#------------------------------------------------------------------------------ #$Date: 2019-07-06 06:56:35 +0300 (Sat, 06 Jul 2019) $ #$Revision: 216789 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021703.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_2021703 loop_ _publ_author_name 'Cabaj, Ma\/lgorzata Katarzyna' 'Gajda, Roman' 'Hoser, Anna' 'Makal, Anna' 'Dominiak, Paulina Maria' _publ_section_title ; Differences and similarities among hypoxanthinium nitrate hydrate structures ; _journal_coeditor_code QP3027 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229619008702 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac 'H3 O +, C5 H5 N4 O +, 2N O3 -, 2H2 O' _chemical_formula_moiety 'H3 O +, C5 H5 N4 O +, 2(N O3 -), 2(H2 O)' _chemical_formula_sum 'C5 H12 N6 O10' _chemical_formula_weight 316.21 _chemical_name_common ; Hydroxonium hypoxanthinium dinitrate dihydrate ; _chemical_name_systematic ; Oxidanium 6-Oxo-1H,7H-purin-9-ium dinitrate dihydrate ; _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' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _audit_creation_method ; OLEX2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 104.812(9) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.8485(8) _cell_length_b 10.1717(6) _cell_length_c 11.2851(11) _cell_measurement_reflns_used 1478 _cell_measurement_temperature 20.00 _cell_measurement_theta_max 27.4980 _cell_measurement_theta_min 2.7400 _cell_volume 1203.90(17) _computing_cell_refinement ; CrysAlisPro 1.171.38.43c (Rigaku OD, 2015) ; _computing_data_collection ; CrysAlisPro 1.171.38.43c (Rigaku OD, 2015) ; _computing_data_reduction ; CrysAlisPro 1.171.38.43c (Rigaku OD, 2015) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2016 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 20.0 _diffrn_detector_area_resol_mean 16.0026 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.895 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type ; Agilent Technologies SuperNova four-circle diffractometer equipped with a micro-focus sealed tube and an Eos CCD detector ; _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_unetI/netI 0.0621 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4511 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.161 _diffrn_reflns_theta_min 2.324 _exptl_absorpt_coefficient_mu 0.169 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.68290 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2015) ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_density_diffrn 1.745 _exptl_crystal_description block _exptl_crystal_F_000 656 _exptl_crystal_size_max 0.178 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.351 _refine_diff_density_min -0.335 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 238 _refine_ls_number_reflns 2640 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.070 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0496 _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^)+(0.0542P)^2^+0.5897P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1174 _refine_ls_wR_factor_ref 0.1348 _reflns_number_gt 2002 _reflns_number_total 2640 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file qp3027sup1.cif _cod_data_source_block hx2_20k _cod_original_cell_volume 1203.91(17) _cod_database_code 2021703 _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 0.971 _shelx_estimated_absorpt_t_max 0.985 _shelx_hkl_file ; 0 0 -1 -0.01 0.02 0 0 -2 213.74 5.75 0 0 -3 -0.04 0.20 0 0 -4 124.23 4.50 0 0 -5 -0.27 0.31 0 0 -6 6.06 1.03 0 0 -7 -0.26 0.39 0 0 -8 29.11 