#------------------------------------------------------------------------------ #$Date: 2019-07-03 21:47:50 +0300 (Wed, 03 Jul 2019) $ #$Revision: 216712 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021696.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_2021696 loop_ _publ_author_name 'Pogoda, Dorota' 'Janczak, Jan' 'Pawlak, Sylwia' 'Zaworotko, Michael' 'Videnova-Adrabinska, Veneta' _publ_section_title ; Tautomeric polymorphism of the neuroactive inhibitor kynurenic acid ; _journal_coeditor_code UK3175 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 793 _journal_page_last 805 _journal_paper_doi 10.1107/S2053229619005990 _journal_volume 75 _journal_year 2019 _chemical_formula_moiety 'C10 H7 N O3, H2 O' _chemical_formula_sum 'C10 H9 N O4' _chemical_formula_weight 207.18 _space_group_crystal_system orthorhombic _space_group_IT_number 56 _space_group_name_Hall '-P 2ab 2ac' _space_group_name_H-M_alt 'P c c n' _symmetry_space_group_name_Hall '-P 2ab 2ac' _symmetry_space_group_name_H-M 'P c c n' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 13.9295(7) _cell_length_b 17.8065(9) _cell_length_c 7.1429(4) _cell_measurement_reflns_used 1562 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.951 _cell_measurement_theta_min 2.288 _cell_volume 1771.69(16) _computing_cell_refinement ; CrysAlis Red 1.171.38.41 (Rigaku Oxford Diffraction, 2015) ; _computing_data_collection ; CrysAlis CCD 1.171.38.41 (Rigaku Oxford Diffraction, 2015) ; _computing_data_reduction ; CrysAlis Red 1.171.38.41 (Rigaku Oxford Diffraction, 2015) ; _computing_molecular_graphics ; Brandenburg & Putz (2006). Diamond 3.0. Crystal and Molecular Structure Visualisation, University of Bonn, Germany ; _computing_publication_material ; SHELXL-2014/7 (Sheldrick, 2014) ; _computing_structure_refinement ; SHELXL-2014/7 (Sheldrick, 2014) ; _computing_structure_solution ; SHELXT (Sheldrick, 2014) ; _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 10.6249 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.900 _diffrn_measurement_device_type 'KUMA KM-4 with CCD detector' _diffrn_measurement_method \w-scan _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_unetI/netI 0.0099 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 32133 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 30.535 _diffrn_reflns_theta_min 2.288 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.122 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.98405 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.553 _exptl_crystal_description parallelepiped _exptl_crystal_F_000 864 _exptl_crystal_size_max 0.280 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_min 0.230 _refine_diff_density_max 0.382 _refine_diff_density_min -0.190 _refine_ls_extinction_coef 0.017(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL-2014/7 (Sheldrick 2014 ; _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 164 _refine_ls_number_reflns 2447 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.001 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0296 _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^)+(0.0444P)^2^+0.7162P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.0799 _reflns_number_gt 2260 _reflns_number_total 2447 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file uk3175sup1.cif _cod_data_source_block ortho_a _cod_database_code 2021696 _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 0.967 _shelx_estimated_absorpt_t_max 0.972 _shelx_hkl_file ; 0 0 -1 -4.30 0.30 0 0 -1 -3.10 0.40 0 0 2 3337.37 70.09 0 0 2 3344.07 70.09 0 0 -2 3271.67 70.09 0 0 2 3348.17 70.09 0 0 -2 3324.47 70.09 0 0 -3 -2.60 0.80 0 0 -3 -1.90 0.80 0 0 -3 -1.40 0.90 0 0 -3 -1.20 0.80 0 0 3 0.00 0.90 0 0 3 -0.50 0.80 0 0 3 -1.50 0.80 0 0 3 -1.20 0.70 0 0 4 66.29 2.60 0 0 4 64.39 2.70 0 0 -4 71.09 2.70 0 0 -4 64.49 2.70 0 0 4 67.19 2.60 0 0 -4 67.79 2.70 0 0 -4 66.79 2.70 0 0 5 0.10 1.00 0 0 5 0.40 1.20 0 0 5 1.50 1.10 0 0 -5 -0.20 1.10 0 0 -5 -1.20 1.10 0 0 5 -1.00 1.00 0 0 -5 -1.50 1.10 0 0 -5 0.20 1.10 0 0 -6 1314.17 29.60 0 0 6 1336.57 29.50 0 0 -6 1350.26 29.60 0 0 6 1320.27 29.60 0 0 6 1349.77 29.60 0 0 -6 1330.57 29.50 0 0 -7 2.40 1.90 0 0 7 -0.20 1.80 0 0 7 -0.60 1.70 0 0 7 -1.80 1.50 0 0 -7 0.30 1.90 0 0 -7 -0.80 1.90 0 0 8 323.47 9.60 0 0 -8 332.87 9.70 0 0 -9 -4.00 2.70 0 0 9 -1.60 2.40 -1 0 -1 -2.70 0.50 1 0 1 -3.80 0.40 1 0 1 -3.30 0.50 -1 0 -1 -3.60 0.40 1 0 -1 -2.60 0.50 1 0 -1 -3.50 0.50 -1 0 1 -4.50 0.30 -1 0 -3 -2.20 0.80 -1 0 -3 -0.30 0.90 1 0 3 -0.60 0.50 1 0 -3 -0.60 0.80 -1 0 -3 -0.80 0.80 1 0 3 -0.30 0.80 -1 0 3 -0.60 0.80 -1 0 3 -0.90 0.80 1 0 -3 -0.50 0.90 1 0 3 -0.90 0.80 1 0 -3 -1.90 0.90 1 0 3 -0.50 0.80 -1 0 3 -0.60 0.90 -1 0 3 -0.10 0.90 -1 0 -3 -0.80 0.70 1 0 -3 -1.70 0.80 -1 0 4 4184.68 89.39 -1 0 4 4137.39 89.39 -1 0 -4 4344.47 89.29 1 0 4 4205.68 89.29 -1 0 4 4319.97 89.39 -1 0 -4 4243.78 89.39 1 0 -4 4333.87 89.39 1 0 -4 4175.18 89.39 -1 0 4 4241.08 89.39 1 0 4 4067.89 89.29 1 0 4 4179.28 89.29 -1 0 -4 4185.38 89.29 1 0 4 4312.57 89.39 1 0 -4 4232.18 89.39 -1 0 -4 4163.08 89.39 1 0 -4 4194.88 89.39 -1 0 5 -0.80 1.10 1 0 5 -0.10 1.10 -1 0 5 1.60 1.20 1 0 -5 -0.20 1.10 1 0 -5 -1.00 1.10 -1 0 5 -1.10 1.00 -1 0 -5 -0.40 1.00 1 0 5 -0.70 1.00 1 0 5 -1.10 1.10 -1 0 5 -1.30 0.90 -1 0 -5 -1.90 1.10 1 0 -5 1.10 1.20 -1 0 -5 -0.60 1.10 1 0 -5 -0.30 1.10 1 0 5 -0.80 0.90 -1 0 -5 1.20 1.20 1 0 6 484.25 11.50 -1 0 6 477.45 11.50 -1 0 6 469.15 12.20 1 0 6 467.15 11.50 -1 0 -6 458.95 11.60 -1 0 6 467.35 11.50 1 0 6 483.45 11.50 -1 0 -6 468.05 11.50 -1 0 -6 460.15 11.50 1 0 -6 461.55 11.50 -1 0 6 463.15 11.60 1 0 -6 462.55 11.60 1 0 -6 463.25 11.60 -1 0 7 -0.90 1.50 -1 0 -7 0.90 2.00 -1 0 7 1.50 1.50 1 0 -7 2.00 1.70 -1 0 7 0.20 1.60 1 0 7 -4.30 1.70 1 0 -7 1.50 1.80 1 0 -7 -0.20 1.90 1 0 7 -0.20 1.70 -1 0 -7 -1.80 3.10 1 0 7 2.70 2.90 -1 0 -7 2.40 1.90 1 0 -8 70.59 4.60 -1 0 8 57.49 4.50 -1 0 -8 57.99 4.50 1 0 8 62.69 4.30 1 0 -9 0.30 2.80 -1 0 9 -0.20 2.50 1 0 9 3.30 2.70 -1 0 -9 -0.30 2.70 2 0 -1 -3.50 0.60 -2 0 1 -3.90 0.60 2 0 -1 -2.20 0.70 2 0 1 -3.30 0.60 2 0 -1 -3.90 0.60 -2 0 1 -3.00 0.60 -2 0 1 -3.20 0.70 -2 0 1 -3.00 0.60 -2 0 -1 -2.70 0.50 2 0 1 -3.00 0.60 -2 0 -1 -2.40 0.50 -2 0 -1 -2.00 0.60 2 0 -1 -2.00 0.60 -2 0 -1 -3.50 0.50 2 0 -2 3213.78 65.39 -2 0 2 3144.29 65.39 2 0 -2 3137.29 65.39 -2 0 2 3056.09 65.39 -2 0 2 3108.29 65.39 -2 0 2 3129.99 65.39 2 0 -2 3073.29 65.39 -2 0 -2 3194.58 65.29 2 0 -2 3019.40 65.39 2 0 2 2772.12 65.49 2 0 2 2989.30 65.39 -2 0 -2 3079.19 65.29 -2 0 -2 3113.59 65.29 2 0 2 3112.89 65.29 -2 0 -3 -2.60 0.90 2 0 -3 -4.60 0.90 -2 0 3 -4.10 0.80 2 0 3 -3.70 0.80 2 0 -3 -3.10 0.90 2 0 3 -1.70 0.90 -2 0 -3 -3.90 0.90 -2 0 -3 -3.00 0.80 -2 0 3 -3.80 0.90 -2 0 3 -3.90 0.80 -2 0 3 -2.80 0.90 -2 0 -3 -2.00 0.80 2 0 -3 -4.40 0.90 2 0 3 -3.60 0.80 2 0 3 -4.70 0.40 2 0 -3 -3.90 0.90 2 0 -4 1539.35 32.80 2 0 4 1458.95 32.70 -2 0 4 1507.65 32.70 -2 0 -4 1493.25 32.70 2 0 4 1521.35 32.70 2 0 -4 1573.34 32.80 2 0 -4 1506.25 32.80 2 0 4 1499.15 32.70 -2 0 -4 1485.85 32.70 -2 0 4 1466.85 32.80 -2 0 4 1528.85 32.80 -2 0 4 1548.84 32.80 2 0 -4 1510.55 32.80 -2 0 -4 1564.54 32.70 -2 0 -4 1480.55 32.70 -2 0 5 2.30 1.30 2 0 5 1.00 0.90 -2 0 -5 0.00 1.20 2 0 -5 0.30 1.20 2 0 -5 0.40 1.10 -2 0 5 0.20 1.20 2 0 5 -1.20 1.10 2 0 -5 -0.20 1.20 -2 0 -5 1.10 1.20 2 0 5 0.70 1.00 -2 0 -5 0.70 1.20 2 0 -5 1.90 1.20 2 0 5 1.60 1.20 -2 0 5 0.50 1.10 -2 0 5 0.50 1.10 -2 0 -5 -1.50 1.20 2 0 6 664.13 17.30 -2 0 6 782.32 17.60 2 0 -6 761.32 17.70 -2 0 6 769.52 17.70 2 0 6 774.42 17.60 -2 0 -6 755.32 17.60 -2 0 -6 761.32 17.50 2 0 -6 766.42 17.70 2 0 6 728.53 17.50 -2 0 -6 779.22 17.70 -2 0 6 760.32 17.60 -2 0 6 789.82 19.50 2 0 -6 785.62 17.60 -2 0 7 2.10 1.70 -2 0 7 -0.80 1.90 2 0 -7 -2.80 1.80 2 0 -7 1.10 1.90 -2 0 -7 -0.50 1.80 -2 0 7 -1.50 1.60 2 0 -7 -1.30 1.70 2 0 7 -2.00 2.10 2 0 7 -2.10 1.40 -2 0 -7 2.80 2.20 -2 0 -7 2.80 1.80 2 0 7 0.00 1.70 -2 0 -8 8.50 2.40 2 0 8 6.30 