#------------------------------------------------------------------------------ #$Date: 2023-07-29 05:02:20 +0300 (Sat, 29 Jul 2023) $ #$Revision: 285384 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/28/2022828.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_2022828 loop_ _publ_author_name 'Naeem, Marilyn' 'Le, Alexander N.' 'Bauer, Barbara E.' 'Chadeayne, Andrew R.' 'Golen, James A.' 'Manke, David R.' _publ_section_title ; N-Cyclohexyltryptamine: freebase, bromide and fumarate ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_page_first 752 _journal_page_last 756 _journal_paper_doi 10.1107/S2056989023006217 _journal_volume 79 _journal_year 2023 _chemical_formula_iupac 'C16 H23 N2 +, C2 H O2 -' _chemical_formula_moiety 'C16 H23 N2 +, C2 H O2 -' _chemical_formula_sum 'C18 H24 N2 O2' _chemical_formula_weight 300.39 _chemical_name_common ; N-Cyclohexyltryptammonium fumarate ; _chemical_name_systematic ; Bis{N-[2-(1H-indol-3-yl)ethyl]cyclohexanaminium} (2E)-but-2-enedioate ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _cell_angle_alpha 90 _cell_angle_beta 99.865(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.2231(10) _cell_length_b 16.1611(16) _cell_length_c 11.4595(12) _cell_measurement_reflns_used 7849 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 26.33 _cell_measurement_theta_min 2.63 _cell_volume 1682.8(3) _computing_cell_refinement ; SAINT (Bruker, 2021) ; _computing_data_collection ; APEX4 (Bruker, 2021) ; _computing_data_reduction ; SAINT (Bruker, 2021) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 297.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker D8 Venture CMOS' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_unetI/netI 0.0184 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 20060 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.404 _diffrn_reflns_theta_min 2.571 _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6941 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour bronze _exptl_crystal_density_diffrn 1.186 _exptl_crystal_description block _exptl_crystal_F_000 648 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.221 _refine_diff_density_min -0.172 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 211 _refine_ls_number_reflns 3446 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0426 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.4152P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1112 _refine_ls_wR_factor_ref 0.1214 _reflns_number_gt 2803 _reflns_number_total 3446 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file tx2070sup1.cif _cod_data_source_block III _cod_database_code 2022828 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.976 _shelx_estimated_absorpt_t_max 0.985 _shelx_hkl_file ; -2 0 0 832.62 29.00 3 0 0 0.80 0.50 3 0 0 0.00 0.50 -3 0 0 0.20 0.50 4 0 0 916.91 16.90 -4 0 0 927.21 16.90 5 0 0 -0.40 0.70 5 0 0 -0.70 0.60 -5 0 0 0.20 0.70 6 0 0 339.77 7.00 -6 0 0 336.27 7.00 6 0 0 333.07 7.00 -7 0 0 -1.80 0.80 7 0 0 0.30 1.10 7 0 0 -1.00 0.90 8 0 0 41.10 2.20 -8 0 0 42.40 2.40 8 0 0 39.90 2.30 9 0 0 0.00 1.10 -9 0 0 0.00 1.10 -10 0 0 2.20 1.40 10 0 0 2.60 1.30 10 0 0 5.20 1.40 -11 0 0 -2.10 1.20 11 0 0 -2.40 1.30 11 0 0 -3.10 1.30 -1 1 0 569.04 16.80 2 -1 0 18.90 0.80 2 -1 0 20.30 0.90 -2 -1 0 18.50 1.00 -2 1 0 17.80 0.90 2 1 0 17.10 1.00 -2 1 0 17.60 0.90 3 -1 0 82.09 2.00 3 -1 0 83.89 2.00 -3 -1 0 75.79 2.10 -3 1 0 81.49 2.00 -3 1 0 82.79 2.00 3 1 0 81.59 2.10 4 -1 0 23.50 1.30 4 -1 0 24.90 1.30 -4 -1 0 22.10 1.40 -4 1 0 25.40 1.30 4 1 0 23.10 1.40 4 1 0 24.00 1.40 -5 -1 0 3.50 0.80 5 -1 0 2.50 0.70 5 -1 0 4.10 0.80 5 1 0 4.00 0.80 -5 1 0 3.20 0.80 5 1 0 4.00 0.90 6 -1 0 38.40 1.80 6 -1 0 36.90 1.70 -6 -1 0 34.30 1.80 6 1 0 31.90 1.80 -6 1 0 37.50 1.80 6 1 0 35.20 1.80 -7 -1 0 8.30 1.20 7 -1 0 9.20 1.20 7 -1 0 4.70 1.30 -7 1 0 8.30 1.20 7 1 0 9.50 1.50 8 -1 0 29.30 2.00 8 -1 0 28.30 2.00 -8 1 0 33.70 2.10 8 1 0 31.90 2.10 8 1 0 30.60 2.10 9 -1 0 73.19 2.90 -9 -1 0 70.99 3.10 -9 1 0 70.69 3.00 9 1 0 74.09 3.10 10 -1 0 23.10 2.30 10 -1 0 28.00 2.40 -10 -1 0 25.60 2.20 10 1 0 23.70 2.30 10 1 0 30.60 3.30 -10 1 0 26.20 2.30 -11 -1 0 0.30 1.50 11 -1 0 -0.50 1.30 11 -1 0 1.20 1.40 11 1 0 -0.20 1.30 -11 1 0 0.70 1.30 11 1 0 0.30 2.20 1 -2 0 948.71 23.40 -1 -2 0 930.01 26.70 -1 2 0 948.31 23.40 2 -2 0 119.79 2.50 2 -2 0 118.19 2.50 -2 -2 0 118.79 2.70 -2 2 0 119.59 2.50 -2 2 0 120.89 2.50 2 2 0 115.89 2.70 3 2 0 929.31 17.00 4 -2 0 2340.57 61.79 -4 -2 0 2374.46 67.09 -4 2 0 2421.46 62.39 5 -2 0 182.88 4.00 5 -2 0 175.78 3.90 -5 -2 0 173.28 4.20 -5 2 0 175.28 4.00 5 2 0 172.18 4.10 6 -2 0 21.00 1.40 6 -2 0 18.60 1.40 -6 -2 0 19.70 1.60 6 2 0 21.60 1.60 -6 2 0 19.60 1.40 6 2 0 18.50 1.60 -7 -2 0 11.10 1.40 7 -2 0 11.20 1.20 7 -2 0 7.90 1.10 7 2 0 6.50 1.30 7 2 0 9.10 1.20 -7 2 0 8.20 1.10 8 -2 0 1.60 1.00 -8 -2 0 3.40 1.20 8 -2 0 2.60 1.10 8 2 0 5.20 1.40 8 2 0 5.70 1.30 -8 2 0 4.20 1.10 9 -2 0 43.10 2.40 -9 -2 0 36.60 2.50 9 2 0 38.10 2.50 -9 2 0 42.80 2.40 10 -2 0 34.10 2.50 10 -2 0 37.50 2.60 -10 -2 0 40.50 2.70 10 2 0 40.10 2.70 10 2 0 31.60 3.00 -10 2 0 34.80 2.40 11 -2 0 0.30 1.20 11 -2 0 1.60 1.40 -11 2 0 0.20 1.20 11 2 0 2.70 1.40 0 -3 0 0.30 0.40 0 -3 0 -0.10 0.40 0 3 0 0.30 0.50 0 3 0 0.30 0.40 1 -3 0 6.50 0.70 1 -3 0 7.30 0.70 -1 -3 0 9.30 0.80 -1 -3 0 6.80 0.70 -1 3 0 6.80 0.60 1 3 0 6.70 0.70 -1 3 0 5.20 0.50 -2 -3 0 20.80 1.30 2 -3 0 24.80 1.40 2 -3 0 23.10 0.90 -2 3 0 22.50 0.90 2 3 0 23.60 1.20 -2 3 0 21.50 0.90 -3 -3 0 47.00 1.70 3 -3 0 48.60 1.40 3 -3 0 48.30 1.40 -3 3 0 45.00 1.40 -3 3 0 45.30 1.40 3 3 0 44.90 1.70 4 -3 0 210.38 4.40 -4 -3 0 206.68 4.70 4 -3 0 215.28 4.40 -4 3 0 221.38 4.40 4 3 0 211.98 4.70 -4 3 0 213.28 4.40 5 -3 0 78.89 2.30 -5 -3 0 83.49 2.60 5 -3 0 79.79 2.30 -5 3 0 76.09 2.30 5 3 0 81.79 2.60 -5 3 0 83.39 2.30 6 -3 0 1.20 0.70 6 -3 0 3.10 0.80 -6 -3 0 2.30 1.00 6 3 0 2.10 1.00 6 3 0 3.10 1.00 -6 3 0 3.40 0.80 7 -3 0 0.20 0.80 7 -3 0 0.70 0.80 -7 -3 0 2.10 1.10 7 3 0 0.10 1.00 -7 3 0 0.80 0.90 7 3 0 2.80 1.20 8 -3 0 62.79 2.50 -8 -3 0 65.59 2.90 8 -3 0 57.29 2.40 8 3 0 61.49 2.80 -8 3 0 59.69 2.50 8 3 0 59.39 2.80 9 -3 0 33.60 2.20 -9 -3 0 35.80 2.60 -9 3 0 33.70 2.30 9 3 0 35.50 2.50 9 3 0 30.90 3.40 -10 -3 0 15.70 1.90 10 -3 0 16.60 1.70 10 -3 0 13.40 1.60 10 3 0 12.70 1.80 10 3 0 13.00 1.70 -10 3 0 13.50 1.70 11 -3 0 6.20 1.50 -11 -3 0 5.10 1.70 11 -3 0 6.90 