2.54 0 0 -9 -0.58 0.46 0 0 -10 2.99 1.12 0 0 -11 -1.19 0.79 0 0 -12 48.02 4.25 0 0 -13 1.26 0.88 0 1 0 0.02 0.02 0 -1 -1 75.97 2.15 0 1 -1 85.78 1.92 0 -1 -2 2.36 0.39 0 1 -2 2.37 0.36 0 1 -3 220.08 6.35 0 -1 -3 225.92 6.39 0 1 -4 26.34 1.71 0 -1 -4 27.15 1.73 0 1 -5 6.93 0.96 0 -1 -5 6.39 0.95 0 -1 -6 -0.04 0.27 0 1 -6 0.80 0.49 0 1 -7 14.82 1.73 0 -1 -7 16.69 1.78 0 1 8 12.54 1.13 0 1 -8 12.18 1.72 0 -1 -8 9.77 1.52 0 1 -9 7.36 1.37 0 -1 -9 7.51 1.37 0 1 -10 72.07 4.72 0 -1 -10 74.53 4.92 0 1 -11 0.61 0.60 0 -1 -11 -0.39 0.60 0 -1 -12 -0.12 0.64 0 1 -12 3.90 1.34 0 -1 -13 1.19 1.13 0 1 -13 0.59 0.79 0 2 0 8.23 0.66 0 -2 0 8.05 0.39 0 2 1 0.70 0.23 0 -2 1 0.59 0.17 0 2 -1 0.56 0.19 0 -2 -2 53.67 2.31 0 2 2 58.97 2.34 0 2 -2 58.35 1.92 0 2 -3 152.31 4.74 0 -2 -3 146.82 4.91 0 -2 -4 42.32 2.38 0 2 -4 36.77 2.10 0 2 -5 53.73 2.86 0 -2 -5 50.78 2.98 0 -2 -6 93.63 4.67 0 2 -6 120.10 4.86 0 2 7 15.24 1.35 0 2 -7 16.13 1.81 0 -2 -7 12.14 1.62 0 -2 -8 4.67 1.25 0 2 8 4.77 0.78 0 2 -8 4.93 1.16 0 2 -9 15.47 2.04 0 -2 -9 11.60 1.94 0 -2 -10 0.31 0.57 0 2 -10 0.66 0.59 0 2 -11 34.69 3.44 0 -2 -11 25.73 3.21 0 2 -12 3.41 1.24 0 -2 -12 3.42 1.40 0 -2 -13 18.23 3.02 0 2 -13 15.23 2.58 0 3 0 0.19 0.23 0 -3 0 0.45 0.13 0 3 1 0.44 0.36 0 -3 -1 0.90 0.22 0 -3 1 0.79 0.24 0 3 -1 0.86 0.37 0 -3 2 24.66 1.64 0 3 -2 22.54 1.24 0 3 2 24.87 1.56 0 -3 -3 26.84 1.80 0 3 3 30.30 1.81 0 3 -3 28.03 1.37 0 3 4 365.27 10.36 0 3 -4 383.11 10.48 0 -3 -4 380.44 10.89 0 -3 -5 3.45 0.82 0 3 -5 3.19 0.70 0 3 5 4.68 0.81 0 3 6 32.15 2.12 0 -3 -6 32.95 2.66 0 3 -6 30.18 2.31 0 3 7 25.94 1.94 0 -3 -7 29.98 2.70 0 3 -7 24.59 2.22 0 3 8 9.13 1.19 0 3 -8 9.92 1.56 0 -3 -8 5.90 1.37 0 3 -9 19.96 2.33 0 -3 -9 23.55 2.74 0 -3 -10 6.83 1.68 0 3 -10 9.58 1.74 0 -3 -11 5.16 1.49 0 3 -11 9.19 1.84 0 3 -12 22.81 3.00 0 -3 -12 26.48 3.51 0 -3 -13 0.52 0.74 0 3 -13 0.25 0.91 0 -4 0 3.00 0.34 0 4 0 3.16 0.59 0 4 -1 4.58 0.66 0 4 1 4.32 0.72 0 -4 -1 5.32 0.42 0 -4 1 4.49 0.53 0 4 -2 -0.07 0.22 0 -4 -2 0.03 0.12 0 -4 2 0.23 0.27 0 4 2 0.45 0.27 0 4 3 35.30 2.21 0 -4 3 32.72 2.30 0 4 -3 34.60 1.77 0 4 -4 54.51 2.32 0 4 4 55.69 2.93 0 4 -5 6.96 1.01 0 4 5 7.24 1.04 0 -4 -5 4.99 1.03 0 4 6 11.22 1.32 0 -4 -6 11.11 1.57 0 4 -6 11.51 1.44 0 4 7 4.30 0.87 0 -4 -7 4.27 1.20 0 4 -7 4.84 1.04 0 4 8 24.07 2.05 0 -4 -8 22.45 2.63 0 4 -8 26.39 2.50 0 4 -9 7.40 1.48 0 4 9 7.45 1.18 0 -4 -9 8.41 1.79 0 -4 -10 0.36 0.86 0 4 -10 0.52 0.63 0 -4 -11 41.51 4.32 0 4 -11 42.34 3.94 0 -4 -12 21.25 3.34 0 4 -12 24.78 3.17 0 -4 -13 0.44 0.96 0 -5 0 0.04 0.10 0 5 0 2.42 0.74 0 5 1 10.44 1.31 0 5 -1 11.11 1.15 0 -5 1 9.48 0.82 0 -5 -1 9.47 0.63 0 5 2 55.72 2.93 0 -5 2 54.92 2.64 0 5 -2 50.85 2.54 0 -5 -2 46.55 1.83 0 5 -3 41.99 2.21 0 -5 3 47.59 2.89 0 -5 -3 39.76 1.91 0 5 3 46.09 2.70 0 5 4 124.60 5.12 0 5 -4 129.18 4.45 0 5 -5 6.17 0.98 0 5 5 5.91 1.04 0 5 6 10.28 1.35 0 5 -6 11.40 1.46 0 5 -7 1.93 0.70 0 5 7 2.24 0.75 0 -5 -7 1.43 0.75 0 5 8 6.85 1.20 0 5 -8 6.17 1.29 0 -5 -8 5.49 1.47 0 -5 -9 2.19 1.15 0 5 9 2.11 0.76 0 5 -9 0.46 0.52 0 -5 -10 6.25 1.59 0 5 -10 6.42 1.53 0 5 -11 4.57 1.31 0 -5 -11 2.04 1.22 0 5 -12 20.61 2.97 0 -5 -12 13.96 2.93 0 -5 -13 -1.94 1.30 0 6 0 6.32 1.03 0 -6 0 5.68 0.57 0 -6 -1 258.27 6.50 0 -6 1 248.71 7.11 0 6 1 240.33 8.15 0 6 -1 243.28 7.98 0 6 2 30.24 2.31 0 -6 -2 34.15 1.48 0 6 -2 32.07 2.15 0 -6 2 35.37 2.18 0 -6 3 7.44 1.19 0 6 -3 7.72 0.98 0 -6 -3 8.44 0.77 0 6 3 7.13 1.13 0 6 4 0.66 0.49 0 6 -4 1.24 0.43 0 -6 -4 1.00 0.40 0 6 5 57.10 3.47 0 6 -5 54.30 2.75 0 6 6 40.97 2.96 0 6 -6 42.76 3.01 0 6 -7 6.16 1.25 0 6 7 5.52 1.12 0 6 8 4.34 