#------------------------------------------------------------------------------ #$Date: 2018-11-14 05:30:28 +0200 (Wed, 14 Nov 2018) $ #$Revision: 211942 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/27/2242738.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_2242738 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 'C14 H14 N2 O4' _chemical_formula_moiety 'C14 H14 N2 O4' _chemical_formula_sum 'C14 H14 N2 O4' _chemical_formula_weight 274.27 _chemical_name_systematic ; Dimethyl 1-(4-methylphenyl)-1H-pyrazole-3,4-dicarboxylate ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014 _cell_angle_alpha 78.988(3) _cell_angle_beta 85.527(3) _cell_angle_gamma 87.548(4) _cell_formula_units_Z 2 _cell_length_a 7.6546(5) _cell_length_b 8.0959(5) _cell_length_c 11.3065(6) _cell_measurement_reflns_used 2526 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 25.459 _cell_measurement_theta_min 2.564 _cell_volume 685.40(7) _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 1.000 _diffrn_measured_fraction_theta_max 0.994 _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 0.0303 _diffrn_reflns_av_unetI/netI 0.0253 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 12818 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.459 _diffrn_reflns_theta_min 2.564 _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 0.099 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_correction_T_min 0.955 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Sheldrick, 2008a) ; _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.329 _exptl_crystal_description block _exptl_crystal_F_000 288 _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.237 _refine_diff_density_min -0.241 _refine_ls_extinction_coef 0.024(4) _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 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 196 _refine_ls_number_reflns 2526 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0444 _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^)+(0.0529P)^2^+0.2439P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1089 _refine_ls_wR_factor_ref 0.1277 _reflns_number_gt 1777 _reflns_number_total 2526 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file zl2741sup1.cif _cod_data_source_block III _cod_database_code 2242738 _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 0 250.87 4.90 -1 0 0 245.48 5.00 -1 0 0 221.18 4.20 -1 0 0 259.57 4.60 1 0 0 229.88 4.20 1 0 0 252.47 4.70 1 0 0 219.98 4.90 1 0 0 253.47 4.50 -2 0 0 47.20 1.80 -2 0 0 44.10 1.90 -2 0 0 47.80 1.70 -2 0 0 45.40 1.80 -2 0 0 45.50 1.20 -2 0 0 47.70 1.80 2 0 0 46.70 1.80 2 0 0 46.00 1.70 2 0 0 45.20 1.20 2 0 0 45.70 1.60 2 0 0 46.20 2.00 2 0 0 46.30 1.80 -3 0 0 135.89 4.20 -3 0 0 133.89 3.90 -3 0 0 125.09 3.50 -3 0 0 131.49 2.80 -3 0 0 128.99 3.90 -3 0 0 128.59 3.70 3 0 0 124.89 4.20 3 0 0 126.39 3.80 3 0 0 125.79 3.40 3 0 0 130.29 2.80 3 0 0 129.89 3.70 3 0 0 129.09 3.80 -4 0 0 214.28 6.30 -4 0 0 218.58 5.80 -4 0 0 208.28 5.40 -4 0 0 207.78 5.70 -4 0 0 215.78 6.00 -4 0 0 210.68 4.40 4 0 0 214.08 5.90 4 0 0 212.58 5.60 4 0 0 194.98 5.70 4 0 0 211.28 5.30 4 0 0 218.88 6.50 -5 0 0 84.09 3.70 -5 0 0 76.99 3.30 -5 0 0 86.79 3.80 -5 0 0 84.69 3.90 -5 0 0 83.09 2.30 5 0 0 87.49 4.30 5 0 0 85.99 3.70 5 0 0 81.49 3.70 -6 0 0 22.10 1.20 -6 0 0 23.10 2.40 -6 0 0 24.90 2.10 -6 0 0 24.50 2.50 6 0 0 25.10 2.50 6 0 0 27.80 2.70 -7 0 0 -0.80 0.80 -7 0 0 0.60 0.90 7 0 0 -0.20 1.20 7 0 0 -0.30 1.30 -8 0 0 7.60 1.80 -8 0 0 2.30 1.40 8 0 0 8.50 2.30 8 0 0 9.60 2.30 -9 0 0 14.50 2.30 -9 0 0 10.80 2.20 9 0 0 8.20 2.70 9 0 0 13.30 2.80 9 -1 0 5.30 2.20 9 -1 0 2.20 1.90 -9 1 0 2.30 1.60 -9 1 0 1.20 1.70 8 -1 0 0.10 1.60 8 -1 0 1.30 1.80 -8 1 0 0.20 1.40 7 -1 0 31.20 3.30 7 -1 0 28.70 3.10 -7 1 0 32.00 2.90 6 -1 0 4.20 1.50 6 -1 0 5.20 1.70 6 -1 0 5.20 1.60 -6 1 0 3.90 1.40 -6 1 0 4.70 0.50 -6 1 0 4.20 1.50 5 -1 0 28.80 2.50 5 -1 0 27.10 2.10 5 -1 0 28.00 2.50 5 -1 0 25.70 2.40 -5 1 0 26.10 1.10 -5 1 0 24.60 2.50 -5 1 0 25.50 2.20 -5 1 0 28.20 2.20 -5 1 0 23.00 2.10 4 -1 0 144.79 4.30 4 -1 0 140.79 4.10 4 -1 0 145.29 4.90 4 -1 0 146.59 4.60 4 -1 0 137.69 4.90 -4 1 0 140.09 5.00 -4 1 0 144.69 4.50 -4 1 0 138.89 3.10 -4 1 0 137.89 4.20 -4 1 0 141.69 4.40 3 -1 0 220.88 5.80 3 -1 0 218.58 6.00 3 -1 0 218.68 5.50 3 -1 0 221.98 5.30 3 -1 0 218.88 5.10 -3 1 0 224.08 6.10 -3 1 0 216.68 4.30 -3 1 0 216.78 5.20 -3 1 0 222.78 5.50 -3 1 0 217.98 5.30 2 -1 0 64.49 2.60 2 -1 0 61.19 2.20 2 -1 0 58.29 1.90 2 -1 0 63.89 2.00 -2 1 0 62.19 2.20 -2 1 0 64.69 2.60 -2 1 0 60.79 2.00 -2 1 0 59.29 2.00 1 -1 0 1309.77 24.00 1 -1 0 1300.87 21.70 1 -1 0 1281.77 21.80 1 -1 0 1274.17 22.40 -1 1 0 1294.07 21.70 -1 1 0 1289.97 22.40 -1 1 0 1323.87 24.00 -1 1 0 1291.57 21.80 0 -1 0 146.49 2.90 0 -1 0 145.79 3.20 0 -1 0 147.39 3.20 0 1 0 147.09 3.10 0 1 0 140.19 3.20 0 1 0 145.09 2.90 -1 -1 0 48.70 1.40 -1 -1 0 48.80 1.50 -1 -1 0 46.80 1.70 1 1 0 46.90 1.40 1 1 0 45.80 1.40 1 1 0 49.70 1.70 1 1 0 49.70 1.50 -2 -1 0 2404.96 44.40 -2 -1 0 2431.96 40.60 -2 -1 0 2415.26 45.20 -2 -1 0 2495.35 40.90 -2 -1 0 2486.55 41.50 2 1 0 2419.06 44.50 2 1 0 2447.96 40.60 2 1 0 2468.05 40.90 2 1 0 2388.16 42.30 2 1 0 2481.05 41.50 -3 -1 0 24.40 1.70 -3 -1 0 22.50 1.40 -3 -1 0 22.30 1.80 -3 -1 0 22.10 1.30 -3 -1 0 23.80 1.20 -3 -1 0 24.40 1.30 3 1 0 21.70 1.70 3 1 0 25.40 1.40 3 1 0 23.60 1.60 3 1 0 24.40 1.20 3 1 0 26.10 1.60 -4 -1 0 134.19 4.90 -4 -1 0 122.89 3.30 -4 -1 0 123.69 4.10 -4 -1 0 120.19 3.40 -4 -1 0 121.89 3.90 -4 -1 0 126.09 3.90 4 1 0 120.89 3.20 