2.20 2 0 -8 10.90 2.50 -2 0 8 9.10 2.30 2 0 9 0.20 2.40 -2 0 9 -1.00 2.70 -2 0 -9 -3.50 2.60 2 0 -9 4.60 2.80 3 0 -1 -0.60 0.70 -3 0 1 0.20 0.60 -3 0 1 0.30 1.00 3 0 -1 -0.70 0.70 -3 0 -1 0.00 0.70 3 0 1 -0.50 0.40 3 0 1 0.50 0.70 3 0 1 0.50 0.70 -3 0 -1 -0.10 0.70 3 0 -1 1.00 0.90 3 0 -1 1.10 1.00 -3 0 1 -0.30 0.60 -3 0 1 0.20 0.70 -3 0 -1 0.10 0.60 -3 0 -1 0.90 0.60 -3 0 2 21.80 1.60 -3 0 -2 23.60 1.50 -3 0 2 21.80 1.60 -3 0 -2 28.40 1.60 -3 0 2 22.50 1.70 -3 0 -2 23.60 1.50 3 0 -2 19.80 1.60 -3 0 2 19.50 1.60 3 0 2 23.30 1.50 3 0 -2 21.10 1.60 -3 0 -2 22.90 1.50 3 0 2 23.20 1.50 3 0 2 25.30 1.60 3 0 -2 21.60 1.60 3 0 3 -0.40 0.90 -3 0 -3 -0.50 0.80 -3 0 3 -0.90 0.90 3 0 -3 -1.40 0.80 -3 0 3 -2.00 0.90 -3 0 -3 -2.30 0.80 3 0 -3 -1.70 0.80 -3 0 3 -1.50 0.90 -3 0 3 -2.20 0.80 3 0 3 -1.20 0.80 -3 0 -3 -2.00 0.90 3 0 3 -1.00 0.80 -3 0 -3 -1.90 0.80 3 0 -3 -0.80 0.90 3 0 3 -1.00 0.90 3 0 -3 -1.70 1.00 -3 0 4 7766.52 164.28 3 0 -4 7625.04 164.28 3 0 -4 7713.53 164.28 3 0 4 7899.71 164.18 3 0 4 7743.03 164.18 3 0 -4 7742.03 164.28 -3 0 4 7626.14 164.28 -3 0 -4 7742.23 164.18 3 0 -4 8146.79 164.28 -3 0 -4 7840.62 164.08 -3 0 4 8005.30 164.28 -3 0 -4 7644.54 164.18 3 0 -5 0.50 1.30 3 0 -5 -0.90 1.10 -3 0 5 -0.30 1.00 3 0 -5 0.60 1.20 3 0 -5 0.20 1.20 3 0 5 0.20 1.00 -3 0 5 -0.40 1.30 3 0 5 -0.10 1.10 3 0 5 0.60 1.20 -3 0 -5 0.20 1.20 -3 0 -5 2.00 1.20 3 0 5 1.00 0.80 -3 0 5 2.10 1.20 -3 0 -5 -1.70 1.10 -3 0 5 1.20 1.20 -3 0 -5 0.50 1.20 -3 0 -6 352.26 9.20 3 0 6 356.36 9.20 3 0 -6 353.06 9.30 -3 0 6 355.06 9.40 -3 0 -6 352.16 9.30 3 0 -6 353.26 9.40 3 0 6 359.46 9.30 -3 0 6 360.46 9.20 -3 0 -6 352.46 9.30 -3 0 6 361.76 9.30 3 0 -6 353.86 9.40 3 0 -7 -2.00 1.60 3 0 7 -1.10 1.70 -3 0 7 -0.60 1.70 -3 0 -7 -2.40 1.90 -3 0 7 -2.20 1.70 3 0 7 2.10 1.80 -3 0 -7 1.50 1.80 3 0 -7 -0.50 1.90 -3 0 -7 -1.10 1.80 -3 0 7 3.30 2.10 3 0 -7 1.30 2.20 -3 0 8 228.68 7.80 -3 0 -8 225.18 7.60 3 0 8 222.28 7.40 3 0 -8 224.68 7.80 3 0 9 -6.40 2.60 3 0 -9 -1.10 3.00 -3 0 -9 -3.40 2.50 -3 0 9 1.40 2.60 4 0 1 -3.10 0.70 -4 0 1 -3.80 1.40 -4 0 -1 -2.80 0.90 -4 0 1 -1.00 0.70 4 0 -1 -2.80 0.80 4 0 -1 -2.10 1.50 4 0 -1 -3.20 0.80 4 0 -1 -2.80 0.70 -4 0 -1 -2.50 0.70 4 0 1 -2.60 0.60 -4 0 1 -1.20 0.90 -4 0 1 -3.00 0.80 4 0 1 -2.40 0.80 -4 0 -1 -3.10 0.70 -4 0 2 2903.31 60.49 4 0 2 2954.00 60.49 4 0 2 2664.43 60.69 4 0 -2 3008.60 60.59 -4 0 -2 2755.72 60.39 4 0 -2 2888.81 60.49 4 0 2 2790.12 60.39 -4 0 -2 2627.14 60.69 -4 0 2 2961.50 60.49 -4 0 -2 2863.31 60.39 -4 0 2 2938.01 60.49 -4 0 -2 2877.01 60.39 -4 0 -3 0.30 0.80 -4 0 -3 0.80 0.90 4 0 3 0.30 0.90 -4 0 -3 0.10 0.90 -4 0 3 -0.30 1.30 4 0 3 -0.10 0.80 -4 0 -3 0.70 1.00 -4 0 3 -0.10 0.90 4 0 -3 0.00 1.00 -4 0 3 -0.20 0.70 4 0 3 -0.50 0.90 4 0 3 -1.50 0.40 -4 0 3 -1.00 0.90 4 0 -3 -0.10 0.80 4 0 -3 0.30 0.80 4 0 -3 -0.90 1.10 -4 0 4 8984.50 192.18 -4 0 4 9336.97 192.18 4 0 -4 9129.89 192.18 -4 0 -4 8794.22 192.08 -4 0 4 9390.76 192.18 -4 0 -4 8937.61 191.98 4 0 -4 9537.05 192.18 4 0 -4 9043.50 192.18 4 0 4 9009.10 191.98 4 0 4 9126.79 192.08 -4 0 -4 9057.79 192.08 4 0 5 -1.60 1.20 -4 0 5 2.60 1.20 4 0 5 0.50 1.30 -4 0 -5 2.60 1.40 -4 0 -5 1.10 1.20 -4 0 -5 -0.50 1.20 4 0 -5 -1.80 1.10 4 0 -5 1.80 1.10 -4 0 5 -1.70 1.10 4 0 -5 2.30 1.30 -4 0 5 1.20 1.20 4 0 5 -0.10 1.20 -4 0 -5 1.00 1.20 4 0 5 1.30 1.10 -4 0 5 1.40 1.40 4 0 -5 -0.90 1.40 -4 0 6 3054.09 63.99 4 0 -6 3000.70 63.89 -4 0 6 2991.50 63.89 4 0 -6 2932.11 63.89 4 0 6 2861.31 63.79 -4 0 -6 3002.70 63.69 4 0 -6 2974.10 63.99 -4 0 6 2932.91 63.99 -4 0 -6 2950.80 63.79 -4 0 -6 2947.61 63.79 4 0 6 2993.80 63.79 -4 0 -7 -0.80 1.90 4 0 -7 0.50 2.10 -4 0 7 -0.70 1.90 -4 0 7 1.60 2.00 4 0 7 -1.90 3.00 4 0 -7 1.50 2.20 4 0 7 -1.70 1.50 -4 0 7 0.20 1.80 -4 0 -7 -0.30 1.80 -4 0 -7 -1.20 1.90 4 0 -7 1.40 1.90 4 0 -8 310.47 9.50 4 0 8 295.97 9.10 -4 0 -8 307.47 9.30 -4 0 8 304.47 9.40 -4 0 9 -1.90 2.60 4 0 -9 1.90 3.00 -4 0 -9 0.80 2.70 4 0 9 2.10 2.80 5 0 1 -4.60 0.70 -5 0 -1 -4.40 0.70 5 0 1 -3.30 0.80 -5 0 1 -3.10 1.10 