1.04 0 6 -8 2.80 0.91 0 6 9 25.79 2.50 0 6 -9 26.21 2.78 0 6 -10 7.67 1.63 0 -6 -11 3.03 1.35 0 6 -11 2.63 1.00 0 6 -12 -0.38 0.74 0 -6 -12 0.68 0.97 0 7 0 0.30 0.47 0 -7 0 0.11 0.15 0 -7 -1 1.21 0.27 0 7 -1 1.33 0.52 0 -7 1 1.35 0.40 0 7 1 1.41 0.63 0 -7 -2 12.94 0.89 0 7 -2 11.68 1.39 0 7 2 10.69 1.46 0 -7 2 13.17 1.36 0 -7 -3 20.48 1.23 0 -7 3 21.82 2.05 0 7 -3 20.36 1.75 0 7 3 19.60 2.00 0 -7 -4 4.63 0.66 0 7 -4 3.11 0.69 0 7 4 3.15 0.88 0 7 5 67.91 4.12 0 7 -5 76.74 3.64 0 7 -6 33.48 2.71 0 7 6 30.35 2.71 0 7 -7 98.80 5.25 0 7 7 95.17 5.12 0 7 -8 18.98 2.30 0 7 8 15.99 2.01 0 7 9 44.12 3.47 0 7 -9 48.24 3.94 0 7 10 6.26 1.32 0 7 -10 7.15 1.66 0 7 -11 2.05 0.99 0 8 0 23.43 2.23 0 8 1 2.49 0.81 0 8 -1 2.35 0.73 0 8 2 4.73 1.07 0 8 -2 4.23 0.90 0 8 3 4.73 1.09 0 8 -3 2.92 0.76 0 8 4 43.78 3.28 0 8 -4 41.92 2.83 0 8 5 13.07 1.79 0 8 -5 12.02 1.45 0 8 6 5.99 1.30 0 8 -6 6.01 1.21 0 8 7 51.51 3.83 0 8 -7 57.19 3.98 0 8 -8 -1.02 0.69 0 8 8 -0.07 0.37 0 8 9 2.61 0.92 0 8 -9 2.46 0.96 0 8 -10 0.95 0.73 0 8 10 1.99 0.95 0 8 -11 2.18 1.18 0 9 0 0.30 0.44 0 9 -1 8.89 1.45 0 9 1 6.25 1.33 0 9 -2 21.46 2.16 0 9 2 21.65 2.36 0 9 -3 118.15 5.50 0 9 3 120.89 6.02 0 9 4 0.05 0.49 0 9 -4 0.20 0.39 0 9 5 22.72 2.50 0 9 6 22.77 2.55 0 9 -6 23.20 2.46 0 9 7 4.21 1.15 0 9 -7 5.16 1.19 0 9 -8 0.73 0.66 0 9 8 -0.38 0.51 0 9 9 0.25 0.55 0 9 -9 1.21 0.78 0 9 10 13.07 2.09 0 9 -10 8.53 1.96 0 10 0 30.29 2.80 0 10 -1 62.00 4.06 0 10 1 59.40 4.07 0 10 2 0.16 0.57 0 10 -2 -1.05 0.57 0 10 3 22.43 2.54 0 10 -3 25.67 2.48 0 10 4 1.88 0.74 0 10 -4 2.00 0.72 0 10 5 0.81 0.60 0 10 6 19.48 2.48 0 10 -6 17.55 2.21 0 10 7 15.90 2.28 0 10 -7 16.27 2.21 0 10 8 -0.10 0.42 0 10 -8 -0.26 0.63 0 10 9 -0.07 0.51 0 10 -9 1.71 1.00 0 11 0 -0.28 0.47 0 11 1 22.91 2.61 0 11 -1 22.62 2.52 0 11 2 20.63 2.48 0 11 -2 19.24 2.28 0 11 3 7.87 1.63 0 11 -3 9.80 1.64 0 11 4 11.96 1.99 0 11 5 10.75 1.88 0 11 6 1.10 0.82 0 11 7 -1.16 0.77 0 12 0 2.04 0.88 0 12 1 2.92 1.03 0 12 -1 2.49 0.94 0 12 2 0.97 0.78 0 12 -2 1.15 0.70 0 12 -3 0.15 0.44 0 12 3 -1.09 0.72 0 12 4 0.87 0.72 0 13 0 -0.17 0.47 0 13 -1 -0.12 0.53 0 13 -2 8.98 1.76 1 0 -13 100.67 7.01 1 0 -12 0.25 0.91 1 0 -11 50.13 4.12 1 0 -10 0.19 0.56 1 0 -9 6.76 1.34 1 0 -8 -0.21 0.39 1 0 -7 88.60 4.36 1 0 -6 0.45 0.45 1 0 -5 51.38 2.70 1 0 -4 -0.12 0.27 1 0 -3 263.63 7.22 1 0 -2 0.03 0.14 1 0 -1 0.11 0.06 1 0 0 0.00 0.01 1 0 1 14.52 0.84 1 0 2 0.22 0.28 -1 0 -2 0.11 0.17 1 0 3 0.71 0.13 -1 0 -3 1.94 0.42 1 0 4 0.07 0.10 -1 0 -4 -0.02 0.22 -1 0 -5 9.77 1.27 1 0 5 6.78 0.54 1 0 6 -0.06 0.10 -1 0 -6 -0.04 0.43 -1 0 -7 284.15 9.66 -1 0 -8 0.53 0.60 -1 0 -9 70.67 4.47 -1 0 -10 -0.74 0.73 -1 0 -11 39.19 3.63 -1 0 -12 0.25 0.84 -1 0 -13 -0.01 0.64 1 -1 -13 -1.37 1.02 1 1 -13 -0.08 0.56 1 1 -12 14.34 2.34 1 -1 -12 11.76 2.39 1 -1 -11 39.53 3.93 1 1 -11 47.60 3.92 1 1 -10 -0.55 0.66 1 -1 -10 -0.46 0.68 1 1 -9 14.04 1.86 1 -1 -9 11.95 1.89 1 1 -8 8.82 1.39 1 -1 -8 5.33 1.20 1 -1 -7 1.41 0.61 1 1 -7 0.57 0.40 1 1 -6 8.89 1.20 1 -1 -6 6.13 1.08 1 1 -5 -0.02 0.35 1 -1 -5 0.71 0.48 1 -1 -4 59.91 2.90 1 1 -4 62.79 2.83 1 -1 -3 143.70 4.57 1 1 -3 127.55 4.26 1 -1 -2 97.29 3.26 1 1 -2 95.91 2.99 1 -1 -1 8.97 0.53 1 1 -1 9.32 0.48 1 -1 0 15.32 0.67 1 1 0 15.47 0.78 1 -1 1 10.84 0.72 1 1 1 10.14 0.63 -1 -1 -1 10.22 0.57 1 1 2 422.42 10.29 1 -1 2 448.44 11.24 -1 -1 -2 418.50 10.56 -1 -1 -3 120.19 4.07 1 -1 3 120.36 4.76 1 1 3 120.77 3.56 -1 1 -3 119.86 4.06 -1 -1 -4 442.54 11.83 1 1 4 431.97 10.83 -1 1 -4 444.73 11.82 -1 -1 -5 22.01 1.79 1 1 5 19.82 1.19 -1 1 -5 20.92 1.74 -1 1 -6 23.63 1.98 1 1 6 25.52 1.43 -1 -1 -6 