#------------------------------------------------------------------------------ #$Date: 2018-11-14 05:30:28 +0200 (Wed, 14 Nov 2018) $ #$Revision: 211942 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/27/2242739.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_2242739 loop_ _publ_author_name Asma 'Kalluraya, Balakrishna' 'Yathirajan, Hemmige S.' 'Rathore, Ravindranath S.' 'Glidewell, Christopher' _publ_section_title ; Four 1-aryl-1H-pyrazole-3,4-dicarboxylate derivatives: synthesis, molecular conformation and hydrogen bonding ; _journal_coeditor_code ZL2741 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 1783 _journal_page_last 1789 _journal_paper_doi 10.1107/S2056989018015864 _journal_volume 74 _journal_year 2018 _chemical_formula_iupac 'C12 H14 N6 O3' _chemical_formula_moiety 'C12 H14 N6 O3' _chemical_formula_sum 'C12 H14 N6 O3' _chemical_formula_weight 290.29 _chemical_name_systematic ; 1-(4-Methoxyphenyl)-1H-pyrazole-3,4-dicarbohydrazide ; _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 mixed _audit_creation_method SHELXL-2014 _cell_angle_alpha 90 _cell_angle_beta 102.284(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.6030(6) _cell_length_b 22.6605(19) _cell_length_c 7.6751(7) _cell_measurement_reflns_used 2521 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 26.065 _cell_measurement_theta_min 2.861 _cell_volume 1292.05(19) _computing_cell_refinement ; APEX2/SAINT (Bruker, 2004) ; _computing_data_collection ; APEX2 (Bruker, 2004) ; _computing_data_reduction ; SAINT/XPREP (Bruker, 2004) ; _computing_molecular_graphics ; PLATON (Spek, 2009) ; _computing_publication_material ; SHELXL2014 (Sheldrick, 2015) and PLATON (Spek, 2009) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008b) ; _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device_type 'Bruker Kappa APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_unetI/netI 0.0377 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 20456 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.065 _diffrn_reflns_theta_min 2.861 _diffrn_source 'fine focus sealed tube' _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.112 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_correction_T_min 0.929 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Sheldrick, 2008a) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.492 _exptl_crystal_description block _exptl_crystal_F_000 608 _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.110 _refine_diff_density_max 0.204 _refine_diff_density_min -0.212 _refine_ls_extinction_coef 0.0045(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2014 (Sheldrick, 2015) ; _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 210 _refine_ls_number_reflns 2521 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0457 _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^)+(0.0270P)^2^+1.1086P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0927 _refine_ls_wR_factor_ref 0.1082 _reflns_number_gt 1722 _reflns_number_total 2521 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file zl2741sup1.cif _cod_data_source_block IV _cod_database_code 2242739 _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 0.984 _shelx_estimated_absorpt_t_max 0.988 _shelx_hkl_file ; 1 0 0 0.30 0.60 1 0 0 0.00 1.10 1 0 0 0.90 0.70 1 0 0 0.20 0.70 -1 0 0 -0.20 0.70 -1 0 0 1.40 0.70 -1 0 0 0.80 0.50 -1 0 0 -0.70 1.00 -1 0 0 0.50 0.50 2 0 0 44.70 2.40 2 0 0 41.60 2.90 2 0 0 38.50 3.00 2 0 0 41.30 4.90 -2 0 0 42.50 2.80 -2 0 0 43.30 2.40 -2 0 0 42.40 2.90 -2 0 0 44.00 5.00 -2 0 0 45.00 2.40 3 0 0 2.10 1.90 3 0 0 1.40 2.70 3 0 0 -1.30 1.20 3 0 0 3.00 2.00 -3 0 0 0.40 1.60 -3 0 0 0.30 1.60 -3 0 0 -5.30 2.30 -3 0 0 2.20 1.30 -3 0 0 2.00 1.30 4 0 0 325.87 11.00 4 0 0 315.47 11.00 4 0 0 304.17 9.70 4 0 0 332.97 17.80 -4 0 0 309.77 8.90 -4 0 0 314.57 10.50 -4 0 0 321.07 17.90 -4 0 0 318.47 10.60 -4 0 0 312.87 9.80 5 0 0 -3.90 2.90 5 0 0 -1.00 1.60 5 0 0 -2.60 2.70 -5 0 0 -0.30 1.70 -5 0 0 -0.30 2.10 -5 0 0 0.70 3.20 6 0 0 113.59 8.20 6 0 0 98.49 7.50 -6 0 0 102.79 12.80 -6 0 0 101.79 7.20 -6 0 0 99.09 5.40 -6 0 0 102.39 5.60 7 0 0 -1.20 4.50 -7 0 0 4.40 3.30 -7 0 0 -1.20 4.40 8 0 0 -0.10 5.30 -8 0 0 8.40 6.40 9 0 0 -0.20 5.90 -8 0 -1 4.00 6.00 8 0 1 -1.30 5.60 -7 0 -1 38.60 6.30 7 0 1 37.20 6.90 -6 0 -1 -2.10 1.60 -6 0 -1 0.70 3.20 -6 0 -1 4.40 5.10 6 0 1 -0.90 2.40 6 0 1 -2.40 4.00 6 0 1 2.90 4.20 -5 0 -1 172.78 8.80 -5 0 -1 156.88 5.60 -5 0 -1 152.68 7.30 -5 0 -1 165.38 14.10 5 0 1 162.18 9.20 5 0 1 162.68 9.00 5 0 1 159.18 7.80 -4 0 -1 8.00 3.80 -4 0 -1 7.90 3.70 -4 0 -1 5.40 2.80 -4 0 -1 2.00 2.50 -4 0 -1 2.90 1.40 4 0 1 5.20 3.00 4 0 1 9.60 3.20 -3 0 -1 9.90 2.10 -3 0 -1 10.10 3.90 -3 0 -1 11.60 3.50 -2 0 -1 4.80 1.90 -2 0 -1 0.20 2.30 -2 0 -1 -1.60 1.10 -2 0 -1 2.50 1.70 -2 0 -1 -1.00 1.80 2 0 1 1.50 1.90 2 0 1 2.70 1.70 2 0 1 -0.70 1.80 2 0 1 0.90 2.40 2 0 1 -0.10 1.70 -1 0 -1 113.79 6.20 -1 0 -1 118.69 4.70 -1 0 -1 118.99 6.60 -1 0 -1 122.09 4.60 -1 0 -1 116.79 4.50 1 0 1 107.69 4.70 1 0 1 122.59 6.80 1 0 1 124.09 4.60 1 0 1 118.59 3.30 1 0 1 103.79 5.90 1 0 1 112.79 