -16 0 -1 16 0 1 -17 0 -1 17 0 1 -17 0 -1 -17 0 1 -18 0 1 -18 0 -1 18 0 -1 -18 0 -1 19 0 1 -19 0 -1 -19 0 -1 -20 0 -1 20 0 -1 -21 0 1 -21 0 -1 21 0 -1 22 0 -1 -22 0 1 -22 0 -1 22 0 -1 -22 0 -1 23 0 -1 -23 0 -1 -23 0 -1 23 0 1 -23 0 1 -24 0 -1 -24 0 -1 -24 0 1 24 0 -1 -25 0 -1 -25 0 1 -25 0 1 25 0 1 -26 0 1 26 0 1 -27 0 1 27 0 1 28 0 1 -28 0 1 29 0 1 -29 0 1 -30 0 -1 30 0 1 30 0 -1 31 0 1 31 0 1 -31 0 -1 32 0 1 32 0 1 -32 0 -1 33 0 1 33 0 1 -33 0 1 34 0 -1 34 0 1 -34 0 1 35 0 -1 35 0 1 36 0 1 -36 0 -1 36 0 1 37 0 -1 -37 0 1 -37 0 -1 37 0 -1 38 0 1 38 0 1 -38 0 -1 -38 0 2 0 0 -2 -1 0 2 -1 0 2 1 0 -2 -2 0 2 2 0 2 -2 0 2 3 0 2 3 0 -2 -3 0 -2 -4 0 -2 4 0 2 4 0 2 4 0 -2 5 0 2 5 0 2 5 0 2 6 0 2 6 0 2 6 0 -2 -6 0 -2 6 0 2 7 0 -2 -7 0 2 7 0 2 7 0 2 8 0 -2 -8 0 2 8 0 2 -8 0 2 8 0 -2 -9 0 2 -9 0 2 9 0 2 9 0 2 9 0 2 10 0 2 10 0 2 -10 0 -2 -10 0 2 10 0 2 11 0 -2 -11 0 2 11 0 2 11 0 2 -11 0 2 12 0 -2 -12 0 2 12 0 2 -12 0 2 12 0 2 13 0 2 13 0 -2 -13 0 2 13 0 2 -13 0 2 14 0 2 14 0 2 14 0 2 -14 0 -2 15 0 2 -15 0 2 15 0 2 -16 0 -2 16 0 2 16 0 -2 17 0 2 17 0 2 -17 0 2 -18 0 2 18 0 -2 18 0 2 19 0 2 -19 0 -2 20 0 2 20 0 2 -20 0 2 -20 0 2 -21 0 2 -21 0 -2 -21 0 2 21 0 2 -22 0 2 22 0 -2 -22 0 2 -22 0 2 23 0 2 -23 0 -2 -23 0 2 -23 0 2 -24 0 -2 -24 0 2 -25 0 2 25 0 2 -26 0 2 26 0 2 27 0 2 -27 0 2 -28 0 2 28 0 2 -29 0 2 29 0 2 30 0 2 -30 0 2 -31 0 2 31 0 2 -32 0 2 32 0 2 33 0 2 -33 0 2 -34 0 2 34 0 2 35 0 2 35 0 2 -35 0 2 -36 0 2 36 0 2 36 0 2 37 0 3 0 0 -3 0 0 3 -1 0 3 1 0 -3 -1 0 -3 1 0 3 2 0 3 2 0 -3 3 0 3 3 0 3 3 0 3 4 0 3 4 0 -3 4 0 3 5 0 -3 5 0 3 5 0 3 6 0 3 6 0 3 7 0 3 7 0 3 8 0 3 8 0 3 9 0 3 9 0 3 -9 0 3 10 0 3 -10 0 3 10 0 3 11 0 3 11 0 3 -11 0 3 12 0 3 12 0 3 -12 0 3 13 0 3 13 0 3 -13 0 3 14 0 3 -14 0 3 14 0 3 14 0 3 15 0 3 15 0 3 -15 0 3 -16 0 3 16 0 3 16 0 3 -17 0 -3 -17 0 3 17 0 -3 -18 0 3 18 0 3 -18 0 -3 19 0 3 19 0 -3 -19 0 3 -19 0 -3 20 0 -3 -20 0 3 20 0 3 -20 0 3 -21 0 -3 -21 0 -3 21 0 3 -22 0 -3 -22 0 -3 -23 0 3 -23 0 3 -24 0 -3 -24 0 3 -25 0 -3 -25 0 -3 -26 0 3 -26 0 -3 -27 0 3 -27 0 3 -28 0 -3 -28 0 -3 -29 0 3 -29 0 3 -30 0 -3 -30 0 -3 -31 0 3 -31 0 3 -32 0 3 33 0 3 -33 0 3 34 0 3 -34 0 3 -35 0 3 35 0 3 -36 0 3 36 0 -4 0 0 4 1 0 -4 1 0 4 2 0 -4 2 0 -4 3 0 -4 3 0 4 3 0 -4 4 0 4 4 0 -4 4 0 4 5 0 -4 5 0 -4 6 0 4 6 0 4 7 0 4 7 0 4 8 0 4 8 0 4 9 0 4 9 0 4 10 0 4 -10 0 4 10 0 -4 -10 0 4 11 0 4 -11 0 4 11 0 -4 -11 0 -4 -12 0 4 12 0 4 -12 0 4 12 0 -4 -13 0 4 13 0 4 -13 0 4 13 0 4 14 0 -4 -14 0 4 -14 0 4 14 0 4 -15 0 -4 -15 0 4 15 0 4 16 0 -4 -16 0 4 -16 0 4 -17 