4 1 0 122.09 3.70 4 1 0 126.89 4.10 4 1 0 120.29 4.70 4 1 0 121.69 4.20 -5 -1 0 0.90 1.00 -5 -1 0 0.30 0.60 -5 -1 0 -1.00 0.70 -5 -1 0 0.00 0.60 -5 -1 0 1.90 0.90 -5 -1 0 0.20 0.80 5 1 0 1.30 0.50 5 1 0 -0.20 1.00 5 1 0 0.80 0.90 -6 -1 0 2.30 1.30 -6 -1 0 1.30 0.90 -6 -1 0 0.00 0.90 -6 -1 0 0.80 0.70 -6 -1 0 0.70 1.00 6 1 0 2.80 1.40 6 1 0 1.60 1.10 6 1 0 2.20 0.60 -7 -1 0 -0.50 1.10 -7 -1 0 0.10 0.90 -7 -1 0 -1.90 0.90 7 1 0 -0.40 1.50 7 1 0 1.10 1.40 -8 -1 0 6.30 1.60 -8 -1 0 7.90 2.00 8 1 0 7.90 2.40 8 1 0 5.80 2.10 -9 -1 0 -2.10 1.50 -9 -1 0 -0.20 1.30 9 1 0 -1.00 1.70 9 1 0 -1.20 1.70 8 -2 0 11.40 2.30 8 -2 0 10.60 2.30 -8 2 0 12.10 2.20 7 -2 0 10.10 2.10 7 -2 0 7.00 1.90 -7 2 0 8.20 1.70 -7 2 0 8.50 1.90 6 -2 0 3.90 1.60 6 -2 0 4.10 1.80 6 -2 0 5.10 1.50 -6 2 0 2.10 1.20 -6 2 0 3.40 1.50 -6 2 0 4.40 0.50 5 -2 0 10.20 2.00 5 -2 0 7.10 1.60 5 -2 0 7.30 1.30 5 -2 0 8.80 1.60 -5 2 0 9.80 0.90 -5 2 0 8.60 1.50 -5 2 0 8.90 1.50 -5 2 0 8.10 1.60 4 -2 0 2.50 0.90 4 -2 0 4.00 1.00 4 -2 0 1.80 0.80 4 -2 0 2.90 0.90 4 -2 0 2.70 1.00 -4 2 0 1.10 0.90 -4 2 0 0.20 0.80 -4 2 0 1.90 1.00 -4 2 0 2.50 0.80 3 -2 0 4.50 1.10 3 -2 0 6.50 1.10 3 -2 0 6.60 0.90 3 -2 0 6.90 1.00 -3 2 0 8.40 1.10 -3 2 0 5.90 1.10 -3 2 0 6.60 1.20 -3 2 0 8.70 1.10 2 -2 0 197.08 4.60 2 -2 0 194.98 4.90 2 -2 0 195.78 5.60 2 -2 0 199.48 4.60 -2 2 0 198.28 5.60 -2 2 0 200.98 4.80 -2 2 0 198.08 4.50 -2 2 0 193.58 4.60 1 -2 0 4809.72 80.69 1 -2 0 4726.83 81.69 1 -2 0 4581.34 84.59 1 -2 0 4759.22 84.59 -1 2 0 4732.63 81.09 -1 2 0 4997.10 84.69 -1 2 0 4652.03 80.19 -1 2 0 4505.55 84.69 0 -2 0 2019.40 34.30 0 -2 0 2082.59 37.40 0 -2 0 2114.99 37.10 0 -2 0 2074.09 34.30 0 2 0 2059.39 37.40 0 2 0 2049.89 37.00 0 2 0 2029.60 34.30 0 2 0 2086.39 35.50 0 2 0 2054.19 34.30 -1 -2 0 1728.73 31.00 -1 -2 0 1704.23 29.00 -1 -2 0 1714.13 29.20 -1 -2 0 1734.23 31.80 -1 -2 0 1707.73 30.10 1 2 0 1724.83 31.80 1 2 0 1733.83 29.10 1 2 0 1730.03 30.10 1 2 0 1738.63 31.00 1 2 0 1772.42 29.00 -2 -2 0 24.30 0.80 -2 -2 0 27.50 1.60 -2 -2 0 28.10 1.20 -2 -2 0 24.50 1.40 -2 -2 0 25.20 1.70 -2 -2 0 26.80 1.50 2 2 0 25.90 1.50 2 2 0 25.30 1.30 2 2 0 26.40 1.90 2 2 0 25.30 1.40 -3 -2 0 7.60 1.10 -3 -2 0 6.70 1.20 -3 -2 0 8.90 0.90 -3 -2 0 8.40 1.20 -3 -2 0 7.30 1.00 -3 -2 0 8.00 0.70 3 2 0 6.60 1.00 3 2 0 9.00 1.30 3 2 0 8.30 1.30 3 2 0 8.20 0.90 3 2 0 7.50 1.00 -4 -2 0 6.00 0.80 -4 -2 0 5.30 1.00 -4 -2 0 4.00 1.10 -4 -2 0 7.40 1.30 -4 -2 0 5.30 1.20 -4 -2 0 7.40 1.00 4 2 0 5.00 1.00 4 2 0 4.50 0.80 4 2 0 4.60 1.20 4 2 0 6.90 1.30 4 2 0 6.40 1.20 -5 -2 0 18.30 2.20 -5 -2 0 10.90 1.30 -5 -2 0 13.90 1.40 -5 -2 0 13.20 1.30 -5 -2 0 13.10 1.70 5 2 0 13.80 1.90 5 2 0 14.20 1.30 5 2 0 12.30 2.10 -6 -2 0 5.40 1.10 -6 -2 0 6.00 1.70 -6 -2 0 6.60 1.30 -6 -2 0 4.90 1.40 -6 -2 0 6.00 1.10 6 2 0 3.60 1.40 6 2 0 5.10 1.00 6 2 0 7.80 1.60 -7 -2 0 1.30 1.30 -7 -2 0 1.40 1.00 7 2 0 3.90 1.60 7 2 0 1.80 1.40 -8 -2 0 3.00 1.20 -8 -2 0 1.40 1.20 8 2 0 -1.30 1.40 8 2 0 1.60 1.80 -9 -2 0 2.00 1.40 -9 -2 0 6.30 1.80 9 2 0 4.00 2.00 9 2 0 5.70 2.60 8 -3 0 1.50 1.40 8 -3 0 0.80 1.90 -8 3 0 4.00 1.90 7 -3 0 7.40 1.80 7 -3 0 8.00 1.90 7 -3 0 8.80 2.20 -7 3 0 7.90 1.70 -7 3 0 5.90 1.80 6 -3 0 21.30 2.70 6 -3 0 21.10 2.50 6 -3 0 20.50 3.00 -6 3 0 18.40 1.30 -6 3 0 20.20 1.30 -6 3 0 22.10 2.40 -6 3 0 19.40 2.10 5 -3 0 24.60 2.40 5 -3 0 21.30 2.00 5 -3 0 19.70 2.70 5 -3 0 23.40 2.50 -5 3 0 23.10 2.20 -5 3 0 21.30 1.40 -5 3 0 22.60 2.10 4 -3 0 19.80 2.60 4 -3 0 17.70 1.50 4 -3 0 16.50 2.00 -4 3 0 20.40 1.90 -4 3 0 18.20 1.90 -4 3 0 19.50 1.80 3 -3 0 142.19 5.50 3 -3 0 153.68 4.30 3 -3 0 148.29 4.10 3 -3 0 134.09 4.50 -3 3 0 144.89 4.10 -3 3 0 141.29 4.20 -3 3 0 141.09 4.40 -3 3 0 142.89 5.40 2 -3 0 14.50 1.30 2 -3 0 11.70 1.70 2 -3 0 12.10 1.00 -2 3 0 17.50 1.50 -2 3 0 16.50 1.80 -2 3 0 13.90 1.20 -2 3 0 12.50 1.10 -2 3 0 13.90 1.20 1 -3 0 2.50 0.70 1 -3 0 3.10 0.70 1 -3 0 2.80 0.80 1 -3 0 2.20 1.10 -1 3 0 2.70 0.60 -1 3 0 3.50 0.80 -1 3 0 1.80 0.90 -1 3 0 2.40 0.80 -1 3 0 3.60 0.80 0 -3 0 17.80 1.40 0 -3 0 19.20 1.60 0 -3 0 19.00 1.20 0 -3 0 24.10 1.60 0 3 0 20.80 1.50 0 3 0 20.10 1.40 0 3 0 20.40 1.40 0 3 0 18.90 1.20 0 3 0 21.10 1.50 -1 -3 0 69.29 2.40 -1 -3 0 71.59 2.50 -1 -3 0 72.99 2.40 -1 -3 0 70.09 2.80 1 3 0 71.39 2.40 1 3 0 71.29 2.30 1 3 0 68.29 2.70 1 3 0 66.69 2.40 1 3 0 68.59 2.80 -2 -3 0 433.96 9.40 -2 -3 0 442.56 9.20 -2 -3 0 443.16 10.40 -2 -3 0 435.66 8.40 -2 -3 0 443.66 8.20 -2 -3 0 439.36 8.90 2 3 0 432.36 9.30 2 3 0 440.96 8.80 2 3 0 434.96 9.10 2 3 0 434.56 10.30 -3 -3 0 272.57 6.60 -3 -3 0 288.57 7.00 -3 -3 0 284.77 7.00 -3 -3 0 286.07 6.10 -3 -3 0 293.37 8.20 3 3 0 288.17 6.90 3 3 0 298.47 6.90 3 3 0 291.27 6.70 3 3 0 281.97 8.00 -4 -3 0 10.80 0.50 -4 -3 0 11.40 1.50 -4 -3 0 12.90 1.60 -4 -3 0 14.10 1.80 -4 -3 0 13.60 1.20 -4 -3 0 13.20 0.50 4 3 0 14.30 1.50 4 3 0 13.60 1.70 4 3 0 15.60 1.60 4 3 0 9.90 1.70 -5 -3 0 118.09 3.80 -5 -3 0 114.19 4.00 -5 -3 0 111.49 4.10 -5 -3 0 114.59 2.90 -5 -3 0 113.99 4.60 5 3 0 113.49 3.90 5 3 0 112.19 4.40 5 3 0 116.59 5.40 -6 -3 0 17.50 1.20 -6 -3 0 15.20 1.80 -6 -3 0 17.90 2.20 6 3 0 15.80 1.60 6 3 0 16.20 2.30 6 3 0 14.00 2.40 -7 -3 0 0.20 1.20 -7 -3 0 -0.10 0.90 7 3 0 -1.30 1.60 7 3 0 -0.80 0.90 -8 -3 0 1.70 1.50 -8 -3 0 1.60 1.20 8 3 0 4.30 1.60 8 3 0 4.00 2.20 8 -4 0 4.20 2.30 8 -4 0 6.30 1.90 -8 4 0 8.10 2.40 -8 4 0 5.30 1.80 7 -4 0 -2.10 1.00 7 -4 0 -1.20 1.50 7 -4 0 -0.90 1.80 -7 4 0 0.40 1.40 -7 4 0 -0.70 1.10 6 -4 0 8.80 2.20 6 -4 0 8.50 2.20 6 -4 0 8.50 1.80 -6 4 0 7.90 1.90 -6 4 0 11.10 1.80 5 -4 0 56.09 3.50 5 -4 0 58.19 4.50 5 -4 0 55.79 3.30 -5 4 0 57.59 2.60 -5 4 0 51.09 3.10 -5 4 0 54.39 3.00 4 -4 0 0.70 0.70 4 -4 0 0.90 1.20 4 -4 0 0.00 1.40 -4 4 0 1.30 1.10 -4 4 0 -0.90 0.70 -4 4 0 1.10 0.80 3 -4 0 16.30 2.00 3 -4 0 20.10 1.80 3 -4 0 20.40 1.60 3 -4 0 15.10 2.10 -3 4 0 15.80 1.80 -3 4 0 17.40 1.60 -3 4 0 16.20 1.80 -3 4 0 15.80 1.60 2 -4 0 24.80 2.30 2 -4 0 26.30 1.90 2 -4 0 26.30 1.90 -2 4 0 22.80 1.60 -2 4 0 26.10 2.00 -2 4 0 27.10 2.00 -2 4 0 26.20 2.50 -2 4 0 24.50 1.70 1 -4 0 1909.41 32.70 1 -4 0 1901.91 34.90 1 -4 0 1831.02 32.80 1 -4 0 1873.11 36.20 -1 4 0 1873.21 36.20 -1 4 0 1894.21 32.70 -1 4 0 1879.51 33.70 -1 4 0 1868.71 32.60 -1 4 0 1877.71 33.40 0 -4 0 26.70 2.10 0 -4 0 26.00 1.80 0 -4 0 29.90 1.70 0 -4 0 28.50 2.00 0 4 0 25.70 1.80 0 4 0 29.00 2.00 0 4 0 28.90 1.90 0 4 0 30.30 1.90 0 4 0 27.30 1.70 -1 -4 0 -0.70 0.70 -1 -4 0 0.70 0.60 -1 -4 0 0.60 0.80 -1 -4 0 0.30 0.70 1 4 0 0.20 0.60 1 4 0 1.30 0.90 1 4 0 -0.30 0.50 1 4 0 -0.60 0.40 1 4 0 -0.20 0.60 -2 -4 0 271.77 6.70 -2 -4 0 253.07 6.30 -2 -4 0 258.67 7.60 -2 -4 0 266.97 5.90 2 4 0 265.07 7.50 2 4 0 260.87 6.50 2 4 0 266.47 6.40 2 4 0 269.97 6.90 2 4 0 269.97 5.80 -3 -4 0 82.19 3.50 -3 -4 0 80.09 2.80 -3 -4 0 80.19 4.10 -3 -4 0 79.29 3.20 3 4 0 77.19 3.90 3 4 0 82.89 3.50 3 4 0 76.89 3.10 3 4 0 82.69 3.40 -4 -4 0 161.68 4.50 -4 -4 0 159.38 5.00 -4 -4 0 168.78 5.60 4 4 0 166.08 5.40 4 4 0 166.98 6.50 4 4 0 166.98 5.30 -5 -4 0 100.59 4.40 -5 -4 0 99.79 3.60 -5 -4 0 100.89 4.20 5 4 0 99.19 5.20 5 4 0 103.49 4.50 -6 -4 0 -2.00 1.00 -6 -4 0 -0.10 0.90 6 4 0 -1.70 1.60 6 4 0 0.50 1.20 -7 -4 0 2.90 1.20 -7 -4 0 0.10 1.40 7 4 0 2.30 2.00 7 4 0 3.90 1.80 -8 -4 0 13.10 2.20 -8 -4 0 18.80 2.80 8 4 0 5.00 2.60 8 4 0 16.30 2.60 7 -5 0 -2.90 2.10 7 -5 0 1.80 1.60 7 -5 0 0.10 1.30 -7 5 0 -1.20 1.00 -7 5 0 0.20 1.50 6 -5 0 16.50 2.60 6 -5 0 10.90 2.70 6 -5 0 12.90 2.00 -6 5 0 16.10 2.50 -6 5 0 11.90 1.90 5 -5 0 0.80 1.40 5 -5 0 2.80 1.60 -5 5 0 1.30 1.10 -5 5 0 1.80 1.00 -5 5 0 3.00 1.30 4 -5 0 3.20 1.00 4 -5 0 3.60 1.30 4 -5 0 1.50 1.40 -4 5 0 5.20 1.30 -4 5 0 2.10 1.00 -4 5 0 0.70 1.00 3 -5 0 34.70 2.80 3 -5 0 35.70 3.20 -3 5 0 31.60 2.10 -3 5 0 34.70 2.50 -3 5 0 33.40 2.30 2 -5 0 75.59 3.30 2 -5 0 85.59 4.60 2 -5 0 75.99 3.50 2 -5 0 76.59 3.30 -2 5 0 74.39 3.30 -2 5 0 77.49 3.00 -2 5 0 80.49 3.50 1 -5 0 2.50 1.20 1 -5 0 1.10 1.00 1 -5 0 0.00 0.80 1 -5 0 0.30 0.90 -1 5 0 -0.50 0.60 -1 5 0 -0.40 0.80 -1 5 0 0.00 0.90 -1 5 0 0.30 0.90 -1 5 0 -0.20 0.80 0 -5 0 5.80 1.50 0 -5 0 6.20 1.30 0 -5 0 7.80 1.40 0 -5 0 4.50 1.10 0 5 0 6.60 1.40 0 5 0 7.00 1.20 0 5 0 5.70 1.20 0 5 0 9.70 1.40 -1 -5 0 74.59 3.20 -1 -5 0 72.29 3.50 -1 -5 0 74.39 3.30 -1 -5 0 74.69 3.30 1 5 0 70.09 3.40 1 5 0 73.89 3.10 1 5 0 76.19 3.20 -2 -5 0 46.80 2.70 -2 -5 0 49.80 2.60 -2 -5 0 51.99 3.40 -2 -5 0 47.10 2.30 2 5 0 46.00 2.60 2 5 0 48.10 3.20 2 5 0 48.60 2.10 -3 -5 0 80.59 3.70 -3 -5 0 74.59 2.10 -3 -5 0 74.49 3.40 3 5 0 72.39 3.30 3 5 0 73.09 4.30 -4 -5 0 42.70 2.70 -4 -5 0 43.10 3.00 4 5 0 46.50 3.90 4 5 0 46.60 3.00 -5 -5 0 1.00 1.00 -5 -5 0 0.20 1.20 5 5 0 -1.70 0.90 5 5 0 -0.80 1.20 -6 -5 0 39.80 3.20 -6 -5 0 34.10 2.60 6 5 0 41.00 4.30 6 5 0 31.00 3.10 -7 -5 0 9.80 2.00 -7 -5 0 11.30 1.90 7 5 0 13.20 2.50 7 5 0 7.10 2.30 -8 -5 0 0.90 1.40 8 5 0 0.20 2.30 7 -6 0 -6.30 2.00 -7 6 0 -0.10 1.30 6 -6 0 1.90 1.60 6 -6 0 2.00 1.30 6 -6 0 -3.00 2.10 -6 6 0 2.80 1.50 -6 6 0 0.00 1.30 5 -6 0 0.70 1.60 5 -6 0 -3.00 1.80 -5 6 0 -0.70 1.20 -5 6 0 -2.00 0.80 4 -6 0 0.20 1.50 4 -6 0 -0.70 1.70 -4 6 0 -0.90 1.20 -4 6 0 0.50 0.90 3 -6 0 1.90 1.20 3 -6 0 3.40 1.60 3 -6 0 3.10 2.10 -3 6 0 4.90 1.30 -3 6 0 2.00 0.90 2 -6 0 61.19 3.70 2 -6 0 67.89 3.60 2 -6 0 63.69 4.50 -2 6 0 70.79 3.60 -2 6 0 66.99 3.10 1 -6 0 3.90 1.50 1 -6 0 2.70 1.20 1 -6 0 4.40 1.60 -1 6 0 5.50 1.20 -1 6 0 4.60 1.20 0 -6 0 7.40 1.70 0 -6 0 8.90 1.50 0 -6 0 8.10 1.60 0 6 0 7.20 1.30 0 6 0 9.30 1.60 -1 -6 0 22.40 2.00 -1 -6 0 21.20 2.00 -1 -6 0 23.40 2.40 1 6 0 23.90 2.00 1 6 0 22.90 2.60 1 6 0 23.50 2.20 -2 -6 0 15.30 1.90 -2 -6 0 16.50 1.90 -2 -6 0 19.30 1.90 2 6 0 19.40 1.90 2 6 0 14.40 1.50 2 6 0 12.80 2.00 -3 -6 0 3.60 1.20 3 6 0 4.40 1.30 3 6 0 5.60 1.70 -4 -6 0 19.30 2.10 4 6 0 16.90 2.80 4 6 0 18.70 2.30 -5 -6 0 0.70 1.40 5 6 0 1.80 1.40 5 6 0 0.40 1.80 -6 -6 0 10.00 2.20 6 6 0 6.70 2.40 6 6 0 6.90 2.00 -7 -6 0 2.50 1.90 -7 -6 0 -0.90 1.30 7 6 0 -1.50 1.50 7 6 0 1.80 1.80 6 -7 0 -0.80 1.80 6 -7 0 -2.40 2.60 -6 7 0 -2.00 1.60 5 -7 0 -3.40 2.20 5 -7 0 1.70 1.80 -5 7 0 0.70 1.50 -5 7 0 0.70 1.00 4 -7 0 -2.10 1.30 4 -7 0 1.00 1.70 -4 7 0 0.30 1.30 -4 7 0 0.50 1.00 3 -7 0 -0.60 1.80 3 -7 0 -0.60 0.90 -3 7 0 0.40 0.90 -3 7 0 0.70 1.40 2 -7 0 0.00 1.80 2 -7 0 1.40 1.60 -2 7 0 3.70 1.10 -2 7 0 1.60 1.40 1 -7 0 2.30 1.50 1 -7 0 6.90 2.10 -1 7 0 3.90 1.20 -1 7 0 4.20 1.30 0 -7 0 2.50 1.70 0 -7 0 1.70 1.20 0 7 0 1.50 1.30 0 7 0 -0.50 0.90 -1 -7 0 17.30 2.40 -1 -7 0 14.70 2.20 1 7 0 15.60 2.20 1 7 0 16.80 1.90 -2 -7 0 6.50 1.80 -2 -7 0 7.20 1.50 2 7 0 9.00 1.30 2 7 0 7.40 1.70 2 7 0 9.50 2.20 -3 -7 0 0.60 1.30 3 7 0 -1.20 1.60 3 7 0 0.30 0.90 -4 -7 0 16.00 2.50 4 7 0 11.60 2.20 4 7 0 12.60 2.50 -5 -7 0 9.30 2.20 5 7 0 3.50 1.90 5 7 0 11.80 2.30 -6 -7 0 -2.60 1.40 6 7 0 1.30 1.30 6 7 0 -3.60 1.30 4 -8 0 -4.00 2.20 4 -8 0 0.50 1.90 -4 8 0 -1.70 1.50 3 -8 0 -1.60 2.20 3 -8 0 1.40 1.40 -3 8 0 0.20 1.50 -3 8 0 1.30 1.00 2 -8 0 8.90 2.60 2 -8 0 11.20 2.40 -2 8 0 8.20 1.80 -2 8 0 8.60 1.60 1 -8 0 5.70 2.00 1 -8 0 0.60 1.80 -1 8 0 2.50 1.20 -1 8 0 4.60 1.80 0 -8 0 0.30 1.50 0 -8 0 0.30 1.50 0 8 0 -0.60 0.90 0 8 0 -0.30 1.20 -1 -8 0 4.90 1.60 -1 -8 0 5.90 1.90 1 8 0 5.80 1.60 -2 -8 0 1.20 1.40 -2 -8 0 3.20 1.60 2 8 0 2.90 1.70 2 8 0 2.10 1.80 -3 -8 0 6.30 1.70 3 8 0 5.90 1.80 3 8 0 6.00 2.00 -4 -8 0 20.60 2.90 4 8 0 14.60 2.60 4 8 0 12.50 3.00 -5 -8 0 1.10 1.80 5 8 0 -2.10 2.20 5 8 0 0.30 1.60 2 -9 0 0.80 1.40 2 -9 0 -2.90 2.20 -2 9 0 -0.60 1.20 1 -9 0 -3.30 1.50 1 -9 0 1.00 2.30 -1 9 0 1.20 1.30 -1 9 0 0.50 1.50 0 -9 0 -4.50 1.60 0 -9 0 -3.50 1.40 0 9 0 0.50 1.70 0 9 0 0.10 1.00 -1 -9 0 1.80 1.90 -1 -9 0 -2.30 1.60 1 9 0 -0.50 1.50 1 9 0 3.30 1.30 -2 -9 0 1.50 1.80 2 9 0 6.60 2.10 -3 -9 0 13.70 2.80 3 9 0 13.60 3.10 3 9 0 14.10 2.50 2 9 -1 3.30 2.00 -2 -9 1 1.30 1.90 1 9 -1 0.10 1.60 1 9 -1 2.50 1.10 -1 -9 1 -0.30 1.80 0 9 -1 -0.20 1.60 0 -9 1 -1.30 1.60 0 -9 1 -3.00 1.60 -1 9 -1 -0.20 1.70 1 -9 1 -2.50 1.70 1 -9 1 -3.10 1.90 -2 9 -1 -1.50 1.60 2 -9 1 -1.90 1.20 2 -9 1 -1.20 2.10 5 8 -1 -1.90 1.60 4 8 -1 1.10 1.70 4 8 -1 3.40 1.80 -4 -8 1 4.20 1.60 3 8 -1 16.40 2.50 3 8 -1 8.30 2.60 -3 -8 1 10.40 2.10 2 8 -1 9.50 2.10 -2 -8 1 6.30 2.00 -2 -8 1 3.40 1.60 1 8 -1 -0.80 1.30 -1 -8 1 -0.30 1.10 0 8 -1 1.70 0.90 0 8 -1 1.10 1.50 0 -8 1 3.30 1.80 0 -8 1 3.30 1.90 -1 8 -1 -1.10 1.00 -1 8 -1 0.50 0.90 1 -8 1 -2.60 1.60 1 -8 1 -1.70 0.90 -2 8 -1 2.70 1.10 -2 8 -1 3.50 1.70 2 -8 1 1.20 2.20 2 -8 1 -0.30 1.10 3 -8 1 -1.70 2.10 3 -8 1 2.00 1.90 -4 8 -1 -1.10 1.10 4 -8 1 -2.00 2.30 4 -8 1 -2.20 1.10 6 7 -1 1.10 2.60 6 7 -1 12.20 2.60 -6 -7 1 8.40 2.40 5 7 -1 -1.60 1.30 5 7 -1 1.10 1.20 -5 -7 1 1.60 1.40 4 7 -1 46.50 4.60 4 7 -1 55.49 3.90 -4 -7 1 49.60 3.50 3 7 -1 16.70 2.50 3 7 -1 14.40 2.70 -3 -7 1 14.60 2.30 -3 -7 1 10.90 1.50 2 7 -1 -0.20 1.20 2 7 -1 1.10 1.30 -2 -7 1 -1.20 1.10 -2 -7 1 -1.00 1.20 1 7 -1 0.00 0.90 1 7 -1 0.20 0.90 -1 -7 1 -0.80 1.20 -1 -7 1 -3.40 1.10 0 7 -1 7.00 1.70 0 7 -1 6.50 1.30 0 -7 1 3.60 1.70 0 -7 1 4.60 1.70 -1 7 -1 7.60 1.30 -1 7 -1 8.70 1.90 1 -7 1 7.30 2.20 1 -7 1 11.50 2.10 -2 7 -1 0.90 0.80 -2 7 -1 1.80 1.20 2 -7 1 -0.10 1.80 2 -7 1 1.90 1.30 -3 7 -1 0.80 0.90 3 -7 1 0.90 1.50 3 -7 1 -2.70 1.80 -4 7 -1 -0.90 1.10 -4 7 -1 -0.20 0.90 4 -7 1 -1.40 1.40 4 -7 1 -3.40 1.20 -5 7 -1 0.50 1.20 5 -7 1 -1.30 2.40 5 -7 1 -0.90 1.30 7 6 -1 -0.60 1.70 7 6 -1 -3.00 1.40 -7 -6 1 -1.70 1.60 6 6 -1 -3.30 1.80 6 6 -1 0.70 1.60 -6 -6 1 -0.10 1.40 5 6 -1 43.50 4.60 5 6 -1 39.10 3.40 -5 -6 1 38.30 3.30 4 6 -1 53.19 3.60 4 6 -1 49.20 4.40 -4 -6 1 61.19 3.70 3 6 -1 17.00 2.70 3 6 -1 19.50 2.40 -3 -6 1 14.90 2.20 -3 -6 1 18.90 1.70 2 6 -1 4.70 1.30 2 6 -1 4.60 1.50 2 6 -1 4.20 1.00 -2 -6 1 3.90 1.20 -2 -6 1 2.80 1.10 1 6 -1 -0.80 0.60 1 6 -1 -0.30 1.00 -1 -6 1 -1.70 1.00 -1 -6 1 -0.10 1.20 0 6 -1 49.30 3.20 0 6 -1 50.39 3.00 0 -6 1 54.99 3.30 0 -6 1 52.79 3.60 -1 6 -1 21.20 2.30 -1 6 -1 18.10 1.60 1 -6 1 20.30 2.40 1 -6 1 19.30 2.60 -2 6 -1 1.90 1.30 -2 6 -1 1.40 0.80 2 -6 1 1.20 1.70 2 -6 1 0.50 1.30 2 -6 1 1.20 1.30 -3 6 -1 4.60 1.00 3 -6 1 5.70 1.80 3 -6 1 3.30 2.20 -4 6 -1 1.40 0.90 -4 6 -1 -0.10 1.30 4 -6 1 -0.30 2.00 4 -6 1 1.80 1.20 -5 6 -1 2.50 1.30 -5 6 -1 0.20 1.00 5 -6 1 -1.40 2.00 5 -6 1 0.40 1.20 -6 6 -1 -0.70 1.10 -6 6 -1 -0.70 1.50 6 -6 1 -3.20 2.00 6 -6 1 -2.50 1.40 7 5 -1 0.20 1.10 7 5 -1 -1.00 1.30 -7 -5 1 -0.50 1.10 -7 -5 1 -0.20 1.10 6 5 -1 7.90 2.50 6 5 -1 5.30 1.90 -6 -5 1 5.60 1.80 -6 -5 1 4.00 1.30 5 5 -1 68.39 5.00 5 5 -1 65.89 4.00 -5 -5 1 69.89 4.10 -5 -5 1 68.09 3.90 4 5 -1 12.30 2.00 4 5 -1 15.50 2.30 -4 -5 1 16.80 2.20 -4 -5 1 15.20 2.20 -4 -5 1 14.20 0.80 3 5 -1 2.90 1.20 3 5 -1 2.00 1.30 -3 -5 1 2.20 1.10 -3 -5 1 1.40 1.20 -3 -5 1 3.20 0.80 -3 -5 1 2.30 1.00 2 5 -1 51.69 3.20 2 5 -1 51.59 2.90 -2 -5 1 57.99 3.30 -2 -5 1 47.60 2.70 -2 -5 1 48.10 2.70 -2 -5 1 53.19 2.60 1 5 -1 12.80 1.50 1 5 -1 11.80 1.80 1 5 -1 15.50 1.60 -1 -5 1 14.20 1.50 -1 -5 1 12.20 1.80 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2.80 1 4 -4 108.79 4.20 1 4 -4 112.39 4.00 1 4 -4 111.39 3.20 -1 -4 4 112.99 4.80 -1 -4 4 111.99 4.60 -1 -4 4 116.19 4.20 0 4 -4 -0.30 0.50 0 4 -4 0.10 0.70 0 4 -4 0.40 0.90 0 4 -4 0.70 0.40 0 -4 4 1.10 0.90 0 -4 4 2.40 1.30 0 -4 4 2.40 1.00 -1 4 -4 2.10 1.00 -1 4 -4 0.60 0.90 -1 4 -4 2.40 0.90 1 -4 4 3.90 1.20 1 -4 4 0.90 0.70 1 -4 4 0.00 1.20 -2 4 -4 77.29 3.40 -2 4 -4 74.19 3.20 -2 4 -4 72.19 3.10 2 -4 4 69.59 3.20 2 -4 4 75.19 3.40 2 -4 4 76.79 4.60 -3 4 -4 7.20 1.30 -3 4 -4 4.80 1.10 -3 4 -4 7.00 1.40 3 -4 4 5.10 1.90 3 -4 4 4.20 1.10 3 -4 4 7.20 1.50 -4 4 -4 30.20 2.00 -4 4 -4 32.70 1.90 -4 4 -4 25.90 2.40 -4 4 -4 33.40 2.50 4 -4 4 32.30 3.40 4 -4 4 33.10 2.70 4 -4 4 33.80 1.40 -5 4 -4 3.40 0.90 -5 4 -4 2.80 1.40 5 -4 4 1.80 1.40 5 -4 4 6.70 2.50 -6 4 -4 -0.20 1.20 6 -4 4 0.10 1.50 6 -4 4 0.30 0.90 -7 4 -4 -0.10 1.40 7 -4 4 -0.70 1.30 7 -4 4 -4.20 1.90 7 -4 4 2.40 1.40 8 3 -4 -2.80 1.90 7 3 -4 -1.70 1.40 7 3 -4 -2.20 1.70 -7 -3 4 -2.20 1.40 -7 -3 4 0.40 1.40 6 3 -4 23.50 3.20 6 3 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5 0.80 1.40 5 -5 5 2.30 2.00 -6 5 -5 -1.40 1.20 6 -5 5 -3.00 1.90 6 -5 5 -1.40 1.30 7 4 -5 1.90 2.50 7 4 -5 7.70 2.30 -7 -4 5 5.60 1.90 -7 -4 5 1.60 1.90 6 4 -5 -1.00 1.20 6 4 -5 -0.80 1.40 -6 -4 5 0.50 1.10 -6 -4 5 -3.00 1.40 5 4 -5 0.00 1.80 5 4 -5 0.20 1.50 -5 -4 5 2.40 1.20 -5 -4 5 1.10 1.50 -5 -4 5 -1.20 1.00 4 4 -5 -0.10 1.10 4 4 -5 -0.80 1.10 -4 -4 5 -0.30 1.50 -4 -4 5 -1.00 1.00 -4 -4 5 -0.80 0.90 3 4 -5 214.28 7.70 3 4 -5 217.28 7.10 -3 -4 5 214.18 7.30 -3 -4 5 220.58 7.20 -3 -4 5 225.38 6.80 2 4 -5 31.60 2.40 2 4 -5 32.00 2.00 -2 -4 5 28.20 2.60 -2 -4 5 38.10 3.00 -2 -4 5 37.30 2.70 1 4 -5 47.60 2.90 1 4 -5 50.49 