4.50 0 0 -1 0.90 0.80 0 0 -1 0.40 0.90 0 0 -1 0.30 0.90 0 0 1 2.20 0.90 0 0 1 2.40 1.00 0 0 1 1.40 0.90 1 0 -1 0.60 1.20 1 0 -1 2.00 0.80 -1 0 1 7.40 1.00 -1 0 1 4.10 0.90 2 0 -1 26.40 5.10 3 0 -1 372.86 17.20 3 0 -1 349.27 9.90 3 0 -1 342.47 9.80 -3 0 1 361.66 9.90 -3 0 1 362.66 17.10 -3 0 1 348.97 9.60 -3 0 1 342.07 9.80 4 0 -1 2.20 3.10 4 0 -1 0.40 2.20 4 0 -1 0.60 1.90 -4 0 1 0.90 1.60 -4 0 1 1.40 1.60 -4 0 1 0.70 2.70 -4 0 1 2.40 1.80 -4 0 1 -0.10 1.00 5 0 -1 172.78 8.10 5 0 -1 156.78 7.60 -5 0 1 151.98 13.40 -5 0 1 157.08 7.30 -5 0 1 149.19 7.20 -5 0 1 148.39 5.50 -5 0 1 162.38 7.00 6 0 -1 -1.50 2.80 6 0 -1 -3.30 3.20 -6 0 1 1.80 3.40 -6 0 1 -2.30 0.90 -6 0 1 -1.50 2.10 -6 0 1 -2.20 2.20 7 0 -1 32.50 6.00 -7 0 1 30.20 4.90 -7 0 1 21.00 3.80 -7 0 1 26.20 7.70 8 0 -1 1.80 4.80 -8 0 1 1.40 5.20 9 0 -1 5.30 6.00 -8 0 -2 130.69 19.10 8 0 2 117.39 12.30 -7 0 -2 4.00 5.50 -7 0 -2 -0.50 4.30 7 0 2 9.80 6.20 -6 0 -2 17.30 4.80 6 0 2 16.90 5.80 -5 0 -2 -0.90 3.10 -5 0 -2 -0.30 4.00 5 0 2 0.90 4.00 5 0 2 1.20 3.20 5 0 2 4.30 4.20 -4 0 -2 246.48 16.30 -4 0 -2 253.87 10.50 -4 0 -2 232.08 10.50 4 0 2 231.28 10.50 4 0 2 257.67 11.40 4 0 2 247.38 6.90 4 0 2 250.67 10.90 -3 0 -2 -1.50 2.80 -3 0 -2 1.40 2.30 -3 0 -2 -0.40 2.90 -3 0 -2 -2.50 1.90 -3 0 -2 7.60 2.30 3 0 2 -0.50 3.40 3 0 2 0.70 1.40 3 0 2 -0.70 2.40 3 0 2 1.70 2.70 3 0 2 0.60 2.90 -2 0 -2 138.59 9.40 -2 0 -2 146.69 6.90 -2 0 -2 134.19 6.50 -2 0 -2 165.78 7.30 -2 0 -2 160.88 10.70 2 0 2 157.68 11.10 2 0 2 171.18 7.50 2 0 2 153.28 7.10 2 0 2 149.59 7.20 2 0 2 153.68 4.90 1 0 2 50.69 4.10 0 0 -2 3.20 1.80 0 0 -2 1.30 0.80 0 0 -2 4.50 2.00 0 0 -2 3.90 1.70 0 0 2 3.30 1.70 0 0 2 3.40 1.60 0 0 2 3.90 2.00 0 0 2 4.80 2.10 1 0 -2 0.20 1.20 1 0 -2 1.30 1.40 1 0 -2 -0.50 1.10 -1 0 2 0.40 1.30 -1 0 2 3.10 1.30 -1 0 2 -1.40 0.80 -1 0 2 0.20 1.50 2 0 -2 8.00 2.40 -2 0 2 -0.60 2.00 3 0 -2 4.90 1.60 3 0 -2 4.50 1.80 3 0 -2 -0.20 3.00 -3 0 2 2.80 2.50 4 0 -2 17.90 5.10 4 0 -2 25.80 3.30 4 0 -2 29.50 3.60 -4 0 2 15.90 5.30 -4 0 2 23.60 3.10 -4 0 2 24.80 3.00 5 0 -2 3.80 2.70 5 0 -2 4.20 2.30 -5 0 2 3.00 2.00 -5 0 2 -0.60 1.70 -5 0 2 2.70 1.30 -5 0 2 -0.30 3.40 6 0 -2 60.89 5.50 6 0 -2 64.79 6.20 -6 0 2 67.49 9.90 -6 0 2 66.69 5.60 -6 0 2 57.19 3.10 -6 0 2 57.89 5.00 7 0 -2 3.10 4.00 -7 0 2 6.00 4.60 -7 0 2 0.50 2.60 8 0 -2 49.30 7.30 -8 0 2 68.89 12.90 9 0 -2 2.10 5.40 -9 0 2 4.70 6.10 -7 0 -3 24.10 6.70 7 0 3 19.30 7.40 -6 0 -3 1.40 4.90 -6 0 -3 -0.50 3.90 6 0 3 -1.00 5.60 -5 0 -3 6.50 4.60 -5 0 -3 5.60 5.20 5 0 3 8.40 5.10 -4 0 -3 -1.70 3.50 -4 0 -3 2.70 3.30 4 0 3 5.00 4.40 4 0 3 4.30 3.70 4 0 3 -0.30 1.80 4 0 3 -0.30 4.00 4 0 3 -2.20 3.20 -3 0 -3 58.29 5.70 -3 0 -3 60.29 8.30 -3 0 -3 51.59 8.70 -3 0 -3 49.80 5.80 3 0 3 56.29 3.90 3 0 3 63.99 6.80 3 0 3 74.09 6.90 3 0 3 58.99 10.40 3 0 3 60.89 6.00 -2 0 -3 9.30 3.20 -2 0 -3 6.20 3.60 2 0 3 6.00 3.00 2 0 3 10.50 3.30 -1 0 -3 1066.69 36.80 -1 0 -3 1099.39 27.10 -1 0 -3 1090.09 38.50 -1 0 -3 1056.09 26.90 1 0 3 1114.09 27.10 1 0 3 1111.99 30.40 1 0 3 1074.49 38.90 1 0 3 1078.89 27.10 0 0 -3 -0.30 2.00 0 0 -3 0.30 1.90 0 0 -3 1.50 2.20 0 0 3 0.50 2.00 0 0 3 2.20 2.00 0 0 3 2.40 2.70 0 0 3 -2.40 1.70 1 0 -3 10.90 2.30 1 0 -3 10.40 2.40 1 0 -3 8.40 2.40 -1 0 3 7.30 2.50 -1 0 3 8.50 2.30 2 0 -3 6.60 2.20 2 0 -3 2.70 2.10 2 0 -3 1.10 1.70 -2 0 3 1.40 1.70 -2 0 3 1.70 2.10 -2 0 3 1.60 1.70 -2 0 3 4.50 1.70 3 0 -3 243.58 7.90 3 0 -3 241.78 8.10 3 0 -3 239.38 12.70 -3 0 3 245.68 7.90 -3 0 3 252.77 12.80 -3 0 3 244.78 8.00 4 0 -3 3.30 3.10 4 0 -3 0.20 2.20 4 0 -3 2.30 1.90 -4 0 3 -0.10 1.60 -4 0 3 2.30 1.70 -4 0 3 -2.70 2.40 5 0 -3 5.00 2.40 5 0 -3 11.30 3.30 -5 0 3 8.20 2.40 -5 0 3 5.60 4.00 -5 0 3 7.10 2.40 6 0 -3 0.20 3.20 6 0 -3 1.30 2.60 -6 0 3 3.50 4.00 -6 0 3 0.50 1.70 -6 0 3 1.30 2.10 7 0 -3 122.29 8.40 -7 0 3 116.59 14.10 8 0 -3 -0.20 4.40 9 0 -3 0.80 5.20 -9 0 3 6.90 6.80 -7 0 -4 1.30 5.20 7 0 4 -6.40 6.50 -6 0 -4 214.18 21.30 -6 0 -4 211.88 13.40 6 0 4 197.78 14.70 -5 0 -4 -0.70 3.90 -5 0 -4 11.00 5.80 5 0 4 0.90 1.90 5 0 4 3.40 5.80 -4 0 -4 167.78 14.70 -4 0 -4 162.98 10.90 4 0 4 188.58 17.70 4 0 4 162.68 6.60 4 0 4 171.08 11.20 -3 0 -4 -0.50 3.20 -3 0 -4 0.40 3.20 3 0 4 1.30 2.10 3 0 4 -1.80 5.00 3 0 4 -1.10 4.00 -2 0 -4 29.80 6.20 -2 0 -4 23.30 5.50 -2 0 -4 28.40 4.80 -2 0 -4 32.00 5.30 2 0 4 30.70 5.20 2 0 4 29.30 5.10 2 0 4 48.30 6.20 2 0 4 40.80 4.20 2 0 4 20.60 5.90 -1 0 -4 -0.70 1.80 -1 0 -4 2.30 2.70 -1 0 -4 0.00 2.60 -1 0 -4 0.20 2.40 1 0 4 1.30 3.60 1 0 4 0.90 2.80 1 0 4 3.00 3.20 1 0 4 -2.40 2.30 0 0 -4 895.71 23.80 0 0 -4 895.61 34.00 0 0 4 879.01 23.60 0 0 4 907.01 23.70 0 0 4 908.91 27.10 0 0 4 905.01 34.90 1 0 -4 5.00 2.30 1 0 -4 2.30 2.50 -1 0 4 10.40 3.40 2 0 -4 189.78 7.70 2 0 -4 185.98 8.00 -2 0 4 188.18 12.80 -2 0 4 198.08 7.70 -2 0 4 194.28 9.30 -2 0 4 189.88 7.70 3 0 -4 5.40 2.90 3 0 -4 5.20 2.80 3 0 -4 2.10 2.10 -3 0 4 5.10 2.10 -3 0 4 4.80 2.30 -3 0 4 4.90 2.20 4 0 -4 153.98 11.20 4 0 -4 155.18 6.80 4 0 -4 155.98 7.60 -4 0 4 157.88 6.80 -4 0 4 157.78 11.10 -4 0 4 157.68 6.90 5 0 -4 3.60 3.40 5 0 -4 -0.30 3.60 5 0 -4 -0.30 1.90 -5 0 4 -0.90 2.70 -5 0 4 0.50 1.90 6 0 -4 3.80 