24.29 2.02 -1 -1 -7 12.48 1.58 -1 1 -7 12.26 1.60 1 1 7 13.39 1.05 -1 1 -8 4.99 1.20 -1 -1 -8 4.08 1.02 -1 1 -9 9.51 1.66 -1 -1 -9 8.12 1.54 -1 -1 -10 18.93 2.42 -1 1 -10 23.71 2.74 -1 1 -11 69.82 4.89 -1 -1 -11 57.58 4.59 -1 -1 -12 9.28 2.06 -1 1 -12 5.40 1.50 -1 1 -13 5.20 1.49 -1 -1 -13 3.10 1.34 1 -2 -13 5.05 1.74 1 2 -13 4.99 1.53 1 -2 -12 1.68 1.07 1 2 -12 1.55 0.90 1 -2 -11 2.57 1.16 1 2 -11 2.33 1.00 1 2 -10 0.04 0.44 1 -2 -10 0.90 0.70 1 -2 -9 2.69 1.06 1 2 -9 -0.14 0.47 1 2 -8 14.33 1.80 1 -2 -8 13.70 1.93 1 -2 -7 49.40 3.40 1 2 -7 50.70 3.25 1 2 -6 11.71 1.39 1 -2 -6 12.70 1.56 1 -2 -5 0.42 0.32 1 2 -5 -0.21 0.43 1 2 -4 18.75 1.41 1 -2 -4 20.82 1.69 1 2 -3 13.96 1.05 1 -2 -3 13.49 1.21 1 2 -2 229.14 6.04 1 -2 -1 154.14 4.07 1 2 -1 156.75 4.40 1 -2 0 1.50 0.22 1 2 0 2.23 0.37 -1 -2 -1 15.38 0.82 1 -2 1 12.31 0.83 1 2 1 13.31 0.95 1 2 2 137.21 4.24 1 -2 2 136.82 4.60 -1 2 -2 137.15 3.68 -1 -2 -2 135.88 4.17 1 -2 3 124.03 4.73 1 2 3 115.59 3.67 -1 -2 -3 111.79 3.79 -1 -2 -4 655.11 16.33 -1 2 -4 638.78 16.40 1 2 4 624.04 15.74 1 2 5 21.08 1.43 -1 2 -5 17.88 1.61 -1 -2 -5 19.78 1.68 1 2 6 44.00 2.26 -1 2 -6 43.81 2.80 -1 -2 -6 46.27 2.88 -1 -2 -7 10.02 1.43 1 2 7 9.75 1.01 -1 2 -7 6.36 1.15 -1 -2 -8 5.14 1.16 -1 2 -8 5.26 1.13 -1 2 -9 0.96 0.58 -1 -2 -9 -0.05 0.63 -1 2 -10 14.70 2.17 -1 -2 -10 8.63 1.81 -1 -2 -11 9.93 2.06 -1 2 -11 10.11 1.93 -1 -2 -12 30.91 3.76 -1 2 -12 47.87 4.29 -1 2 -13 1.77 0.88 -1 -2 -13 3.37 1.31 1 3 -13 9.48 1.94 1 -3 -13 8.17 2.19 1 3 -12 13.72 2.28 1 -3 -12 17.42 2.84 1 3 -11 1.65 0.91 1 -3 -11 2.46 1.13 1 -3 -10 4.94 1.50 1 3 -10 6.99 1.51 1 3 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-0.78 0.96 1 4 -13 10.64 2.11 1 -4 -13 8.50 2.16 1 -4 -12 5.21 1.83 1 4 -12 8.67 1.88 1 4 -11 2.68 1.13 1 -4 -11 3.22 1.26 1 -4 -10 22.53 2.99 1 4 -10 19.85 2.53 1 4 -9 4.22 1.14 -1 4 9 4.10 0.96 1 -4 -9 5.69 1.47 1 -4 -8 -0.05 0.55 -1 4 8 0.68 0.54 1 4 -8 1.12 0.72 1 -4 -7 38.94 3.36 1 4 -7 44.61 3.03 1 -4 -6 1.50 0.71 1 4 -6 0.42 0.30 1 4 -5 12.52 1.32 1 4 -4 101.12 3.96 1 -4 -3 35.01 1.78 1 4 -3 39.80 2.03 1 -4 -2 26.15 1.30 1 4 -2 25.05 1.59 1 4 -1 500.78 13.41 -1 -4 1 537.96 12.80 1 -4 -1 530.41 12.56 -1 4 1 515.97 13.75 1 4 0 346.43 9.30 -1 -4 0 322.94 7.73 -1 4 0 347.43 9.32 1 -4 0 336.07 8.33 1 -4 1 0.00 0.14 -1 4 -1 -0.16 0.23 1 4 1 0.01 0.27 -1 -4 -1 0.34 0.12 1 4 2 48.07 2.52 1 -4 2 46.83 2.36 -1 4 -2 44.47 2.15 1 4 3 4.83 0.78 1 -4 3 4.03 0.81 -1 4 -3 4.11 0.56 1 -4 4 42.55 2.98 -1 -4 -4 34.94 2.43 1 4 4 40.34 2.41 -1 4 -4 42.70 1.84 1 4 5 19.64 1.71 -1 -4 -5 20.46 1.96 -1 -4 -6 57.71 3.74 1 4 6 57.34 3.12 -1 4 -6 54.43 3.36 -1 4 -7 4.51 1.02 -1 -4 -7 4.17 1.18 1 4 7 3.94 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-1 0 -0.37 0.51 11 1 0 0.29 0.43 11 -1 1 4.11 1.14 11 1 1 3.74 1.08 11 -1 2 5.27 1.30 11 1 2 4.87 1.24 11 -1 3 18.58 2.57 11 1 3 19.08 2.58 11 -1 4 18.65 2.80 11 1 4 17.26 2.63 11 -1 5 1.72 1.06 11 1 5 1.47 1.00 11 1 6 1.46 1.05 11 2 -12 12.12 2.03 11 2 -11 -0.33 0.47 11 2 -10 25.94 2.74 11 -2 -10 28.36 3.02 11 2 -9 3.87 1.01 11 -2 -9 3.78 1.13 11 2 -8 2.76 0.83 11 -2 -8 2.46 0.87 11 2 -7 1.62 0.70 11 -2 -7 2.59 0.88 11 2 -6 6.12 1.11 11 -2 -6 5.85 1.21 11 -2 -5 3.92 0.98 11 2 -5 4.61 0.95 11 -2 -4 -0.18 0.41 11 2 -4 -0.66 0.44 11 -2 -3 1.42 0.69 11 2 -3 1.13 0.51 11 -2 -2 0.81 0.63 11 2 -2 -0.28 0.36 11 -2 -1 8.22 1.43 11 2 -1 8.26 1.31 11 -2 0 28.47 2.76 11 -2 1 0.86 0.73 11 -2 2 8.51 1.66 11 -2 3 8.14 1.68 11 -2 4 0.43 0.71 11 -2 5 1.50 0.94 11 -3 -10 0.44 0.60 11 -3 -9 9.89 1.80 11 -3 -8 -0.48 0.53 11 -3 -7 6.84 1.39 11 -3 -6 8.97 1.56 