2.80 1 4 -5 46.70 2.00 -1 -4 5 47.80 3.30 -1 -4 5 46.30 2.80 -1 -4 5 50.09 3.40 0 4 -5 1.60 0.40 0 4 -5 1.50 0.80 0 4 -5 1.60 1.00 0 -4 5 2.10 0.80 0 -4 5 1.60 1.30 0 -4 5 -0.60 1.10 -1 4 -5 12.30 1.70 -1 4 -5 13.80 1.70 1 -4 5 11.90 1.70 1 -4 5 9.90 1.70 1 -4 5 10.90 2.10 -2 4 -5 127.99 5.20 -2 4 -5 128.89 4.50 -2 4 -5 137.19 4.60 2 -4 5 132.69 6.20 2 -4 5 125.59 4.70 2 -4 5 125.69 4.50 -3 4 -5 23.20 2.20 -3 4 -5 21.90 2.00 -3 4 -5 21.20 2.00 3 -4 5 20.20 2.10 3 -4 5 21.90 2.20 3 -4 5 16.30 2.80 -4 4 -5 21.20 2.20 -4 4 -5 19.70 1.80 -4 4 -5 16.90 2.10 -4 4 -5 20.30 1.70 4 -4 5 16.90 3.00 4 -4 5 21.40 2.30 -5 4 -5 10.60 1.90 5 -4 5 8.00 2.30 5 -4 5 9.30 1.90 -6 4 -5 13.50 2.20 6 -4 5 9.00 2.90 6 -4 5 15.00 2.50 -7 4 -5 15.00 2.50 7 -4 5 12.40 3.10 7 3 -5 3.30 2.00 7 3 -5 -2.30 1.80 -7 -3 5 1.10 1.60 -7 -3 5 -1.90 1.70 6 3 -5 -1.40 1.70 6 3 -5 -1.30 1.50 -6 -3 5 -0.90 1.40 -6 -3 5 0.40 1.40 5 3 -5 71.29 4.50 5 3 -5 73.49 4.50 -5 -3 5 79.79 4.20 -5 -3 5 76.49 4.40 4 3 -5 10.80 2.30 4 3 -5 10.60 1.90 -4 -3 5 11.80 1.80 -4 -3 5 15.30 2.30 3 3 -5 25.80 2.00 3 3 -5 26.90 2.90 3 3 -5 26.90 2.60 -3 -3 5 32.70 2.30 -3 -3 5 31.10 2.80 -3 -3 5 32.50 2.70 2 3 -5 116.39 4.20 2 3 -5 113.59 4.30 2 3 -5 124.29 3.90 -2 -3 5 116.99 4.20 -2 -3 5 123.19 4.90 -2 -3 5 121.89 4.80 1 3 -5 142.89 4.40 1 3 -5 138.39 3.70 1 3 -5 133.09 4.50 -1 -3 5 139.09 5.10 -1 -3 5 129.99 4.30 -1 -3 5 139.49 5.40 0 3 -5 152.48 3.30 0 3 -5 147.59 4.90 0 3 -5 157.88 4.60 0 3 -5 152.48 4.60 0 -3 5 149.99 5.10 0 -3 5 150.28 5.70 0 -3 5 154.18 4.60 -1 3 -5 19.80 2.20 -1 3 -5 18.10 1.60 -1 3 -5 17.70 1.70 -1 3 -5 18.70 1.50 1 -3 5 15.00 2.10 1 -3 5 16.60 1.60 1 -3 5 14.20 1.80 -2 3 -5 1.00 0.80 -2 3 -5 -0.40 0.70 -2 3 -5 -0.40 0.60 2 -3 5 0.50 0.90 2 -3 5 0.20 0.70 2 -3 5 -1.00 1.10 -3 3 -5 65.09 2.90 -3 3 -5 67.99 3.00 -3 3 -5 69.29 2.90 3 -3 5 69.09 3.00 3 -3 5 72.39 3.20 3 -3 5 65.39 4.40 -4 3 -5 12.10 1.40 -4 3 -5 10.80 1.60 -4 3 -5 11.10 1.50 -4 3 -5 10.90 1.60 4 -3 5 10.00 2.40 4 -3 5 11.50 1.40 4 -3 5 12.60 1.90 4 -3 5 10.10 0.80 -5 3 -5 4.20 0.80 -5 3 -5 5.70 1.40 -5 3 -5 4.70 1.10 -5 3 -5 4.40 1.30 5 -3 5 3.40 0.70 5 -3 5 4.90 1.40 5 -3 5 3.10 1.70 -6 3 -5 8.40 1.80 6 -3 5 5.10 1.60 6 -3 5 5.80 2.00 -7 3 -5 -0.10 1.30 7 -3 5 -0.10 1.40 7 -3 5 2.30 1.70 7 2 -5 -1.80 1.50 7 2 -5 1.50 1.40 -7 -2 5 -1.00 1.00 -7 -2 5 -2.20 1.20 6 2 -5 12.50 2.50 6 2 -5 11.50 2.40 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20.40 3.10 -3 4 11 17.10 2.90 2 -4 -11 2.50 1.30 2 -4 -11 -0.20 1.40 -2 4 11 -0.90 0.90 -2 4 11 -1.90 1.50 1 -4 -11 17.10 2.80 1 -4 -11 19.70 1.80 -1 4 11 14.90 2.60 -1 4 11 17.10 2.70 0 -4 -11 35.20 1.40 0 -4 -11 26.70 3.40 0 4 11 37.50 3.30 0 4 11 36.20 3.70 0 4 11 37.90 2.80 -1 -4 -11 2.40 1.60 -1 -4 -11 1.40 1.30 1 4 11 2.80 1.50 1 4 11 4.20 1.70 1 4 11 3.50 1.30 -2 -4 -11 2.30 1.70 -2 -4 -11 6.20 1.80 2 4 11 5.70 1.80 2 4 11 4.60 1.60 2 4 11 3.70 1.50 -3 -4 -11 -0.70 1.40 -3 -4 -11 -1.20 1.20 3 4 11 1.70 1.20 3 4 11 0.40 1.10 3 4 11 -0.10 1.00 3 4 11 0.40 1.20 -4 -4 -11 3.30 1.80 -4 -4 -11 -0.60 1.50 4 4 11 -0.10 1.30 4 4 11 0.20 1.30 4 4 11 0.20 1.10 4 4 11 2.20 1.10 -5 -4 -11 -0.50 1.70 -5 -4 -11 -0.60 1.50 5 4 11 -1.40 0.80 5 4 11 0.90 1.30 5 4 11 -0.10 1.00 3 -5 -11 1.40 1.30 3 -5 -11 0.60 1.50 -3 5 11 2.10 2.00 -3 5 11 2.40 2.00 2 -5 -11 13.70 2.00 2 -5 -11 12.80 2.60 -2 5 11 9.30 2.50 -2 5 11 12.40 2.60 1 -5 -11 76.99 4.80 1 -5 -11 75.79 3.20 -1 5 11 81.69 5.30 -1 5 11 70.09 4.70 0 -5 -11 11.10 2.50 0 -5 -11 9.60 1.10 0 5 11 10.10 2.30 -1 -5 -11 0.80 1.60 1 5 11 2.40 1.50 1 5 11 0.70 1.00 -2 -5 -11 0.00 1.50 -2 -5 -11 1.00 1.70 2 5 11 1.40 1.30 2 5 11 0.40 1.20 -3 -5 -11 2.40 1.80 -3 -5 -11 0.80 1.10 3 5 11 0.00 1.00 3 5 11 -0.20 1.00 -4 -5 -11 -0.20 1.50 -4 -5 -11 0.60 1.80 4 5 11 1.70 1.70 4 5 11 1.50 1.10 4 5 11 1.20 1.20 -5 -5 -11 -0.80 1.70 5 5 11 1.40 1.50 2 -6 -11 3.00 1.50 2 -6 -11 0.10 1.50 -2 6 11 2.70 1.80 1 -6 -11 5.40 2.00 1 -6 -11 5.10 1.40 -1 6 11 5.40 2.10 0 -6 -11 6.40 1.10 0 -6 -11 4.80 2.00 0 6 11 2.30 1.90 -1 -6 -11 5.10 1.90 1 6 11 3.70 1.60 -2 -6 -11 3.80 1.90 2 6 11 5.10 1.80 -3 -6 -11 -0.10 1.40 -3 -6 -11 0.40 1.10 3 6 11 3.50 1.60 3 6 11 0.80 1.30 -4 -6 -11 1.20 2.00 -4 -6 -11 -0.90 1.40 4 6 11 1.40 1.40 0 -7 -11 0.70 1.00 0 -7 -11 0.40 1.60 0 7 11 1.40 1.40 -1 -7 -11 1.90 1.70 1 7 11 5.20 2.00 -2 -7 -11 12.80 2.80 -2 -2 12 2.90 2.20 -2 -2 12 0.30 2.10 1 2 -12 3.60 1.30 -1 -2 12 0.70 2.00 -1 -2 12 2.90 1.80 0 2 -12 -0.50 0.90 0 -2 12 -1.60 2.10 0 -2 12 0.30 1.30 -1 2 -12 1.80 1.00 -1 2 -12 2.40 1.70 1 -2 12 1.50 2.20 1 -2 12 1.30 1.70 -2 2 -12 1.50 1.70 -2 2 -12 2.20 1.00 -2 2 -12 2.80 1.30 2 -2 12 2.20 2.20 2 -2 12 2.50 1.70 -3 2 -12 -2.30 1.10 -3 2 -12 0.50 1.20 -3 2 -12 0.40 0.90 3 -2 12 -0.80 1.50 3 -2 12 -1.50 1.30 2 1 -12 2.10 1.30 -2 -1 12 0.40 1.20 -2 -1 12 1.20 2.00 -2 -1 12 2.80 2.00 1 1 -12 0.60 1.00 -1 -1 12 -0.70 1.60 -1 -1 12 2.60 1.70 0 1 -12 5.50 1.30 0 1 -12 6.60 1.80 0 -1 12 4.90 1.90 0 -1 12 2.80 2.10 -1 1 -12 4.10 1.00 -1 1 -12 4.10 1.70 1 -1 12 3.10 1.80 1 -1 12 8.50 2.20 -2 1 -12 6.30 1.50 -2 1 -12 8.00 1.90 -2 1 -12 4.30 0.90 2 -1 12 2.70 1.60 2 -1 12 7.80 2.70 -3 1 -12 0.60 0.70 -3 1 -12 1.10 1.40 -3 1 -12 0.70 1.20 3 -1 12 0.00 1.40 3 -1 12 2.00 1.90 -4 1 -12 7.00 2.10 -4 1 -12 1.80 1.50 4 -1 12 4.80 2.20 4 -1 12 1.80 1.50 3 0 -12 -0.60 1.20 -3 0 12 2.30 2.10 -3 0 12 0.80 1.40 2 0 -12 26.10 3.50 2 0 -12 23.10 2.30 -2 0 12 18.60 2.40 -2 0 12 22.60 3.40 1 0 -12 3.70 1.80 1 0 -12 3.30 1.10 -1 0 12 4.50 2.00 -1 0 12 2.20 1.30 0 0 -12 0.20 1.10 0 0 -12 1.30 