0 -4 -17 0 4 -18 0 -4 -18 0 4 -19 0 -4 -19 0 -4 -20 0 -4 -20 0 4 -20 0 -4 -21 0 -4 -21 0 4 -21 0 -4 -22 0 4 -22 0 4 -23 0 -4 -23 0 4 -24 0 -4 -24 0 -4 -25 0 4 -25 0 -4 -26 0 4 -26 0 4 -27 0 -4 -27 0 4 -28 0 -4 -28 0 4 -29 0 4 29 0 4 -30 0 -4 -30 0 4 30 0 -4 -31 0 4 -31 0 4 31 0 4 32 0 4 -32 0 -4 -32 0 -4 -33 0 4 -33 0 4 33 0 -5 0 0 -5 1 0 -5 -1 0 -5 -2 0 -5 2 0 -5 -2 0 -5 -3 0 -5 -3 0 -5 -4 0 -5 -4 0 -5 -5 0 -5 -5 0 -5 -6 0 5 -6 0 5 6 0 5 7 0 5 -7 0 -5 -7 0 -5 -7 0 5 -8 0 -5 8 0 -5 -8 0 -5 -9 0 5 -9 0 -5 -10 0 5 -10 0 -5 -11 0 5 -11 0 5 -12 0 -5 -12 0 5 -13 0 -5 -13 0 -5 -14 0 5 -14 0 -5 -15 0 5 -15 0 5 -16 0 -5 -16 0 5 -17 0 -5 -17 0 5 -18 0 -5 -18 0 -5 -19 0 -5 -19 0 5 -19 0 -5 -20 0 -5 -20 0 5 -20 0 5 -21 0 -5 -21 0 -5 -21 0 5 -22 0 -5 -22 0 -5 -23 0 5 -23 0 5 -24 0 -5 -24 0 -5 -25 0 5 -25 0 5 -26 0 -5 -26 0 5 -27 0 -5 -27 0 5 -28 0 -5 -28 0 5 -29 0 -5 -29 0 -5 -30 0 5 -30 0 -6 0 0 -6 -1 0 -6 1 0 -6 2 0 -6 -2 0 -6 -3 0 -6 3 0 6 -3 0 6 -4 0 -6 -4 0 -6 -5 0 6 -5 0 -6 -6 0 6 -6 0 6 -7 0 -6 -7 0 6 -8 0 -6 -8 0 -6 -9 0 6 -9 0 -6 -10 0 6 -10 0 -6 -11 0 6 -11 0 6 -12 0 -6 -12 0 -6 -13 0 6 -13 0 6 -14 0 -6 -14 0 -6 -15 0 6 -15 0 -6 -16 0 6 -16 0 -6 -17 0 6 -17 0 6 -18 0 -6 -18 0 -6 -19 0 6 -19 0 6 -20 0 6 -21 0 6 -22 0 6 -23 0 6 -24 0 6 -25 0 6 -26 0 7 0 0 -7 0 0 -7 -1 0 7 1 0 -7 1 0 7 -1 0 -7 -2 0 -7 2 0 7 2 0 7 -2 0 7 -3 0 -7 -3 0 -7 3 0 -7 4 0 7 -4 0 -7 -4 0 -7 5 0 -7 -5 0 7 -5 0 7 -6 0 -7 6 0 -7 -6 0 7 -7 0 -7 -7 0 -7 7 0 7 -8 0 -7 8 0 -7 -8 0 -7 9 0 -7 -9 0 7 -9 0 -7 10 0 -7 -10 0 7 -10 0 7 -11 0 -7 11 0 -7 -11 0 -7 -12 0 7 -12 0 -7 12 0 7 -13 0 -7 13 0 -7 -13 0 7 -14 0 -7 -14 0 -7 14 0 -7 15 0 7 -15 0 -7 -15 0 7 -16 0 -7 16 0 7 -17 0 -7 18 0 7 -18 0 -7 19 0 7 -19 0 8 0 0 8 1 0 8 -1 0 8 2 0 8 -2 0 8 3 0 8 -3 0 8 -4 -1 0 39 1 0 -39 -1 0 38 -1 0 37 -1 0 36 -1 0 35 -1 0 34 -1 0 33 -1 0 32 -1 0 31 -1 0 31 -1 0 30 -1 0 30 -1 0 29 -1 0 29 -1 0 28 -1 0 28 -1 0 27 -1 0 27 -1 0 26 -1 0 26 -1 0 25 1 0 -25 -1 0 25 -1 0 24 1 0 -24 -1 0 24 -1 0 23 1 0 -23 -1 0 22 1 0 -22 1 0 -21 1 0 -20 1 0 -19 -1 0 19 1 0 -18 1 0 -18 -1 0 18 1 0 -17 1 0 -17 -1 0 17 -1 0 16 1 0 -16 1 0 -16 1 0 -15 -1 0 15 1 0 -15 1 0 -14 -1 0 14 1 0 -13 -1 0 13 1 0 -13 1 0 -12 -1 0 12 1 0 -12 1 0 -11 1 0 -11 -1 0 11 1 0 -10 1 0 -10 -1 0 9 1 0 -9 1 0 -8 -1 0 8 -1 0 7 1 0 -7 1 0 -7 -1 0 7 -1 0 6 1 0 -6 -1 0 6 1 0 -6 -1 0 5 1 0 -5 1 0 -5 -1 0 5 -1 0 4 1 0 -4 1 0 -4 -1 0 4 1 0 -3 -1 0 3 1 0 -3 -1 0 3 -1 0 3 -1 0 2 -1 0 2 -1 0 1 -1 0 1 -1 0 1 -1 0 1 -1 0 1 -1 0 1 -1 0 0 -1 0 0 -1 0 0 -1 0 0 -1 0 