11 -3 -5 26.81 2.59 11 -3 -4 -1.14 0.61 11 -3 -3 18.42 2.09 11 -3 -2 2.58 0.85 11 -3 -1 13.88 1.90 11 -3 0 25.18 2.66 11 -3 1 12.29 1.94 11 -3 2 1.46 0.82 11 -3 3 1.37 0.83 11 -3 4 16.78 2.58 11 -4 -9 4.80 1.29 11 -4 -8 11.54 1.91 11 -4 -7 0.64 0.55 11 -4 -6 4.72 1.19 11 -4 -5 20.48 2.33 11 -4 -4 8.28 1.51 11 -4 -3 1.03 0.62 11 -4 -2 20.52 2.32 11 -4 -1 15.03 2.04 11 -4 0 5.78 1.30 11 -4 1 20.16 2.53 11 -4 2 0.29 0.62 11 -4 3 1.36 0.85 11 -5 -8 13.11 2.04 11 -5 -7 -0.18 0.46 11 -5 -6 2.98 0.98 11 -5 -5 1.98 0.75 11 -5 -4 2.62 0.93 11 -5 -3 29.21 2.82 11 -5 -2 0.82 0.73 11 -5 -1 2.31 0.80 11 -5 0 19.78 2.48 11 -5 1 0.77 0.66 11 -5 2 20.56 2.70 11 -6 -7 0.48 0.54 11 -6 -6 22.97 2.64 11 -6 -5 11.51 1.79 11 -6 -4 0.30 0.42 11 -6 -3 -0.14 0.41 11 -6 -2 -0.73 0.58 11 -6 -1 0.14 0.56 11 -6 0 11.83 2.00 11 -6 1 38.43 3.68 11 -7 -5 35.71 3.30 11 -7 -4 1.39 0.62 11 -7 -3 1.71 0.68 11 -7 -2 0.11 0.62 11 -7 -1 17.88 2.41 12 0 -10 56.04 4.30 12 0 -9 1.14 0.70 12 0 -8 30.40 2.92 12 0 -7 -0.74 0.55 12 0 -6 0.79 0.55 12 0 -5 -0.10 0.31 12 0 -4 0.65 0.49 12 0 -3 0.12 0.36 12 0 -2 15.56 1.95 12 0 -1 -0.31 0.46 12 0 0 80.30 5.05 12 0 1 0.76 0.63 12 0 2 0.96 0.71 12 0 3 0.69 0.68 12 0 4 0.20 0.71 12 1 -11 0.74 0.70 12 1 -10 -1.64 0.82 12 -1 -10 -0.91 0.82 12 1 -9 25.85 2.72 12 -1 -9 25.94 2.84 12 1 -8 5.00 1.17 12 -1 -8 5.83 1.30 12 1 -7 0.08 0.35 12 -1 -7 0.84 0.58 12 -1 -6 0.67 0.53 12 1 -6 -0.46 0.48 12 -1 -5 1.69 0.70 12 1 -5 1.14 0.57 12 -1 -4 7.12 1.28 12 1 -4 5.17 1.08 12 1 -3 -1.66 0.69 12 -1 -3 0.43 0.48 12 -1 -2 26.28 2.61 12 1 -2 28.67 2.67 12 -1 -1 0.12 0.44 12 1 -1 0.12 0.40 12 -1 0 14.01 2.06 12 1 0 10.30 1.72 12 -1 1 11.92 1.95 12 1 1 9.98 1.73 12 -1 2 12.79 2.13 12 1 2 11.89 2.06 12 -1 3 20.04 2.82 12 -1 4 38.45 4.18 12 -2 -9 -0.29 0.54 12 -2 -8 8.76 1.67 12 -2 -7 3.32 1.00 12 -2 -6 2.65 0.82 12 -2 -5 11.56 1.77 12 -2 -4 1.73 0.68 12 -2 -3 4.48 1.12 12 -2 -2 0.09 0.42 12 -2 -1 20.74 2.46 12 -2 0 13.46 2.09 12 -2 1 21.04 2.62 12 -2 2 0.97 0.88 12 -2 3 -0.62 0.69 12 -3 -8 5.89 1.41 12 -3 -7 12.70 1.98 12 -3 -6 15.48 2.13 12 -3 -5 0.82 0.60 12 -3 -4 0.07 0.40 12 -3 -3 -0.04 0.48 12 -3 -2 -0.34 0.50 12 -3 -1 36.18 3.32 12 -3 0 1.60 0.79 12 -3 1 -0.27 0.57 12 -3 2 1.55 0.86 12 -4 -7 -0.84 0.62 12 -4 -6 4.29 1.18 12 -4 -5 7.75 1.52 12 -4 -4 1.62 0.77 12 -4 -3 -0.40 0.51 12 -4 -2 0.67 0.69 12 -4 -1 44.98 3.81 12 -4 0 16.40 2.39 12 -4 1 0.56 0.65 12 -5 -6 0.23 0.55 12 -5 -5 5.49 1.36 12 -5 -4 9.04 1.64 12 -5 -3 16.43 2.25 12 -5 -2 10.10 1.80 12 -5 -1 0.58 0.48 12 -5 0 5.83 1.49 13 0 -9 10.70 1.88 13 0 -8 -0.71 0.56 13 0 -7 1.57 0.78 13 0 -6 -1.34 0.72 13 0 -5 66.78 4.42 13 0 -4 0.55 0.57 13 0 -3 31.49 2.97 13 0 -2 -1.47 0.77 13 0 -1 20.01 2.51 13 0 0 0.07 0.48 13 0 1 5.93 1.41 13 0 2 -1.62 0.94 13 1 -9 12.16 2.01 13 1 -8 1.60 0.76 13 -1 -8 1.16 0.79 13 -1 -7 0.73 0.61 13 1 -7 1.84 0.75 13 -1 -6 1.59 0.78 13 1 -6 -0.40 0.47 13 -1 -5 1.09 0.61 13 1 -5 -0.01 0.38 13 -1 -4 1.00 0.65 13 1 -4 0.10 0.39 13 -1 -3 -0.29 0.49 13 -1 -2 7.03 1.50 13 -1 -1 28.54 3.05 13 -1 0 2.17 0.93 13 -1 1 13.49 2.18 13 -1 2 0.69 0.72 13 -2 -7 7.26 1.53 13 -2 -6 12.32 1.95 13 -2 -5 5.23 1.29 13 -2 -4 4.49 1.17 13 -2 -3 6.73 1.44 13 -2 -2 0.59 0.60 13 -2 -1 -0.72 0.64 13 -2 0 32.47 3.41 13 -2 1 4.16 1.33 13 -3 -6 22.87 2.71 13 -3 -5 38.75 3.50 13 -3 -4 4.33 1.19 13 -3 -3 0.62 0.62 13 -3 -2 -0.36 0.57 13 -3 -1 38.51 3.67 14 0 -7 0.14 0.50 14 0 -6 16.01 2.23 14 0 -5 -2.24 0.93 14 0 -4 37.33 3.44 14 0 -3 -2.08 0.92 14 0 -2 84.70 5.53 14 0 -1 -0.54 0.65 14 -1 -5 15.60 2.23 14 -1 -4 5.51 1.41 14 -1 -3 1.90 0.90 14 -1 -2 2.24 0.95 0 0 0 0.00 0.00 TITL exp_858 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.71073 10.848521 10.171718 11.285072 90.0000 104.8118 90.0000 ZERR 5.00 0.000776 0.000635 0.001070 0.0000 0.0093 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O UNIT 55.00 50.00 5.00 5.