0.80 0 0 12 -2.70 1.40 0 0 12 -0.90 1.40 0 0 12 0.80 1.00 -1 0 -12 3.00 1.60 -1 0 -12 1.80 0.70 -1 0 -12 0.30 1.00 1 0 12 3.00 1.60 1 0 12 -0.70 1.70 1 0 12 0.60 1.00 -2 0 -12 9.50 1.70 -2 0 -12 5.10 1.80 2 0 12 9.90 2.10 2 0 12 8.30 2.60 -3 0 -12 2.90 1.40 -3 0 -12 6.00 2.00 3 0 12 5.90 1.70 3 0 12 4.20 2.20 -4 0 -12 2.70 1.50 -4 0 -12 2.20 1.70 4 0 12 1.60 2.00 4 0 12 1.10 1.20 3 -1 -12 18.50 3.00 3 -1 -12 15.80 2.20 -3 1 12 19.40 2.80 -3 1 12 17.80 3.10 2 -1 -12 1.60 1.20 2 -1 -12 0.50 1.10 -2 1 12 0.20 1.20 -2 1 12 1.50 1.50 1 -1 -12 -1.00 0.70 1 -1 -12 1.30 1.20 -1 1 12 0.90 1.30 -1 1 12 -2.20 0.80 0 -1 -12 1.50 0.60 0 -1 -12 -1.20 1.10 0 1 12 -0.30 0.90 0 1 12 1.00 1.60 -1 -1 -12 21.10 2.00 -1 -1 -12 26.90 2.90 -1 -1 -12 22.10 1.00 1 1 12 21.40 2.90 1 1 12 22.40 3.50 1 1 12 21.70 2.20 -2 -1 -12 3.00 1.40 -2 -1 -12 2.30 1.30 2 1 12 2.90 1.90 2 1 12 2.70 1.20 2 1 12 0.80 1.30 -3 -1 -12 4.30 1.80 -3 -1 -12 3.40 1.50 3 1 12 1.60 1.60 3 1 12 2.00 1.30 3 1 12 4.90 1.30 -4 -1 -12 4.40 1.80 -4 -1 -12 0.40 1.40 4 1 12 0.00 1.10 4 1 12 0.90 1.20 -5 -1 -12 24.70 3.10 3 -2 -12 0.80 1.50 3 -2 -12 3.50 1.40 -3 2 12 2.40 2.10 -3 2 12 2.70 1.80 2 -2 -12 3.70 1.60 2 -2 -12 6.00 1.40 -2 2 12 3.10 1.60 -2 2 12 3.00 2.00 1 -2 -12 4.20 1.00 1 -2 -12 3.70 1.80 -1 2 12 2.50 1.30 -1 2 12 4.00 2.00 0 -2 -12 1.60 1.20 0 -2 -12 1.40 0.50 0 -2 -12 0.60 1.10 0 2 12 2.00 1.10 0 2 12 1.90 1.60 -1 -2 -12 15.10 2.10 -1 -2 -12 12.10 2.60 1 2 12 11.60 2.30 1 2 12 10.90 1.90 -2 -2 -12 0.00 1.40 -2 -2 -12 -0.30 1.10 2 2 12 1.20 1.40 2 2 12 0.30 1.50 2 2 12 -0.10 0.80 -3 -2 -12 9.80 2.40 -3 -2 -12 16.10 2.40 3 2 12 12.90 2.10 3 2 12 15.30 2.90 3 2 12 12.40 2.20 -4 -2 -12 0.30 1.60 -4 -2 -12 -0.80 0.90 4 2 12 1.20 1.50 4 2 12 0.10 1.00 4 2 12 -0.90 1.00 4 2 12 -0.40 1.30 -5 -2 -12 -0.20 1.50 -5 -2 -12 0.50 1.30 5 2 12 1.50 1.50 5 2 12 2.00 1.60 3 -3 -12 -0.50 1.40 3 -3 -12 1.40 1.30 -3 3 12 0.70 1.60 -3 3 12 3.00 2.30 2 -3 -12 1.70 1.10 2 -3 -12 0.50 1.40 -2 3 12 -0.70 0.80 -2 3 12 0.40 1.70 1 -3 -12 0.20 0.80 1 -3 -12 1.30 1.30 -1 3 12 0.00 1.60 -1 3 12 0.80 1.20 0 -3 -12 2.00 1.20 0 3 12 5.60 2.00 0 3 12 3.30 1.40 -1 -3 -12 0.50 1.40 -1 -3 -12 -0.10 1.10 1 3 12 1.50 1.00 1 3 12 1.10 1.50 -2 -3 -12 3.10 1.50 -2 -3 -12 4.10 1.60 2 3 12 4.20 1.80 2 3 12 7.00 1.70 2 3 12 4.10 1.70 -3 -3 -12 5.80 1.80 -3 -3 -12 4.80 1.80 3 3 12 4.10 1.70 3 3 12 3.50 1.60 3 3 12 4.10 1.70 3 3 12 4.30 1.50 -4 -3 -12 1.30 1.70 -4 -3 -12 4.30 1.90 4 3 12 -0.10 1.20 4 3 12 2.20 1.10 4 3 12 0.50 1.20 4 3 12 -0.10 1.30 3 -4 -12 3.90 1.90 -3 4 12 1.80 1.80 2 -4 -12 2.60 1.30 2 -4 -12 -0.80 1.20 -2 4 12 0.70 1.80 -2 4 12 -0.20 1.50 1 -4 -12 1.20 1.50 1 -4 -12 0.40 0.80 -1 4 12 0.30 1.30 -1 4 12 0.50 1.70 0 -4 -12 0.30 1.60 0 4 12 0.50 1.30 0 4 12 0.40 1.70 -1 -4 -12 0.40 1.50 -1 -4 -12 2.50 1.50 1 4 12 1.20 1.20 1 4 12 1.20 1.40 1 4 12 1.10 1.00 -2 -4 -12 7.40 1.90 -2 -4 -12 2.70 1.50 2 4 12 4.40 1.50 2 4 12 4.80 1.80 2 4 12 4.40 1.60 -3 -4 -12 -1.00 1.50 -3 -4 -12 -2.80 1.00 3 4 12 1.90 1.40 3 4 12 1.00 1.10 3 4 12 0.60 1.20 3 4 12 0.50 1.00 -4 -4 -12 0.80 1.70 -4 -4 -12 0.40 1.70 4 4 12 0.60 0.90 4 4 12 1.40 1.20 4 4 12 1.20 1.60 4 4 12 0.20 1.20 2 -5 -12 2.80 1.30 2 -5 -12 2.70 1.80 -2 5 12 2.50 2.00 -2 5 12 2.10 1.80 1 -5 -12 0.60 0.90 1 -5 -12 3.70 1.80 -1 5 12 -0.80 1.50 -1 5 12 2.50 1.90 0 -5 -12 2.80 1.70 0 5 12 3.40 1.60 0 5 12 2.60 1.60 -1 -5 -12 0.70 1.60 1 5 12 1.50 1.30 1 5 12 2.60 1.70 -2 -5 -12 3.00 1.80 -2 -5 -12 1.60 1.40 2 5 12 0.20 1.30 2 5 12 3.30 1.60 2 5 12 3.10 1.50 -3 -5 -12 0.60 1.60 -3 -5 -12 -1.60 1.00 3 5 12 0.00 1.20 3 5 12 0.20 1.20 3 5 12 1.40 1.40 3 5 12 1.50 1.40 0 -6 -12 3.80 1.80 0 6 12 0.60 1.70 -1 -6 -12 0.30 1.30 1 6 12 -1.00 1.40 -2 -6 -12 1.70 1.50 0 1 -13 5.80 2.10 0 -1 13 4.60 2.30 0 -1 13 1.80 1.90 -1 1 -13 1.00 1.70 1 -1 13 0.10 1.70 1 -1 13 -2.70 1.80 1 0 -13 9.70 1.50 1 0 -13 7.30 2.00 -1 0 13 7.30 2.70 -1 0 13 9.80 2.40 0 0 -13 -0.80 1.40 0 0 -13 0.80 0.80 0 0 13 3.70 2.00 0 0 13 -0.90 1.90 -1 0 -13 5.90 2.20 1 0 13 4.70 2.60 1 0 13 9.00 2.30 -2 0 -13 8.80 2.40 -2 0 -13 4.00 1.70 2 0 13 6.50 2.00 2 0 13 2.30 1.80 2 -1 -13 18.10 3.10 1 -1 -13 1.40 1.60 1 -1 -13 3.80 1.10 -1 1 13 2.30 2.00 -1 1 13 -0.20 1.30 0 -1 -13 3.60 1.80 0 -1 -13 6.60 0.90 0 1 13 6.30 2.50 0 1 13 4.00 1.50 0 1 13 7.20 2.20 -1 -1 -13 3.40 1.80 -1 -1 -13 2.10 1.30 1 1 13 1.20 1.80 1 1 13 0.80 1.10 1 1 13 1.10 1.30 -2 -1 -13 1.30 1.30 -2 -1 -13 -1.70 1.30 2 1 13 0.00 1.30 2 1 13 2.90 1.90 -3 -1 -13 5.90 1.70 -3 -1 -13 7.80 2.40 3 1 13 8.50 2.70 3 1 13 5.40 1.80 2 -2 -13 -0.50 1.10 -2 2 13 -0.60 1.30 -2 2 13 -0.10 1.90 1 -2 -13 0.00 1.40 1 -2 -13 2.60 0.80 -1 2 13 2.80 2.10 -1 2 13 1.20 1.40 0 -2 -13 6.10 2.10 0 2 13 10.70 2.50 0 2 13 8.00 1.80 -1 -2 -13 1.20 1.10 -1 -2 -13 -0.10 1.10 1 2 13 0.80 1.50 1 2 13 0.90 1.70 1 2 13 -1.40 0.90 -2 -2 -13 2.80 1.50 -2 -2 -13 3.80 1.90 2 2 13 -0.50 1.30 2 2 13 3.00 1.30 2 2 13 1.80 1.80 -3 -2 -13 1.50 1.60 -3 -2 -13 1.10 1.70 3 2 13 3.10 1.70 3 2 13 2.30 1.90 3 2 13 2.00 1.20 1 -3 -13 -1.60 1.10 1 -3 -13 1.70 0.90 -1 3 13 -2.00 1.70 -1 3 13 -2.40 1.00 0 -3 -13 13.30 2.70 0 3 13 10.90 2.20 0 3 13 17.20 2.90 -1 -3 -13 -2.40 1.10 -1 -3 -13 -1.70 1.20 1 3 13 -1.10 1.20 1 3 13 -0.10 1.40 -2 -3 -13 1.30 1.30 -2 -3 -13 -2.20 1.20 2 3 13 -0.70 1.00 2 3 13 0.50 1.40 2 3 13 -0.90 1.10 -3 -3 -13 5.50 2.10 -3 -3 -13 0.50 1.50 3 3 13 0.50 1.40 3 3 13 2.80 1.90 3 3 13 1.70 1.30 3 3 13 2.00 1.30 1 -4 -13 2.90 1.90 -1 4 13 2.20 1.60 0 -4 -13 1.70 1.70 0 4 13 0.80 1.30 0 4 13 2.20 1.60 -1 -4 -13 -2.20 1.30 