5 0 -1 -3.60 0.80 5 0 -1 -2.60 0.80 -5 0 1 -5.10 0.80 -5 0 1 -4.00 0.70 5 0 1 -4.00 0.70 5 0 1 -4.80 0.70 5 0 -1 -4.20 0.80 -5 0 -1 -3.00 0.80 -5 0 1 -4.40 0.80 -5 0 -1 -4.10 0.80 -5 0 -1 -3.20 0.80 5 0 -1 -4.40 0.80 -5 0 -2 288.17 6.90 5 0 2 271.77 6.80 -5 0 2 287.77 6.90 5 0 2 242.28 6.70 -5 0 2 273.47 7.10 5 0 -2 272.57 7.10 -5 0 -2 284.37 6.90 -5 0 -2 290.87 6.80 5 0 -2 287.87 7.00 5 0 2 293.87 6.90 5 0 2 289.77 6.90 -5 0 2 293.97 7.00 5 0 -2 298.97 7.00 -5 0 -2 287.57 6.90 -5 0 2 282.87 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4.00 -5 -5 6 57.29 3.10 5 -5 -6 57.49 4.20 -5 5 -6 49.40 3.10 5 -5 -6 52.99 3.70 5 5 6 50.49 3.80 -5 5 -6 48.30 3.00 -5 -5 6 54.59 3.10 -5 5 -6 46.90 2.90 5 5 6 52.19 3.90 5 -5 -6 45.70 4.10 -5 5 7 8.40 4.40 -5 -5 -7 8.70 2.70 -5 -5 -7 9.50 2.70 5 -5 7 6.20 1.80 -5 5 7 7.90 2.60 5 5 -7 6.40 2.10 -5 5 7 6.50 2.50 5 5 7 6.00 2.50 5 -5 -7 3.80 2.20 5 5 7 9.00 2.80 -5 5 -7 8.40 1.90 5 -5 -7 6.20 2.40 -5 -5 7 7.20 2.00 5 -5 8 34.10 3.80 -5 -5 -8 39.00 5.10 5 5 -8 32.90 4.20 -5 5 8 34.90 3.80 5 5 8 36.60 3.80 -5 -5 8 38.80 4.20 5 -5 -8 37.70 3.90 -5 5 -8 29.90 3.80 -5 -5 -9 19.50 3.70 -5 -5 9 18.10 5.10 5 5 9 15.40 3.50 5 -5 -9 19.30 5.10 6 -5 0 0.00 0.80 -6 5 0 -0.20 0.70 6 5 0 -0.40 0.80 -6 5 0 -0.50 0.80 6 -5 0 -0.10 0.70 6 -5 0 0.60 0.80 -6 -5 0 -0.30 0.70 -6 5 0 -0.20 0.80 -6 -5 0 0.90 0.90 -6 5 0 0.00 0.70 6 -5 0 -0.60 0.60 -6 -5 0 0.50 0.90 6 5 0 -0.20 0.80 6 5 0 -0.20 0.90 6 5 0 -0.90 0.90 -6 -5 0 -0.20 1.20 -6 -5 -1 1963.70 41.40 6 5 -1 2034.30 41.40 -6 5 1 1901.91 41.30 -6 -5 -1 1913.61 41.40 -6 5 1 1900.71 41.20 6 5 -1 1937.11 41.40 6 5 -1 1958.30 41.30 6 -5 1 1921.91 41.00 6 -5 1 1890.41 40.90 -6 5 1 1949.90 41.20 6 5 -1 1942.11 41.30 -6 5 1 1887.91 41.20 6 -5 1 1790.62 41.00 6 -5 1 1929.11 41.10 -6 -5 -1 1974.90 41.40 -6 -5 1 1917.01 41.30 -6 -5 1 1966.00 41.30 6 5 1 1950.30 41.40 -6 -5 1 1973.30 41.40 6 -5 -1 1963.30 41.20 6 5 1 1914.41 41.40 -6 5 -1 1923.81 40.90 -6 5 -1 1900.21 41.10 -6 5 -1 1827.92 41.10 6 5 1 1970.20 41.40 6 -5 -1 1877.81 41.20 6 -5 -1 1957.00 41.30 -6 -5 1 1913.01 41.40 -6 5 -1 1923.81 40.90 6 5 1 1925.41 41.40 -6 5 2 799.12 18.00 -6 -5 -2 793.22 18.10 6 -5 2 815.12 17.60 -6 -5 -2 802.92 18.10 6 -5 2 779.92 17.60 6 5 -2 822.32 18.00 -6 5 2 829.52 18.00 6 5 -2 842.82 18.00 -6 5 2 797.52 18.00 6 -5 2 816.42 17.70 6 5 -2 794.82 18.00 -6 5 2 789.22 18.00 6 5 -2 821.12 17.90 6 -5 2 801.62 17.50 6 5 2 695.53 19.40 6 -5 -2 824.62 18.00 6 5 2 809.02 18.20 -6 5 -2 824.12 17.50 -6 -5 2 824.92 18.00 6 -5 -2 796.12 18.00 6 -5 -2 815.42 18.00 -6 5 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32.70 1.90 -2 -9 2 35.00 1.40 2 9 2 35.60 1.90 2 9 2 36.10 2.10 2 9 2 42.30 2.20 -2 -9 2 33.20 1.50 2 -9 -2 34.90 2.00 2 -9 -2 36.50 2.10 -2 -9 2 37.80 1.60 2 9 2 35.50 2.30 -2 9 3 2005.10 42.70 -2 9 3 2010.40 42.60 -2 -9 -3 2015.80 42.70 -2 9 3 1990.10 42.60 -2 -9 -3 2019.70 42.70 2 9 -3 1948.91 41.70 -2 -9 -3 1984.30 42.70 2 9 -3 1946.81 42.10 -2 -9 -3 1927.61 42.70 -2 9 3 1971.40 42.70 2 9 -3 1926.61 42.10 -2 -9 3 1896.01 42.10 -2 -9 3 2003.90 41.90 -2 -9 3 1980.60 41.90 2 -9 -3 1996.80 42.60 2 9 3 1983.20 42.60 2 9 3 1993.10 42.70 2 -9 -3 1909.61 42.60 2 9 3 1994.00 42.70 2 9 3 1976.50 42.80 2 -9 -3 2040.40 42.70 -2 -9 3 1895.01 42.10 2 -9 -3 2041.80 42.70 2 9 -4 379.96 8.10 2 -9 4 356.16 8.10 2 9 -4 356.16 8.10 2 -9 4 354.66 8.10 -2 9 4 356.96 9.20 -2 9 4 350.96 9.20 -2 -9 -4 355.76 9.30 2 9 -4 361.26 8.40 -2 9 4 359.86 9.10 -2 -9 -4 356.26 9.20 -2 -9 -4 364.66 9.20 2 9 -4 360.86 8.50 -2 -9 -4 364.46 9.30 -2 9 4 351.06 9.00 2 -9 -4 368.26 9.20 2 9 4 356.56 9.10 2 -9 -4 354.96 9.20 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213.68 6.20 -3 20 2 2.00 1.70 -3 -20 -2 -0.90 1.90 3 20 -2 2.60 1.30 3 20 -2 2.20 1.50 -3 -20 2 2.20 1.40 -3 -20 2 -0.70 2.60 3 -20 -2 2.40 1.80 3 20 2 1.60 1.70 3 20 -3 23.70 2.10 -3 20 3 22.60 2.70 -3 -20 -3 22.10 2.80 3 -20 -3 27.90 3.50 -3 -20 3 25.70 2.30 3 20 3 21.20 2.80 -3 20 4 -2.00 