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 25292 _shelx_res_file ; TITL exp_858 hx2_20k.res created by SHELXL-2016/4 at 19:07:33 on 08-Apr-2019 CELL 0.71073 10.848521 10.171718 11.285072 90 104.8118 90 ZERR 4 0.000776 0.000635 0.00107 0 0.0093 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 20 48 24 40 EQIV $1 -0.5+X,1.5-Y,-0.5+Z EQIV $2 0.5+X,0.5-Y,0.5+Z EQIV $3 0.5+X,1.5-Y,0.5+Z EQIV $4 1.5-X,0.5+Y,0.5-Z EQIV $5 +X,-1+Y,+Z L.S. 4 0 0 PLAN 20 SIZE 0.178 0.1 0.09 TEMP 20 HTAB C2 O6_$2 HTAB O1 O6_$2 HTAB N1 O12_$5 HTAB C2 O12_$5 HTAB C8 O1_$1 HTAB N1 O11_$5 HTAB N7 O12_$1 HTAB N7 O13_$1 HTAB N9 O11 HTAB N9 O13 HTAB O1 N3 HTAB O2 O1 HTAB O2 O23_$3 HTAB O2 O3 HTAB O3 O21_$4 HTAB O3 O22_$4 HTAB O3 O23 BOND $H CONF fmap 2 53 acta REM REM REM WGHT 0.054200 0.589700 FVAR 0.23364 O6 4 0.296866 0.226344 0.130915 11.00000 0.00870 0.00957 = 0.01541 -0.00299 0.00081 -0.00239 N1 3 0.467795 0.243994 0.300046 11.00000 0.00760 0.00987 = 0.01411 0.00148 0.00230 -0.00003 H1 2 0.476359 0.148299 0.302517 11.00000 0.03242 N3 3 0.559066 0.443035 0.390267 11.00000 0.00788 0.01068 = 0.01449 0.00018 0.00397 0.00033 N7 3 0.304251 0.533360 0.137691 11.00000 0.00627 0.01052 = 0.01280 0.00094 0.00122 0.00061 H7 2 0.231101 0.524722 0.066229 11.00000 0.05060 N9 3 0.447203 0.633313 0.281531 11.00000 0.00968 0.00680 = 0.01305 -0.00128 0.00329 -0.00080 H9 2 0.488710 0.697525 0.327845 11.00000 0.01927 C2 1 0.554585 0.314938 0.384727 11.00000 0.00537 0.01348 = 0.01348 0.00100 0.00358 -0.00033 H2 2 0.614137 0.263819 0.443638 11.00000 0.01483 C4 1 0.466683 0.500293 0.299957 11.00000 0.00844 0.00767 = 0.01367 0.00099 0.00510 0.00144 C5 1 0.376967 0.436869 0.210080 11.00000 0.00767 0.00933 = 0.01350 -0.00067 0.00374 0.00085 C6 1 0.371984 0.297362 0.204194 11.00000 0.00620 0.01330 = 0.01142 0.00106 0.00419 0.00152 C8 1 0.349046 0.649517 0.182826 11.00000 0.00588 0.01197 = 0.01259 0.00085 0.00307 0.00125 H8 2 0.316332 0.734362 0.149847 11.00000 0.00714 N11 3 0.552990 0.927109 0.391704 11.00000 0.00726 0.01048 = 0.01492 0.00042 0.00399 0.00080 O12 4 0.610717 1.028167 0.443186 11.00000 0.00981 0.00926 = 0.01596 -0.00263 0.00133 -0.00363 O11 4 0.461904 0.939356 0.299221 11.00000 0.00949 0.01554 = 0.01321 0.00077 -0.00186 0.00077 O13 4 0.589552 0.815592 0.435042 11.00000 0.01226 0.00835 = 0.01482 0.00184 0.00109 0.00193 O1 4 0.784171 0.541529 0.556312 11.00000 0.01087 0.01368 = 0.01566 0.00282 -0.00096 -0.00063 H1A 2 0.720940 0.528804 0.491584 11.00000 0.06681 H1B 2 0.807266 0.464280 0.593004 11.00000 0.03474 O2 4 0.964651 0.644819 0.479898 11.00000 0.00896 0.01114 = 0.01613 0.00273 0.00128 0.00104 H2A 2 0.905066 0.595910 0.504062 11.00000 0.04050 H2B 2 0.927099 0.704783 0.441850 11.00000 0.05595 H2C 2 1.041226 0.646081 0.545216 11.00000 0.04651 O3 4 0.863723 0.841148 0.369473 11.00000 0.01480 0.00790 = 0.01972 -0.00123 -0.00155 -0.00168 H3A 2 0.876007 0.911664 0.388412 11.00000 0.00527 H3B 2 0.795134 0.840885 0.302789 11.00000 0.06609 N21 3 0.666615 0.661053 0.163433 11.00000 0.00807 0.00948 = 0.01667 -0.00084 0.00436 -0.00238 O21 4 0.739857 0.602419 0.248385 11.00000 0.01039 0.01327 = 0.01588 0.00326 -0.00283 0.00059 O22 4 0.595033 0.600955 0.074163 11.00000 0.01136 0.01252 = 0.01475 -0.00335 -0.00068 -0.00213 O23 4 0.660116 0.788007 0.164254 11.00000 0.01035 0.00921 = 0.01748 -0.00117 0.00065 0.00152 HKLF 4 REM exp_858 REM R1 = 0.0496 for 2002 Fo > 4sig(Fo) and 0.0714 for all 2640 data REM 238 parameters refined using 0 restraints END WGHT 0.0542 0.5915 REM Highest difference peak 0.351, deepest hole -0.335, 1-sigma level 0.081 Q1 1 0.6187 0.8614 0.3890 11.00000 0.05 0.35 Q2 1 0.7380 0.6847 0.2781 11.00000 0.05 0.34 Q3 1 0.9011 0.5010 0.4460 11.00000 0.05 0.32 Q4 1 0.7568 0.4666 0.2656 11.00000 0.05 0.30 Q5 1 0.4432 0.5731 0.3130 11.00000 0.05 0.29 Q6 1 0.3980 0.3697 0.1807 11.00000 0.05 0.28 Q7 1 0.8998 0.6372 0.5178 11.00000 0.05 0.28 Q8 1 0.3363 0.4761 0.1822 11.00000 0.05 0.27 Q9 1 0.8667 0.6033 0.2378 11.00000 0.05 0.26 Q10 1 0.9566 0.5721 0.4389 11.00000 0.05 0.26 Q11 1 0.5396 0.3772 0.4093 11.00000 0.05 0.26 Q12 1 0.5984 0.4546 0.4389 11.00000 0.05 0.26 Q13 1 0.5457 0.8637 0.4794 11.00000 0.05 0.25 Q14 1 0.4597 0.8529 0.2798 11.00000 0.05 0.25 Q15 1 0.8077 0.6021 0.4964 11.00000 0.05 0.25 Q16 1 0.7147 0.5656 0.5995 11.00000 0.05 0.25 Q17 1 0.8489 0.9559 0.3510 11.00000 0.05 0.25 Q18 1 1.0065 0.6605 0.5458 11.00000 0.05 0.25 Q19 1 0.3591 0.3810 0.2288 11.00000 0.05 0.25 Q20 1 0.6485 1.0153 0.5151 11.00000 0.05 0.25 ; _shelx_res_checksum 91678 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 O O6 0.29687(15) 0.22634(16) 0.13091(16) 0.0116(4) Uani d 1 N N1 0.46780(19) 0.2440(2) 0.30005(19) 0.0106(5) Uani d 1 H H1 0.476(3) 0.148(3) 0.303(3) 0.032(9) Uiso d 1 N N3 0.55907(19) 0.44304(19) 0.3903(2) 0.0108(5) Uani d 1 N N7 0.30425(19) 0.5334(2) 0.1377(2) 0.0101(4) Uani d 1 H H7 0.231(4) 0.525(4) 0.066(4) 0.051(11) Uiso d 1 N N9 0.44720(19) 0.6333(2) 0.2815(2) 0.0098(4) Uani d 1 H H9 0.489(3) 0.698(3) 0.328(3) 0.019(8) Uiso d 1 C C2 0.5546(2) 0.3149(2) 0.3847(2) 0.0106(5) Uani d 1 H H2 0.614(3) 0.264(3) 0.444(3) 0.015(7) Uiso d 1 C C4 0.4667(2) 0.5003(2) 0.3000(2) 0.0095(5) Uani d 1 C C5 0.3770(2) 0.4369(2) 0.2101(2) 0.0100(5) Uani d 1 C C6 0.3720(2) 0.2974(2) 0.2042(2) 0.0100(5) Uani d 1 C C8 0.3490(2) 0.6495(2) 0.1828(2) 0.0100(5) Uani d 1 H H8 0.316(2) 0.734(3) 0.150(2) 0.007(6) Uiso d 1 N N11 0.55299(19) 0.92711(19) 0.3917(2) 0.0107(5) Uani d 1 O O12 0.61072(16) 1.02817(16) 0.44319(16) 0.0120(4) Uani d 1 O O11 0.46190(16) 0.93936(17) 0.29922(16) 0.0136(4) Uani d 1 O O13 0.58955(16) 0.81559(16) 0.43504(16) 0.0122(4) Uani d 1 O O1 0.78417(18) 0.54153(19) 0.55631(18) 0.0142(4) Uani d 1 H H1A 0.721(4) 0.529(4) 0.492(4) 0.067(14) Uiso d 1 H H1B 0.807(3) 0.464(4) 0.593(3) 0.035(10) Uiso d 1 O O2 0.96465(18) 0.64482(19) 0.47990(18) 0.0124(4) Uani d 1 H H2A 0.905(4) 0.596(3) 0.504(3) 0.040(10) Uiso d 1 H H2B 0.927(4) 0.705(4) 0.442(4) 0.056(13) Uiso d 1 H H2C 1.041(4) 0.646(3) 0.545(4) 0.047(11) Uiso d 1 O O3 0.86372(19) 0.84115(19) 0.36947(19) 0.0152(4) Uani d 1 H H3A 0.876(3) 0.912(3) 0.388(3) 0.005(7) Uiso d 1 H H3B 0.795(4) 0.841(4) 0.303(4) 0.066(14) Uiso d 1 N N21 0.66662(19) 0.6611(2) 0.1634(2) 0.0112(5) Uani d 1 O O21 0.73986(16) 0.60242(17) 0.24839(16) 0.0143(4) Uani d 1 O O22 0.59503(16) 0.60095(17) 0.07416(16) 0.0136(4) Uani d 1 O O23 0.66012(16) 0.78801(16) 0.16425(16) 0.0129(4) Uani 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 O6 0.0087(8) 0.0096(8) 0.0154(9) -0.0024(7) 0.0008(7) -0.0030(7) N1 0.0076(10) 0.0099(10) 0.0141(11) 0.0000(8) 0.0023(8) 0.0015(8) N3 0.0079(10) 0.0107(10) 0.0145(11) 0.0003(8) 0.0040(9) 0.0002(8) N7 0.0063(10) 0.0105(10) 0.0128(11) 0.0006(8) 0.0012(8) 0.0009(8) N9 0.0097(10) 0.0068(10) 0.0130(11) -0.0008(8) 0.0033(9) -0.0013(8) C2 0.0054(11) 0.0135(12) 0.0135(13) -0.0003(10) 0.0036(10) 0.0010(10) C4 0.0084(11) 