2.80 6 0 -4 7.60 4.10 -6 0 4 6.20 4.70 -6 0 4 6.90 2.60 7 0 -4 -1.50 4.00 -7 0 4 -2.50 3.80 8 0 -4 10.20 5.10 -8 0 4 -0.90 5.50 -9 0 4 -3.50 5.10 -6 0 -5 4.80 5.10 6 0 5 3.60 7.40 -5 0 -5 58.69 12.40 -5 0 -5 62.59 9.10 5 0 5 60.39 10.10 5 0 5 84.09 15.50 -4 0 -5 4.40 4.50 -4 0 -5 1.40 4.50 4 0 5 7.40 6.00 4 0 5 7.40 6.50 4 0 5 -0.90 2.60 -3 0 -5 172.58 13.00 -3 0 -5 190.78 11.80 3 0 5 178.58 8.00 3 0 5 181.28 18.40 3 0 5 189.08 11.70 -2 0 -5 3.40 3.10 -2 0 -5 3.40 3.90 2 0 5 2.80 2.50 2 0 5 3.00 4.40 2 0 5 2.20 5.80 -1 0 -5 20.90 4.60 -1 0 -5 14.00 4.30 -1 0 -5 19.90 4.00 1 0 5 20.60 5.00 1 0 5 14.90 5.70 0 0 -5 -1.10 3.00 0 0 -5 -0.90 3.00 0 0 5 -0.40 3.20 0 0 5 2.70 4.30 1 0 -5 1.10 3.30 1 0 -5 4.40 3.10 -1 0 5 3.40 3.10 -1 0 5 2.60 4.10 2 0 -5 2.80 2.60 2 0 -5 2.80 3.30 -2 0 5 3.90 2.90 -2 0 5 2.50 3.70 -2 0 5 3.40 2.60 3 0 -5 63.99 6.20 3 0 -5 54.69 5.00 -3 0 5 73.29 9.60 -3 0 5 55.29 5.10 -3 0 5 58.39 6.10 4 0 -5 0.10 2.10 4 0 -5 1.90 3.40 -4 0 5 0.50 2.50 -4 0 5 3.00 3.50 -4 0 5 0.50 2.50 -4 0 5 0.00 2.30 5 0 -5 63.39 5.20 5 0 -5 64.49 6.90 -5 0 5 52.59 5.60 -5 0 5 57.69 5.00 -5 0 5 62.59 8.60 6 0 -5 -1.00 4.20 -6 0 5 1.40 3.60 -7 0 5 62.29 11.40 -5 0 -6 -1.20 4.80 5 0 6 5.70 7.10 5 0 6 4.00 7.10 -4 0 -6 3.60 5.10 4 0 6 0.90 6.50 4 0 6 5.50 7.10 -3 0 -6 0.30 4.60 3 0 6 -3.30 5.30 3 0 6 1.00 2.90 3 0 6 -5.00 6.70 -2 0 -6 221.08 12.90 -2 0 -6 203.78 12.20 2 0 6 214.48 10.00 2 0 6 209.68 13.10 2 0 6 222.58 21.10 -1 0 -6 0.80 4.90 1 0 6 6.40 4.70 1 0 6 -5.70 5.30 0 0 -6 329.97 14.30 0 0 -6 318.37 14.00 0 0 6 326.87 14.30 0 0 6 317.37 21.50 1 0 -6 3.60 4.30 1 0 -6 2.00 3.80 -1 0 6 -0.80 4.10 -1 0 6 6.30 4.00 2 0 -6 5.40 3.60 2 0 -6 6.60 4.30 -2 0 6 11.40 5.70 -2 0 6 7.50 3.70 3 0 -6 -5.60 3.80 3 0 -6 -1.50 2.70 -3 0 6 -3.50 2.40 -3 0 6 -1.00 4.20 -3 0 6 -1.30 2.80 4 0 -6 119.79 7.30 4 0 -6 121.69 8.70 -4 0 6 139.49 14.30 -4 0 6 128.49 7.70 5 0 -6 0.40 4.40 -5 0 6 1.10 4.70 -5 0 6 -3.80 3.00 -6 0 6 -2.70 3.60 -7 0 6 -1.30 4.60 -4 0 -7 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4.80 -3 4 6 3.50 2.70 4 -4 -6 1.10 3.40 4 -4 -6 2.90 2.40 -4 4 6 2.60 2.30 -4 4 6 2.00 2.50 -4 4 6 2.30 4.40 5 -4 -6 2.10 3.60 -5 4 6 4.80 5.40 -5 4 6 1.10 3.00 -6 4 6 7.70 5.30 -6 4 6 7.60 4.40 -7 4 6 10.00 5.30 -4 -4 -7 29.70 8.90 4 4 7 30.20 7.70 4 4 7 13.30 9.30 -3 -4 -7 -0.40 5.60 3 4 7 -5.70 7.60 3 4 7 -1.10 3.80 3 4 7 -2.80 5.60 -2 -4 -7 -4.00 4.80 2 4 7 7.40 5.70 2 4 7 -4.10 7.90 2 4 7 6.40 4.00 -1 -4 -7 67.79 9.30 1 4 7 59.69 7.60 1 4 7 73.79 9.10 0 -4 -7 68.09 8.60 0 4 7 41.40 10.80 0 4 7 65.29 8.20 1 -4 -7 61.59 8.00 1 -4 -7 46.90 6.90 -1 4 7 42.80 6.40 -1 4 7 33.30 8.50 2 -4 -7 387.16 15.80 -2 4 7 352.56 14.50 -2 4 7 386.16 26.00 3 -4 -7 155.48 9.90 -3 4 7 150.68 16.90 -3 4 7 143.49 8.90 4 -4 -7 -0.10 4.10 -4 4 7 0.60 5.70 5 -4 -7 9.10 4.70 -5 4 7 18.10 7.70 -6 4 7 1.40 4.80 -7 4 7 15.90 7.30 -2 -4 -8 33.50 8.40 2 4 8 44.70 9.40 2 4 8 39.20 6.80 2 4 8 12.50 10.40 -1 -4 -8 -9.30 4.90 1 4 8 -13.80 8.10 1 4 8 -0.40 4.90 1 4 8 2.20 3.90 0 -4 -8 16.60 6.30 0 4 8 15.90 5.70 0 4 8 4.00 9.50 1 -4 -8 48.70 7.90 -1 4 8 31.00 10.90 -1 4 8 45.00 7.20 2 -4 -8 12.80 5.80 -2 4 8 9.20 8.20 3 -4 -8 30.30 6.50 -3 4 8 17.10 8.30 4 -4 -8 -3.60 5.20 -4 4 8 5.10 7.60 5 -4 -8 7.70 5.20 -5 4 8 10.00 7.50 -6 4 8 3.10 6.80 0 -4 -9 5.10 7.00 0 4 9 -7.60 10.60 1 -4 -9 7.70 6.40 -1 4 9 -14.20 9.60 2 -4 -9 12.90 6.30 -2 4 9 -0.40 9.90 -3 4 9 36.70 12.70 -4 4 9 -0.20 8.70 -3 -5 9 -12.30 7.00 3 5 -9 -10.80 6.20 -2 -5 9 -15.70 6.90 2 5 -9 5.00 7.20 -1 -5 9 -3.00 5.50 1 5 -9 9.10 7.70 0 -5 9 -21.10 8.80 -6 -5 8 8.00 6.90 -5 -5 8 111.89 17.40 5 5 -8 85.69 11.50 -4 -5 8 42.80 9.90 4 5 -8 72.19 10.40 -3 -5 8 -1.20 6.30 -3 -5 8 6.10 4.90 3 5 -8 -0.80 6.60 -2 -5 8 -7.30 6.10 -2 -5 8 -1.00 5.00 2 5 -8 -2.90 5.60 -1 -5 8 -8.90 7.10 -1 -5 8 2.40 4.80 1 5 -8 7.70 6.90 0 -5 8 -13.10 7.30 0 -5 8 3.30 5.80 0 5 -8 -2.20 6.00 1 -5 8 4.90 8.60 1 -5 8 15.10 7.40 -1 5 -8 14.30 6.90 2 -5 8 3.00 9.60 2 -5 8 25.80 8.70 -2 5 -8 12.30 7.00 -7 -5 7 14.40 6.30 -6 -5 7 6.40 6.00 6 5 -7 2.70 6.60 -5 -5 7 -5.70 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3.50 -3 -5 4 16.90 3.40 -3 -5 4 8.40 3.90 3 5 -4 12.70 3.30 3 5 -4 12.60 3.90 3 5 -4 16.10 3.90 -2 -5 4 75.99 8.30 -2 -5 4 76.89 6.10 -2 -5 4 76.19 5.90 -2 -5 4 79.99 5.80 2 5 -4 74.49 7.30 2 5 -4 78.89 5.60 2 5 -4 83.19 6.30 -1 -5 4 16.10 3.90 -1 -5 4 10.20 3.60 -1 -5 4 20.70 4.00 -1 -5 4 13.50 3.50 1 5 -4 15.50 3.30 1 5 -4 18.80 3.90 1 5 -4 15.40 4.10 1 5 -4 19.20 4.60 0 -5 4 113.89 7.60 0 -5 4 102.29 9.80 0 -5 4 109.99 7.90 0 -5 4 107.59 7.30 0 5 -4 105.69 7.10 0 5 -4 104.09 8.20 0 5 -4 94.79 6.40 0 5 -4 123.49 8.50 1 -5 4 30.60 5.10 1 -5 4 29.80 5.60 1 -5 4 40.50 5.60 1 -5 4 45.50 5.40 -1 5 -4 46.70 6.40 -1 5 -4 43.50 5.80 -1 5 -4 41.10 5.20 -1 5 -4 46.00 6.40 2 -5 4 48.20 6.60 2 -5 4 52.29 6.50 2 -5 4 58.99 10.40 -2 5 -4 55.29 7.20 -2 5 -4 49.00 7.60 -2 5 -4 59.89 6.70 3 -5 4 59.59 8.10 3 -5 4 64.79 11.20 3 -5 4 57.69 3.70 -3 5 -4 78.69 8.20 -3 5 -4 71.39 7.60 -3 5 -4 76.49 9.50 4 -5 4 0.20 4.80 4 -5 4 7.60 5.70 -4 5 -4 0.30 4.30 -4 5 -4 1.60 4.40 -4 5 -4 5.60 4.10 5 -5 4 1.80 5.70 -5 5 -4 -3.00 4.70 -5 5 -4 1.60 4.00 -5 5 -4 3.60 4.60 6 -5 4 10.60 6.50 -6 5 -4 8.80 6.50 -6 5 -4 14.90 6.30 -6 5 -4 7.10 5.20 7 -5 4 -1.20 6.90 -9 -5 3 11.30 10.00 9 5 -3 16.00 7.00 -8 -5 3 4.70 6.70 8 5 -3 2.20 5.40 -7 -5 3 -2.30 4.80 -7 -5 3 1.70 3.20 7 5 -3 0.30 4.70 -6 -5 3 312.67 21.50 -6 -5 3 268.27 11.90 6 5 -3 288.47 12.10 6 5 -3 310.87 13.50 -5 -5 3 21.60 6.50 -5 -5 3 19.30 4.10 5 5 -3 14.70 4.40 5 5 -3 16.00 3.70 -4 -5 3 237.28 7.90 -4 -5 3 217.18 9.20 -4 -5 3 168.58 13.70 4 5 -3 225.28 14.50 4 5 -3 217.38 9.20 4 5 -3 231.58 9.90 -3 -5 3 142.59 7.30 -3 -5 3 134.69 6.90 -3 -5 3 128.39 6.70 -3 -5 3 141.39 6.40 3 5 -3 126.59 6.60 3 5 -3 135.29 7.20 3 5 -3 136.49 10.20 -2 -5 3 254.87 9.60 -2 -5 3 293.27 14.30 -2 -5 3 271.97 10.10 -2 -5 3 263.37 9.90 2 5 -3 268.37 10.50 2 5 -3 285.17 14.00 2 5 -3 262.47 9.40 2 5 -3 254.87 9.70 -1 -5 3 814.22 21.20 -1 -5 3 839.52 23.60 -1 -5 3 790.82 21.20 -1 -5 3 814.72 29.20 1 5 -3 810.92 21.10 1 5 -3 803.62 23.70 1 5 -3 842.82 30.40 1 5 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4.30 2 10 -5 1.90 5.30 -1 -10 5 159.68 12.80 -1 -10 5 144.19 9.80 1 10 -5 136.99 10.20 1 10 -5 136.79 13.10 1 10 -5 159.18 11.60 0 -10 5 130.19 13.00 0 -10 5 136.89 10.30 0 10 -5 132.09 11.60 0 10 -5 134.59 9.80 1 -10 5 21.50 6.20 1 -10 5 29.30 4.70 1 -10 5 37.30 7.10 -1 10 -5 31.00 5.90 -1 10 -5 38.30 7.90 -1 10 -5 32.00 6.10 2 -10 5 467.55 19.30 2 -10 5 456.05 14.10 2 -10 5 465.05 24.00 -2 10 -5 447.66 22.10 -2 10 -5 474.15 18.70 -2 10 -5 454.25 21.30 3 -10 5 34.40 8.00 3 -10 5 25.00 6.70 -3 10 -5 35.10 6.90 -3 10 -5 38.40 8.30 4 -10 5 83.59 11.20 -4 10 -5 84.29 13.30 -4 10 -5 83.89 10.10 -4 10 -5 80.69 10.70 5 -10 5 -6.30 6.10 -5 10 -5 -3.20 5.20 -5 10 -5 -0.80 5.90 -5 10 -5 -5.00 4.50 8 10 -4 12.20 7.50 -7 -10 4 133.69 10.40 7 10 -4 152.58 12.40 -6 -10 4 38.60 6.30 -6 -10 4 37.60 11.60 6 10 -4 75.79 9.40 -5 -10 4 34.30 9.10 -5 -10 4 42.00 6.80 -5 -10 4 29.40 3.90 5 10 -4 46.10 7.10 -4 -10 4 0.90 3.50 -4 -10 4 1.80 4.90 -4 -10 4 0.90 2.00 4 10 -4 -6.10 3.70 4 10 -4 5.60 4.80 4 10 -4 -0.70 2.80 -3 -10 4 78.69 7.10 -3 -10 4 91.49 11.80 -3 -10 4 80.19 6.40 3 10 -4 90.39 11.40 3 10 -4 94.19 8.50 3 10 -4 94.29 8.50 3 10 -4 84.29 6.80 -2 -10 4 28.50 4.80 -2 -10 4 41.80 6.20 -2 -10 4 37.80 6.90 2 10 -4 22.30 6.30 2 10 -4 27.60 4.40 2 10 -4 46.50 6.70 2 10 -4 29.00 5.10 -1 -10 4 76.69 7.30 -1 -10 4 76.09 7.70 -1 -10 4 75.89 8.00 -1 -10 4 73.69 6.30 1 10 -4 85.09 8.00 1 10 -4 78.49 7.00 1 10 -4 62.89 9.70 0 -10 4 10.80 3.30 0 -10 4 10.20 4.20 0 -10 4 7.00 3.60 0 10 -4 4.00 3.70 0 10 -4 10.50 4.00 1 -10 4 27.50 4.20 1 -10 4 25.40 5.80 1 -10 4 19.60 4.90 -1 10 -4 25.80 4.70 -1 10 -4 30.00 5.40 -1 10 -4 27.50 6.00 2 -10 4 186.48 7.80 2 -10 4 198.88 13.80 2 -10 4 182.58 11.40 -2 10 -4 175.38 10.30 -2 10 -4 193.18 12.30 -2 10 -4 179.58 11.70 3 -10 4 19.10 5.70 3 -10 4 25.90 3.10 3 -10 4 33.70 7.10 -3 10 -4 28.20 6.30 -3 10 -4 21.10 5.10 -3 10 -4 13.70 4.60 4 -10 4 221.28 13.00 -4 10 -4 249.08 19.80 -4 10 -4 207.58 12.70 -4 10 -4 204.68 14.40 5 -10 4 8.90 6.50 -5 10 -4 11.50 5.60 -5 10 -4 7.40 5.20 -5 10 -4 16.30 7.50 6 -10 4 46.80 9.30 -6 10 -4 28.60 7.10 8 10 -3 5.10 6.30 -7 -10 3 27.50 6.30 -7 -10 3 8.50 7.00 7 10 -3 18.90 6.70 -6 -10 3 336.27 26.60 -6 -10 3 460.85 17.60 6 10 -3 462.95 18.00 -5 -10 3 36.30 6.10 -5 -10 3 24.10 8.40 5 10 -3 27.20 5.70 5 10 -3 27.00 5.10 -4 -10 3 43.10 4.10 -4 -10 3 47.40 6.50 -4 -10 3 51.79 10.30 4 10 -3 48.40 5.60 4 10 -3 52.69 6.50 4 10 -3 51.79 6.10 -3 -10 3 11.60 5.20 -3 -10 3 4.80 3.00 3 10 -3 10.90 3.30 3 10 -3 8.50 5.30 3 10 -3 6.60 2.60 -2 -10 3 157.68 8.30 -2 -10 3 148.79 8.00 -2 -10 3 140.19 8.10 -2 -10 3 148.09 8.40 2 10 -3 147.69 8.70 2 10 -3 145.99 7.70 2 10 -3 145.39 8.30 -1 -10 3 33.20 5.10 -1 -10 3 29.40 4.50 -1 -10 3 32.10 4.40 -1 -10 3 31.50 5.10 -1 -10 3 34.50 5.20 1 10 -3 37.80 4.20 1 10 -3 22.00 5.60 1 10 -3 28.00 4.50 1 10 -3 29.40 4.80 0 -10 3 79.39 6.70 0 -10 3 95.19 6.00 0 -10 3 81.09 6.90 0 -10 3 90.39 6.80 0 -10 3 82.19 6.80 0 10 -3 84.59 6.60 0 10 -3 76.69 7.30 0 10 -3 86.39 6.00 1 -10 3 22.10 4.00 1 -10 3 34.70 4.30 1 -10 3 40.80 5.70 -1 10 -3 37.70 4.10 -1 10 -3 34.50 5.70 -1 10 -3 33.00 4.90 2 -10 3 38.30 6.60 2 -10 3 40.70 6.00 2 -10 3 29.70 4.90 2 -10 3 34.70 4.10 -2 10 -3 33.10 5.30 -2 10 -3 40.90 5.80 -2 10 -3 41.80 6.50 3 -10 3 10.80 4.80 3 -10 3 16.30 2.10 3 -10 3 17.20 5.30 -3 10 -3 10.80 3.80 -3 10 -3 15.50 4.70 -3 10 -3 19.30 4.70 4 -10 3 203.78 11.20 4 -10 3 199.88 11.80 -4 10 -3 214.28 11.40 -4 10 -3 178.48 14.50 -4 10 -3 181.78 12.40 5 -10 3 5.50 5.50 -5 10 -3 3.90 4.40 -5 10 -3 -1.00 5.00 -5 10 -3 4.50 3.90 6 -10 3 19.10 7.10 -6 10 -3 10.50 7.00 -6 10 -3 30.80 7.10 7 -10 3 18.80 7.80 -7 10 -3 10.70 5.70 -7 10 -3 5.50 7.70 -8 -10 2 3.10 7.50 8 10 -2 10.20 6.80 -7 -10 2 2.60 5.80 -7 -10 2 12.20 5.30 7 10 -2 -2.30 5.20 -6 -10 2 9.10 4.50 -6 -10 2 10.90 7.20 6 10 -2 8.90 5.60 -5 -10 2 45.40 6.50 -5 -10 2 20.60 7.80 5 10 -2 36.10 5.50 5 10 -2 26.40 5.40 -4 -10 2 36.70 8.30 -4 -10 2 33.90 5.30 4 10 -2 47.60 6.50 4 10 -2 44.00 4.20 4 10 -2 44.00 5.40 -3 -10 2 713.73 32.90 -3 -10 2 743.83 21.50 -3 -10 2 766.72 21.60 -3 -10 2 739.83 21.10 -3 -10 2 714.83 20.60 3 10 -2 842.12 34.30 3 10 -2 712.63 21.00 3 10 -2 701.13 20.70 3 10 -2 727.83 21.40 3 10 -2 712.43 21.00 -2 -10 2 68.69 5.60 -2 -10 2 80.29 5.80 -2 -10 2 74.69 10.30 -2 -10 2 80.09 5.60 -2 -10 2 79.99 5.80 2 10 -2 91.19 6.30 2 10 -2 82.79 5.80 2 10 -2 51.69 9.30 2 10 -2 84.59 6.50 2 10 -2 76.59 6.20 -1 -10 2 323.67 11.30 -1 -10 2 305.87 11.70 -1 -10 2 293.37 11.10 -1 -10 2 297.57 10.60 1 10 -2 281.77 10.80 1 10 -2 313.07 17.10 1 10 -2 291.87 11.90 1 10 -2 277.77 10.50 1 10 -2 281.27 10.50 0 -10 2 36.70 4.70 0 -10 2 23.70 3.50 0 -10 2 27.10 3.30 0 -10 2 29.90 4.20 0 -10 2 22.20 4.10 0 10 -2 32.70 3.90 0 10 -2 27.80 3.70 0 10 -2 23.90 3.80 0 10 -2 31.60 4.90 1 -10 2 2.80 2.50 1 -10 2 4.00 3.00 1 -10 2 3.10 2.30 1 -10 2 1.80 2.70 -1 10 -2 5.90 2.80 -1 10 -2 6.30 2.20 -1 10 -2 4.80 1.20 -1 10 -2 4.40 3.30 -1 10 -2 6.20 2.30 2 -10 2 21.70 4.30 2 -10 2 23.50 3.00 2 -10 2 26.00 4.50 2 -10 2 26.70 4.30 -2 10 -2 19.00 3.40 -2 10 -2 15.50 2.80 -2 10 -2 24.90 3.10 -2 10 -2 17.60 4.20 -2 10 -2 22.10 3.80 3 -10 2 3.50 1.50 3 -10 2 2.10 3.40 3 -10 2 4.70 3.60 -3 10 -2 0.60 2.70 -3 10 -2 0.10 3.00 -3 10 -2 1.70 2.70 4 -10 2 -1.90 3.80 4 -10 2 -0.60 3.70 -4 10 -2 -4.30 2.70 -4 10 -2 0.80 2.70 -4 10 -2 -6.60 2.90 5 -10 2 -5.50 3.80 5 -10 2 -2.00 4.50 -5 10 -2 1.50 3.80 -5 10 -2 1.40 3.30 -5 10 -2 -2.40 4.20 6 -10 2 -9.40 4.40 -6 10 -2 1.80 5.30 -6 10 -2 0.20 3.80 -6 10 -2 -0.20 3.40 7 -10 2 10.90 6.00 -7 10 -2 10.80 4.40 -7 10 -2 3.70 7.20 -8 -10 1 3.80 8.10 -8 -10 1 25.00 6.60 8 10 -1 20.80 7.40 -7 -10 1 93.89 9.60 7 10 -1 93.39 10.00 -6 -10 1 -0.90 3.90 -6 -10 1 -4.90 4.90 6 10 -1 1.00 4.90 -5 -10 1 -2.10 4.20 -5 -10 1 1.80 3.70 5 10 -1 -3.00 3.70 5 10 -1 -2.50 3.80 -4 -10 1 69.09 6.60 -4 -10 1 44.80 9.50 4 10 -1 55.29 6.60 4 10 -1 62.89 4.20 4 10 -1 47.40 5.90 4 10 -1 60.79 5.60 -3 -10 1 91.19 6.40 -3 -10 1 109.29 11.70 -3 -10 1 86.99 6.50 -3 -10 1 86.49 6.30 3 10 -1 99.39 5.60 3 10 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2.40 5.90 -1 12 -7 -2.20 6.00 -1 12 -7 -5.40 6.20 2 -12 7 5.40 7.10 2 -12 7 -6.70 5.90 -2 12 -7 3.20 5.90 -2 12 -7 -0.90 6.50 3 -12 7 -0.70 7.20 -3 12 -7 -7.70 6.60 -3 12 -7 -8.00 5.80 -6 -12 6 7.70 5.60 6 12 -6 7.30 6.90 -5 -12 6 42.30 7.50 5 12 -6 54.69 9.60 -4 -12 6 0.50 4.10 -4 -12 6 4.20 4.70 4 12 -6 3.20 6.40 -3 -12 6 22.20 6.40 -3 -12 6 28.50 6.90 3 12 -6 18.70 6.50 3 12 -6 18.00 7.30 -2 -12 6 1.50 4.70 -2 -12 6 0.50 4.40 2 12 -6 -2.60 5.60 2 12 -6 -2.00 6.80 -1 -12 6 0.80 4.90 1 12 -6 -2.20 6.10 1 12 -6 -3.70 4.50 0 -12 6 252.97 18.90 0 -12 6 240.08 14.80 0 12 -6 255.27 17.00 0 12 -6 247.78 14.80 1 -12 6 -9.90 5.10 1 -12 6 -0.80 5.80 -1 12 -6 -2.50 4.70 -1 12 -6 10.80 6.60 2 -12 6 9.20 6.70 2 -12 6 10.30 6.40 -2 12 -6 23.60 8.10 -2 12 -6 14.30 6.00 3 -12 6 4.00 5.70 3 -12 6 2.60 6.00 -3 12 -6 3.00 6.10 -3 12 -6 -0.80 5.30 4 -12 6 7.10 7.00 -4 12 -6 6.00 7.30 -4 12 -6 13.60 7.30 -4 12 -6 3.00 6.20 7 12 -5 -1.30 6.50 -6 -12 5 -5.30 6.00 -6 -12 5 0.60 4.30 6 12 -5 -4.70 6.00 -5 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5.60 -5 -12 4 2.50 4.30 -5 -12 4 5.30 6.50 5 12 -4 2.40 4.90 -4 -12 4 2.50 2.50 -4 -12 4 2.90 4.10 -4 -12 4 6.90 6.40 4 12 -4 0.40 4.90 4 12 -4 2.60 4.70 -3 -12 4 128.79 8.30 -3 -12 4 136.19 9.80 3 12 -4 131.39 9.60 3 12 -4 146.99 10.00 -2 -12 4 5.60 3.10 -2 -12 4 13.20 4.80 2 12 -4 13.70 4.40 2 12 -4 13.30 4.60 -1 -12 4 0.80 2.70 -1 -12 4 0.80 3.40 1 12 -4 2.70 3.50 1 12 -4 -4.90 4.30 1 12 -4 5.30 4.30 0 -12 4 57.69 8.10 0 -12 4 66.49 6.40 0 -12 4 53.09 7.30 0 12 -4 60.59 7.80 0 12 -4 62.09 6.90 1 -12 4 26.90 5.10 1 -12 4 27.00 6.00 1 -12 4 28.10 4.40 -1 12 -4 34.20 6.80 -1 12 -4 38.60 6.60 2 -12 4 5.60 5.00 2 -12 4 4.00 3.70 2 -12 4 -0.70 2.80 -2 12 -4 0.60 2.10 -2 12 -4 3.40 4.30 -2 12 -4 -3.50 3.80 3 -12 4 47.00 4.70 3 -12 4 65.79 8.30 -3 12 -4 38.50 7.40 -3 12 -4 65.49 9.20 -3 12 -4 50.89 7.70 4 -12 4 106.89 11.00 -4 12 -4 108.49 9.80 -4 12 -4 100.59 10.40 5 -12 4 5.10 6.10 -5 12 -4 5.30 6.40 -5 12 -4 3.90 4.50 -5 12 -4 -1.10 4.70 6 -12 4 2.10 6.60 -6 12 -4 6.80 7.20 -6 12 -4 7.00 5.50 -8 -12 3 4.60 9.90 8 12 -3 28.60 8.90 -7 -12 3 98.69 9.80 -7 -12 3 51.79 13.50 7 12 -3 75.09 10.50 -6 -12 3 -3.90 7.30 -6 -12 3 6.00 4.80 6 12 -3 6.00 5.30 -5 -12 3 24.30 5.60 -5 -12 3 23.20 8.40 5 12 -3 24.90 6.50 -4 -12 3 1.30 1.90 -4 -12 3 4.60 5.50 -4 -12 3 4.80 3.60 4 12 -3 -2.30 4.30 4 12 -3 11.80 3.40 -3 -12 3 196.88 9.30 -3 -12 3 201.18 16.80 -3 -12 3 197.28 10.30 3 12 -3 196.08 10.20 3 12 -3 190.68 10.80 -2 -12 3 26.70 4.60 -2 -12 3 22.30 4.50 2 12 -3 32.50 5.90 2 12 -3 18.00 6.70 2 12 -3 22.90 4.70 -1 -12 3 114.19 7.50 -1 -12 3 122.99 8.00 -1 -12 3 104.89 7.90 -1 -12 3 121.39 7.60 -1 -12 3 121.59 8.30 1 12 -3 128.89 12.40 1 12 -3 136.79 9.10 1 12 -3 128.99 8.40 0 -12 3 4.60 2.50 0 -12 3 7.00 3.90 0 -12 3 1.20 3.40 0 -12 3 2.30 2.90 0 12 -3 7.30 3.90 0 12 -3 4.20 3.40 1 -12 3 12.40 3.00 1 -12 3 13.10 3.30 1 -12 3 15.90 4.60 1 -12 3 18.50 4.80 -1 12 -3 12.90 4.40 -1 12 -3 19.60 4.40 2 -12 3 1.50 2.60 2 -12 3 6.70 4.20 2 -12 3 -0.40 4.00 -2 12 -3 1.00 3.40 -2 12 -3 0.90 2.90 -2 