2.30 -3 -20 -4 5.20 2.50 3 20 4 -1.30 2.50 -3 -20 4 5.10 1.40 3 -20 -4 3.90 2.40 -3 -20 -5 197.38 8.10 3 -20 -5 169.38 9.40 3 20 5 194.58 7.90 4 20 0 373.66 9.60 -4 20 0 369.46 9.00 -4 20 0 358.06 8.80 4 -20 0 373.46 9.10 4 -20 0 368.36 9.00 -4 -20 0 369.36 9.70 -4 -20 -1 32.90 3.30 4 20 -1 34.90 2.80 4 -20 1 32.00 2.10 -4 20 1 33.80 2.80 4 20 1 35.90 3.20 4 -20 -1 35.00 2.90 -4 -20 1 37.00 2.90 4 20 -2 29.20 2.50 -4 -20 -2 27.00 3.50 -4 20 2 27.30 3.10 4 20 2 27.20 3.30 4 -20 -2 26.60 3.20 -4 -20 2 27.20 2.70 -4 -20 -3 183.28 6.80 4 20 -3 175.98 5.20 -4 20 3 180.08 6.40 4 -20 -3 178.48 6.40 -4 -20 3 178.58 5.30 4 20 3 187.88 6.80 4 20 -4 3.30 1.40 -4 20 4 6.50 2.40 -4 -20 -4 0.20 2.60 4 -20 -4 1.20 2.60 4 20 4 3.10 2.70 -4 -20 4 5.00 1.60 -4 -20 -5 1.20 3.10 4 20 5 7.10 3.50 5 -20 0 -0.50 1.50 5 -20 0 -1.90 1.30 -5 20 0 -0.90 1.40 5 20 0 -0.20 1.70 -5 20 0 -1.40 1.20 -5 -20 0 0.40 1.60 -5 -20 -1 11.10 2.20 5 20 -1 12.90 1.90 -5 20 1 14.00 1.90 5 -20 -1 12.50 1.90 -5 -20 1 8.10 1.80 5 20 1 9.70 2.00 -5 20 2 135.69 5.10 -5 -20 -2 138.89 5.70 5 20 -2 143.49 4.80 5 -20 -2 139.69 5.20 -5 -20 2 137.59 4.80 5 20 2 147.49 5.70 -5 -20 -3 2.80 2.40 5 20 -3 8.40 1.70 -5 20 3 5.60 2.30 5 20 3 8.10 2.60 -5 -20 3 9.10 1.80 5 -20 -3 6.20 2.30 -5 -20 -4 184.18 7.50 -5 20 4 183.38 7.10 5 20 4 174.98 7.30 5 -20 -4 176.18 7.00 -5 -20 -5 72.89 6.30 5 20 5 89.09 6.90 6 -20 0 106.09 3.80 -6 20 0 102.39 3.80 -6 -20 0 103.39 4.70 6 20 0 113.39 4.70 -6 20 0 100.99 3.60 -6 -20 -1 17.80 2.60 6 20 -1 14.00 2.10 -6 20 1 12.90 1.90 6 -20 -1 14.10 2.00 6 20 1 10.60 2.30 -6 -20 1 14.70 2.20 -6 -20 -2 6.20 2.40 6 20 -2 8.00 1.90 -6 20 2 2.50 2.00 6 -20 -2 -1.80 2.00 -6 -20 2 3.20 1.70 6 20 2 5.90 2.20 -6 20 3 545.75 13.90 -6 -20 -3 560.04 14.40 6 20 -3 524.95 13.10 -6 -20 3 541.95 13.20 6 20 3 552.74 14.40 6 -20 -3 540.35 13.90 -6 -20 -4 25.90 3.50 6 20 4 33.30 3.90 -6 -20 -5 -2.20 4.30 -7 -20 0 0.70 2.00 7 20 0 -4.50 1.90 7 -20 0 -0.90 1.50 -7 20 0 -0.70 1.40 -7 20 0 -1.20 1.60 -7 -20 -1 9.70 2.40 7 -20 1 11.00 1.40 7 20 -1 8.10 2.10 -7 20 1 12.60 2.00 7 20 1 9.30 2.30 -7 -20 1 11.30 2.30 7 -20 -1 12.00 2.10 -7 20 2 76.89 4.30 7 20 -2 87.89 4.10 -7 -20 -2 79.59 5.20 -7 -20 2 81.79 4.20 7 -20 -2 74.49 4.30 7 20 2 84.09 5.10 -7 20 3 282.37 11.60 -7 -20 -3 280.87 9.40 7 20 3 282.07 9.20 7 -20 -3 303.67 10.60 -7 -20 -4 7.10 3.00 7 20 4 4.10 3.00 -8 20 0 300.37 8.30 8 -20 0 301.07 8.50 8 20 0 301.07 9.70 -8 -20 0 300.77 9.70 -8 20 1 863.12 19.70 -8 -20 -1 861.21 20.80 8 -20 1 864.92 19.00 8 20 -1 860.51 20.40 8 -20 -1 852.41 19.80 -8 -20 1 859.12 20.40 8 20 1 862.11 20.80 -8 -20 -2 1.60 2.70 8 20 -2 5.90 3.60 -8 20 2 1.10 3.40 -8 -20 2 5.10 2.40 8 -20 -2 5.80 3.00 8 20 2 4.00 2.60 -8 -20 -3 161.08 7.20 8 20 3 148.99 7.00 -8 -20 -4 -1.50 3.80 9 -20 0 -0.50 2.00 -9 -20 0 -2.30 2.20 9 20 0 1.30 2.30 -9 20 0 1.80 1.70 9 -20 1 202.78 5.80 -9 -20 -1 220.18 7.60 9 20 1 214.88 7.60 -9 -20 1 214.58 8.10 -9 -20 -2 0.50 2.80 9 20 2 -2.60 2.50 -9 -20 -3 39.00 4.90 9 20 3 25.40 4.40 0 -21 1 -0.30 1.30 0 21 -1 0.20 1.30 0 -21 -1 0.20 1.70 0 21 1 0.90 1.60 0 -21 1 0.10 1.40 0 21 -1 -0.20 1.20 0 -21 -2 77.89 4.30 0 21 2 82.99 4.20 0 21 3 0.10 2.10 0 -21 -3 -2.20 2.10 0 -21 -4 601.44 15.70 0 21 4 620.74 15.90 -1 21 0 48.20 2.80 1 21 0 45.70 2.90 -1 21 0 49.50 3.10 -1 -21 0 46.60 3.10 1 -21 0 45.40 2.90 -1 21 1 1.10 1.50 1 21 -1 0.60 1.50 1 -21 1 3.60 1.40 1 -21 1 0.80 1.20 -1 -21 -1 1.30 1.70 1 21 -1 1.60 1.30 -1 -21 1 1.40 2.60 -1 -21 1 2.10 1.40 1 -21 -1 -0.70 1.60 1 21 1 2.90 1.70 -1 21 2 353.26 9.60 -1 -21 -2 359.36 9.70 -1 -21 2 357.36 8.60 1 -21 -2 354.26 9.60 1 21 2 362.26 9.80 -1 -21 2 357.96 8.60 -1 -21 -3 136.59 5.80 -1 21 3 129.69 5.50 1 -21 -3 132.69 5.60 1 21 3 133.29 5.60 -1 21 4 9.10 2.90 -1 -21 -4 8.90 2.60 1 21 4 9.40 2.80 1 -21 -4 5.50 2.70 -2 21 0 -1.20 1.50 -2 -21 0 1.40 1.60 -2 21 0 1.10 1.40 2 21 0 1.60 1.50 2 -21 0 1.70 1.40 -2 -21 -1 30.90 3.30 2 21 -1 28.60 2.50 2 -21 1 33.50 2.20 2 -21 1 28.70 2.30 2 21 -1 