1.60 -11 3 0 6.30 1.50 11 3 0 7.80 1.70 0 4 0 1926.61 48.10 1 -4 0 200.28 4.10 -1 -4 0 201.68 4.10 1 -4 0 198.78 3.90 -1 -4 0 207.18 4.10 1 4 0 195.08 4.10 -1 4 0 199.78 4.00 -1 4 0 197.98 3.90 -2 -4 0 130.59 3.10 2 -4 0 129.39 2.70 2 -4 0 130.49 2.70 -2 4 0 124.69 2.70 2 4 0 129.69 3.00 -2 4 0 128.09 2.70 -3 -4 0 185.28 4.10 3 -4 0 184.78 3.80 3 -4 0 179.18 3.80 -3 4 0 182.88 3.80 -3 4 0 189.28 4.40 3 4 0 180.38 4.10 4 -4 0 591.84 11.10 4 -4 0 592.04 11.10 -4 -4 0 584.34 11.50 -4 4 0 599.74 11.10 4 4 0 606.84 11.50 -4 4 0 594.64 11.10 5 -4 0 323.37 6.50 5 -4 0 325.67 6.50 -5 -4 0 327.77 7.00 -5 4 0 321.37 6.60 -5 4 0 326.37 6.50 5 4 0 337.17 7.00 -6 -4 0 29.90 2.00 6 -4 0 29.00 1.60 6 -4 0 27.40 1.50 6 4 0 27.50 1.90 -6 4 0 26.70 1.60 -6 4 0 26.60 1.50 -7 -4 0 58.09 2.60 7 -4 0 55.09 2.20 7 -4 0 58.99 2.20 7 4 0 61.89 2.70 -7 4 0 58.69 2.30 7 4 0 62.89 2.70 8 -4 0 6.50 1.20 -8 -4 0 6.70 1.50 8 -4 0 6.10 1.10 8 4 0 5.70 1.50 8 4 0 5.50 1.40 -8 4 0 2.40 1.10 -9 -4 0 29.40 2.60 9 4 0 32.50 2.60 9 4 0 31.80 2.50 -9 4 0 29.10 2.20 10 -4 0 12.70 1.60 10 -4 0 13.10 1.60 -10 -4 0 13.50 1.90 10 4 0 12.50 1.90 10 4 0 9.20 1.70 -10 4 0 13.90 1.60 11 -4 0 -0.30 1.20 11 -4 0 -0.30 1.20 -11 -4 0 2.50 1.50 -11 4 0 -1.40 1.20 11 4 0 3.60 1.70 0 -5 0 -0.30 0.60 0 -5 0 0.50 0.50 0 5 0 -0.10 0.60 0 5 0 -0.10 0.60 -1 -5 0 12.40 1.10 1 -5 0 13.70 0.90 1 -5 0 14.90 0.90 -1 -5 0 13.30 1.10 -1 5 0 13.40 0.90 1 5 0 14.10 1.10 -1 5 0 14.60 1.00 2 -5 0 126.69 2.80 -2 -5 0 136.49 3.40 -2 -5 0 127.49 3.10 2 -5 0 125.09 2.80 -2 5 0 130.49 2.80 2 5 0 124.09 3.10 -2 5 0 130.69 2.80 3 -5 0 44.30 1.50 -3 -5 0 45.50 1.90 3 -5 0 45.90 1.50 3 5 0 44.60 1.90 -3 5 0 45.40 1.50 -3 5 0 48.50 1.50 4 -5 0 176.08 3.80 4 -5 0 170.48 3.80 -4 -5 0 176.08 4.20 4 5 0 185.98 4.30 -4 5 0 173.58 3.80 -4 5 0 177.48 3.80 -5 -5 0 2.20 1.00 5 -5 0 3.20 0.70 5 -5 0 3.40 0.70 5 5 0 2.10 0.90 -5 5 0 1.20 0.70 -5 5 0 2.90 0.70 6 -5 0 68.39 2.20 -6 -5 0 70.89 2.70 6 -5 0 70.19 2.20 -6 5 0 67.49 2.20 -6 5 0 68.79 2.20 6 5 0 65.09 2.60 7 -5 0 6.30 1.10 7 -5 0 6.30 1.00 -7 -5 0 7.80 1.40 -7 5 0 4.80 1.00 7 5 0 6.60 1.30 7 5 0 8.30 1.40 8 -5 0 3.40 1.00 8 -5 0 4.60 1.10 -8 -5 0 3.50 1.40 -8 5 0 2.20 1.10 8 5 0 3.50 1.40 -9 -5 0 12.30 1.70 9 5 0 14.30 1.80 9 5 0 13.50 1.90 -9 5 0 15.90 1.50 -10 -5 0 7.80 1.70 10 -5 0 8.20 1.40 10 -5 0 7.20 2.20 10 5 0 8.20 1.80 -10 5 0 11.00 1.50 10 5 0 7.60 1.90 11 -5 0 0.00 1.10 -11 -5 0 1.10 1.60 -11 -5 0 1.40 1.60 11 -5 0 2.00 1.20 -11 5 0 -0.40 1.20 11 5 0 -1.00 1.50 0 -6 0 657.23 12.20 0 -6 0 651.13 12.20 0 6 0 652.23 12.50 0 6 0 651.03 12.20 -1 -6 0 862.91 15.80 1 -6 0 854.91 15.70 -1 -6 0 838.62 15.80 1 6 0 833.72 15.80 -1 6 0 868.61 15.90 1 6 0 880.11 15.90 2 -6 0 117.19 2.70 -2 -6 0 114.29 3.00 2 -6 0 115.69 2.70 -2 -6 0 117.49 3.00 -2 6 0 114.99 2.70 2 6 0 120.49 3.00 -2 6 0 113.29 2.70 -3 -6 0 193.48 4.60 3 -6 0 202.18 4.20 -3 -6 0 194.48 4.60 3 -6 0 197.28 4.20 -3 6 0 199.78 4.20 -3 6 0 200.28 4.20 3 6 0 203.38 4.60 4 -6 0 35.10 1.40 -4 -6 0 35.60 1.90 4 -6 0 32.90 1.40 4 6 0 36.60 2.00 -4 6 0 32.80 1.40 -4 6 0 33.00 1.40 5 -6 0 29.80 1.40 -5 -6 0 28.60 2.00 5 -6 0 30.60 1.50 -5 6 0 27.90 1.40 5 6 0 31.30 2.00 -5 6 0 27.40 1.40 6 -6 0 -0.50 0.70 -6 -6 0 0.80 1.10 6 -6 0 -0.90 0.70 -6 6 0 -0.20 0.70 -6 6 0 -0.30 0.80 6 6 0 -0.30 1.00 7 -6 0 162.88 4.00 -7 6 0 166.68 4.30 -7 6 0 162.08 4.10 8 -6 0 6.70 1.10 -8 -6 0 5.00 1.40 8 -6 0 4.80 1.10 8 6 0 6.30 1.50 -8 6 0 6.40 1.20 9 -6 0 1.90 1.00 9 -6 0 0.40 0.60 -9 -6 0 -0.70 1.40 -9 6 0 0.20 1.10 9 6 0 1.10 1.40 9 6 0 0.10 1.40 -10 -6 0 4.80 1.70 10 -6 0 3.50 1.20 10 -6 0 4.70 1.20 -10 -6 0 3.20 1.60 10 6 0 0.80 1.70 10 6 0 2.90 1.80 -10 6 0 2.00 1.20 0 -7 0 -1.00 0.60 0 -7 0 -1.00 0.70 0 7 0 0.40 0.70 0 7 0 -0.40 0.70 -1 -7 0 38.80 1.70 -1 -7 0 37.80 1.60 1 -7 0 40.30 1.50 1 -7 0 37.60 1.50 1 7 0 40.60 1.70 1 7 0 37.60 1.70 -1 7 0 39.90 1.50 -1 7 0 42.00 1.60 -2 -7 0 147.09 3.60 -2 -7 0 143.69 3.60 2 -7 0 151.38 3.40 2 -7 0 149.59 3.30 2 7 0 149.09 3.70 -2 7 0 147.19 3.30 -2 7 0 147.29 3.40 3 -7 0 78.99 2.10 -3 -7 0 80.89 2.60 -3 -7 0 79.19 2.60 3 -7 0 76.19 2.20 -3 7 0 75.09 2.20 3 7 0 80.19 2.60 -3 7 0 79.59 2.20 -4 -7 0 134.69 3.70 4 -7 0 130.49 3.10 4 -7 0 129.09 3.10 -4 -7 0 132.09 3.60 -4 7 0 130.79 3.10 4 7 0 130.39 3.60 -4 7 0 127.19 3.10 5 -7 0 60.59 2.00 5 -7 0 62.39 2.00 -5 -7 0 60.79 2.60 -5 -7 0 63.09 2.60 -5 7 0 58.99 2.00 -5 7 0 62.59 2.00 5 7 0 59.89 2.50 -6 -7 0 143.19 4.20 6 -7 0 140.09 3.50 6 -7 0 144.49 3.50 -6 -7 0 141.69 4.20 -6 7 0 139.39 3.50 6 7 0 134.59 4.10 -6 7 0 141.09 3.50 7 -7 0 18.40 1.60 7 -7 0 18.50 1.60 -7 -7 0 19.50 1.90 -7 -7 0 18.40 1.90 -7 7 0 18.00 1.70 -7 7 0 19.10 1.60 -8 -7 0 16.50 2.00 8 -7 0 13.00 1.30 8 -7 0 13.30 1.30 -8 -7 0 11.30 1.80 8 7 0 11.10 1.70 -9 -7 0 63.39 3.40 -9 -7 0 49.20 3.10 9 -7 0 49.80 2.40 9 7 0 49.30 3.60 9 7 0 50.89 3.70 -9 7 0 53.79 2.50 10 -7 0 3.90 1.20 10 -7 0 3.20 1.10 -10 -7 0 1.70 2.40 -10 7 0 1.30 1.10 10 7 0 5.90 1.80 0 -8 0 282.87 5.80 0 -8 0 278.87 5.80 0 8 0 277.47 5.80 0 8 0 274.07 5.80 -1 -8 0 24.70 1.50 1 -8 0 25.70 1.40 -1 -8 0 26.20 1.60 1 -8 0 24.60 1.40 -1 8 0 25.20 1.40 1 8 0 24.80 1.60 1 8 0 24.30 1.60 -1 8 0 23.80 1.40 -2 -8 0 130.59 3.50 2 -8 0 129.59 3.10 -2 -8 0 127.99 3.40 2 -8 0 127.49 3.10 2 8 0 129.29 3.40 -2 8 0 126.39 3.10 -2 8 0 125.09 3.10 3 -8 0 291.27 5.90 -3 -8 0 294.07 6.40 3 -8 0 286.07 5.90 -3 -8 0 287.27 6.40 -3 8 0 290.87 5.90 -3 8 0 295.07 6.00 3 8 0 290.37 6.40 4 -8 0 6.90 0.90 4 -8 0 5.40 0.80 -4 -8 0 7.90 1.20 -4 -8 0 7.70 1.30 4 8 0 6.70 1.20 -4 8 0 7.10 0.90 -4 8 0 7.80 0.90 5 -8 0 212.78 4.70 -5 -8 0 215.88 5.40 -5 -8 0 201.18 5.30 5 -8 0 210.78 4.70 -5 8 0 213.28 4.70 -5 8 0 213.38 4.70 5 8 0 215.38 5.30 -6 -8 0 0.20 1.20 6 -8 0 1.00 0.80 -6 -8 0 -1.10 1.20 6 -8 0 0.20 0.80 6 8 0 1.80 1.20 -6 8 0 0.30 0.80 -6 8 0 -0.10 0.80 -7 -8 0 41.00 2.80 -7 -8 0 43.40 2.70 7 -8 0 39.70 2.00 7 -8 0 41.50 2.00 -7 8 0 41.50 2.10 -7 8 0 40.90 2.00 -8 -8 0 1.60 1.50 8 -8 0 1.40 1.00 8 -8 0 0.70 1.00 -8 -8 0 0.10 1.50 -8 8 0 2.20 1.10 -8 8 0 1.30 1.20 -9 -8 0 24.50 2.40 -9 -8 0 30.60 2.90 9 -8 0 27.60 1.90 9 8 0 30.50 2.90 9 8 0 23.60 2.40 -9 8 0 28.70 2.10 -10 -8 0 6.00 1.80 10 -8 0 5.90 1.30 -10 -8 0 5.00 1.80 10 8 0 6.60 1.80 -10 8 0 5.60 1.20 0 -9 0 -0.20 0.90 0 -9 0 -0.20 0.70 0 9 0 -0.40 0.70 0 9 0 0.60 0.80 1 -9 0 52.59 2.00 1 -9 0 53.49 1.90 -1 -9 0 51.09 2.00 -1 -9 0 51.89 2.10 1 9 0 54.39 