12 -3 -0.10 1.70 3 -12 3 135.79 9.70 3 -12 3 125.89 5.60 3 -12 3 130.89 9.00 -3 12 -3 131.99 9.80 -3 12 -3 136.09 10.80 -3 12 -3 129.79 8.80 4 -12 3 4.90 5.40 4 -12 3 0.60 4.40 -4 12 -3 -4.20 3.50 -4 12 -3 3.30 4.40 -4 12 -3 4.40 3.90 5 -12 3 -3.80 5.00 -5 12 -3 0.40 4.30 -5 12 -3 -0.10 4.00 -5 12 -3 -4.20 4.70 6 -12 3 -6.10 5.30 -6 12 -3 5.60 4.50 -6 12 -3 1.10 6.20 -7 12 -3 13.20 5.20 -7 12 -3 2.80 7.60 -8 -12 2 5.20 5.30 8 12 -2 -3.30 6.10 -7 -12 2 -4.00 6.40 -7 -12 2 1.60 4.20 7 12 -2 0.00 5.50 -6 -12 2 6.40 8.40 -6 -12 2 22.00 6.20 6 12 -2 18.00 6.30 -5 -12 2 7.70 4.10 -5 -12 2 8.50 6.70 5 12 -2 11.80 5.30 -4 -12 2 74.29 12.10 -4 -12 2 64.29 7.20 4 12 -2 62.69 7.70 4 12 -2 63.19 7.70 4 12 -2 61.09 5.50 -3 -12 2 11.70 6.20 -3 -12 2 11.80 3.90 3 12 -2 13.90 3.70 3 12 -2 11.90 4.20 3 12 -2 12.90 3.70 3 12 -2 11.90 4.10 -2 -12 2 14.40 3.30 -2 -12 2 19.40 4.30 -2 -12 2 17.60 4.20 2 12 -2 5.40 5.80 2 12 -2 14.70 4.00 2 12 -2 20.50 3.80 2 12 -2 10.20 3.50 2 12 -2 15.30 4.10 -1 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53.69 10.60 2 26 -2 50.79 9.60 2 26 -2 60.39 10.20 -1 -26 2 6.30 5.70 1 26 -2 3.40 5.80 1 26 -2 9.60 6.60 1 26 -2 -1.60 5.30 0 -26 2 1.00 6.30 0 26 -2 -4.00 5.60 0 26 -2 1.50 4.80 1 -26 2 -6.20 5.90 -1 26 -2 5.70 5.10 -1 26 -2 2.00 6.40 2 -26 2 -9.40 5.60 -2 26 -2 1.40 4.40 -2 26 -2 -3.80 5.90 -3 -26 1 12.90 7.10 3 26 -1 9.20 6.60 3 26 -1 22.70 7.50 3 26 -1 15.60 7.30 -2 -26 1 1.70 5.70 2 26 -1 -7.40 4.30 2 26 -1 -4.50 5.10 2 26 -1 0.80 5.70 -1 -26 1 6.90 6.00 1 26 -1 1.90 5.50 1 26 -1 -6.60 5.00 1 26 -1 1.30 4.90 0 -26 1 57.59 8.90 0 26 -1 39.90 7.40 0 26 -1 43.60 9.20 1 -26 1 -3.40 5.30 -1 26 -1 -3.80 5.20 -1 26 -1 -1.50 4.60 2 -26 1 7.70 5.90 -2 26 -1 3.60 6.00 -2 26 -1 1.10 4.60 -3 -26 0 7.80 5.60 3 26 0 2.20 5.50 3 26 0 9.30 6.30 3 26 0 2.90 6.50 -2 -26 0 16.90 6.80 2 26 0 27.80 8.40 2 26 0 20.40 7.20 2 26 0 13.10 6.50 -1 -26 0 0.90 5.40 1 26 0 0.50 5.20 1 26 0 -2.50 5.70 0 -26 0 26.20 6.90 0 26 0 36.50 9.20 0 26 0 23.40 7.00 1 -26 0 -4.50 4.70 -1 26 0 -3.80 5.10 -1 26 0 2.60 5.30 2 -26 0 11.80 5.80 -2 26 0 15.70 5.80 -2 26 0 17.50 7.80 3 -26 0 -6.80 4.60 -3 26 0 -1.50 5.80 -3 26 0 -3.30 4.40 -2 -26 -1 11.10 6.40 2 26 1 -3.40 4.80 2 26 1 3.20 6.60 -1 -26 -1 5.00 5.20 1 26 1 2.10 5.20 1 26 1 2.40 5.80 0 -26 -1 68.99 9.30 0 26 1 55.09 10.50 0 26 1 42.00 8.50 1 -26 -1 -1.70 4.70 -1 26 1 3.50 5.50 -1 26 1 0.30 5.80 2 -26 -1 -0.50 4.60 -2 26 1 -3.40 4.50 -2 26 1 5.20 6.20 3 -26 -1 8.30 5.00 -3 26 1 8.80 6.90 -3 26 1 7.80 5.30 -2 -26 -2 -2.20 5.80 2 26 2 0.90 5.80 2 26 2 3.20 5.70 -1 -26 -2 2.90 5.30 1 26 2 2.00 5.50 1 26 2 -1.60 6.10 0 -26 -2 3.70 4.80 0 26 2 -3.10 5.20 0 26 2 -9.70 4.90 1 -26 -2 1.60 4.50 -1 26 2 6.30 6.30 -1 26 2 0.40 5.50 2 -26 -2 66.09 8.20 -2 26 2 57.49 11.30 -2 26 2 43.40 8.90 -3 26 2 0.50 6.00 1 26 3 -1.90 5.60 0 -26 -3 1.80 4.60 0 26 3 5.30 5.80 0 26 3 -5.90 5.40 1 -26 -3 24.00 6.00 -1 26 3 38.80 8.80 -1 26 3 14.20 7.50 -2 26 3 6.40 5.60 -1 -27 2 7.70 6.60 1 27 -2 5.30 5.70 1 27 -2 1.80 6.10 0 -27 2 11.50 7.40 0 27 -2 7.40 5.50 0 27 -2 6.20 6.90 -2 -27 1 37.20 8.70 2 27 -1 31.50 8.60 2 27 -1 20.20 7.30 -1 -27 1 33.10 8.10 1 27 -1 34.40 8.10 1 27 -1 31.30 8.90 0 -27 1 15.00 6.80 0 27 -1 15.10 7.80 0 27 -1 21.50 7.20 1 -27 1 -0.90 6.00 -1 27 -1 4.20 5.10 -1 27 -1 1.60 6.60 -2 -27 0 5.00 5.50 2 27 0 -1.50 5.70 2 27 0 1.80 5.80 -1 -27 0 -0.30 5.40 1 27 0 0.40 5.20 1 27 0 0.90 6.00 0 -27 0 -1.20 5.20 0 27 0 -9.60 4.60 0 27 0 0.80 5.40 1 -27 0 -1.70 5.20 -1 27 0 0.80 5.40 -1 27 0 -5.70 5.30 2 -27 0 3.70 5.60 -2 27 0 -2.00 5.90 -2 27 0 -4.50 4.80 -1 -27 -1 7.90 6.50 1 27 1 -0.40 5.70 1 27 1 8.30 6.20 0 -27 -1 22.50 6.50 0 27 1 11.10 6.50 0 27 1 12.90 7.50 1 -27 -1 33.20 7.20 -1 27 1 38.80 8.50 -1 27 1 29.50 9.20 -2 27 1 14.50 6.40 -2 27 1 23.00 8.80 0 -27 -2 17.10 6.40 0 27 2 6.60 7.20 0 27 2 5.00 7.00 1 -27 -2 0.30 4.40 -1 27 2 0.60 5.80 -1 27 2 2.70 6.30 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 19195 _shelx_res_file ; TITL 51ecg CELL 0.71073 7.6030 22.6605 7.6751 90.000 102.284 90.000 ZERR 4.00 0.0006 0.0019 0.0007 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 48 56 24 12 MERG 2 FMAP 2 OMIT -2 180.0 PLAN 20 SIZE 0.11 0.13 0.14 ACTA BOND $H CONF HTAB L.S. 20 TEMP 23.00 WGHT 0.027000 1.108600 EXTI 0.004463 FVAR 0.59776 N1 3 0.765990 0.369694 0.643663 11.00000 0.02982 0.02998 = 0.02394 -0.00140 0.00308 0.00285 N2 3 0.794797 0.322238 0.547340 11.00000 0.03411 0.03098 = 0.02651 -0.00316 0.00058 0.00327 C3 1 0.701804 0.332286 0.382227 11.00000 0.02598 0.02866 = 0.02639 0.00038 0.00218 -0.00157 C4 1 0.611484 0.387648 0.371663 11.00000 0.02744 0.02881 = 0.02656 0.00216 0.00273 -0.00234 C5 1 0.656389 0.409411 0.543322 11.00000 0.02888 0.02771 = 0.03169 0.00214 0.00399 0.00185 AFIX 43 H5 2 0.618093 0.445010 0.582809 11.00000 -1.20000 AFIX 0 C11 1 0.857175 0.373550 0.826782 11.00000 0.02648 0.03194 = 0.02379 0.00099 0.00397 -0.00033 C12 1 0.844927 0.423405 0.924354 11.00000 0.03560 0.03422 = 0.03058 0.00182 0.00056 0.00609 AFIX 43 H12 2 0.774704 0.454998 0.872655 11.00000 -1.20000 AFIX 0 C13 1 0.937988 0.426665 1.101337 11.00000 