27.60 2.90 -2 21 1 29.40 2.80 -2 -21 1 29.30 2.60 2 -21 -1 28.90 2.90 2 21 1 32.10 3.10 -2 21 2 311.17 8.70 -2 -21 -2 319.17 9.10 2 21 2 323.27 9.00 -2 -21 2 316.27 7.90 2 -21 -2 321.37 8.90 -2 21 3 2.50 2.10 -2 -21 -3 5.90 2.40 2 21 3 7.50 2.30 -2 -21 3 8.40 1.60 2 -21 -3 5.30 2.30 -2 -21 3 6.40 1.30 -2 21 4 12.40 4.60 -2 -21 -4 9.20 2.80 2 21 4 3.40 2.70 2 -21 -4 9.30 3.40 -3 21 0 30.10 2.70 3 21 0 28.40 3.00 -3 -21 0 27.10 3.10 -3 21 0 25.90 2.40 3 -21 0 29.20 2.50 3 21 -1 22.60 2.60 -3 -21 -1 26.40 3.30 -3 21 1 23.60 2.80 3 21 1 23.90 3.00 3 -21 -1 20.70 2.80 -3 -21 1 23.20 2.60 -3 21 2 50.19 3.60 -3 -21 -2 46.90 4.10 3 21 -2 45.40 4.50 3 21 -2 46.60 2.70 3 -21 -2 41.50 3.60 -3 -21 2 46.10 2.90 3 21 2 54.89 3.80 -3 -21 -3 41.30 4.30 -3 21 3 38.90 4.00 3 -21 -3 31.30 3.90 3 21 3 41.60 4.20 -3 -21 3 41.70 2.60 -3 -21 -4 17.10 3.30 -3 -21 4 22.90 2.60 3 21 4 22.50 3.20 -4 -21 0 -3.00 1.60 4 21 0 -1.10 1.60 -4 21 0 1.60 1.50 4 -21 0 1.10 1.40 -4 21 0 -0.70 1.30 4 21 -1 73.79 3.70 -4 -21 -1 72.59 4.30 -4 21 1 75.09 3.60 4 21 1 74.29 4.10 4 -21 -1 82.19 3.70 -4 -21 1 68.99 3.60 -4 21 2 763.42 18.00 4 21 -2 761.62 17.50 -4 -21 -2 778.92 18.60 4 -21 -2 768.12 18.10 -4 -21 2 762.02 17.60 4 21 2 773.72 18.50 4 21 -3 16.20 1.80 -4 -21 -3 20.40 3.00 -4 21 3 13.00 2.60 4 21 3 15.60 3.00 -4 -21 3 15.50 1.90 4 -21 -3 15.80 2.70 -4 -21 -4 168.28 7.60 4 21 4 186.48 9.30 -5 21 0 926.71 20.50 -5 21 0 899.61 20.20 -5 -21 0 925.11 21.30 5 -21 0 908.91 20.40 5 21 0 922.91 21.20 5 21 -1 36.80 3.20 -5 -21 -1 36.10 3.80 -5 21 1 37.20 3.00 5 -21 -1 38.00 3.20 5 21 1 49.30 4.00 -5 -21 1 31.20 3.20 -5 -21 -2 587.74 14.70 -5 21 2 564.84 14.00 5 21 -2 559.24 13.60 5 21 2 598.44 14.70 5 -21 -2 570.04 14.10 -5 -21 2 565.44 13.80 -5 -21 -3 100.49 5.40 5 21 3 82.79 5.20 6 -21 0 -2.80 1.50 6 21 0 3.00 1.90 -6 21 0 -3.30 1.40 -6 -21 0 -2.90 1.80 -6 21 1 153.78 5.20 6 21 -1 150.28 5.50 -6 -21 -1 155.28 6.20 -6 -21 1 155.18 5.70 6 -21 -1 153.78 5.30 6 21 1 163.58 6.20 6 21 -2 109.79 5.00 -6 -21 -2 101.99 5.50 -6 21 2 110.19 5.30 -6 -21 2 109.99 4.90 6 -21 -2 108.19 5.30 6 21 2 107.29 5.30 -6 -21 -3 -0.40 2.80 6 21 3 0.60 2.90 7 -21 0 -1.40 1.60 7 21 0 0.10 2.20 -7 -21 0 -2.00 2.00 -7 21 0 0.60 1.50 -7 -21 -1 -3.90 2.20 -7 21 1 1.40 1.90 7 21 -1 -1.00 2.30 7 21 1 4.60 2.30 7 -21 -1 -1.80 2.00 -7 -21 1 4.20 2.30 -7 -21 -2 -2.10 2.50 7 21 2 -1.80 2.50 -8 21 0 -1.10 1.90 8 -21 1 285.47 7.20 0 -22 0 81.69 3.70 0 22 0 81.59 3.50 0 22 1 -0.90 1.80 0 -22 1 -0.10 1.30 0 -22 -1 3.90 1.80 0 22 -1 0.50 1.30 0 22 2 30.50 3.40 0 -22 -2 27.70 3.60 0 -22 -3 1.40 2.90 -1 22 0 3.20 1.50 1 22 0 3.20 1.60 1 -22 0 -2.20 1.50 -1 -22 0 2.80 1.60 1 22 -1 110.29 5.30 -1 22 1 95.89 4.20 -1 -22 -1 97.09 4.50 1 -22 1 97.99 3.50 1 22 -1 94.09 3.50 1 -22 -1 96.89 4.20 -1 -22 1 104.09 3.80 1 22 1 96.29 4.30 -1 22 2 64.89 4.00 -1 -22 -2 55.49 4.10 -1 -22 2 70.19 2.90 1 22 2 60.79 4.10 1 -22 -2 56.09 4.00 -1 -22 -3 30.20 5.70 2 22 0 404.96 10.10 -2 22 0 398.16 9.60 2 -22 0 391.86 9.70 -2 -22 0 395.96 10.20 -2 -22 -1 11.50 2.00 2 22 -1 11.50 1.50 2 -22 1 11.60 1.30 2 -22 1 12.10 1.70 -2 22 1 11.50 1.70 -2 -22 1 11.80 1.60 2 22 1 12.00 1.80 2 -22 -1 11.90 1.80 -2 22 2 22.80 2.60 -2 -22 -2 24.40 2.70 -2 -22 2 29.40 2.50 2 22 2 33.60 3.60 2 -22 -2 28.10 3.50 -2 -22 -3 67.59 7.70 -2 -22 3 72.69 2.90 3 -22 0 0.20 1.50 3 22 0 2.00 1.70 -3 22 0 0.10 1.30 -3 -22 0 1.10 1.80 3 22 -1 16.50 2.10 -3 22 1 17.80 2.10 -3 -22 -1 17.10 2.40 -3 -22 1 20.50 2.70 3 22 1 13.10 2.20 3 -22 -1 18.00 2.10 -3 -22 -2 145.29 5.90 -3 22 2 146.69 5.90 3 22 -2 143.99 4.50 3 22 2 142.29 5.80 3 -22 -2 144.69 5.60 -3 -22 2 139.39 4.70 -4 -22 0 284.97 8.30 4 22 0 285.07 8.10 -4 22 0 285.07 7.20 4 -22 0 277.87 7.40 4 22 -1 205.58 6.30 -4 -22 -1 223.28 7.10 -4 22 1 200.18 6.20 4 -22 -1 210.58 6.30 4 22 1 211.58 6.90 -4 -22 1 203.28 6.40 4 22 -2 6.80 1.90 -4 -22 -2 3.60 2.60 4 22 2 6.10 2.60 -4 -22 2 4.60 3.10 -5 -22 0 -0.90 2.00 5 -22 0 0.50 1.50 5 22 0 1.50 2.30 -5 -22 -1 198.48 7.60 -5 22 1 180.48 6.30 5 -22 -1 184.28 7.10 -5 -22 1 183.68 8.30 5 22 1 200.78 9.30 6 -22 0 147.79 5.80 0 -23 1 0.40 1.50 1 -23 0 476.65 11.70 1 23 0 480.75 12.20 -1 23 0 465.25 11.40 -1 -23 0 487.55 12.40 1 23 -1 14.50 2.60 1 -23 1 14.60 2.60 -1 -23 1 13.80 2.70 -1 -23 2 19.80 2.60 -2 23 0 1.00 1.50 2 -23 0 1.80 1.80 2 23 -1 9.90 2.10 -3 23 0 174.38 5.