2.10 -1 9 0 55.19 2.00 -1 9 0 55.39 2.00 2 -9 0 -0.50 0.70 2 -9 0 0.30 0.70 -2 -9 0 0.80 0.90 -2 -9 0 -0.50 0.90 -2 9 0 -1.40 0.70 -2 9 0 -0.90 0.80 2 9 0 0.00 0.90 3 -9 0 179.98 4.10 -3 -9 0 186.68 4.60 -3 -9 0 182.98 4.50 3 -9 0 180.48 4.10 -3 9 0 171.88 4.10 -3 9 0 175.28 4.10 3 9 0 175.88 4.50 -4 -9 0 41.10 2.30 4 -9 0 43.40 1.70 4 -9 0 41.80 1.80 -4 -9 0 42.60 2.30 4 9 0 42.30 2.30 -4 9 0 39.30 1.70 -4 9 0 41.70 1.80 -5 -9 0 3.40 1.30 5 -9 0 3.20 0.90 5 -9 0 4.20 0.90 -5 -9 0 3.40 1.30 5 9 0 2.20 1.30 -5 9 0 4.20 1.00 -5 9 0 2.40 0.80 -6 -9 0 27.50 2.70 -6 -9 0 25.80 2.40 6 -9 0 27.50 2.00 6 -9 0 27.30 1.70 -6 9 0 26.60 1.80 -6 9 0 26.00 1.70 6 9 0 33.20 2.60 -7 -9 0 113.19 4.20 7 -9 0 115.09 3.30 -7 -9 0 113.49 4.20 7 -9 0 115.19 3.30 -7 9 0 113.99 3.30 7 9 0 111.99 4.10 -7 9 0 114.79 3.30 8 -9 0 64.89 2.50 -8 -9 0 63.99 3.40 8 -9 0 61.49 2.50 -8 -9 0 67.19 3.60 -8 9 0 61.29 2.50 -8 9 0 58.99 2.50 8 9 0 61.69 3.40 -9 -9 0 1.10 1.60 -9 -9 0 1.10 1.60 9 -9 0 2.00 1.00 9 9 0 0.50 1.60 -9 9 0 2.50 1.10 9 9 0 -0.80 1.60 10 -9 0 47.70 2.40 10 -9 0 42.00 3.80 -10 -9 0 46.40 3.50 -10 -9 0 44.30 3.30 10 9 0 44.60 3.40 -10 9 0 44.90 2.40 0 -10 0 297.57 6.30 0 -10 0 303.37 6.40 0 10 0 290.07 6.30 0 10 0 290.47 6.30 -1 -10 0 48.50 2.10 1 -10 0 51.89 2.00 -1 -10 0 50.69 2.10 1 -10 0 50.19 2.00 -1 10 0 50.89 2.00 -1 10 0 51.99 2.00 1 10 0 50.09 2.20 2 -10 0 195.98 4.50 -2 -10 0 195.18 4.90 2 -10 0 199.58 4.50 -2 -10 0 200.88 4.80 2 10 0 193.48 4.80 -2 10 0 198.18 4.50 -2 10 0 194.88 4.50 -3 -10 0 19.80 1.90 3 -10 0 23.50 1.50 3 -10 0 23.20 1.50 -3 -10 0 20.80 1.80 -3 10 0 23.30 1.80 -3 10 0 24.00 1.60 3 10 0 23.80 1.90 4 -10 0 93.19 2.70 -4 -10 0 92.79 3.40 4 -10 0 96.29 2.80 -4 -10 0 89.19 3.30 -4 10 0 96.39 2.70 -4 10 0 92.29 2.80 4 10 0 93.29 3.40 -5 -10 0 14.30 1.70 -5 -10 0 12.20 1.70 5 -10 0 12.90 1.20 5 -10 0 12.80 1.20 -5 10 0 15.40 1.30 -5 10 0 12.70 1.20 5 10 0 15.80 1.90 -6 -10 0 278.37 6.90 6 -10 0 278.27 6.00 6 -10 0 273.97 6.00 -6 -10 0 258.67 6.80 -6 10 0 278.57 6.00 6 10 0 275.37 6.90 -6 10 0 272.87 6.00 -7 -10 0 13.90 2.00 7 -10 0 12.80 1.30 7 -10 0 13.80 1.40 -7 -10 0 12.60 1.90 -7 10 0 11.80 1.60 7 10 0 19.10 2.20 -7 10 0 13.20 1.30 8 -10 0 6.60 1.10 8 -10 0 4.10 1.10 -8 -10 0 5.00 1.80 -8 -10 0 4.10 1.70 -8 10 0 6.70 1.20 -8 10 0 7.10 1.20 9 -10 0 1.10 1.00 -9 -10 0 1.00 1.60 -9 -10 0 2.00 1.70 9 -10 0 1.20 1.20 -9 10 0 1.70 1.00 9 10 0 -1.90 1.50 9 10 0 1.70 1.90 0 -11 0 1.10 0.80 0 -11 0 0.20 0.90 0 11 0 -0.50 0.90 0 11 0 1.60 0.90 1 -11 0 144.39 3.80 1 -11 0 149.29 3.80 -1 -11 0 144.59 4.00 -1 -11 0 147.69 3.90 -1 11 0 147.89 3.80 1 11 0 151.58 4.00 -1 11 0 144.99 3.80 2 -11 0 202.98 4.80 -2 -11 0 200.58 5.10 2 -11 0 208.28 4.80 -2 -11 0 203.18 5.00 -2 11 0 207.38 4.80 -2 11 0 200.78 4.70 2 11 0 208.88 5.10 -3 -11 0 90.29 4.10 3 -11 0 91.39 2.80 3 -11 0 90.29 2.80 -3 -11 0 89.89 3.20 -3 11 0 95.19 2.80 -3 11 0 93.79 2.80 3 11 0 92.19 3.30 4 -11 0 120.49 3.40 -4 -11 0 125.09 4.00 4 -11 0 127.29 3.40 -4 -11 0 127.09 4.00 -4 11 0 135.29 3.80 -4 11 0 125.79 3.40 4 11 0 113.49 5.90 5 -11 0 36.40 1.90 -5 -11 0 34.30 2.60 -5 -11 0 33.90 2.60 5 -11 0 37.10 1.90 5 11 0 37.60 2.60 -5 11 0 35.20 2.10 -5 11 0 36.60 2.00 6 -11 0 127.39 3.50 6 -11 0 124.19 3.50 -6 -11 0 129.09 4.30 -6 -11 0 120.89 4.30 6 11 0 122.49 4.40 -6 11 0 124.19 3.50 -6 11 0 128.09 3.50 7 -11 0 82.59 2.80 -7 -11 0 83.69 3.80 7 -11 0 81.89 2.80 -7 -11 0 84.89 3.90 -7 11 0 81.49 2.80 7 11 0 82.79 3.80 -7 11 0 80.79 2.80 8 -11 0 4.70 1.10 8 -11 0 0.20 0.70 -8 -11 0 1.70 1.60 -8 -11 0 0.60 1.70 8 11 0 1.00 1.70 -8 11 0 3.40 1.10 9 -11 0 -1.10 0.90 9 -11 0 1.60 1.00 -9 -11 0 -3.60 1.80 -9 11 0 0.20 1.00 0 -12 0 84.19 3.30 0 -12 0 88.39 3.00 0 12 0 87.79 3.00 0 12 0 90.59 3.00 1 -12 0 4.90 1.10 1 -12 0 5.90 1.10 -1 -12 0 3.20 1.10 -1 -12 0 5.00 1.30 -1 12 0 3.10 1.00 1 12 0 4.00 1.20 -1 12 0 4.40 1.00 2 -12 0 2.00 1.10 -2 -12 0 1.30 1.10 2 -12 0 0.10 1.60 -2 -12 0 2.50 1.20 -2 12 0 0.70 0.90 -2 12 0 -0.20 0.90 2 12 0 1.10 1.20 3 -12 0 -1.40 1.50 -3 -12 0 0.00 1.20 3 -12 0 0.90 1.00 -3 -12 0 2.20 1.30 -3 12 0 1.10 1.00 -3 12 0 1.10 1.00 3 12 0 0.20 1.30 -4 -12 0 1.30 1.40 4 -12 0 2.30 1.00 4 -12 0 1.70 0.90 -4 -12 0 1.30 1.30 4 12 0 2.50 1.40 -4 12 0 1.00 1.00 -4 12 0 2.10 1.00 -5 -12 0 64.09 3.80 -5 -12 0 70.69 3.30 5 -12 0 69.29 2.50 5 -12 0 65.79 2.50 -5 12 0 71.39 2.90 5 12 0 62.59 3.30 -5 12 0 64.69 2.50 -6 -12 0 1.40 1.50 6 -12 0 0.90 0.90 6 -12 0 -0.50 0.90 -6 -12 0 1.10 1.50 6 12 0 -0.10 1.50 -6 12 0 1.80 1.20 -6 12 0 -1.00 1.10 -7 -12 0 -1.00 1.50 -7 -12 0 -0.10 1.60 7 -12 0 -0.30 0.90 7 -12 0 -0.70 0.90 -7 12 0 0.50 1.00 -7 12 0 1.30 0.90 7 12 0 -0.20 1.60 -8 -12 0 6.80 2.10 -8 -12 0 5.30 1.80 8 -12 0 7.10 1.10 8 12 0 8.90 2.00 -8 12 0 7.70 1.20 -8 12 0 9.10 1.30 -9 -12 0 4.90 2.10 9 -12 0 1.50 1.00 9 -12 0 4.20 1.10 -9 -12 0 2.20 1.80 -9 12 0 5.20 1.20 -9 12 0 2.60 1.10 0 -13 0 -0.90 1.00 0 -13 0 -0.20 1.00 0 13 0 -0.90 1.10 0 13 0 -0.20 1.10 -1 -13 0 107.49 3.60 1 -13 0 109.59 3.40 -1 -13 0 113.29 3.60 1 -13 0 109.89 3.40 1 13 0 113.69 3.70 -1 13 0 114.09 3.50 -1 13 0 113.49 3.50 -2 -13 0 -1.20 1.20 2 -13 0 0.20 0.90 2 -13 0 0.60 1.00 -2 -13 0 0.80 1.10 2 13 0 -0.70 1.20 -2 13 0 -1.00 0.90 -2 13 0 -1.40 1.00 3 -13 0 3.00 1.10 -3 -13 0 4.50 1.50 3 -13 0 1.70 1.60 -3 -13 0 7.20 1.70 -3 13 0 3.00 1.10 -3 13 0 3.00 1.10 3 13 0 4.60 2.80 4 -13 0 -0.10 1.00 -4 -13 0 1.70 1.40 -4 -13 0 0.40 1.40 4 -13 0 0.10 0.90 -4 13 0 -0.60 0.90 -4 13 0 -0.40 1.00 4 13 0 0.10 1.40 -5 -13 0 30.90 2.80 5 -13 0 40.90 2.10 5 -13 0 37.70 2.10 -5 -13 0 36.00 2.80 -5 13 0 32.60 2.00 5 13 0 38.40 2.90 -5 13 0 36.90 2.50 6 -13 0 36.80 2.10 6 -13 0 32.30 2.00 -6 -13 0 23.90 2.40 -6 -13 0 30.60 2.90 -6 13 0 35.20 2.10 6 13 0 30.60 3.10 -6 13 0 31.80 3.10 -7 -13 0 -0.10 1.60 -7 -13 0 -0.70 1.60 7 -13 0 -1.00 0.90 7 13 0 -2.90 1.70 -7 13 0 0.30 0.90 -7 13 0 -0.80 0.90 -8 -13 0 -0.20 1.80 -8 -13 0 0.00 1.90 8 -13 0 1.00 1.00 8 -13 0 0.40 0.90 -8 13 0 -1.60 0.90 -8 13 0 0.60 0.90 0 -14 0 303.27 7.00 0 -14 0 300.07 7.00 0 14 0 296.87 7.00 -1 -14 0 58.19 2.70 1 -14 0 71.99 2.90 1 -14 0 70.09 2.90 -1 -14 0 68.19 3.00 -1 14 0 73.49 2.90 1 14 0 69.09 3.10 -1 14 0 77.49 4.60 2 -14 0 200.38 5.10 -2 -14 0 196.88 5.50 2 -14 0 203.48 5.10 2 14 0 199.48 5.40 -2 14 0 208.68 6.80 -2 14 0 200.28 5.10 3 -14 0 22.70 1.90 3 -14 0 21.30 2.00 -3 -14 0 19.00 2.00 -3 14 0 23.50 2.30 3 14 0 21.80 2.10 -3 14 0 26.50 2.10 -4 -14 0 94.89 3.90 4 -14 0 100.49 3.20 4 -14 0 99.39 3.30 -4 -14 0 98.49 4.70 -4 14 0 99.69 3.20 4 14 0 102.39 4.10 -4 14 0 103.09 3.30 5 -14 0 1.30 1.00 -5 -14 0 1.90 1.50 -5 -14 0 3.90 1.70 5 -14 0 0.90 1.00 -5 14 0 1.00 1.00 -5 14 0 -0.10 1.00 5 14 0 2.00 1.70 -6 -14 0 23.30 2.50 -6 -14 0 15.70 2.20 6 -14 0 19.30 1.80 -6 14 0 22.20 1.90 6 14 0 19.80 2.40 -6 14 0 22.80 1.90 -7 -14 0 0.90 1.70 -7 -14 0 -1.40 1.50 7 -14 0 0.70 1.00 7 -14 0 2.40 1.30 -7 14 0 1.10 1.40 -7 14 0 -1.10 1.00 7 14 0 0.40 1.80 -8 -14 0 0.60 2.00 8 -14 0 -0.80 0.90 -8 -14 0 0.10 1.70 8 -14 0 0.80 1.00 -8 14 0 1.30 1.00 -8 14 0 2.10 1.00 0 -15 0 -1.80 1.10 0 -15 0 -1.60 1.20 0 15 0 0.70 1.30 1 -15 0 25.90 2.20 1 -15 0 27.40 2.30 -1 -15 0 27.70 2.40 1 15 0 30.00 2.50 -1 15 0 31.70 2.40 -1 15 0 28.20 2.30 2 -15 0 21.20 2.00 -2 -15 0 26.60 2.50 2 -15 0 20.40 2.10 -2 15 0 22.20 2.10 2 15 0 21.60 2.10 -2 15 0 21.50 2.20 3 -15 0 14.00 1.50 -3 -15 0 16.00 2.00 -3 15 0 18.90 1.70 3 15 0 18.40 2.10 -3 15 0 13.50 1.50 -4 -15 0 0.30 1.40 4 -15 0 0.00 0.60 -4 -15 0 2.20 1.50 4 -15 0 0.40 1.10 -4 15 0 0.20 1.00 4 15 0 1.30 1.60 -4 15 0 1.00 1.10 5 -15 0 1.70 1.00 -5 -15 0 4.90 1.90 -5 -15 0 -0.30 1.50 5 15 0 3.80 1.90 -5 15 0 1.20 1.10 -5 15 0 0.80 1.10 -6 -15 0 2.10 1.70 6 -15 0 2.10 1.10 6 -15 0 2.60 1.20 -6 -15 0 1.70 1.70 6 15 0 3.30 2.30 -6 15 0 1.20 1.00 -6 15 0 1.90 1.10 7 -15 0 0.90 1.00 7 -15 0 2.00 1.10 -7 -15 0 3.60 1.80 -7 -15 0 1.80 1.90 7 15 0 -0.70 2.10 -7 15 0 3.00 1.10 0 -16 0 156.38 4.70 0 16 0 150.48 4.70 -1 -16 0 0.20 1.40 1 -16 0 0.70 1.20 -1 16 0 0.70 1.30 -1 16 0 0.80 1.20 1 16 0 2.50 2.40 -2 -16 0 32.40 2.80 2 -16 0 31.70 2.40 -2 16 0 27.00 2.40 -2 16 0 27.30 2.30 2 16 0 29.90 2.80 -3 -16 0 43.70 2.90 3 -16 0 42.20 2.50 -3 -16 0 45.60 3.10 -3 16 0 44.10 2.50 3 16 0 47.40 3.20 -3 16 0 41.40 2.50 -4 -16 0 57.09 3.40 4 -16 0 59.69 3.30 4 -16 0 56.59 2.70 -4 -16 0 60.89 5.20 -4 16 0 53.19 2.70 -4 16 0 57.69 2.80 4 16 0 58.19 3.50 -5 -16 0 1.10 1.70 5 -16 0 0.30 1.10 -5 -16 0 -0.40 1.60 -5 16 0 1.10 1.10 5 16 0 -0.60 1.70 -5 16 0 2.00 1.20 6 -16 0 6.70 1.30 6 -16 0 5.90 1.20 -6 -16 0 7.10 2.30 -6 -16 0 4.80 1.90 -6 16 0 5.50 1.30 -6 16 0 4.30 1.20 6 16 0 7.50 2.10 0 -17 0 -0.60 1.30 0 -17 0 -1.00 1.30 0 17 0 -0.40 1.30 -1 -17 0 -0.10 1.40 -1 -17 0 0.90 1.30 1 -17 0 -0.50 1.30 1 -17 0 -0.70 1.20 -1 17 0 2.80 1.50 1 17 0 -2.00 1.50 -2 -17 0 39.70 4.40 2 -17 0 33.60 2.50 2 -17 0 37.10 2.50 -2 -17 0 37.00 3.60 -2 17 0 36.00 2.60 -2 17 0 37.30 2.50 2 17 0 33.70 3.00 3 -17 0 28.60 2.30 -3 -17 0 35.70 3.00 -3 -17 0 32.00 2.80 3 -17 0 31.60 2.30 -3 17 0 26.70 2.30 3 17 0 37.10 3.20 -3 17 0 29.50 2.40 4 -17 0 3.70 1.30 -4 -17 0 2.40 1.70 4 -17 0 1.40 1.10 -4 -17 0 1.40 1.60 4 17 0 1.60 1.80 -4 17 0 1.30 1.20 -4 17 0 1.70 1.30 5 -17 0 6.30 1.30 -5 -17 0 5.20 1.90 -5 17 0 5.30 1.30 -5 17 0 5.30 1.30 5 17 0 5.70 2.00 -6 -17 0 -1.60 1.60 6 -17 0 1.40 1.10 6 -17 0 1.10 1.10 -6 17 0 0.20 1.10 -6 17 0 0.50 1.10 0 -18 0 5.30 1.50 0 -18 0 4.10 1.60 0 18 0 7.40 1.70 -1 -18 0 12.50 1.80 1 -18 0 15.60 1.90 1 -18 0 16.60 1.90 -1 -18 0 12.70 1.90 -1 18 0 16.20 1.90 1 18 0 15.60 2.10 -2 -18 0 0.40 1.40 2 -18 0 1.40 1.30 -2 -18 0 2.00 1.70 2 -18 0 0.90 1.30 -2 18 0 0.00 1.30 2 18 0 1.10 1.60 -3 -18 0 4.40 1.80 -3 -18 0 3.90 1.80 3 -18 0 5.10 1.40 3 -18 0 8.70 1.50 3 18 0 6.10 2.00 -3 18 0 6.10 1.50 -3 18 0 3.60 1.40 4 -18 0 18.30 1.80 -4 -18 0 15.50 2.40 4 -18 0 12.00 1.60 -4 18 0 12.10 1.60 4 18 0 16.30 2.80 -4 18 0 13.50 1.80 5 -18 0 3.40 1.20 -5 -18 0 4.10 1.90 5 -18 0 5.00 1.30 5 18 0 7.40 2.10 -5 18 0 6.20 1.40 -5 18 0 4.10 1.40 0 -19 0 -1.90 1.40 0 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3.30 5 -11 3 68.49 2.10 -5 11 -3 68.19 1.70 5 11 3 67.59 3.30 6 -11 3 2.20 0.40 -6 -11 -3 2.10 1.60 -6 -11 -3 2.00 1.50 6 -11 3 1.80 0.40 6 11 3 -0.90 1.30 -6 11 -3 1.20 0.50 -7 -11 -3 9.50 1.90 -7 -11 -3 10.30 1.90 7 11 3 10.10 1.90 -7 11 -3 10.50 0.70 -8 -11 -3 3.10 2.30 -8 -11 -3 -0.50 1.60 9 -12 -3 2.40 1.40 -9 -12 3 5.70 2.40 9 -12 -3 7.10 1.70 -9 -12 3 7.70 3.10 -9 12 3 3.60 1.60 -9 12 3 2.20 1.40 9 12 -3 5.70 2.00 -8 -12 3 10.00 2.10 8 -12 -3 8.90 1.60 -8 -12 3 10.00 2.00 8 -12 -3 9.40 1.70 8 12 -3 8.40 1.90 -8 12 3 9.00 1.60 8 12 -3 9.10 2.20 -8 12 3 8.30 1.60 7 -12 -3 10.30 1.60 7 -12 -3 7.10 1.40 -7 -12 3 9.50 1.90 -7 -12 3 9.70 1.90 -7 12 3 6.30 1.50 -7 12 3 8.50 1.60 7 12 -3 8.60 2.00 6 -12 -3 64.89 3.00 -6 -12 3 64.69 3.30 -6 -12 3 70.69 3.40 6 12 -3 60.79 3.40 -6 12 3 64.19 3.00 -6 12 3 57.49 2.90 -5 -12 3 35.40 2.80 5 -12 -3 37.20 2.40 5 -12 -3 31.10 2.20 -5 12 3 35.90 2.50 -5 12 3 36.40 2.40 5 12 -3 35.40 2.80 4 -12 -3 67.29 2.90 -4 -12 3 74.59 3.20 4 -12 -3 74.09 2.90 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4.00 1.70 7 9 -4 4.60 1.70 6 -9 -4 4.70 1.30 6 -9 -4 4.50 1.30 -6 -9 4 2.40 1.50 -6 9 4 5.50 1.40 -6 9 4 5.40 1.40 6 9 -4 4.00 1.50 6 9 -4 6.60 1.60 -5 -9 4 187.98 5.10 5 -9 -4 186.88 4.80 5 -9 -4 181.48 4.80 5 9 -4 183.88 5.00 5 9 -4 180.48 5.00 -5 9 4 182.08 4.80 -5 9 4 182.28 4.80 4 -9 -4 7.50 1.30 4 -9 -4 8.40 1.20 -4 -9 4 6.40 1.30 -4 9 4 11.50 1.50 4 9 -4 9.70 1.40 -4 9 4 8.20 1.30 -3 -9 4 97.99 3.10 3 -9 -4 97.29 3.10 3 -9 -4 93.59 3.10 3 9 -4 92.29 3.10 -3 9 4 90.99 3.10 -3 9 4 98.89 3.20 2 -9 -4 194.38 4.80 2 -9 -4 192.28 4.70 -2 -9 4 192.48 4.60 -2 9 4 197.28 4.80 -2 9 4 181.48 4.70 2 9 -4 188.38 4.60 -1 -9 4 4.60 0.80 -1 -9 4 4.20 0.90 1 -9 -4 5.00 1.10 1 -9 -4 5.00 1.10 1 9 -4 2.90 0.90 -1 9 4 7.60 1.30 -1 9 4 4.90 1.10 0 -9 4 12.80 1.00 0 -9 -4 12.10 1.40 0 -9 -4 13.40 1.40 0 -9 4 11.40 1.20 0 9 -4 11.80 1.20 0 9 4 11.40 1.30 0 9 4 14.30 1.50 1 -9 4 254.87 5.80 -1 -9 -4 275.57 6.20 1 -9 4 265.97 5.40 -1 -9 -4 273.87 6.20 1 9 4 269.67 6.20 -1 9 -4 269.97 5.40 1 9 4 273.37 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4 41.80 2.70 3 11 4 42.90 2.80 -4 -11 -4 177.58 5.20 -4 -11 -4 179.08 5.10 4 11 4 172.78 5.10 -5 -11 -4 41.70 2.70 -5 -11 -4 43.40 2.90 -6 -11 -4 27.70 2.50 6 11 4 23.80 3.10 -7 -11 -4 2.00 1.60 -7 -11 -4 1.30 1.50 7 11 4 -1.10 1.60 -8 -11 -4 0.70 1.70 -8 -11 -4 0.40 1.60 9 -12 -4 -1.00 1.40 -9 -12 4 1.80 2.20 -9 12 4 6.30 2.10 9 12 -4 2.60 2.40 -9 12 4 1.40 1.50 -8 -12 4 10.10 2.00 8 -12 -4 10.50 1.80 8 -12 -4 9.80 1.70 8 12 -4 11.30 2.20 -8 12 4 8.00 1.70 8 12 -4 12.20 2.20 -8 12 4 11.20 1.80 7 -12 -4 22.00 2.10 -7 -12 4 15.60 2.20 7 -12 -4 22.90 2.20 7 12 -4 21.80 2.50 -7 12 4 