0 -1 0 -1 -1 0 -1 -1 0 -1 -1 0 -2 -1 0 -2 1 0 2 -1 0 -2 -1 0 -2 1 0 3 1 0 3 -1 0 -3 -1 0 -3 -1 0 -4 1 0 4 1 0 4 1 0 5 1 0 5 -1 0 -5 1 0 6 -1 0 -6 1 0 6 -1 0 -7 1 0 7 -1 0 -8 1 0 8 -1 0 -9 1 0 9 1 0 10 -1 0 -10 -1 0 -11 1 0 11 -1 0 -12 1 0 12 1 0 13 -1 0 -13 -1 0 -14 1 0 14 -1 0 -15 1 0 15 1 0 16 -1 0 -16 1 0 17 -1 0 -17 -1 0 -18 1 0 18 -1 0 -19 1 0 19 1 0 20 -1 0 -20 1 0 21 -1 0 -21 1 0 22 -1 0 -22 1 0 23 -1 0 -23 -1 0 -24 1 0 24 -1 0 -25 -1 0 -26 -1 0 -27 -1 0 -28 -1 0 -29 -1 0 -30 1 0 31 1 0 32 1 0 33 1 0 34 -1 0 -34 1 0 35 -1 0 -35 -1 0 -36 1 0 36 -1 0 -37 1 0 37 1 0 38 -1 0 -38 1 -1 -39 -1 1 39 -1 1 38 -1 1 37 -1 1 36 -1 1 35 -1 1 34 -1 1 33 -1 -1 33 -1 1 32 -1 -1 32 -1 -1 31 -1 1 31 -1 -1 30 -1 1 30 -1 -1 29 -1 1 29 -1 1 28 -1 -1 28 -1 1 27 -1 -1 27 -1 -1 27 -1 1 26 -1 -1 26 -1 1 25 1 -1 -25 -1 1 24 -1 -1 24 1 -1 -24 -1 -1 23 -1 1 23 1 1 -23 1 -1 -23 1 1 -23 1 1 -22 -1 1 22 1 -1 -22 1 1 -22 -1 1 22 -1 -1 22 1 1 -21 -1 1 21 1 -1 -21 -1 1 21 1 1 -21 1 -1 -20 1 1 -20 1 1 -20 1 -1 -19 1 1 -19 1 1 -19 1 1 -18 1 1 -18 1 -1 -18 1 1 -17 1 1 -17 1 -1 -17 1 1 -16 1 1 -16 1 -1 -16 1 1 -15 1 -1 -15 1 1 -15 1 -1 -14 1 1 -14 1 1 -14 -1 -1 13 1 1 -13 1 -1 -13 1 1 -13 1 1 -12 1 -1 -12 1 1 -12 -1 -1 12 -1 -1 11 1 1 -11 1 1 -11 1 -1 -11 1 1 -10 1 1 -10 1 -1 -10 -1 -1 10 -1 1 10 -1 1 9 -1 -1 9 1 1 -9 -1 1 9 1 1 -9 1 -1 -9 1 -1 -8 -1 1 8 -1 1 8 1 1 -8 1 1 -8 -1 1 7 1 1 -7 -1 1 7 1 -1 -7 -1 1 6 -1 1 6 1 1 -6 -1 1 6 -1 1 6 -1 -1 6 1 -1 -6 -1 1 5 -1 1 5 1 1 -5 -1 -1 5 -1 1 5 1 1 -4 -1 -1 4 -1 -1 4 -1 1 4 -1 1 4 -1 1 4 1 1 -4 -1 -1 3 -1 1 3 1 1 -3 -1 1 3 -1 1 3 -1 -1 3 1 1 -3 -1 -1 3 1 1 -2 -1 1 2 -1 -1 2 -1 -1 2 -1 1 2 -1 -1 2 -1 1 2 -1 1 1 -1 -1 1 -1 -1 1 1 1 -1 -1 -1 1 -1 -1 1 -1 1 1 -1 1 0 -1 1 0 -1 -1 0 -1 -1 0 -1 -1 0 1 1 0 -1 -1 0 -1 -1 -1 -1 1 -1 1 1 1 -1 1 -1 1 1 1 -1 -1 -1 -1 1 -1 -1 -1 -1 -1 -1 -1 -1 1 -2 -1 1 -2 -1 -1 -2 -1 -1 -2 1 1 2 -1 -1 -2 -1 -1 -2 -1 -1 -2 -1 1 -2 1 1 2 -1 1 -2 1 1 3 -1 1 -3 -1 -1 -3 1 1 3 -1 -1 -3 -1 1 -3 -1 -1 -3 -1 -1 -4 1 1 4 -1 1 -4 -1 -1 -4 -1 1 -5 1 1 5 -1 1 -5 -1 -1 -5 -1 -1 -5 -1 -1 -6 1 1 6 -1 1 -6 -1 1 -6 -1 -1 -6 -1 -1 -7 1 1 7 -1 1 -7 -1 1 -7 -1 -1 -7 -1 1 -8 1 1 8 -1 -1 -8 -1 -1 -8 -1 1 -8 -1 1 -9 -1 -1 -9 1 1 9 -1 1 -9 -1 -1 -9 -1 -1 -10 -1 1 -10 1 1 10 -1 1 -10 -1 1 -11 -1 -1 -11 1 1 11 -1 -1 -12 1 -1 12 -1 1 -12 1 1 12 -1 -1 -13 1 -1 13 -1 1 -13 1 -1 14 -1 1 -14 -1 -1 -14 -1 1 -15 -1 -1 -15 1 -1 15 -1 1 -16 1 -1 16 -1 -1 -16 1 -1 17 -1 1 -17 -1 -1 -17 1 -1 18 -1 -1 -18 -1 -1 -19 1 -1 19 1 -1 20 1 -1 21 -1 1 -21 -1 -1 -21 -1 1 -22 -1 -1 -22 -1 1 -23 1 -1 23 -1 -1 -23 1 -1 24 -1 -1 -24 -1 1 -24 -1 1 -25 -1 1 -26 1 1 27 -1 1 -27 1 1 28 -1 1 -28 -1 1 -29 1 1 29 1 1 30 -1 1 -30 1 1 31 -1 1 -31 1 1 32 -1 1 -32 1 1 33 -1 1 -33 1 -1 33 -1 -1 -33 -1 1 -33 -1 1 -34 -1 -1 -34 1 1 34 1 -1 34 -1 1 -34 -1 -1 -35 1 1 35 1 -1 35 -1 1 -35 1 -1 36 -1 1 -36 1 1 36 -1 -1 -36 1 1 37 -1 -1 -37 -1 1 -37 1 -1 37 1 -1 38 1 1 38 -1 1 -38 -1 -1 -38 -1 2 38 -1 2 37 -1 2 37 -1 2 36 -1 2 36 -1 2 35 -1 2 35 -1 2 34 -1 2 34 -1 2 33 -1 2 33 -1 2 32 -1 2 32 -1 2 31 -1 2 30 -1 2 29 -1 2 28 -1 2 27 -1 2 26 -1 2 25 1 2 -25 1 2 -24 -1 2 24 1 -2 -24 -1 2 23 1 2 -23 1 -2 -23 1 2 -23 -1 2 23 1 2 -22 1 2 -22 -1 2 22 -1 -2 22 -1 2 22 1 -2 -22 -1 -2 21 -1 2 21 1 -2 -21 -1 2 21 1 2 -21 1 2 -21 1 2 -20 -1 -2 20 1 2 -20 -1 2 20 -1 2 20 1 -2 -20 1 -2 -19 1 2 -19 -1 2 19 -1 2 18 1 2 -18 1 -2 -18 -1 2 17 1 2 -17 1 -2 -17 -1 2 16 1 2 -16 1 -2 -16 -1 2 15 1 2 -15 1 -2 -15 1 2 -14 1 -2 -14 -1 2 14 1 2 -13 -1 2 13 1 -2 -13 1 2 -12 1 -2 -12 -1 2 12 1 -2 -11 -1 2 11 1 2 -11 -1 2 11 -1 2 10 -1 2 10 1 2 -10 -1 2 10 1 -2 -10 -1 2 9 -1 2 9 1 -2 -9 -1 2 9 -1 2 8 1 -2 -8 -1 2 8 -1 2 8 -1 -2 8 -1 2 7 -1 -2 7 -1 2 7 -1 2 6 -1 2 6 -1 -2 6 -1 -2 5 -1 2 5 -1 2 5 -1 2 4 -1 -2 4 -1 2 4 -1 -2 3 -1 2 3 -1 2 3 1 2 -3 -1 -2 3 -1 2 2 -1 -2 2 -1 2 2 -1 -2 2 1 2 -2 1 2 -1 -1 -2 1 -1 2 1 -1 -2 1 -1 -2 0 1 2 0 -1 -2 0 1 2 1 -1 -2 -1 -1 -2 -1 -1 -2 -2 1 2 2 -1 -2 -3 1 2 3 1 2 4 1 2 4 1 2 4 -1 -2 -4 1 2 5 1 2 5 -1 -2 -5 1 2 5 1 2 6 1 2 6 -1 -2 -6 1 2 6 1 2 7 -1 -2 -7 1 2 7 1 2 7 1 2 8 1 2 8 1 2 8 1 2 9 1 2 9 1 2 9 1 2 10 1 2 10 1 2 10 1 2 11 1 2 11 1 2 11 1 2 12 1 2 12 1 2 12 1 2 13 1 2 13 1 2 13 1 2 14 1 2 14 1 2 14 1 2 15 1 2 15 1 2 15 1 -2 15 1 -2 16 1 2 16 1 2 16 1 2 17 1 -2 17 1 2 17 1 -2 18 1 2 18 1 2 18 -1 -2 -19 1 -2 19 -1 2 -19 1 2 19 1 2 20 1 -2 20 -1 2 -20 -1 -2 -20 -1 -2 -21 1 -2 21 -1 2 -21 1 2 21 -1 -2 -22 1 2 22 -1 2 -22 1 -2 22 1 -2 23 -1 -2 -23 -1 2 -23 -1 2 -24 -1 -2 -24 -1 -2 -25 -1 2 -25 -1 2 -26 -1 -2 -26 -1 -2 -27 -1 2 -27 -1 2 -28 -1 2 -29 -1 2 -30 -1 2 -31 -1 2 -32 -1 2 -33 -1 2 -34 -1 2 -35 1 2 36 1 2 37 -1 3 36 -1 3 35 -1 3 34 -1 3 33 -1 3 32 -1 3 31 -1 3 30 1 3 -30 1 -3 -29 1 3 -29 1 -3 -28 1 3 -28 1 -3 -27 1 3 -27 1 -3 -26 1 3 -26 1 3 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3 14 -8 3 14 -8 3 13 -8 3 13 -8 3 13 -8 3 12 -8 3 12 -8 3 11 -8 3 11 -8 3 11 -8 -3 10 -8 3 10 -8 3 10 -8 -3 9 -8 3 9 -8 3 9 -8 -3 8 -8 3 8 -8 3 8 -8 -3 7 -8 3 7 -8 -3 6 -8 3 6 -8 -3 5 -8 3 5 -8 -3 4 -8 3 4 -8 -3 3 -8 3 3 -8 -3 2 -8 -3 1 -8 3 1 -8 -3 0 -8 3 0 -8 -3 -1 -8 3 -1 -8 -3 -2 -8 3 -2 -8 -3 -3 -8 3 -3 -8 -3 -4 -8 3 -4 -8 -3 -5 -8 -3 -6 -8 -3 -7 -8 3 -7 -8 -3 -8 -8 3 -8 -8 -3 -9 -8 3 -9 -8 -3 -10 -8 3 -10 -8 -3 -11 -8 3 -11 -8 -3 -12 -8 3 -12 -8 -3 -13 -8 3 -13 -8 -3 -14 -8 3 -14 -8 -3 -15 -8 3 -15 -8 -3 -16 -8 3 -16 -8 3 -17 -8 3 -18 -8 3 -19 -8 4 21 -8 4 20 -8 4 20 -8 4 19 -8 4 19 -8 4 18 -8 4 18 -8 4 17 -8 4 17 -8 4 16 -8 4 16 -8 4 15 -8 4 15 -8 4 14 -8 4 14 -8 4 13 -8 4 13 -8 4 12 -8 4 12 -8 4 11 -8 4 11 -8 4 10 -8 4 9 -8 -4 8 -8 4 8 -8 -4 7 -8 4 7 -8 -4 6 -8 4 6 -8 -4 5 -8 4 5 -8 -4 4 -8 4 4 -8 -4 3 -8 4 3 -8 -4 2 -8 -4 1 -8 -4 0 -8 -4 -1 -8 -4 -2 -8 -4 -3 -8 -4 -4 -8 -4 -5 -8 -4 -6 -8 -4 -7 -8 -4 -8 -8 -4 -9 -8 -4 -10 -8 -4 -11 -8 -4 -12 -8 -4 -13 -8 -4 -14 -8 -4 -15 -8 5 13 -8 5 12 -8 5 12 -8 5 11 -8 5 11 -8 5 10 -8 5 9 -8 5 8 -8 5 7 -8 5 6 -8 5 5 -8 -5 4 -8 -5 3 -8 -5 2 -8 -5 1 -8 -5 0 -8 -5 -1 -8 -5 -2 -8 -5 -3 -8 -5 -4 -8 -5 -5 -8 -5 -6 -8 -5 -7 -9 0 25 -9 0 24 -9 0 23 -9 0 22 -9 0 21 -9 0 21 -9 0 20 -9 0 20 -9 0 19 -9 0 19 -9 0 18 -9 0 18 -9 0 17 -9 0 17 -9 0 16 -9 0 16 -9 0 16 -9 0 15 -9 0 15 -9 0 14 -9 0 14 -9 0 13 -9 0 13 -9 0 12 -9 0 12 -9 0 11 -9 0 11 -9 0 10 -9 0 10 -9 0 9 -9 0 9 -9 0 8 -9 0 8 -9 0 7 -9 0 7 -9 0 6 -9 0 6 -9 0 5 -9 0 5 -9 0 5 -9 0 4 -9 0 4 -9 0 4 -9 0 3 -9 0 3 -9 0 2 -9 0 2 -9 0 1 -9 0 0 -9 0 0 -9 0 -1 -9 0 -1 -9 0 -2 -9 0 -2 -9 0 -3 -9 0 -4 -9 0 -4 -9 0 -4 -9 0 -5 -9 0 -5 -9 0 -5 -9 0 -6 -9 0 -6 -9 0 -6 -9 0 -7 -9 0 -7 -9 0 -7 -9 0 -8 -9 0 -8 -9 0 -9 -9 0 -9 -9 0 -10 -9 0 -10 -9 0 -11 -9 0 -11 -9 0 -12 -9 0 -12 -9 0 -13 -9 0 -13 -9 0 -14 -9 0 -14 -9 0 -15 -9 0 -15 -9 0 -16 -9 0 -17 -9 0 -18 -9 1 24 -9 1 23 -9 -1 22 -9 1 22 -9 1 22 -9 -1 21 -9 1 21 -9 1 21 -9 1 21 -9 -1 20 -9 1 20 -9 1 20 -9 1 20 -9 1 19 -9 1 19 -9 1 19 -9 1 18 -9 1 18 -9 -1 18 -9 1 17 -9 1 17 -9 1 17 -9 -1 17 -9 1 16 -9 1 16 -9 -1 16 -9 1 15 -9 1 15 -9 -1 15 -9 1 14 -9 1 14 -9 -1 14 -9 1 13 -9 -1 13 -9 1 13 -9 1 12 -9 1 12 -9 -1 12 -9 1 11 -9 -1 11 -9 1 11 -9 1 10 -9 -1 10 -9 1 10 -9 -1 10 -9 1 9 -9 -1 9 -9 1 9 -9 -1 9 -9 1 8 -9 -1 8 -9 1 8 -9 -1 8 -9 1 7 -9 -1 7 -9 -1 7 -9 1 7 -9 1 6 -9 -1 6 -9 1 6 -9 1 5 -9 1 5 -9 1 5 -9 1 4 -9 1 4 -9 1 4 -9 1 3 -9 1 3 -9 1 3 -9 1 2 -9 -1 2 -9 1 2 -9 1 2 -9 1 1 -9 1 1 -9 -1 1 -9 1 0 -9 1 0 -9 1 -1 -9 1 -1 -9 1 -2 -9 1 -2 -9 1 -2 -9 1 -3 -9 1 -3 -9 1 -3 -9 1 -4 -9 1 -4 -9 1 -5 -9 -1 -5 -9 1 -5 -9 1 -5 -9 1 -5 -9 1 -6 -9 -1 -6 -9 1 -6 -9 1 -6 -9 1 -7 -9 -1 -7 -9 1 -7 -9 1 -7 -9 1 -8 -9 -1 -8 -9 1 -8 -9 1 -8 -9 -1 -9 -9 1 -9 -9 