1 4 13 -0.10 1.20 1 4 13 1.20 1.60 -2 -4 -13 2.20 1.80 -2 -4 -13 1.10 1.60 2 4 13 2.80 1.60 2 4 13 2.70 1.50 2 4 13 3.80 1.60 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 23779 _shelx_res_file ; TITL 53ecg CELL 0.71073 7.6546 8.0959 11.3065 78.988 85.527 87.548 ZERR 2.00 0.0005 0.0005 0.0006 0.003 0.003 0.004 LATT 1 SFAC C H N O UNIT 28 28 4 8 MERG 2 FMAP 2 PLAN 20 OMIT -2 180.0 SIZE 0.12 0.15 0.16 ACTA BOND $H CONF HTAB L.S. 20 TEMP 23.00 OMIT 0 0 1 EXYZ C31A C31B EADP C31A C31B EADP O31A O31B EADP O32A O32B EADP C32A C32B FLAT C3 C31A O31A O32A FLAT C3 C31B O31B O32B WGHT 0.052900 0.243900 EXTI 0.023730 FVAR 0.79111 0.71396 N1 3 0.393796 0.722754 0.381593 11.00000 0.04400 0.05607 = 0.03310 -0.00411 -0.00500 -0.00928 N2 3 0.445804 0.777349 0.262969 11.00000 0.04584 0.06127 = 0.03450 -0.00296 -0.00282 -0.01053 C3 1 0.316267 0.741287 0.202667 11.00000 0.03975 0.05106 = 0.03691 -0.00665 -0.00468 -0.00315 C4 1 0.179071 0.662317 0.281269 11.00000 0.04069 0.05053 = 0.03718 -0.00635 -0.00455 -0.00505 C5 1 0.236214 0.652498 0.394797 11.00000 0.04361 0.05672 = 0.03733 -0.00356 -0.00088 -0.01104 AFIX 43 H5 2 0.176500 0.605690 0.467465 11.00000 -1.20000 AFIX 0 C11 1 0.503582 0.748243 0.472867 11.00000 0.04493 0.05053 = 0.03896 -0.00729 -0.00838 -0.00441 C12 1 0.452896 0.697940 0.592694 11.00000 0.05392 0.09372 = 0.04244 -0.00854 -0.00510 -0.01740 AFIX 43 H12 2 0.346839 0.644981 0.615741 11.00000 -1.20000 AFIX 0 C13 1 0.559628 0.726078 0.679039 11.00000 0.06733 0.09236 = 0.04031 -0.01168 -0.01084 -0.00546 AFIX 43 H13 2 0.523991 0.691062 0.760193 11.00000 -1.20000 AFIX 0 C14 1 0.716817 0.804122 0.649065 11.00000 0.06441 0.05432 = 0.05548 -0.01425 -0.02186 0.00135 C15 1 0.764695 0.850010 0.528921 11.00000 0.06711 0.09679 = 0.06487 -0.00632 -0.01634 -0.03670 AFIX 43 H15 2 0.871733 0.901107 0.505858 11.00000 -1.20000 AFIX 0 C16 1 0.661157 0.823847 0.440297 11.00000 0.06606 0.09508 = 0.04411 -0.00351 -0.00823 -0.03343 AFIX 43 H16 2 0.697922 0.857200 0.359180 11.00000 -1.20000 AFIX 0 C141 1 0.832762 0.835426 0.743598 11.00000 0.09235 0.07866 = 0.07819 -0.02595 -0.04410 0.00089 AFIX 137 H14A 2 0.767735 0.819004 0.820837 11.00000 -1.50000 H14B 2 0.872587 0.948866 0.723262 11.00000 -1.50000 H14C 2 0.931923 0.758377 0.746995 11.00000 -1.50000 AFIX 0 PART 1 C31A 1 0.334152 0.790731 0.068742 21.00000 0.04088 0.07273 = 0.03798 -0.00934 -0.00308 -0.00641 O31A 4 0.458722 0.755431 0.004800 21.00000 0.06962 0.15919 = 0.04343 -0.01031 0.00307 0.03492 O32A 4 0.204421 0.893603 0.028820 21.00000 0.05447 0.06218 = 0.03949 0.00600 0.00091 -0.00771 C32A 1 0.211327 0.957517 -0.099842 21.00000 0.07501 0.07392 = 0.04064 0.01034 -0.00889 -0.01683 AFIX 137 H32A 2 0.219485 0.864992 -0.142117 21.00000 -1.50000 H32B 2 0.312068 1.026092 -0.123263 21.00000 -1.50000 H32C 2 0.107015 1.023913 -0.119593 21.00000 -1.50000 AFIX 0 PART 0 PART 2 SAME 0.005 0.01 C31A > C32A C31B 1 0.334152 0.790731 0.068742 -21.00000 0.04088 0.07273 = 0.03798 -0.00934 -0.00308 -0.00641 O31B 4 0.412873 0.697893 0.011254 -21.00000 0.06962 0.15919 = 0.04343 -0.01031 0.00307 0.03492 O32B 4 0.233235 0.919859 0.025033 -21.00000 0.05447 0.06218 = 0.03949 0.00600 0.00091 -0.00771 C32B 1 0.234291 0.965861 -0.104967 -21.00000 0.07501 0.07392 = 0.04064 0.01034 -0.00889 -0.01683 AFIX 137 H32D 2 0.147626 0.903520 -0.133357 -21.00000 -1.50000 H32E 2 0.347937 0.940414 -0.140408 -21.00000 -1.50000 H32F 2 0.208011 1.084207 -0.127492 -21.00000 -1.50000 AFIX 0 PART 0 C41 1 0.014999 0.592917 0.258086 11.00000 0.04213 0.05570 = 0.03874 -0.00771 -0.00253 -0.00474 O41 4 -0.085951 0.522089 0.335635 11.00000 0.05810 0.12115 = 0.04491 -0.00312 0.00174 -0.03940 O42 4 -0.010862 0.615048 0.141226 11.00000 0.05188 0.07291 = 0.04026 -0.00476 -0.00880 -0.01771 C42 1 -0.173818 0.555083 0.111150 11.00000 0.05504 0.09417 = 0.05897 -0.01689 -0.01731 -0.01866 AFIX 137 H42A 2 -0.270140 0.603477 0.153794 11.00000 -1.50000 H42B 2 -0.174837 0.434638 0.133915 11.00000 -1.50000 H42C 2 -0.184731 0.587297 0.025762 11.00000 -1.50000 AFIX 0 HKLF 4 REM 53ecg REM R1 = 0.0444 for 1777 Fo > 4sig(Fo) and 0.0716 for all 2526 data REM 196 parameters refined using 7 restraints END WGHT 0.0529 0.2441 REM Instructions for potential hydrogen bonds EQIV $1 -x, -y+1, -z+1 HTAB C5 O41_$1 HTAB C12 O41_$1 EQIV $2 -x, -y+2, -z HTAB C32A O32A_$2 REM Highest difference peak 0.237, deepest hole -0.241, 1-sigma level 0.036 Q1 1 0.8506 0.7346 0.8024 11.00000 0.05 0.24 Q2 1 0.9687 0.8646 0.7021 11.00000 0.05 0.19 Q3 1 0.4662 0.8348 0.0329 11.00000 0.05 0.19 Q4 1 0.2428 0.6797 0.2345 11.00000 0.05 0.17 Q5 1 0.2288 0.7267 0.2340 11.00000 0.05 0.16 Q6 1 0.6489 0.9280 0.3580 11.00000 0.05 0.15 Q7 1 0.7624 0.7646 0.6015 11.00000 0.05 0.14 Q8 1 0.5041 0.6684 0.5372 11.00000 0.05 0.14 Q9 1 0.7753 0.9276 0.7964 11.00000 0.05 0.13 Q10 1 0.6806 0.7404 0.6597 11.00000 0.05 0.13 Q11 1 0.3584 0.7027 0.0174 11.00000 0.05 0.13 Q12 1 0.1079 0.6719 0.2584 11.00000 0.05 0.13 Q13 1 -0.2094 0.6953 0.0304 11.00000 0.05 0.13 Q14 1 0.1684 0.7237 0.3250 11.00000 0.05 0.13 Q15 1 0.8309 0.9848 0.4960 11.00000 0.05 0.13 Q16 1 0.2167 0.6063 0.3253 11.00000 0.05 0.12 Q17 1 0.4400 0.7993 0.5408 11.00000 0.05 0.12 Q18 1 -0.1234 0.5077 0.0279 11.00000 0.05 0.12 Q19 1 0.5648 0.8280 0.2251 11.00000 0.05 0.12 Q20 1 -0.2644 0.4852 0.1815 11.00000 0.05 0.12 ; _shelx_res_checksum 56688 _shelxl_version_number 2.014 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N N1 0.3938(2) 0.7228(2) 0.38159(13) 0.0446(4) Uani d 1 . . N N2 0.4458(2) 0.7773(2) 