16.80 1.80 -7 12 4 19.80 2.00 7 12 -4 22.00 2.30 6 -12 -4 14.50 1.80 6 -12 -4 19.70 2.10 -6 -12 4 15.30 2.00 -6 -12 4 17.40 2.10 6 12 -4 18.50 2.10 -6 12 4 17.70 2.00 -6 12 4 18.00 2.00 6 12 -4 18.10 2.20 5 -12 -4 -0.90 1.20 5 -12 -4 -0.30 1.20 -5 -12 4 0.30 1.50 -5 12 4 -0.80 1.30 5 12 -4 -2.30 1.30 -5 12 4 -0.40 1.20 -4 -12 4 70.49 3.10 4 -12 -4 56.49 2.70 4 -12 -4 64.79 3.00 -4 12 4 65.49 2.90 -4 12 4 64.59 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12 -4 0.80 0.40 4 12 4 -0.70 1.50 -5 -12 -4 2.30 1.40 -5 -12 -4 1.10 1.40 5 12 4 -0.40 1.40 -6 -12 -4 15.20 2.00 -6 -12 -4 15.00 2.10 6 12 4 15.40 2.10 -7 -12 -4 1.10 1.50 -7 -12 -4 0.90 1.40 7 12 4 1.00 1.80 -8 -12 -4 3.80 1.70 -8 -12 -4 0.40 1.40 8 -13 -4 1.20 1.40 8 -13 -4 0.50 1.50 -8 -13 4 -1.20 1.60 8 13 -4 -1.40 1.90 8 13 -4 -1.90 1.70 -8 13 4 -0.90 1.40 -8 13 4 0.20 1.40 7 -13 -4 13.10 1.80 7 -13 -4 13.90 1.90 -7 -13 4 16.90 2.20 -7 -13 4 14.00 2.20 7 13 -4 15.10 2.20 -7 13 4 12.30 1.80 -7 13 4 14.00 1.90 7 13 -4 16.60 2.30 6 -13 -4 0.40 1.30 6 -13 -4 1.60 1.40 -6 -13 4 3.60 1.80 -6 -13 4 2.50 1.60 -6 13 4 -1.00 1.30 6 13 -4 0.40 1.70 -6 13 4 0.80 1.40 -5 -13 4 9.70 1.80 5 -13 -4 3.80 1.50 5 -13 -4 6.50 2.00 5 13 -4 8.40 1.80 -5 13 4 7.20 1.60 -5 13 4 4.20 1.60 -4 -13 4 31.30 2.50 4 -13 -4 26.60 2.50 -4 13 4 24.30 2.50 4 13 -4 25.70 2.40 -4 13 4 24.10 2.40 -3 -13 4 1.20 1.20 3 -13 -4 0.80 1.30 -3 -13 4 1.10 1.30 3 13 -4 -0.50 1.20 -3 13 4 0.20 1.30 -3 13 4 -1.30 1.30 -2 -13 4 28.30 2.20 2 -13 -4 28.60 2.30 -2 -13 4 27.60 2.20 -2 13 4 24.90 2.10 -2 13 4 23.70 2.40 2 13 -4 28.00 2.20 1 -13 -4 -0.20 1.20 -1 -13 4 1.60 1.00 1 -13 -4 -1.20 1.40 -1 -13 4 -0.10 1.00 -1 13 4 0.60 1.40 1 13 -4 0.00 1.00 0 -13 -4 67.39 3.10 0 -13 -4 64.29 3.10 0 -13 4 63.89 2.50 0 -13 4 61.39 2.40 0 13 4 65.79 3.60 0 13 4 63.89 3.20 0 13 -4 65.49 2.50 1 -13 4 301.77 6.40 -1 -13 -4 286.97 7.10 1 -13 4 285.97 6.20 -1 -13 -4 293.37 7.20 1 13 4 292.37 7.10 1 13 4 295.87 7.60 -1 13 -4 289.57 6.30 2 -13 4 2.70 0.80 -2 -13 -4 4.00 1.80 -2 -13 -4 4.20 1.40 2 -13 4 3.10 0.90 2 13 4 4.20 1.70 -2 13 -4 3.60 0.90 2 13 4 4.50 1.50 -3 -13 -4 -0.80 1.30 -3 -13 -4 0.50 1.40 3 -13 4 0.40 0.60 3 -13 4 0.30 0.40 3 13 4 -1.70 1.40 -3 13 -4 -0.50 0.70 -4 -13 -4 4.70 1.60 -4 -13 -4 7.70 1.60 4 -13 4 7.40 0.70 4 13 4 7.90 1.90 -4 13 -4 8.20 0.70 -5 -13 -4 -0.80 1.30 -5 -13 -4 -2.40 1.40 5 13 4 -0.50 1.60 -6 -13 -4 3.40 1.50 -6 -13 -4 5.50 1.90 6 13 4 3.90 1.90 -7 -13 -4 0.00 1.60 -7 -13 -4 0.00 1.40 -8 -14 4 6.80 2.00 8 -14 -4 4.60 1.60 -8 14 4 7.50 1.80 8 14 -4 6.30 1.90 8 14 -4 9.90 3.10 -8 14 4 8.80 2.90 -7 -14 4 5.70 2.00 -7 -14 4 5.20 2.20 7 -14 -4 5.40 1.60 7 -14 -4 3.70 1.50 -7 14 4 4.20 1.80 7 14 -4 4.80 1.80 -7 14 4 5.00 1.60 -6 -14 4 4.00 1.80 6 -14 -4 3.90 1.50 6 -14 -4 3.20 1.50 -6 -14 4 2.60 1.80 -6 14 4 4.10 1.50 6 14 -4 4.90 1.90 -6 14 4 4.60 1.60 5 -14 -4 20.00 2.00 -5 -14 4 19.80 3.20 5 -14 -4 25.60 2.60 5 14 -4 23.50 2.50 -5 14 4 24.90 2.30 -5 14 4 19.50 2.10 -4 -14 4 145.29 4.70 4 -14 -4 141.89 4.60 4 -14 -4 142.09 4.60 4 14 -4 145.09 4.80 -4 14 4 146.09 4.70 -4 14 4 151.38 4.60 3 -14 -4 10.80 1.70 -3 -14 4 12.10 1.70 -3 14 4 11.80 2.20 -3 14 4 10.80 1.70 3 14 -4 15.30 1.90 2 -14 -4 108.89 4.10 -2 -14 4 121.19 3.90 -2 14 4 123.49 4.20 -2 14 4 130.99 4.50 2 14 -4 124.19 4.00 -1 -14 4 52.99 2.60 1 -14 -4 50.79 2.90 -1 -14 4 52.49 2.50 -1 14 4 50.99 3.10 1 14 -4 55.19 2.60 -1 14 4 54.79 2.90 0 -14 4 101.99 3.30 0 -14 4 104.39 3.30 0 -14 -4 96.99 3.80 0 -14 -4 106.79 3.90 0 14 4 105.69 3.90 0 14 4 101.89 3.80 0 14 -4 101.99 3.30 1 -14 4 45.20 2.10 -1 -14 -4 47.40 3.00 1 -14 4 47.80 2.10 -1 -14 -4 40.80 4.30 1 14 4 46.80 2.90 1 14 4 51.69 3.00 -1 14 -4 51.79 2.60 -2 -14 -4 35.80 2.80 2 -14 4 34.90 1.80 2 -14 4 37.10 1.80 -2 -14 -4 35.50 2.80 -2 14 -4 38.50 1.80 2 14 4 35.70 3.00 2 14 4 38.60 2.80 -3 -14 -4 14.80 2.00 3 -14 4 18.00 1.70 -3 -14 -4 18.40 2.10 3 14 4 15.10 2.00 4 -14 4 61.39 2.20 -4 -14 -4 69.09 3.60 4 -14 4 67.29 1.90 -4 -14 -4 66.09 3.50 -4 14 -4 64.49 1.90 4 14 4 68.99 3.60 -5 -14 -4 2.00 1.60 -5 -14 -4 0.90 1.40 5 14 4 3.20 1.80 -6 -14 -4 -0.80 1.60 -7 -14 -4 5.00 1.60 -7 -14 -4 4.40 1.90 7 -15 -4 0.40 1.50 -7 -15 4 0.90 1.80 -7 15 4 0.60 1.60 -7 15 4 0.30 2.20 7 15 -4 -1.30 1.60 7 15 -4 0.70 1.90 6 -15 -4 1.60 1.50 6 -15 -4 -0.50 1.40 -6 -15 4 1.40 1.70 -6 -15 4 3.30 1.70 -6 15 4 2.60 1.90 6 15 -4 1.00 1.80 -6 15 4 0.90 1.50 -5 -15 4 44.00 3.20 5 -15 -4 36.80 2.80 5 -15 -4 43.60 3.00 -5 -15 4 41.30 3.10 -5 15 4 37.00 3.50 -5 15 4 35.80 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10 8 -5 48.10 3.60 -10 8 5 52.79 3.30 -10 8 5 54.39 3.50 9 -8 -5 27.80 2.70 9 -8 -5 29.10 2.70 -9 -8 5 22.50 2.50 9 8 -5 27.40 2.70 -9 8 5 23.70 2.30 9 8 -5 25.30 2.50 -9 8 5 25.80 2.40 8 -8 -5 7.30 1.60 -8 -8 5 6.30 1.70 8 -8 -5 5.60 1.60 8 8 -5 3.90 1.60 8 8 -5 7.10 2.00 -8 8 5 5.20 1.50 -8 8 5 7.00 2.10 -7 -8 5 13.00 1.90 7 -8 -5 11.10 1.60 -7 8 5 15.30 1.90 -7 8 5 14.10 1.70 7 8 -5 12.50 1.90 7 8 -5 14.20 2.00 -6 -8 5 291.17 7.20 6 -8 -5 299.67 7.00 -6 8 5 294.07 7.00 6 8 -5 300.57 7.60 -6 8 5 294.47 7.00 6 8 -5 286.57 7.10 -5 -8 5 5.30 1.40 5 -8 -5 5.90 1.30 5 -8 -5 8.50 1.30 -5 8 5 8.00 1.40 5 8 -5 5.70 1.40 5 8 -5 7.40 1.50 -5 8 5 8.40 1.40 -4 -8 5 1.50 1.20 4 -8 -5 0.40 1.10 4 -8 -5 1.10 1.10 -4 8 5 1.00 1.10 4 8 -5 0.30 1.00 -4 8 5 0.00 1.10 4 8 -5 -1.80 1.00 -3 -8 5 40.70 2.10 3 -8 -5 46.00 2.20 3 -8 -5 41.20 2.20 -3 8 5 42.10 2.20 -3 8 5 37.90 2.20 3 8 -5 37.30 2.00 3 8 -5 40.50 2.10 2 -8 -5 108.19 3.30 2 -8 -5 106.99 3.30 -2 -8 5 98.19 3.10 -2 8 5 102.29 3.20 2 8 -5 100.09 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5 13.40 1.20 0 -11 -5 11.50 1.60 0 11 5 13.70 1.70 0 11 5 9.80 1.70 0 11 -5 11.10 1.10 -1 -11 -5 1.90 1.30 1 -11 5 2.00 0.80 1 -11 5 2.10 0.70 -1 -11 -5 1.50 1.30 1 11 5 0.90 1.30 1 11 5 1.90 1.30 -1 11 -5 3.00 0.70 -2 -11 -5 139.59 4.40 -2 -11 -5 141.29 4.40 2 -11 5 144.29 3.10 2 -11 5 141.79 3.10 2 11 5 141.89 4.40 -2 11 -5 141.59 3.10 2 11 5 139.09 4.40 -2 11 -5 141.39 3.10 -3 -11 -5 8.50 1.70 -3 -11 -5 9.90 1.70 3 11 5 9.60 1.80 3 11 5 13.40 1.80 -4 -11 -5 31.80 2.70 -4 -11 -5 38.10 2.70 -5 -11 -5 12.60 1.80 -5 -11 -5 15.40 2.10 -6 -11 -5 6.40 1.80 -6 -11 -5 3.30 1.40 6 11 5 8.10 1.90 -7 -11 -5 40.00 3.20 -7 -11 -5 40.80 3.00 7 11 5 44.30 4.20 -8 -12 5 -0.40 1.60 8 -12 -5 1.30 1.50 8 -12 -5 0.40 1.40 -8 12 5 -1.00 1.40 8 12 -5 -2.50 1.80 -8 12 5 1.80 1.60 