0.04015 0.03688 = 0.03163 -0.00526 0.00551 0.00137 AFIX 43 H13 2 0.928918 0.460348 1.168091 11.00000 -1.20000 AFIX 0 C14 1 1.043612 0.380019 1.177830 11.00000 0.02856 0.04117 = 0.02348 0.00285 0.00103 -0.00337 C15 1 1.055457 0.330042 1.077712 11.00000 0.03709 0.03561 = 0.03375 0.00396 -0.00108 0.00783 AFIX 43 H15 2 1.126988 0.298606 1.128484 11.00000 -1.20000 AFIX 0 C16 1 0.962188 0.326439 0.903423 11.00000 0.03871 0.03254 = 0.03253 -0.00356 0.00352 0.00552 AFIX 43 H16 2 0.969584 0.292496 0.837244 11.00000 -1.20000 AFIX 0 O14 4 1.140360 0.378833 1.350369 11.00000 0.05035 0.04954 = 0.02725 -0.00067 -0.00508 0.00300 C141 1 1.130667 0.429309 1.458002 11.00000 0.05457 0.05870 = 0.03126 -0.00577 0.00156 -0.00207 AFIX 137 H14A 2 1.176206 0.463085 1.406298 11.00000 -1.50000 H14B 2 1.201560 0.422717 1.575693 11.00000 -1.50000 H14C 2 1.007692 0.436203 1.464676 11.00000 -1.50000 AFIX 0 C31 1 0.710322 0.286368 0.246273 11.00000 0.02892 0.02814 = 0.02956 0.00006 0.00177 -0.00246 O31 4 0.606910 0.286236 0.096123 11.00000 0.04334 0.03869 = 0.03398 -0.00656 -0.01035 0.00290 N31 3 0.832911 0.245134 0.295395 11.00000 0.04165 0.02990 = 0.03088 -0.00357 -0.00178 0.00555 H31 2 0.910896 0.247690 0.396507 11.00000 -1.20000 N32 3 0.863742 0.199952 0.178741 11.00000 0.07013 0.03663 = 0.04399 -0.00929 0.00031 0.01270 H32A 2 0.781803 0.204703 0.063791 11.00000 -1.20000 H32B 2 0.841088 0.161178 0.232253 11.00000 -1.20000 C41 1 0.502390 0.422289 0.223555 11.00000 0.02972 0.03113 = 0.02880 0.00239 0.00500 0.00031 O41 4 0.460957 0.473955 0.247075 11.00000 0.06399 0.03306 = 0.03643 0.00142 0.00298 0.01413 N41 3 0.456240 0.395346 0.067237 11.00000 0.03910 0.03667 = 0.02739 0.00218 -0.00219 0.00635 H41 2 0.499643 0.356346 0.057596 11.00000 -1.20000 N42 3 0.353682 0.422538 -0.086916 11.00000 0.04361 0.05093 = 0.03142 0.00860 -0.00192 0.00389 H42A 2 0.411988 0.457678 -0.110038 11.00000 -1.20000 H42B 2 0.262182 0.436087 -0.059601 11.00000 -1.20000 HKLF 4 REM 51ecg REM R1 = 0.0457 for 1722 Fo > 4sig(Fo) and 0.0832 for all 2521 data REM 210 parameters refined using 0 restraints END WGHT 0.0274 1.1077 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y+1, -z+1 HTAB C5 O41_$1 HTAB C12 O41_$1 EQIV $2 x+1, y, z+2 HTAB C141 N42_$2 EQIV $3 x+1/2, -y+1/2, z+1/2 HTAB N31 O31_$3 EQIV $4 x-1/2, -y+1/2, z-3/2 HTAB N32 O14_$4 HTAB N32 N42_$3 HTAB N41 O31 EQIV $5 -x+1, -y+1, -z HTAB N42 O41_$5 REM Highest difference peak 0.204, deepest hole -0.212, 1-sigma level 0.046 Q1 1 0.6767 0.3677 0.3432 11.00000 0.05 0.20 Q2 1 0.6983 0.1981 0.1125 11.00000 0.05 0.20 Q3 1 0.8551 0.4173 1.0271 11.00000 0.05 0.18 Q4 1 0.3173 0.4759 -0.0752 11.00000 0.05 0.17 Q5 1 0.9455 0.3925 1.1404 11.00000 0.05 0.17 Q6 1 0.7745 0.4056 0.6180 11.00000 0.05 0.17 Q7 1 0.6836 0.4077 0.4517 11.00000 0.05 0.17 Q8 1 0.8658 0.2813 0.5627 11.00000 0.05 0.16 Q9 1 0.4434 0.3608 0.0843 11.00000 0.05 0.16 Q10 1 0.3837 0.4755 0.0454 11.00000 0.05 0.16 Q11 1 0.9579 0.3664 0.8544 11.00000 0.05 0.16 Q12 1 0.7554 0.2759 0.5595 11.00000 0.05 0.16 Q13 1 1.1388 0.3986 1.6087 11.00000 0.05 0.16 Q14 1 0.3037 0.4244 -0.2407 11.00000 0.05 0.16 Q15 1 0.7689 0.2920 0.6539 11.00000 0.05 0.16 Q16 1 0.9602 0.3310 1.0119 11.00000 0.05 0.16 Q17 1 0.5814 0.3827 0.4194 11.00000 0.05 0.16 Q18 1 0.4950 0.2932 0.1379 11.00000 0.05 0.16 Q19 1 0.3957 0.3853 -0.1396 11.00000 0.05 0.16 Q20 1 1.1252 0.3251 1.3576 11.00000 0.05 0.15 ; _shelx_res_checksum 91336 _shelxl_version_number 2.014 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 N N1 0.7660(2) 0.36969(8) 0.6437(2) 0.0283(4) Uani d 1 N N2 0.7948(2) 0.32224(8) 0.5473(2) 0.0314(5) Uani d 1 C C3 0.7018(3) 0.33229(9) 0.3822(3) 0.0275(5) Uani d 1 C C4 0.6115(3) 0.38765(9) 0.3717(3) 0.0280(5) Uani d 1 C C5 0.6564(3) 0.40941(10) 0.5433(3) 0.0298(5) Uani d 1 H H5 0.6181 0.4450 0.5828 0.036 Uiso calc 1 C C11 0.8572(3) 0.37355(9) 0.8268(3) 0.0276(5) Uani d 1 C C12 0.8449(3) 0.42341(10) 0.9244(3) 0.0344(6) Uani d 1 H H12 0.7747 0.4550 0.8727 0.041 Uiso calc 1 C C13 0.9380(3) 0.42666(11) 1.1013(3) 0.0365(6) Uani d 1 H H13 0.9289 0.4603 1.1681 0.044 Uiso calc 1 C C14 1.0436(3) 0.38002(10) 1.1778(3) 0.0317(5) Uani d 1 C C15 1.0555(3) 0.33004(10) 1.0777(3) 0.0368(6) Uani d 1 H H15 1.1270 0.2986 1.1285 0.044 Uiso calc 1 C C16 0.9622(3) 0.32644(10) 0.9034(3) 0.0352(6) Uani d 1 H H16 0.9696 0.2925 0.8372 0.042 Uiso calc 1 O O14 1.1404(2) 0.37883(8) 1.3504(2) 0.0444(5) Uani d 1 C C141 1.1307(4) 0.42931(12) 1.4580(3) 0.0493(7) Uani d 1 H H14A 1.1762 0.4631 1.4063 0.074 Uiso calc 1 H H14B 1.2016 0.4227 1.5757 0.074 Uiso calc 1 H H14C 1.0077 0.4362 1.4647 0.074 Uiso calc 1 C C31 0.7103(3) 0.28637(9) 0.2463(3) 0.0295(5) Uani d 1 O O31 0.6069(2) 0.28624(7) 0.0961(2) 0.0414(5) Uani d 1 N N31 0.8329(3) 0.24513(8) 0.2954(3) 0.0356(5) Uani d 1 H H31 0.911(3) 0.2477(11) 0.397(3) 0.043 Uiso d 1 N N32 0.8637(3) 0.19995(10) 0.1787(3) 0.0520(6) Uani d 1 H H32A 0.782(4) 0.2047(12) 0.064(4) 0.062 Uiso d 1 H H32B 0.841(4) 0.1612(13) 0.232(4) 0.062 Uiso d 1 C C41 0.5024(3) 0.42229(10) 0.2236(3) 0.0301(5) Uani d 1 O O41 0.4610(2) 0.47395(7) 0.2471(2) 0.0456(5) Uani d 1 N