1 -9 -9 1 -9 -9 1 -10 -9 -1 -10 -9 1 -10 -9 1 -10 -9 1 -11 -9 1 -11 -9 -1 -11 -9 1 -11 -9 1 -12 -9 -1 -12 -9 1 -12 -9 1 -12 -9 1 -13 -9 -1 -13 -9 1 -13 -9 1 -13 -9 1 -14 -9 -1 -14 -9 1 -14 -9 1 -14 -9 1 -15 -9 -1 -15 -9 1 -15 -9 1 -15 -9 1 -16 -9 1 -16 -9 -1 -16 -9 1 -16 -9 1 -17 -9 -1 -17 -9 1 -17 -9 1 -17 -9 1 -18 -9 2 23 -9 2 23 -9 2 22 -9 2 22 -9 2 21 -9 2 21 -9 2 20 -9 2 20 -9 2 19 -9 2 19 -9 2 18 -9 2 18 -9 2 17 -9 2 17 -9 2 17 -9 2 16 -9 2 16 -9 2 16 -9 2 15 -9 2 15 -9 2 15 -9 2 14 -9 2 14 -9 2 13 -9 2 13 -9 2 12 -9 2 12 -9 2 11 -9 2 11 -9 2 10 -9 2 9 -9 2 9 -9 2 8 -9 2 8 -9 2 7 -9 2 7 -9 2 6 -9 2 6 -9 2 5 -9 2 5 -9 2 4 -9 2 4 -9 2 3 -9 2 3 -9 2 3 -9 2 2 -9 2 2 -9 2 1 -9 2 1 -9 2 0 -9 2 0 -9 2 -1 -9 2 -1 -9 2 -2 -9 2 -2 -9 2 -3 -9 2 -3 -9 2 -3 -9 2 -4 -9 2 -4 -9 2 -4 -9 2 -5 -9 2 -5 -9 2 -5 -9 2 -6 -9 2 -6 -9 2 -6 -9 2 -7 -9 2 -7 -9 2 -8 -9 2 -8 -9 2 -9 -9 2 -9 -9 2 -10 -9 2 -10 -9 2 -11 -9 2 -11 -9 2 -12 -9 2 -12 -9 2 -13 -9 2 -13 -9 2 -14 -9 2 -14 -9 2 -15 -9 2 -15 -9 2 -16 -9 2 -16 -9 3 19 -9 3 18 -9 3 17 -9 3 17 -9 3 16 -9 3 16 -9 3 15 -9 3 15 -9 3 14 -9 3 13 -9 3 12 -9 3 11 -9 3 10 -9 3 9 -9 3 9 -9 3 8 -9 3 8 -9 3 7 -9 3 7 -9 -3 6 -9 3 6 -9 3 6 -9 -3 5 -9 3 5 -9 3 5 -9 -3 4 -9 3 4 -9 3 4 -9 -3 3 -9 3 3 -9 -3 2 -9 3 2 -9 -3 1 -9 3 1 -9 -3 0 -9 3 0 -9 -3 -1 -9 3 -1 -9 -3 -2 -9 3 -2 -9 -3 -3 -9 3 -3 -9 -3 -4 -9 3 -4 -9 -3 -5 -9 3 -5 -9 -3 -6 -9 3 -7 -9 3 -8 -9 3 -9 -9 3 -10 -9 3 -11 -9 3 -12 -9 4 13 -9 4 13 -9 4 12 -9 4 12 -9 4 11 -9 4 11 -9 4 10 -9 4 10 -9 4 9 -9 4 9 -9 4 8 -9 4 8 -9 4 7 -9 4 7 -9 4 6 -9 4 6 -9 4 5 -9 4 5 -9 4 4 -9 -4 3 -9 4 3 -9 -4 2 -9 -4 1 -9 -4 0 -9 -4 -1 -9 -4 -2 -9 -4 -3 -9 -4 -4 -9 -4 -5 -9 -4 -6 -10 0 18 -10 0 17 -10 0 16 -10 0 15 -10 0 14 -10 0 13 -10 0 12 -10 0 12 -10 0 11 -10 0 11 -10 0 10 -10 0 10 -10 0 9 -10 0 8 -10 0 7 -10 0 6 -10 0 5 -10 0 0 -10 0 -1 -10 0 -2 -10 0 -3 -10 0 -4 -10 0 -5 -10 0 -6 -10 0 -7 -10 0 -8 -10 0 -9 -10 0 -10 -10 1 18 -10 1 17 -10 1 17 -10 1 16 -10 1 16 -10 1 15 -10 1 15 -10 1 14 -10 1 14 -10 1 13 -10 1 13 -10 1 12 -10 1 12 -10 1 11 -10 1 11 -10 1 10 -10 1 10 -10 1 9 -10 1 8 -10 1 7 -10 1 6 -10 1 5 -10 1 4 -10 1 4 -10 1 3 -10 1 2 -10 1 1 -10 1 1 -10 1 0 -10 1 -1 -10 1 -2 -10 1 -3 -10 1 -4 -10 1 -5 -10 1 -6 -10 1 -7 -10 1 -8 -10 1 -9 -10 1 -10 -10 1 -11 -10 2 15 -10 2 15 -10 2 14 -10 2 14 -10 2 13 -10 2 12 -10 2 11 -10 2 10 -10 2 10 -10 2 9 -10 2 9 -10 2 8 -10 2 8 -10 2 7 -10 2 7 -10 2 6 -10 2 6 -10 2 5 -10 2 5 -10 2 4 -10 2 3 -10 2 2 -10 2 1 -10 2 0 -10 2 -1 -10 2 -1 -10 2 -2 -10 2 -3 -10 2 -4 -10 2 -5 -10 2 -6 -10 2 -7 -10 3 8 -10 3 8 -10 3 7 -10 3 7 -10 3 6 -10 3 6 -10 3 5 -10 3 4 -10 3 3 -10 3 2 -10 3 1 -10 3 0 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C10 N1 C2 . . 