8 12 -5 1.70 1.70 -7 -12 5 -0.10 1.50 7 -12 -5 -0.10 1.50 7 -12 -5 0.20 1.50 -7 12 5 -0.20 1.40 7 12 -5 0.20 1.60 7 12 -5 -0.10 1.60 -7 12 5 0.10 1.40 6 -12 -5 1.20 1.40 -6 -12 5 2.20 1.60 6 -12 -5 1.90 1.50 6 12 -5 1.50 1.60 -6 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-13 16.00 1.70 0 -4 13 2.50 1.10 0 -4 -13 -1.60 1.40 0 -4 -13 1.70 1.50 0 -4 13 1.50 1.10 0 4 13 1.00 1.40 0 4 13 1.00 1.40 0 4 -13 1.20 1.00 -1 -4 -13 6.60 1.60 -1 -4 -13 3.40 1.50 -1 4 -13 2.90 1.00 1 4 13 1.30 1.40 -1 4 -13 2.60 1.00 1 4 13 2.20 1.30 -2 -4 -13 0.70 1.50 -2 -4 -13 0.90 1.30 2 -4 13 1.30 0.90 2 4 13 0.30 1.60 -2 4 -13 0.90 0.80 2 4 13 2.30 1.40 -2 4 -13 0.80 0.80 5 -5 -13 4.30 1.90 5 -5 -13 8.50 2.20 5 5 -13 6.70 1.90 5 5 -13 9.60 1.80 -4 -5 13 -0.70 1.40 4 -5 -13 1.70 1.80 4 -5 -13 3.10 1.80 4 5 -13 0.90 1.60 -4 5 13 5.60 1.90 4 5 -13 0.30 1.80 3 -5 -13 4.20 1.90 -3 -5 13 3.20 1.50 3 -5 -13 2.70 3.10 -3 5 13 4.60 1.80 3 5 -13 3.90 1.50 3 5 -13 3.50 1.50 -2 -5 13 16.20 1.80 2 -5 -13 14.80 2.00 2 -5 -13 14.50 2.40 2 5 -13 16.00 1.80 -2 5 13 13.80 2.10 2 5 -13 16.40 1.80 -1 -5 13 -0.40 1.10 1 -5 -13 3.60 1.50 1 -5 -13 1.00 1.40 -1 5 13 -1.60 1.90 1 5 -13 -0.60 1.10 -1 5 13 -1.20 1.40 1 5 -13 2.10 1.30 0 -5 13 31.60 2.00 0 -5 -13 33.50 3.00 0 -5 -13 35.90 2.90 0 5 13 33.30 4.20 0 5 -13 38.80 2.20 0 5 -13 33.40 2.10 0 5 13 34.70 2.80 1 -5 13 -0.60 0.40 -1 -5 -13 -1.40 1.50 -1 5 -13 2.10 0.90 1 5 13 -0.40 1.40 -1 5 -13 0.50 1.30 2 -5 13 1.90 0.60 -2 -5 -13 0.40 1.40 2 5 13 1.60 1.30 -2 5 -13 3.40 0.70 -2 5 -13 0.60 0.70 5 -6 -13 10.40 2.20 -5 -6 13 4.90 2.60 5 -6 -13 10.80 2.20 5 6 -13 10.80 1.90 5 6 -13 9.20 2.00 -5 6 13 11.90 2.20 -4 -6 13 0.40 1.40 4 -6 -13 -1.50 1.50 4 -6 -13 1.10 1.80 4 6 -13 -2.40 2.60 -4 6 13 0.00 1.70 3 -6 -13 -0.70 1.60 3 -6 -13 4.80 1.80 -3 -6 13 4.00 1.50 3 6 -13 2.50 1.40 -3 6 13 2.70 1.70 3 6 -13 3.30 1.50 2 -6 -13 3.50 2.10 -2 -6 13 4.20 1.40 2 -6 -13 4.90 1.70 2 6 -13 4.70 1.40 -2 6 13 4.60 1.80 2 6 -13 2.90 1.30 -1 -6 13 7.60 1.40 1 -6 -13 6.20 1.90 1 -6 -13 5.70 2.70 1 6 -13 7.40 1.40 1 6 -13 6.30 1.30 -1 6 13 7.60 1.90 0 -6 -13 2.40 1.60 0 -6 -13 5.60 1.90 0 -6 13 3.20 1.00 0 6 -13 2.50 1.00 0 6 13 3.30 1.50 0 6 -13 4.20 1.10 -1 -6 -13 14.70 2.10 -1 -6 -13 10.20 1.90 1 -6 13 8.80 1.00 -1 6 -13 8.30 1.00 -1 6 -13 6.50 1.00 1 6 13 8.70 1.80 4 -7 -13 0.20 1.70 -4 -7 13 -0.20 1.30 4 -7 -13 -1.60 1.60 4 7 -13 0.10 1.70 4 7 -13 -0.30 1.40 -4 7 13 -1.90 1.60 -3 -7 13 1.90 1.40 3 -7 -13 0.10 1.80 3 -7 -13 -2.10 1.60 3 7 -13 1.60 1.40 -3 7 13 2.10 1.70 3 7 -13 -0.70 1.30 2 -7 -13 -0.10 1.50 -2 -7 13 0.10 1.20 2 -7 -13 1.50 1.60 2 7 -13 -0.40 1.20 2 7 -13 0.70 1.30 1 -7 -13 2.30 1.60 1 -7 -13 2.30 1.70 -1 -7 13 1.80 1.10 -1 7 13 3.60 1.70 1 7 -13 4.40 1.30 1 7 -13 2.90 1.20 0 -7 -13 5.30 1.80 0 -7 -13 3.60 1.70 0 7 13 4.50 1.70 0 7 -13 3.20 1.00 0 7 -13 1.90 1.00 3 -8 -13 4.80 2.00 -3 -8 13 7.10 1.60 3 -8 -13 6.40 1.90 3 8 -13 6.80 2.00 -3 8 13 7.80 2.10 3 8 -13 11.40 1.90 2 -8 -13 6.70 1.90 -2 -8 13 6.70 1.40 2 -8 -13 5.70 1.80 -2 8 13 4.60 1.80 2 8 -13 8.80 1.50 2 8 -13 6.40 1.50 1 -8 -13 2.80 1.70 1 -8 -13 2.30 1.60 -1 -8 13 5.80 1.20 -1 8 13 2.70 1.70 1 8 -13 4.60 1.50 1 8 -13 4.90 1.20 4 0 -14 3.00 1.80 4 0 -14 5.50 1.80 -4 0 14 5.10 1.80 -3 0 14 1.50 1.60 3 0 -14 3.50 1.70 3 0 -14 -1.50 1.40 -2 0 14 1.00 1.40 2 0 -14 1.20 2.20 2 0 -14 2.40 1.90 1 0 -14 2.00 1.50 -1 0 14 3.20 1.50 1 0 -14 0.10 1.40 -1 0 14 -0.20 1.50 0 0 -14 2.60 1.40 0 0 -14 2.60 1.30 0 0 14 1.60 1.30 0 0 14 1.60 1.30 4 -1 -14 1.40 1.70 4 -1 -14 5.30 1.80 -4 -1 14 1.50 1.70 -4 1 14 1.90 1.70 4 1 -14 1.30 1.60 4 1 -14 3.80 1.70 -3 -1 14 7.00 1.80 3 -1 -14 8.70 1.90 3 -1 -14 5.10 1.80 -3 1 14 6.50 2.20 3 1 -14 7.20 1.90 3 1 -14 11.10 2.00 -2 -1 14 -0.20 1.40 2 -1 -14 -1.90 1.60 2 -1 -14 0.10 1.50 2 1 -14 -1.80 2.20 2 1 -14 1.00 1.40 -2 1 14 -0.90 1.50 -1 -1 14 0.20 1.30 1 -1 -14 -0.60 1.40 -1 -1 14 2.30 1.40 1 1 -14 0.10 1.30 -1 1 14 1.80 1.50 1 1 -14 3.40 1.40 0 -1 14 2.00 1.20 0 -1 14 4.10 1.40 0 -1 -14 3.70 1.40 0 1 -14 4.10 1.40 0 1 14 5.50 1.50 0 1 -14 2.80 1.40 4 -2 -14 0.10 1.80 4 -2 -14 4.10 1.90 4 2 -14 1.30 1.50 4 2 -14 1.10 1.50 3 -2 -14 1.90 1.70 3 -2 -14 1.30 1.60 -3 -2 14 4.00 1.70 -3 2 14 3.30 1.70 3 2 -14 2.50 1.60 3 2 -14 0.60 1.50 2 -2 -14 4.80 1.70 2 -2 -14 4.10 1.60 -2 -2 14 2.90 1.50 -2 2 14 3.50 1.60 2 2 -14 3.30 1.80 2 2 -14 3.40 1.60 -1 -2 14 0.70 1.20 -1 -2 14 -0.10 1.20 1 -2 -14 3.60 2.90 1 -2 -14 2.90 1.60 1 2 -14 1.10 1.30 1 2 -14 1.40 1.30 -1 2 14 0.00 1.40 0 -2 -14 0.60 1.40 0 -2 -14 -0.80 1.70 0 -2 14 0.70 1.20 0 2 -14 -0.60 1.20 0 2 14 1.90 1.40 0 2 -14 0.40 1.20 3 -3 -14 -2.40 1.40 -3 -3 14 -1.10 1.40 3 -3 -14 3.40 1.60 -3 3 14 -2.50 1.50 3 3 -14 0.10 1.50 3 3 -14 0.90 1.70 2 -3 -14 -1.00 1.40 -2 -3 14 0.60 1.40 2 -3 -14 1.20 1.50 -2 -3 14 2.30 2.10 -2 3 14 -1.10 1.90 2 3 -14 -0.80 1.50 2 3 -14 0.50 1.30 -1 -3 14 33.30 2.60 1 -3 -14 33.80 2.90 -1 -3 14 36.80 2.60 1 -3 -14 32.80 3.00 1 3 -14 31.80 2.60 1 3 -14 35.80 2.60 2 -4 -14 2.80 1.70 -2 -4 14 1.80 1.40 2 -4 -14 2.70 1.70 -2 -4 14 6.80 2.60 -2 4 14 1.30 1.70 2 4 -14 4.30 1.50 2 4 -14 2.70 1.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 91265 _shelx_res_file ; TITL umd2591d_a.res in P2(1)/n umd2591d_a.res created by SHELXL-2018/3 at 15:29:17 on 21-Mar-2022 REM Old TITL umd2591d in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.191, Rweak 0.010, Alpha 0.027 REM 0.524 for 134 systematic absences, Orientation as input REM Formula found by SHELXT: C17 N2 O3 CELL 0.71073 9.2231 16.1611 11.4595 90 99.865 90 ZERR 4 0.001 0.0016 0.0012 0 0.004 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 72 96 8 8 EQIV $1 -0.5+X,1.5-Y,-0.5+Z EQIV $2 1-X,1-Y,2-Z DFIX 0.87 0.01 N1 H1 DFIX 0.9 0.01 N2 H2b N2 H2a L.S. 10 PLAN 4 SIZE 0.2 0.22 0.32 TEMP 24 CONF HTAB N2 O2 HTAB N1 O4_$1 HTAB N2 O4_$2 BOND $H LIST 6 htab 2 fmap 2 acta MORE -1 OMIT -4 12 5 OMIT 1 0 1 REM REM REM WGHT 0.057000 0.415200 FVAR 0.76787 O2 4 0.727525 0.474205 0.973677 11.00000 0.03867 0.05336 = 0.09484 -0.01677 0.00384 -0.00787 O4 4 0.749970 0.604527 1.033079 11.00000 0.05203 0.03737 = 0.09720 -0.00305 0.03160 0.00499 N1 3 0.337590 0.730025 0.547169 11.00000 0.07064 0.03642 = 0.05169 0.00329 0.00965 0.00326 N2 3 0.469956 0.428769 0.837480 11.00000 0.03488 0.04172 = 0.04318 0.00418 0.00450 0.00279 C1 1 0.437442 0.684081 0.622145 11.00000 0.05887 0.05011 = 0.04568 0.00049 0.00328 -0.00220 