0.0077(11) 0.0137(12) 0.0014(9) 0.0051(9) 0.0010(9) C5 0.0077(12) 0.0093(12) 0.0135(12) 0.0009(9) 0.0037(10) -0.0007(10) C6 0.0062(11) 0.0133(12) 0.0114(12) 0.0015(10) 0.0042(9) 0.0011(10) C8 0.0059(11) 0.0120(12) 0.0126(13) 0.0013(10) 0.0031(10) 0.0008(10) N11 0.0073(10) 0.0105(10) 0.0149(11) 0.0008(8) 0.0040(9) 0.0004(8) O12 0.0098(8) 0.0093(8) 0.0160(9) -0.0036(7) 0.0013(7) -0.0026(7) O11 0.0095(9) 0.0155(9) 0.0132(9) 0.0008(7) -0.0019(7) 0.0008(7) O13 0.0123(9) 0.0084(8) 0.0148(9) 0.0019(7) 0.0011(7) 0.0018(7) O1 0.0109(9) 0.0137(9) 0.0157(10) -0.0006(8) -0.0010(8) 0.0028(8) O2 0.0090(9) 0.0111(9) 0.0161(10) 0.0010(8) 0.0013(8) 0.0027(8) O3 0.0148(10) 0.0079(10) 0.0197(11) -0.0017(8) -0.0016(8) -0.0012(8) N21 0.0081(10) 0.0095(10) 0.0167(11) -0.0024(8) 0.0044(9) -0.0008(9) O21 0.0104(9) 0.0133(9) 0.0159(10) 0.0006(7) -0.0028(7) 0.0033(8) O22 0.0114(9) 0.0125(9) 0.0148(10) -0.0021(7) -0.0007(7) -0.0034(7) O23 0.0103(9) 0.0092(9) 0.0175(9) 0.0015(7) 0.0007(7) -0.0012(7) 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 H1 117.6(19) C2 N1 C6 125.3(2) C6 N1 H1 117(2) C2 N3 C4 112.3(2) C5 N7 H7 130(2) C8 N7 H7 122(2) C8 N7 C5 107.8(2) C4 N9 H9 126.9(19) C8 N9 H9 125.2(19) C8 N9 C4 107.8(2) N1 C2 H2 115.0(17) N3 C2 N1 124.9(2) N3 C2 H2 120.0(17) N3 C4 N9 126.0(2) N3 C4 C5 126.7(2) C5 C4 N9 107.3(2) N7 C5 C6 132.1(2) C4 C5 N7 106.9(2) C4 C5 C6 121.0(2) O6 C6 N1 121.4(2) O6 C6 C5 128.8(2) N1 C6 C5 109.8(2) N7 C8 N9 110.1(2) N7 C8 H8 125.6(16) N9 C8 H8 124.3(16) O11 N11 O12 119.8(2) O11 N11 O13 121.3(2) O13 N11 O12 119.0(2) H1A O1 H1B 109(4) H2A O2 H2B 106(3) H2A O2 H2C 109(3) H2B O2 H2C 129(4) H3A O3 H3B 107(3) O21 N21 O22 122.0(2) O21 N21 O23 120.2(2) O22 N21 O23 117.8(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O6 C6 1.235(3) N1 H1 0.98(3) N1 C2 1.364(3) N1 C6 1.404(3) N3 C2 1.305(3) N3 C4 1.364(3) N7 H7 0.98(4) N7 C5 1.387(3) N7 C8 1.329(3) N9 H9 0.88(3) N9 C4 1.377(3) N9 C8 1.340(3) C2 H2 0.95(3) C4 C5 1.374(3) C5 C6 1.421(3) C8 H8 0.97(3) N11 O12 1.265(3) N11 O11 1.247(3) N11 O13 1.259(3) O1 H1A 0.87(5) O1 H1B 0.89(4) O2 H2A 0.91(4) O2 H2B 0.80(4) O2 H2C 0.96(4) O3 H3A 0.75(3) O3 H3B 0.91(5) N21 O21 1.232(3) N21 O22 1.262(3) N21 O23 1.293(3) 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 H1 O12_$5 1_545 0.98(3) 2.23(3) 2.924(3) 127(3) N1 H1 O11_$5 1_545 0.98(3) 2.13(3) 3.099(3) 171(3) N7 H7 O13_$1 4_575 0.98(4) 2.45(4) 3.208(3) 133(3) N7 H7 O12_$1 4_575 0.98(4) 1.73(4) 2.695(3) 167(3) N9 H9 O11 . 0.88(3) 2.49(3) 3.121(3) 129(2) N9 H9 O13 . 0.88(3) 1.85(3) 2.731(3) 173(3) C2 H2 O6_$2 4_666 0.95(3) 2.50(3) 3.327(3) 145(2) C2 H2 O12_$5 1_545 0.95(3) 2.40(3) 3.018(3) 122(2) C8 H8 O1_$1 4_575 0.97(3) 2.50(3) 3.449(3) 166(2) O1 H1A N3 . 0.87(5) 2.03(5) 2.853(3) 156(4) O1 H1B O6_$2 4_666 0.89(4) 2.00(4) 2.845(3) 158(3) O2 H2A O1 . 0.91(4) 1.66(4) 2.558(3) 166(3) O2 H2B O3 . 0.80(4) 1.67(4) 2.458(3) 173(4) O2 H2C O23_$3 4_676 0.96(4) 1.74(4) 2.653(3) 157(3) O3 H3A O22_$4 2_655 0.75(3) 1.98(3) 2.728(3) 176(3) O3 H3A O21_$4 2_655 0.75(3) 2.60(3) 3.055(3) 121(3) O3 H3B O23 . 0.91(5) 1.93(5) 2.814(3) 164(4) 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 N3 C4 C5 N7 -179.1(2) N3 C4 C5 C6 0.7(4) N7 C5 C6 O6 -1.3(5) N7 C5 C6 N1 180.0(2) N9 C4 C5 N7 0.2(3) N9 C4 C5 C6 -180.0(2) C2 N1 C6 O6 179.9(2) C2 N1 C6 C5 -1.3(3) C2 N3 C4 N9 -179.8(2) C2 N3 C4 C5 -0.5(4) C4 N3 C2 N1 -0.6(3) C4 N9 C8 N7 0.4(3) C4 C5 C6 O6 178.9(2) C4 C5 C6 N1 0.3(3) C5 N7 C8 N9 -0.3(3) C6 N1 C2 N3 1.6(4) C8 N7 C5 C4 0.0(3) C8 N7 C5 C6 -179.8(3) C8 N9 C4 N3 179.0(2) C8 N9 C4 C5 -0.4(3) _cod_database_fobs_code 2021703