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 71490 _shelx_res_file ; ortho_a.res created by SHELXL-2014/7 TITL ortho_a_a.res in Pccn CELL 0.71073 13.9295 17.8065 7.1429 90 90 90 ZERR 8 0.0007 0.0009 0.0004 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,-Y,0.5-Z SFAC C H N O UNIT 80 72 8 32 L.S. 10 PLAN 20 TEMP -173 BOND $H EQIV $1 -X+1.5, -Y+0.5, Z HTAB N1 O2_$1 HTAB O3 O4 EQIV $2 -X+1, -Y+1, -Z+1 HTAB O4 O1_$2 EQIV $3 X-0.5, -Y+1, -Z+0.5 HTAB O4 O1_$3 FMAP 2 SIZE 0.28 0.26 0.23 ACTA 52 WGHT 0.044400 0.716200 EXTI 0.017393 FVAR 0.90141 N1 3 0.608139 0.254603 0.260295 11.00000 0.00829 0.00828 = 0.01196 0.00010 0.00036 0.00059 H1N 2 0.658640 0.235196 0.210868 11.00000 -1.20000 C2 1 0.600121 0.329514 0.269656 11.00000 0.00873 0.00892 = 0.01020 0.00036 -0.00097 -0.00046 C3 1 0.517479 0.363104 0.338143 11.00000 0.00975 0.00784 = 0.01254 0.00008 -0.00024 0.00024 H3 2 0.512910 0.416257 0.345136 11.00000 -1.20000 C4 1 0.440193 0.318256 0.394708 11.00000 0.00876 0.01100 = 0.01046 -0.00040 -0.00052 0.00064 C5 1 0.449449 0.238146 0.387337 11.00000 0.00910 0.00956 = 0.01085 -0.00013 -0.00136 -0.00039 C6 1 0.374992 0.188879 0.443898 11.00000 0.00975 0.01263 = 0.01570 0.00042 -0.00011 -0.00109 H6 2 0.317058 0.209133 0.493637 11.00000 -1.20000 C7 1 0.386928 0.112560 0.428986 11.00000 0.01282 0.01242 = 0.01725 0.00118 -0.00076 -0.00397 H7 2 0.337477 0.078357 0.465691 11.00000 -1.20000 C8 1 0.473484 0.082464 0.357919 11.00000 0.01599 0.00785 = 0.01500 -0.00050 -0.00197 -0.00092 H8 2 0.479442 0.028546 0.349346 11.00000 -1.20000 C9 1 0.547911 0.128724 0.304321 11.00000 0.01248 0.00952 = 0.01246 -0.00061 -0.00087 0.00080 H9 2 0.606767 0.110268 0.252872 11.00000 -1.20000 C10 1 0.536035 0.207206 0.318336 11.00000 0.00948 0.00931 = 0.00984 0.00033 -0.00118 -0.00079 C1 1 0.685465 0.374168 0.193769 11.00000 0.00854 0.01015 = 0.01114 0.00206 -0.00110 -0.00024 O1 4 0.683499 0.444219 0.219069 11.00000 0.01361 0.00807 = 0.01777 0.00036 0.00204 -0.00088 O2 4 0.748123 0.337000 0.110003 11.00000 0.00995 0.01130 = 0.01626 0.00157 0.00212 0.00175 O3 4 0.357880 0.345707 0.454198 11.00000 0.00876 0.00996 = 0.02133 -0.00055 0.00315 0.00129 H3O 2 0.353650 0.397276 0.445920 11.00000 -1.50000 O4 4 0.341591 0.487821 0.442712 11.00000 0.01382 0.01020 = 0.01876 -0.00109 -0.00128 0.00233 H4A 2 0.340830 0.508818 0.552052 11.00000 -1.50000 H4B 2 0.292071 0.506194 0.384469 11.00000 -1.50000 HKLF 4 REM ortho_a_a.res in Pccn REM R1 = 0.0296 for 2260 Fo > 4sig(Fo) and 0.0325 for all 2447 data REM 164 parameters refined using 0 restraints END WGHT 0.0442 0.6408 REM Highest difference peak 0.382, deepest hole -0.190, 1-sigma level 0.042 Q1 1 0.6395 0.3535 0.2322 11.00000 0.05 0.38 Q2 1 0.4782 0.3405 0.3696 11.00000 0.05 0.38 Q3 1 0.5596 0.3440 0.3060 11.00000 0.05 0.37 Q4 1 0.4957 0.2247 0.3595 11.00000 0.05 0.35 Q5 1 0.4143 0.2123 0.4169 11.00000 0.05 0.34 Q6 1 0.5089 0.1097 0.3295 11.00000 0.05 0.32 Q7 1 0.5405 0.1674 0.3156 11.00000 0.05 0.32 Q8 1 0.4335 0.0995 0.4035 11.00000 0.05 0.30 Q9 1 0.5725 0.2339 0.2981 11.00000 0.05 0.28 Q10 1 0.4458 0.2757 0.3806 11.00000 0.05 0.28 Q11 1 0.6010 0.2919 0.2698 11.00000 0.05 0.25 Q12 1 0.3959 0.1493 0.4653 11.00000 0.05 0.22 Q13 1 0.3986 0.3320 0.4258 11.00000 0.05 0.22 Q14 1 0.7175 0.3572 0.1511 11.00000 0.05 0.20 Q15 1 0.3817 0.1506 0.4181 11.00000 0.05 0.20 Q16 1 0.3388 0.4437 0.4344 11.00000 0.05 0.13 Q17 1 0.6439 0.4592 0.2663 11.00000 0.05 0.13 Q18 1 0.6830 0.4112 0.1936 11.00000 0.05 0.12 Q19 1 0.7402 0.2886 0.1269 11.00000 0.05 0.11 Q20 1 0.7252 0.4657 0.1786 11.00000 0.05 0.11 ; _shelx_res_checksum 32490 