AFIX 43 H1A 2 0.513836 0.706133 0.676833 11.00000 -1.20000 AFIX 0 C2 1 0.242357 0.677382 0.480124 11.00000 0.05082 0.04451 = 0.04028 0.00376 0.01433 0.00628 C3 1 0.122699 0.694609 0.391565 11.00000 0.06007 0.06712 = 0.04962 0.01161 0.00938 0.01816 AFIX 43 H3 2 0.095302 0.748764 0.371017 11.00000 -1.20000 AFIX 0 C4 1 0.047105 0.628791 0.336033 11.00000 0.05501 0.10133 = 0.06424 0.00258 -0.00474 0.00703 AFIX 43 H4 2 -0.032377 0.638517 0.275820 11.00000 -1.20000 AFIX 0 C5 1 0.086269 0.547592 0.367471 11.00000 0.06912 0.08064 = 0.07854 -0.01561 -0.00366 -0.01416 AFIX 43 H5 2 0.032566 0.504233 0.327913 11.00000 -1.20000 AFIX 0 C6 1 0.203016 0.530359 0.456027 11.00000 0.06321 0.04850 = 0.07062 -0.00659 0.01055 -0.00311 AFIX 43 H6 2 0.227496 0.475901 0.477033 11.00000 -1.20000 AFIX 0 C7 1 0.284089 0.595688 0.513817 11.00000 0.04622 0.04082 = 0.04302 0.00126 0.01399 0.00458 C8 1 0.410223 0.601848 0.606137 11.00000 0.04891 0.04376 = 0.04433 0.00549 0.01176 0.00688 C9 1 0.488897 0.531454 0.675176 11.00000 0.04889 0.05353 = 0.05560 0.01262 0.01248 0.01189 AFIX 23 H9A 2 0.584225 0.550063 0.715932 11.00000 -1.20000 H9B 2 0.504732 0.487268 0.621464 11.00000 -1.20000 AFIX 0 C10 1 0.399078 0.499206 0.764779 11.00000 0.04474 0.04593 = 0.05279 0.00939 0.01071 0.01342 AFIX 23 H10A 2 0.382929 0.544073 0.817299 11.00000 -1.20000 H10B 2 0.303662 0.481452 0.723096 11.00000 -1.20000 AFIX 0 C11 1 0.500694 0.351263 0.773648 11.00000 0.04012 0.04260 = 0.04522 0.00338 0.01001 0.00520 AFIX 13 H11 2 0.565930 0.364743 0.717251 11.00000 -1.20000 AFIX 0 C12 1 0.578673 0.291190 0.864699 11.00000 0.05766 0.04625 = 0.06398 0.00856 -0.00465 0.00697 AFIX 23 H12A 2 0.519809 0.282701 0.926173 11.00000 -1.20000 H12B 2 0.672434 0.314467 0.901290 11.00000 -1.20000 AFIX 0 C13 1 0.604489 0.208104 0.807908 11.00000 0.09677 0.05207 = 0.08857 0.01327 0.02133 0.02538 AFIX 23 H13A 2 0.671411 0.215725 0.752071 11.00000 -1.20000 H13B 2 0.649859 0.169933 0.868687 11.00000 -1.20000 AFIX 0 C14 1 0.461263 0.171714 0.744216 11.00000 0.12273 0.04746 = 0.07133 -0.01065 0.03460 -0.00685 AFIX 23 H14A 2 0.480951 0.120240 0.706292 11.00000 -1.20000 H14B 2 0.397404 0.159654 0.801073 11.00000 -1.20000 AFIX 0 C15 1 0.385558 0.230939 0.652692 11.00000 0.10547 0.07392 = 0.05459 -0.01915 0.01120 -0.01161 AFIX 23 H15A 2 0.291923 0.207658 0.615817 11.00000 -1.20000 H15B 2 0.445353 0.238438 0.591619 11.00000 -1.20000 AFIX 0 C16 1 0.359332 0.314886 0.706601 11.00000 0.05683 0.06422 = 0.04992 -0.00616 -0.00261 0.00032 AFIX 23 H16A 2 0.317379 0.352639 0.644040 11.00000 -1.20000 H16B 2 0.289125 0.308535 0.760051 11.00000 -1.20000 AFIX 0 C17 1 0.801633 0.537173 1.003677 11.00000 0.03555 0.03567 = 0.04819 0.00012 0.00820 0.00129 C18 1 0.964694 0.533025 1.011703 11.00000 0.03634 0.03460 = 0.04928 -0.00437 0.00699 -0.00390 AFIX 43 H18 2 1.019151 0.580476 1.034817 11.00000 -1.20000 AFIX 0 H2A 2 0.555792 0.446967 0.880479 11.00000 0.06054 H1 2 0.329752 0.784043 0.545477 11.00000 0.07524 H2B 2 0.408889 0.414285 0.888058 11.00000 0.05720 HKLF 4 REM umd2591d_a.res in P2(1)/n REM wR2 = 0.1214, GooF = S = 1.028, Restrained GooF = 1.028 for all data REM R1 = 0.0426 for 2803 Fo > 4sig(Fo) and 0.0546 for all 3446 data REM 211 parameters refined using 3 restraints END WGHT 0.0570 0.4153 REM Instructions for potential hydrogen bonds HTAB N2 O2 HTAB N1 O4_$1 HTAB N2 O4_$2 REM Highest difference peak 0.221, deepest hole -0.172, 1-sigma level 0.034 Q1 1 0.7265 0.5050 0.9004 11.00000 0.05 0.22 Q2 1 0.8232 0.5883 1.0910 11.00000 0.05 0.18 Q3 1 0.9334 0.4874 0.9729 11.00000 0.05 0.14 Q4 1 0.0482 0.6624 0.3849 11.00000 0.05 0.13 ; _shelx_res_checksum 91028 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O2 0.72753(11) 0.47420(7) 0.97368(12) 0.0632(3) Uani d 1 . . O O4 0.74997(12) 0.60453(6) 1.03308(11) 0.0600(3) Uani d 1 . . N N1 0.33759(16) 0.73002(8) 0.54717(12) 0.0530(3) Uani d 1 . . N N2 0.46996(12) 0.42877(7) 0.83748(10) 0.0402(3) Uani d 1 . . C C1 0.43744(18) 0.68408(10) 0.62215(13) 0.0522(4) Uani d 1 . . H H1A 0.513836 0.706133 0.676833 0.063 Uiso calc 1 . . C C2 0.24236(16) 0.67738(9) 0.48012(12) 0.0444(3) Uani d 1 . . C C3 0.12270(18) 0.69461(11) 0.39157(14) 0.0589(4) Uani d 1 . . H H3 0.095302 0.748764 0.371017 0.071 Uiso calc 1 . . C C4 0.0471(2) 0.62879(15) 0.33603(17) 0.0753(5) Uani d 1 . . H H4 -0.032377 0.638517 0.275820 0.090 Uiso calc 1 . . C C5 0.0863(2) 0.54759(14) 0.36747(19) 0.0780(6) Uani d 1 . . H H5 0.032566 0.504233 0.327913 0.094 Uiso calc 1 . . C C6 0.20302(19) 0.53036(10) 0.45603(16) 0.0609(4) Uani d 1 . . H H6 0.227496 0.475901 0.477033 0.073 Uiso calc 1 . . C C7 0.28409(15) 0.59569(8) 0.51382(12) 0.0426(3) Uani d 1 . . C C8 0.41022(16) 0.60185(9) 0.60614(12) 0.0452(3) Uani d 1 . . C C9 0.48890(17) 0.53145(10) 0.67518(14) 0.0523(4) Uani d 1 . . H H9A 0.584225 0.550063 0.715932 0.063 Uiso calc 1 . . H H9B 0.504732 0.487268 0.621464 0.063 Uiso calc 1 . . C C10 0.39908(16) 0.49921(9) 0.76478(13) 0.0475(3) Uani d 1 . . H H10A 0.382929 0.544073 0.817299 0.057 Uiso calc 1 . . H H10B 0.303662 0.481452 0.723096 0.057 Uiso calc 1 . . C C11 0.50069(15) 0.35126(8) 0.77365(12) 0.0423(3) Uani d 1 . . H H11 0.565930 0.364743 0.717251 0.051 Uiso calc 1 . . C C12 0.57867(19) 0.29119(10) 0.86470(15) 0.0577(4) Uani d 1 . . H H12A 0.519809 0.282701 0.926173 0.069 Uiso calc 1 . . H H12B 0.672434 0.314467 0.901290 0.069 Uiso calc 1 . . C C13 0.6045(2) 0.20810(11) 0.80791(19) 0.0785(6) Uani d 1 . . H H13A 0.671411 0.215725 0.752071 0.094 Uiso calc 1 . . H H13B 0.649859 0.169933 0.868687 0.094 Uiso calc 1 . . C C14 0.4613(3) 0.17171(11) 0.74422(18) 0.0784(6) Uani d 1 . . H H14A 0.480951 0.120240 0.706292 0.094 Uiso calc 1 . . H H14B 0.397404 0.159654 0.801073 0.094 Uiso calc 1 . . C C15 0.3856(3) 0.23094(13) 0.65269(16) 0.0783(6) Uani d 1 . . H H15A 0.291923 0.207658 0.615817 0.094 Uiso calc 1 . . H H15B 0.445353 0.238438 0.591619 0.094 Uiso calc 1 . . C C16 0.35933(18) 0.31489(11) 0.70660(14) 0.0584(4) Uani d 1 . . H H16A 0.317379 0.352639 0.644040 0.070 Uiso calc 1 . . H H16B 0.289125 0.308535 0.760051 0.070 Uiso calc 1 . . C C17 0.80163(14) 0.53717(8) 1.00368(12) 0.0397(3) Uani d 1 . . C C18 0.96469(14) 0.53303(8) 1.01170(12) 0.0401(3) Uani d 1 . . H H18 1.019151 0.580476 1.034817 0.048 Uiso calc 1 . . H H2A 0.5558(13) 0.4470(10) 0.8805(13) 0.061(5) Uiso d 1 . . H H1 0.330(2) 0.7840(6) 0.5455(17) 0.075(6) Uiso