119.83(10) ? C3 C2 N1 . . 121.62(10) ? C11 C2 N1 . . 117.02(9) ? C11 C2 C3 . . 121.27(10) ? C4 C3 C2 . . 122.15(10) ? C8 C3 C2 . . 118.28(10) ? C8 C3 C4 . . 119.55(10) ? H4 C4 C3 . . 119.75(6) ? C5 C4 C3 . . 120.49(10) ? C5 C4 H4 . . 119.75(7) ? C6 C5 C4 . . 120.02(10) ? O22 C5 C4 . . 125.12(11) ? O22 C5 C6 . . 114.86(10) ? C7 C6 C5 . . 120.18(10) ? O24 C6 C5 . . 114.08(10) ? O24 C6 C7 . . 125.74(11) ? H7 C7 C6 . . 119.75(7) ? C8 C7 C6 . . 120.51(10) ? C8 C7 H7 . . 119.75(7) ? C7 C8 C3 . . 119.20(10) ? C9 C8 C3 . . 118.26(10) ? C9 C8 C7 . . 122.54(10) ? H9 C9 C8 . . 120.43(6) ? C10 C9 C8 . . 119.14(10) ? C10 C9 H9 . . 120.43(7) ? C9 C10 N1 . . 122.73(11) ? H10 C10 N1 . . 118.63(6) ? H10 C10 C9 . . 118.63(7) ? H11a C11 C2 . . 108.51(6) ? H11b C11 C2 . . 108.51(6) ? H11b C11 H11a . . 107.5 ? C12 C11 C2 . . 115.05(9) ? C12 C11 H11a . . 108.51(5) ? C12 C11 H11b . . 108.51(6) ? C13 C12 C11 . . 119.63(10) ? C17 C12 C11 . . 121.16(10) ? C17 C12 C13 . . 119.20(10) ? H13 C13 C12 . . 119.55(6) ? C14 C13 C12 . . 120.90(10) ? C14 C13 H13 . . 119.55(7) ? C15 C14 C13 . . 119.43(10) ? O18 C14 C13 . . 125.11(10) ? O18 C14 C15 . . 115.46(10) ? C16 C15 C14 . . 119.43(10) ? O20 C15 C14 . . 115.67(10) ? O20 C15 C16 . . 124.90(10) ? H16 C16 C15 . . 119.68(7) ? C17 C16 C15 . . 120.64(10) ? C17 C16 H16 . . 119.68(7) ? C16 C17 C12 . . 120.38(10) ? H17 C17 C12 . . 119.81(7) ? H17 C17 C16 . . 119.81(7) ? C19 O18 C14 . . 117.12(9) ? H19a C19 O18 . . 109.5 ? H19b C19 O18 . . 109.5 ? H19b C19 H19a . . 109.5 ? H19c C19 O18 . . 109.5 ? H19c C19 H19a . . 109.5 ? H19c C19 H19b . . 109.5 ? C21 O20 C15 . . 116.43(9) ? H21a C21 O20 . . 109.5 ? H21b C21 O20 . . 109.5 ? H21b C21 H21a . . 109.5 ? H21c C21 O20 . . 109.5 ? H21c C21 H21a . . 109.5 ? H21c C21 H21b . . 109.5 ? C23 O22 C5 . . 116.42(9) ? H23a C23 O22 . . 109.5 ? H23b C23 O22 . . 109.5 ? H23b C23 H23a . . 109.5 ? H23c C23 O22 . . 109.5 ? H23c C23 H23a . . 109.5 ? H23c C23 H23b . . 109.5 ? C25 O24 C6 . . 117.14(10) ? H25a C25 O24 . . 109.5 ? H25b C25 O24 . . 109.5 ? H25b C25 H25a . . 109.5 ? H25c C25 O24 . . 109.5 ? H25c C25 H25a . . 109.5 ? H25c C25 H25b . . 109.5 ? O32 C30 O31 . . 124.73(10) ? C33 C30 O31 . . 113.12(10) ? C33 C30 O32 . . 122.15(10) ? H31 O31 C30 . . 109.5 ? C33 C33 C30 3_566 . 122.17(13) ? H33 C33 C30 . . 