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, 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 N N1 0.60814(5) 0.25460(4) 0.26030(10) 0.00951(15) Uani d 1 H H1N 0.6586(9) 0.2352(6) 0.2109(16) 0.011 Uiso d 1 C C2 0.60012(5) 0.32951(4) 0.26966(11) 0.00928(16) Uani d 1 C C3 0.51748(5) 0.36310(4) 0.33814(11) 0.01005(16) Uani d 1 H H3 0.5129(8) 0.4163(6) 0.3451(16) 0.012 Uiso d 1 C C4 0.44019(5) 0.31826(4) 0.39471(11) 0.01007(16) Uani d 1 C C5 0.44945(5) 0.23815(4) 0.38734(11) 0.00983(16) Uani d 1 C C6 0.37499(6) 0.18888(5) 0.44390(12) 0.01269(17) Uani d 1 H H6 0.3171(9) 0.2091(6) 0.4936(17) 0.015 Uiso d 1 C C7 0.38693(6) 0.11256(5) 0.42899(12) 0.01416(17) Uani d 1 H H7 0.3375(9) 0.0784(6) 0.4657(17) 0.017 Uiso d 1 C C8 0.47348(6) 0.08246(4) 0.35792(12) 0.01295(17) Uani d 1 H H8 0.4794(8) 0.0285(7) 0.3493(16) 0.016 Uiso d 1 C C9 0.54791(6) 0.12872(4) 0.30432(11) 0.01149(16) Uani d 1 H H9 0.6068(8) 0.1103(7) 0.2529(16) 0.014 Uiso d 1 C C10 0.53604(5) 0.20721(4) 0.31834(11) 0.00954(16) Uani d 1 C C1 0.68546(5) 0.37417(4) 0.19377(11) 0.00994(16) Uani d 1 O O1 0.68350(4) 0.44422(3) 0.21907(8) 0.01315(14) Uani d 1 O O2 0.74812(4) 0.33700(3) 0.11000(9) 0.01250(14) Uani d 1 O O3 0.35788(4) 0.34571(3) 0.45420(9) 0.01335(14) Uani d 1 H H3O 0.3536(9) 0.3973(7) 0.4459(17) 0.020 Uiso d 1 O O4 0.34159(4) 0.48782(3) 0.44271(10) 0.01426(14) Uani d 1 H H4A 0.3408(9) 0.5088(7) 0.5521(19) 0.021 Uiso d 1 H H4B 0.2921(9) 0.5062(7) 0.3845(18) 0.021 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 N1 0.0083(3) 0.0083(3) 0.0120(3) 0.0006(2) 0.0004(2) 0.0001(2) C2 0.0087(3) 0.0089(3) 0.0102(3) -0.0005(3) -0.0010(3) 0.0004(3) C3 0.0098(3) 0.0078(3) 0.0125(3) 0.0002(3) -0.0002(3) 0.0001(3) C4 0.0088(3) 0.0110(4) 0.0105(3) 0.0006(3) -0.0005(3) -0.0004(3) C5 0.0091(3) 0.0096(4) 0.0109(3) -0.0004(2) -0.0014(3) -0.0001(3) C6 0.0097(3) 0.0126(4) 0.0157(4) -0.0011(3) -0.0001(3) 0.0004(3) C7 0.0128(4) 0.0124(4) 0.0173(4) -0.0040(3) -0.0008(3) 0.0012(3) C8 0.0160(4) 0.0079(4) 0.0150(4) -0.0009(3) -0.0020(3) -0.0005(3) C9 0.0125(3) 0.0095(4) 0.0125(3) 0.0008(3) -0.0009(3) -0.0006(3) C10 0.0095(3) 0.0093(4) 0.0098(3) -0.0008(3) -0.0012(3) 0.0003(3) C1 0.0085(3) 0.0102(4) 0.0111(3) -0.0002(2) -0.0011(3) 0.0021(3) O1 0.0136(3) 0.0081(3) 0.0178(3) -0.0009(2) 0.0020(2) 0.0004(2) O2 0.0100(3) 0.0113(3) 0.0163(3) 0.0018(2) 0.0021(2) 0.0016(2) O3 0.0088(3) 0.0100(3) 0.0213(3) 0.00129(19) 0.0032(2) -0.0005(2) O4 0.0138(3) 0.0102(3) 0.0188(3) 0.0023(2) -0.0013(2) -0.0011(2) 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 C2 N1 C10 122.32(7) C2 N1 H1N 119.3(7) C10 N1 H1N 118.3(7) N1 C2 C3 121.08(7) N1 C2 C1 115.78(7) C3 C2 C1 123.10(7) C2 C3 C4 119.62(7) C2 C3 H3 120.3(7) C4 C3 H3 120.1(7) O3 C4 C3 123.43(7) O3 C4 C5 117.36(7) C3 C4 C5 119.21(7) C10 C5 C6 118.83(7) C10 C5 C4 118.50(7) C6 C5 C4 122.67(7) C7 C6 C5 120.12(7) C7 C6 H6 120.4(7) C5 C6 H6 119.5(7) C6 C7 C8 120.41(7) C6 C7 H7 121.5(7) C8 C7 H7 118.1(7) C9 C8 C7 120.97(7) C9 C8 H8 120.8(7) C7 C8 H8 118.2(7) C8 C9 C10 118.95(7) C8 C9 H9 123.1(7) C10 C9 H9 117.9(7) N1 C10 C9 120.04(7) N1 C10 C5 119.24(7) C9 C10 C5 120.70(7) O2 C1 O1 127.49(7) O2 C1 C2 115.96(7) O1 C1 C2 116.53(7) C4 O3 H3O 113.9(8) H4A O4 H4B 105.0(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C2 1.3402(10) N1 C10 1.3758(10) N1 H1N 0.860(12) C2 C3 1.3865(10) C2 C1 1.5295(10) C3 C4 1.4000(10) C3 H3 0.950(11) C4 O3 1.3169(9) C4 C5 1.4333(10) C5 C10 1.4146(10) C5 C6 1.4172(11) C6 C7 1.3732(11) C6 H6 0.953(12) C7 C8 1.4137(12) C7 H7 0.956(12) C8 C9 1.3784(11) C8 H8 0.966(12) C9 C10 1.4108(11) C9 H9 0.957(12) C1 O2 1.2481(10) C1 O1 1.2607(10) O3 H3O 0.922(13) O4 H4A 0.866(14) O4 H4B 0.869(13) 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 N1 H1N O2 2_655 0.860(12) 1.964(12) 2.7968(9) 162.7(11) O3 H3O O4 . 0.922(13) 1.621(13) 2.5420(8) 176.3(12) O4 H4A O1 5_666 0.866(14) 1.867(14) 2.7245(9) 170.1(12) O4 H4B O1 4_465 0.869(13) 1.901(13) 2.7657(8) 172.8(12) _cod_database_fobs_code 2021696