d 1 . . H H2B 0.4089(16) 0.4143(10) 0.8881(12) 0.057(5) Uiso d 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 O2 0.0387(6) 0.0534(6) 0.0948(9) -0.0079(5) 0.0038(5) -0.0168(6) O4 0.0520(6) 0.0374(5) 0.0972(9) 0.0050(4) 0.0316(6) -0.0031(5) N1 0.0706(9) 0.0364(6) 0.0517(7) 0.0033(6) 0.0096(6) 0.0033(5) N2 0.0349(6) 0.0417(6) 0.0432(6) 0.0028(5) 0.0045(5) 0.0042(5) C1 0.0589(9) 0.0501(8) 0.0457(8) -0.0022(7) 0.0033(7) 0.0005(7) C2 0.0508(8) 0.0445(7) 0.0403(7) 0.0063(6) 0.0143(6) 0.0038(6) C3 0.0601(10) 0.0671(10) 0.0496(8) 0.0182(8) 0.0094(7) 0.0116(8) C4 0.0550(10) 0.1013(15) 0.0642(11) 0.0070(10) -0.0047(8) 0.0026(11) C5 0.0691(12) 0.0806(14) 0.0785(13) -0.0142(10) -0.0037(10) -0.0156(11) C6 0.0632(10) 0.0485(9) 0.0706(10) -0.0031(7) 0.0106(8) -0.0066(8) C7 0.0462(7) 0.0408(7) 0.0430(7) 0.0046(6) 0.0140(6) 0.0013(6) C8 0.0489(8) 0.0438(7) 0.0443(7) 0.0069(6) 0.0118(6) 0.0055(6) C9 0.0489(8) 0.0535(9) 0.0556(8) 0.0119(7) 0.0125(7) 0.0126(7) C10 0.0447(8) 0.0459(8) 0.0528(8) 0.0134(6) 0.0107(6) 0.0094(6) C11 0.0401(7) 0.0426(7) 0.0452(7) 0.0052(6) 0.0100(6) 0.0034(6) C12 0.0577(9) 0.0463(8) 0.0640(9) 0.0070(7) -0.0046(7) 0.0086(7) C13 0.0968(15) 0.0521(10) 0.0886(13) 0.0254(10) 0.0213(12) 0.0133(10) C14 0.1227(18) 0.0475(10) 0.0713(12) -0.0069(10) 0.0346(12) -0.0107(9) C15 0.1055(16) 0.0739(13) 0.0546(10) -0.0116(11) 0.0112(10) -0.0191(9) C16 0.0568(9) 0.0642(10) 0.0499(8) 0.0003(8) -0.0026(7) -0.0062(7) C17 0.0356(6) 0.0357(7) 0.0482(7) 0.0013(5) 0.0082(5) 0.0001(5) C18 0.0363(7) 0.0346(6) 0.0493(7) -0.0039(5) 0.0070(5) -0.0044(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 N1 H1 . . 126.9(13) ? C2 N1 C1 . . 108.39(12) ? C2 N1 H1 . . 124.6(13) ? C10 N2 C11 . . 117.72(11) ? C10 N2 H2A . . 108.3(11) ? C10 N2 H2B . . 107.1(11) ? C11 N2 H2A . . 108.4(11) ? C11 N2 H2B . . 106.6(11) ? H2A N2 H2B . . 108.5(15) ? N1 C1 H1A . . 124.5 ? C8 C1 N1 . . 110.95(14) ? C8 C1 H1A . . 124.5 ? N1 C2 C3 . . 129.78(14) ? N1 C2 C7 . . 108.12(12) ? C3 C2 C7 . . 122.10(15) ? C2 C3 H3 . . 121.3 ? C4 C3 C2 . . 117.42(16) ? C4 C3 H3 . . 121.3 ? C3 C4 H4 . . 119.2 ? C3 C4 C5 . . 121.59(16) ? C5 C4 H4 . . 119.2 ? C4 C5 H5 . . 119.4 ? C6 C5 C4 . . 121.16(18) ? C6 C5 H5 . . 119.4 ? C5 C6 H6 . . 120.5 ? C5 C6 C7 . . 119.05(16) ? C7 C6 H6 . . 120.5 ? C2 C7 C8 . . 106.59(12) ? C6 C7 C2 . . 118.68(14) ? C6 C7 C8 . . 134.73(14) ? C1 C8 C7 . . 105.96(12) ? C1 C8 C9 . . 127.52(14) ? C7 C8 C9 . . 126.43(13) ? C8 C9 H9A . . 109.6 ? C8 C9 H9B . . 109.6 ? C8 C9 C10 . . 110.27(12) ? H9A C9 H9B . . 108.1 ? C10 C9 H9A . . 109.6 ? C10 C9 H9B . . 109.6 ? N2 C10 C9 . . 113.68(11) ? N2 C10 H10A . . 108.8 ? N2 C10 H10B . . 108.8 ? C9 C10 H10A . . 108.8 ? C9 C10 H10B . . 108.8 ? H10A C10 H10B . . 107.7 ? N2 C11 H11 . . 108.9 ? N2 C11 C12 . . 107.83(12) ? N2 C11 C16 . . 110.67(11) ? C12 C11 H11 . . 108.9 ? C12 C11 C16 . . 111.52(13) ? C16 C11 H11 . . 108.9 ? C11 C12 H12A . . 109.4 ? C11 C12 H12B . . 109.4 ? C11 C12 C13 . . 111.11(14) ? H12A C12 H12B . . 108.0 ? C13 C12 H12A . . 109.4 ? C13 C12 H12B . . 109.4 ? C12 C13 H13A . . 109.4 ? C12 C13 H13B . . 109.4 ? H13A C13 H13B . . 108.0 ? C14 C13 C12 . . 111.08(16) ? C14 C13 H13A . . 109.4 ? C14 C13 H13B . . 109.4 ? C13 C14 H14A . . 109.5 ? C13 C14 H14B . . 109.5 ? H14A C14 H14B . . 108.1 ? C15 C14 C13 . . 110.62(16) ? C15 C14 H14A . . 109.5 ? C15 C14 H14B . . 109.5 ? C14 C15 H15A . . 109.3 ? C14 C15 H15B . . 109.3 ? C14 C15 C16 . . 111.77(14) ? H15A C15 H15B . . 107.9 ? C16 C15 H15A . . 109.3 ? C16 C15 H15B . . 109.3 ? C11 C16 C15 . . 111.59(15) ? C11 C16 H16A . . 109.3 ? C11 C16 H16B . . 109.3 ? C15 C16 H16A . . 109.3 ? C15 C16 H16B . . 109.3 ? H16A C16 H16B . . 108.0 ? O2 C17 O4 . . 124.62(13) ? O2 C17 C18 . . 118.79(12) ? O4 C17 C18 . . 116.52(12) ? C17 C18 H18 . . 118.0 ? C18 C18 C17 3_767 . 123.95(16) ? C18 C18 H18 3_767 . 118.0 ? 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 O2 C17 . 1.2411(16) ? O4 C17 . 1.2572(16) ? N1 C1 . 1.366(2) ? N1 C2 . 1.362(2) ? N1 H1 . 0.876(9) ? N2 C10 . 1.4935(17) ? N2 C11 . 1.5018(18) ? N2 H2A . 0.907(9) ? N2 H2B . 0.905(9) ? C1 H1A . 0.9300 ? C1 C8 . 1.359(2) ? C2 C3 . 1.393(2) ? C2 C7 . 1.4105(19) ? C3 H3 . 0.9300 ? C3 C4 . 1.368(3) ? C4 H4 . 0.9300 ? C4 C5 . 1.392(3) ? C5 H5 . 0.9300 ? C5 C6 . 1.376(3) ? C6 H6 . 0.9300 ? C6 C7 . 1.394(2) ? C7 C8 . 1.436(2) ? C8 C9 . 1.5000(19) ? C9 H9A . 0.9700 ? C9 H9B . 0.9700 ? C9 C10 . 1.518(2) ? C10 H10A . 0.9700 ? C10 H10B . 0.9700 ? C11 H11 . 0.9800 ? C11 C12 . 1.514(2) ? C11 C16 . 1.514(2) ? C12 H12A . 0.9700 ? C12 H12B . 0.9700 ? C12 C13 . 1.529(2) ? C13 H13A . 0.9700 ? C13 H13B . 0.9700 ? C13 C14 . 1.514(3) ? C14 H14A . 0.9700 ? C14 H14B . 0.9700 ? C14 C15 . 1.501(3) ? C15 H15A . 0.9700 ? C15 H15B . 0.9700 ? C15 C16 . 1.527(2) ? C16 H16A . 0.9700 ? C16 H16B . 0.9700 ? C17 C18 . 1.4924(18) ? C18 C18 3_767 1.302(3) ? 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 _geom_hbond_publ_flag N2 H2A O2 . 0.907(9) 1.807(9) 2.7107(15) 174.6(16) yes N1 H1 O4 4_575 0.876(9) 1.941(11) 2.7899(16) 162.7(18) yes N2 H2B O4 3_667 0.905(9) 1.873(10) 2.7632(16) 167.0(15) yes 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 O2 C17 C18 C18 . . . 3_767 0.5(3) ? O4 C17 C18 C18 . . . 3_767 177.60(18) ? N1 C1 C8 C7 . . . . 0.23(17) ? N1 C1 C8 C9 . . . . -176.30(14) ? N1 C2 C3 C4 . . . . 178.46(16) ? N1 C2 C7 C6 . . . . -179.33(14) ? N1 C2 C7 C8 . . . . 0.35(16) ? N2 C11 C12 C13 . . . . 176.04(14) ? N2 C11 C16 C15 . . . . -173.47(13) ? C1 N1 C2 C3 . . . . -179.77(15) ? C1 N1 C2 C7 . . . . -0.21(16) ? C1 C8 C9 C10 . . . . 101.09(19) ? C2 N1 C1 C8 . . . . -0.02(18) ? C2 C3 C4 C5 . . . . 0.9(3) ? C2 C7 C8 C1 . . . . -0.35(16) ? C2 C7 C8 C9 . . . . 176.23(13) ? C3 C2 C7 C6 . . . . 0.3(2) ? C3 C2 C7 C8 . . . . 179.95(13) ? C3 C4 C5 C6 . . . . 0.0(3) ? C4 C5 C6 C7 . . . . -0.8(3) ? C5 C6 C7 C2 . . . . 0.7(2) ? C5 C6 C7 C8 . . . . -178.90(17) ? C6 C7 C8 C1 . . . . 179.25(17) ? C6 C7 C8 C9 . . . . -4.2(3) ? C7 C2 C3 C4 . . . . -1.0(2) ? C7 C8 C9 C10 . . . . -74.77(19) ? C8 C9 C10 N2 . . . . 180.00(12) ? C10 N2 C11 C12 . . . . 177.27(12) ? C10 N2 C11 C16 . . . . -60.50(16) ? C11 N2 C10 C9 . . . . -60.41(17) ? C11 C12 C13 C14 . . . . -56.1(2) ? C12 C11 C16 C15 . . . . -53.43(19) ? C12 C13 C14 C15 . . . . 56.9(2) ? C13 C14 C15 C16 . . . . -56.1(2) ? C14 C15 C16 C11 . . . . 54.6(2) ? C16 C11 C12 C13 . . . . 54.34(19) ? _cod_database_fobs_code 2022828