N41 0.4562(3) 0.39535(9) 0.0672(2) 0.0358(5) Uani d 1 H H41 0.500(3) 0.3563(12) 0.058(3) 0.043 Uiso d 1 N N42 0.3537(3) 0.42254(10) -0.0869(3) 0.0435(6) Uani d 1 H H42A 0.412(4) 0.4577(13) -0.110(3) 0.052 Uiso d 1 H H42B 0.262(4) 0.4361(13) -0.060(4) 0.052 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 0.0298(10) 0.0300(10) 0.0239(10) 0.0028(8) 0.0031(8) -0.0014(8) N2 0.0341(11) 0.0310(10) 0.0265(11) 0.0033(8) 0.0006(9) -0.0032(8) C3 0.0260(12) 0.0287(11) 0.0264(12) -0.0016(9) 0.0022(10) 0.0004(9) C4 0.0274(12) 0.0288(11) 0.0266(12) -0.0023(9) 0.0027(10) 0.0022(9) C5 0.0289(12) 0.0277(11) 0.0317(13) 0.0018(10) 0.0040(10) 0.0021(10) C11 0.0265(12) 0.0319(12) 0.0238(12) -0.0003(9) 0.0040(10) 0.0010(9) C12 0.0356(14) 0.0342(13) 0.0306(13) 0.0061(11) 0.0006(11) 0.0018(10) C13 0.0401(14) 0.0369(13) 0.0316(14) 0.0014(11) 0.0055(11) -0.0053(11) C14 0.0286(13) 0.0412(13) 0.0235(12) -0.0034(10) 0.0010(10) 0.0028(10) C15 0.0371(14) 0.0356(13) 0.0337(14) 0.0078(11) -0.0011(11) 0.0040(11) C16 0.0387(14) 0.0325(12) 0.0325(13) 0.0055(11) 0.0035(11) -0.0036(10) O14 0.0503(11) 0.0495(11) 0.0273(9) 0.0030(9) -0.0051(8) -0.0007(8) C141 0.0546(18) 0.0587(18) 0.0313(14) -0.0021(14) 0.0016(13) -0.0058(13) C31 0.0289(13) 0.0281(12) 0.0296(13) -0.0025(10) 0.0018(10) 0.0001(10) O31 0.0433(10) 0.0387(10) 0.0340(10) 0.0029(8) -0.0103(8) -0.0066(7) N31 0.0417(12) 0.0299(10) 0.0309(11) 0.0056(9) -0.0018(9) -0.0036(9) N32 0.0701(17) 0.0366(13) 0.0440(14) 0.0127(12) 0.0003(12) -0.0093(11) C41 0.0297(12) 0.0311(12) 0.0288(13) 0.0003(10) 0.0050(10) 0.0024(10) O41 0.0640(12) 0.0331(9) 0.0364(10) 0.0141(8) 0.0030(9) 0.0014(8) N41 0.0391(12) 0.0367(11) 0.0274(11) 0.0063(9) -0.0022(9) 0.0022(9) N42 0.0436(14) 0.0509(14) 0.0314(12) 0.0039(11) -0.0019(10) 0.0086(10) 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 N2 N1 C5 111.78(17) N2 N1 C11 119.05(17) C5 N1 C11 129.07(18) C3 N2 N1 105.65(17) N2 C3 C4 110.88(19) N2 C3 C31 117.06(19) C4 C3 C31 132.06(19) C5 C4 C3 104.01(18) C5 C4 C41 121.8(2) C3 C4 C41 134.0(2) N1 C5 C4 107.67(19) N1 C5 H5 126.2 C4 C5 H5 126.2 C12 C11 C16 120.2(2) C12 C11 N1 120.81(19) C16 C11 N1 118.97(19) C11 C12 C13 119.8(2) C11 C12 H12 120.1 C13 C12 H12 120.1 C14 C13 C12 120.2(2) C14 C13 H13 119.9 C12 C13 H13 119.9 O14 C14 C13 124.7(2) O14 C14 C15 115.8(2) C13 C14 C15 119.5(2) C16 C15 C14 120.5(2) C16 C15 H15 119.7 C14 C15 H15 119.7 C15 C16 C11 119.8(2) C15 C16 H16 120.1 C11 C16 H16 120.1 C14 O14 C141 117.50(19) O14 C141 H14A 109.5 O14 C141 H14B 109.5 H14A C141 H14B 109.5 O14 C141 H14C 109.5 H14A C141 H14C 109.5 H14B C141 H14C 109.5 O31 C31 N31 122.0(2) O31 C31 C3 122.5(2) N31 C31 C3 115.47(19) C31 N31 N32 122.4(2) C31 N31 H31 120.9(17) N32 N31 H31 116.0(17) N31 N32 H32A 109.5(17) N31 N32 H32B 108.1(16) H32A N32 H32B 110(2) O41 C41 N41 122.8(2) O41 C41 C4 120.6(2) N41 C41 C4 116.59(19) C41 N41 N42 123.4(2) C41 N41 H41 118.0(15) N42 N41 H41 118.6(15) N41 N42 H42A 109.1(16) N41 N42 H42B 107(2) H42A N42 H42B 101(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 N2 1.349(2) N1 C5 1.351(3) N1 C11 1.431(3) N2 C3 1.333(3) C3 C4 1.424(3) C3 C31 1.485(3) C4 C5 1.380(3) C4 C41 1.482(3) C5 H5 0.9300 C11 C12 1.369(3) C11 C16 1.387(3) C12 C13 1.394(3) C12 H12 0.9300 C13 C14 1.381(3) C13 H13 0.9300 C14 O14 1.371(3) C14 C15 1.382(3) C15 C16 1.377(3) C15 H15 0.9300 C16 H16 0.9300 O14 C141 1.422(3) C141 H14A 0.9600 C141 H14B 0.9600 C141 H14C 0.9600 C31 O31 1.249(3) C31 N31 1.317(3) N31 N32 1.412(3) N31 H31 0.87(3) N32 H32A 0.97(3) N32 H32B 1.00(3) C41 O41 1.236(3) C41 N41 1.325(3) N41 N42 1.412(3) N41 H41 0.95(3) N42 H42A 0.95(3) N42 H42B 0.83(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 _geom_hbond_publ_flag N31 H31 O31 4_666 0.88(2) 2.04(2) 2.851(3) 153(2) no N32 H32A O14 4_564 0.97(3) 2.58(3) 3.256(3) 127(2) no N32 H32B N42 4_666 1.00(2) 2.34(3) 3.317(3) 165(2) no N41 H41 O31 . 0.95(3) 1.78(3) 2.714(3) 166(2) no N42 H42A O41 3_665 0.95(3) 2.21(3) 3.120(3) 162(2) no N42 H42B Cg1 1_454 0.83(3) 2.85(3) 3.442(3) 130(2) no C5 H5 O41 3_666 0.93 2.40 3.314(3) 166 no C12 H12 O41 3_666 0.93 2.44 3.354(3) 168 no 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 C5 N1 N2 C3 0.2(2) C11 N1 N2 C3 -176.56(18) N1 N2 C3 C4 0.2(2) N1 N2 C3 C31 179.81(18) N2 C3 C4 C5 -0.6(2) C31 C3 C4 C5 179.9(2) N2 C3 C4 C41 175.1(2) C31 C3 C4 C41 -4.4(4) N2 N1 C5 C4 -0.6(2) C11 N1 C5 C4 175.8(2) C3 C4 C5 N1 0.7(2) C41 C4 C5 N1 -175.66(19) N2 N1 C11 C12 173.8(2) C5 N1 C11 C12 -2.3(3) N2 N1 C11 C16 -4.7(3) C5 N1 C11 C16 179.2(2) C16 C11 C12 C13 -0.2(3) N1 C11 C12 C13 -178.6(2) C11 C12 C13 C14 0.6(4) C12 C13 C14 O14 180.0(2) C12 C13 C14 C15 -0.3(3) O14 C14 C15 C16 179.4(2) C13 C14 C15 C16 -0.4(4) C14 C15 C16 C11 0.8(4) C12 C11 C16 C15 -0.5(3) N1 C11 C16 C15 178.0(2) C13 C14 O14 C141 0.1(3) C15 C14 O14 C141 -179.6(2) N2 C3 C31 O31 168.0(2) C4 C3 C31 O31 -12.5(4) N2 C3 C31 N31 -11.1(3) C4 C3 C31 N31 168.4(2) O31 C31 N31 N32 3.9(4) C3 C31 N31 N32 -177.0(2) C5 C4 C41 O41 6.1(3) C3 C4 C41 O41 -169.0(2) C5 C4 C41 N41 -175.2(2) C3 C4 C41 N41 9.8(4) O41 C41 N41 N42 -0.8(4) C4 C41 N41 N42 -179.5(2) _cod_database_fobs_code 2242739