118.91(6) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 C2 . 1.3245(14) ? N1 C10 . 1.3652(15) ? C2 C3 . 1.4195(15) ? C2 C11 . 1.5053(15) ? C3 C4 . 1.4187(16) ? C3 C8 . 1.4172(16) ? C4 H4 . 0.9500 ? C4 C5 . 1.3670(15) ? C5 C6 . 1.4386(17) ? C5 O22 . 1.3561(14) ? C6 C7 . 1.3670(17) ? C6 O24 . 1.3533(14) ? C7 H7 . 0.9500 ? C7 C8 . 1.4211(16) ? C8 C9 . 1.4145(16) ? C9 H9 . 0.9500 ? C9 C10 . 1.3602(17) ? C10 H10 . 0.9500 ? C11 H11a . 0.9900 ? C11 H11b . 0.9900 ? C11 C12 . 1.5183(15) ? C12 C13 . 1.4011(16) ? C12 C17 . 1.3819(16) ? C13 H13 . 0.9500 ? C13 C14 . 1.3880(16) ? C14 C15 . 1.4120(16) ? C14 O18 . 1.3684(14) ? C15 C16 . 1.3817(16) ? C15 O20 . 1.3688(13) ? C16 H16 . 0.9500 ? C16 C17 . 1.3984(16) ? C17 H17 . 0.9500 ? O18 C19 . 1.4288(15) ? C19 H19a . 0.9800 ? C19 H19b . 0.9800 ? C19 H19c . 0.9800 ? O20 C21 . 1.4285(14) ? C21 H21a . 0.9800 ? C21 H21b . 0.9800 ? C21 H21c . 0.9800 ? O22 C23 . 1.4296(15) ? C23 H23a . 0.9800 ? C23 H23b . 0.9800 ? C23 H23c . 0.9800 ? O24 C25 . 1.4372(15) ? C25 H25a . 0.9800 ? C25 H25b . 0.9800 ? C25 H25c . 0.9800 ? C30 O31 . 1.3064(14) ? C30 O32 . 1.2230(14) ? C30 C33 . 1.4884(16) ? O31 H31 . 0.8400 ? C33 C33 3_566 1.319(2) ? C33 H33 . 0.9500 ? 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 O31 H31 N1 1_555 0.840(7) 1.730(7) 2.5687(12) 175.4(12) C9 H9 O32 3_676 0.9500(16) 2.2706(14) 3.2191(14) 176.13(11) 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N1 C2 C3 C4 . . . . -177.32(10) ? N1 C2 C3 C8 . . . . 4.06(12) ? N1 C2 C11 C12 . . . . 113.81(10) ? N1 C10 C9 C8 . . . . 2.72(13) ? C2 C3 C4 C5 . . . . -178.66(11) ? C2 C3 C8 C7 . . . . 177.22(10) ? C2 C3 C8 C9 . . . . -1.70(12) ? C2 C11 C12 C13 . . . . 133.10(9) ? C2 C11 C12 C17 . . . . -47.48(11) ? C3 C4 C5 C6 . . . . 2.05(12) ? C3 C4 C5 O22 . . . . -177.78(10) ? C3 C8 C7 C6 . . . . 0.89(12) ? C3 C8 C9 C10 . . . . -1.52(12) ? C4 C5 C6 C7 . . . . -2.60(13) ? C4 C5 C6 O24 . . . . 177.69(11) ? C4 C5 O22 C23 . . . . 9.21(14) ? C5 C6 C7 C8 . . . . 1.10(13) ? C5 C6 O24 C25 . . . . -175.75(11) ? C6 C7 C8 C9 . . . . 179.76(11) ? C7 C8 C9 C10 . . . . 179.60(11) ? C11 C12 C13 C14 . . . . -179.55(10) ? C11 C12 C17 C16 . . . . 179.76(10) ? C12 C13 C14 C15 . . . . -0.40(12) ? C12 C13 C14 O18 . . . . 179.50(10) ? C12 C17 C16 C15 . . . . 0.01(13) ? C13 C14 C15 C16 . . . . -0.41(12) ? C13 C14 C15 O20 . . . . -179.63(10) ? C13 C14 O18 C19 . . . . -0.69(14) ? C14 C15 C16 C17 . . . . 0.61(12) ? C14 C15 O20 C21 . . . . -177.02(10) ? C30 C33 C33 C30 . . 3_566 3_566 180.00(14) ?