0.26297(14) 0.0477(4) Uani d 1 . . C C3 0.3163(2) 0.7413(3) 0.20267(16) 0.0426(5) Uani d 1 . . C C4 0.1791(2) 0.6623(2) 0.28127(16) 0.0428(5) Uani d 1 . . C C5 0.2362(3) 0.6525(3) 0.39480(17) 0.0464(5) Uani d 1 . . H H5 0.1765 0.6057 0.4675 0.056 Uiso calc 1 . . C C11 0.5036(3) 0.7482(3) 0.47287(17) 0.0446(5) Uani d 1 . . C C12 0.4529(3) 0.6979(3) 0.59269(19) 0.0634(7) Uani d 1 . . H H12 0.3468 0.6450 0.6157 0.076 Uiso calc 1 . . C C13 0.5596(3) 0.7261(3) 0.6790(2) 0.0663(7) Uani d 1 . . H H13 0.5240 0.6911 0.7602 0.080 Uiso calc 1 . . C C14 0.7168(3) 0.8041(3) 0.6491(2) 0.0567(6) Uani d 1 . . C C15 0.7647(3) 0.8500(4) 0.5289(2) 0.0758(8) Uani d 1 . . H H15 0.8717 0.9011 0.5059 0.091 Uiso calc 1 . . C C16 0.6612(3) 0.8238(3) 0.4403(2) 0.0686(7) Uani d 1 . . H H16 0.6979 0.8572 0.3592 0.082 Uiso calc 1 . . C C141 0.8328(4) 0.8354(3) 0.7436(2) 0.0797(8) Uani d 1 . . H H14A 0.7677 0.8190 0.8208 0.119 Uiso calc 1 . . H H14B 0.8726 0.9489 0.7233 0.119 Uiso calc 1 . . H H14C 0.9319 0.7584 0.7470 0.119 Uiso calc 1 . . C C31A 0.3342(3) 0.7907(3) 0.06874(18) 0.0505(5) Uani d 0.71(2) A 1 O O31A 0.4587(11) 0.7554(17) 0.0048(5) 0.093(3) Uani d 0.71(2) A 1 O O32A 0.2044(10) 0.8936(9) 0.0288(6) 0.0542(14) Uani d 0.71(2) A 1 C C32A 0.2113(19) 0.9575(17) -0.0998(7) 0.0653(16) Uani d 0.71(2) A 1 H H32A 0.2195 0.8650 -0.1421 0.098 Uiso calc 0.71(2) A 1 H H32B 0.3121 1.0261 -0.1233 0.098 Uiso calc 0.71(2) A 1 H H32C 0.1070 1.0239 -0.1196 0.098 Uiso calc 0.71(2) A 1 C C31B 0.3342(3) 0.7907(3) 0.06874(18) 0.0505(5) Uani d 0.29(2) A 2 O O31B 0.413(2) 0.6979(19) 0.0113(14) 0.093(3) Uani d 0.29(2) A 2 O O32B 0.233(2) 0.9199(19) 0.0250(15) 0.0542(14) Uani d 0.29(2) A 2 C C32B 0.234(5) 0.966(4) -0.1050(17) 0.0653(16) Uani d 0.29(2) A 2 H H32D 0.1476 0.9035 -0.1334 0.098 Uiso calc 0.29(2) A 2 H H32E 0.3479 0.9404 -0.1404 0.098 Uiso calc 0.29(2) A 2 H H32F 0.2080 1.0842 -0.1275 0.098 Uiso calc 0.29(2) A 2 C C41 0.0150(3) 0.5929(3) 0.25809(17) 0.0456(5) Uani d 1 . . O O41 -0.0860(2) 0.5221(2) 0.33564(14) 0.0756(6) Uani d 1 . . O O42 -0.01086(18) 0.61505(19) 0.14123(12) 0.0550(4) Uani d 1 . . C C42 -0.1738(3) 0.5551(3) 0.1112(2) 0.0679(7) Uani d 1 . . H H42A -0.2701 0.6035 0.1538 0.102 Uiso calc 1 . . H H42B -0.1748 0.4346 0.1339 0.102 Uiso calc 1 . . H H42C -0.1847 0.5873 0.0258 0.102 Uiso calc 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 0.0440(9) 0.0561(11) 0.0331(8) -0.0093(8) -0.0050(7) -0.0041(7) N2 0.0458(10) 0.0613(11) 0.0345(9) -0.0105(8) -0.0028(7) -0.0030(8) C3 0.0397(11) 0.0511(12) 0.0369(10) -0.0032(9) -0.0047(8) -0.0067(9) C4 0.0407(10) 0.0505(12) 0.0372(10) -0.0050(9) -0.0045(8) -0.0063(9) C5 0.0436(11) 0.0567(13) 0.0373(10) -0.0110(10) -0.0009(8) -0.0036(9) C11 0.0449(11) 0.0505(12) 0.0390(11) -0.0044(9) -0.0084(8) -0.0073(9) C12 0.0539(13) 0.0937(19) 0.0424(12) -0.0174(12) -0.0051(10) -0.0085(12) C13 0.0673(16) 0.0924(19) 0.0403(12) -0.0055(14) -0.0108(11) -0.0117(12) C14 0.0644(15) 0.0543(13) 0.0555(14) 0.0014(11) -0.0219(11) -0.0142(10) C15 0.0671(16) 0.097(2) 0.0649(16) -0.0367(14) -0.0163(12) -0.0063(14) C16 0.0661(15) 0.0951(19) 0.0441(12) -0.0334(14) -0.0082(11) -0.0035(12) C141 0.092(2) 0.0787(19) 0.0782(18) 0.0009(15) -0.0441(15) -0.0260(14) C31A 0.0409(11) 0.0727(15) 0.0380(11) -0.0064(11) -0.0031(9) -0.0093(10) O31A 0.070(3) 0.159(6) 0.0434(12) 0.035(4) 0.0031(17) -0.010(2) O32A 0.054(2) 0.062(2) 0.0395(9) -0.008(2) 0.0009(13) 0.0060(12) C32A 0.075(4) 0.0739(19) 0.0406(14) -0.017(3) -0.0089(17) 0.0103(13) C31B 0.0409(11) 0.0727(15) 0.0380(11) -0.0064(11) -0.0031(9) -0.0093(10) O31B 0.070(3) 0.159(6) 0.0434(12) 0.035(4) 0.0031(17) -0.010(2) O32B 0.054(2) 0.062(2) 0.0395(9) -0.008(2) 0.0009(13) 0.0060(12) C32B 0.075(4) 0.0739(19) 0.0406(14) -0.017(3) -0.0089(17) 0.0103(13) C41 0.0421(11) 0.0557(13) 0.0387(11) -0.0047(10) -0.0025(9) -0.0077(9) O41 0.0581(10) 0.1211(15) 0.0449(9) -0.0394(10) 0.0017(7) -0.0031(9) O42 0.0519(9) 0.0729(10) 0.0403(8) -0.0177(7) -0.0088(6) -0.0048(7) C42 0.0550(14) 0.0942(19) 0.0590(14) -0.0187(13) -0.0173(11) -0.0169(13) 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 C5 N1 N2 111.67(15) C5 N1 C11 128.79(16) N2 N1 C11 119.52(15) C3 N2 N1 105.05(15) N2 C3 C4 111.50(16) N2 C3 C31A 117.41(17) C4 C3 C31A 131.07(17) C5 C4 C3 104.27(16) C5 C4 C41 123.78(17) C3 C4 C41 131.86(17) N1 C5 C4 107.50(17) N1 C5 H5 126.2 C4 C5 H5 126.2 C12 C11 C16 119.48(19) C12 C11 N1 120.75(18) C16 C11 N1 119.77(18) C11 C12 C13 119.7(2) C11 C12 H12 120.1 C13 C12 H12 120.1 C14 C13 C12 122.1(2) C14 C13 H13 119.0 C12 C13 H13 119.0 C15 C14 C13 116.7(2) C15 C14 C141 121.4(2) C13 C14 C141 121.9(2) C14 C15 C16 122.7(2) C14 C15 H15 118.6 C16 C15 H15 118.6 C11 C16 C15 119.3(2) C11 C16 H16 120.4 C15 C16 H16 120.4 C14 C141 H14A 109.5 C14 C141 H14B 109.5 H14A C141 H14B 109.5 C14 C141 H14C 109.5 H14A C141 H14C 109.5 H14B C141 H14C 109.5 O31A C31A O32A 123.5(3) O31A C31A C3 125.0(3) O32A C31A C3 111.1(3) C31A O32A C32A 116.5(3) O32A C32A H32A 109.5 O32A C32A H32B 109.5 H32A C32A H32B 109.5 O32A C32A H32C 109.5 H32A C32A H32C 109.5 H32B C32A H32C 109.5 O32B C32B H32D 109.5 O32B C32B H32E 109.5 H32D C32B H32E 109.5 O32B C32B H32F 109.5 H32D C32B H32F 109.5 H32E C32B H32F 109.5 O41 C41 O42 123.08(18) O41 C41 C4 123.97(18) O42 C41 C4 112.95(17) C41 O42 C42 116.23(16) O42 C42 H42A 109.5 O42 C42 H42B 109.5 H42A C42 H42B 109.5 O42 C42 H42C 109.5 H42A C42 H42C 109.5 H42B C42 H42C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C5 1.341(2) N1 N2 1.363(2) N1 C11 1.430(2) N2 C3 1.319(2) C3 C4 1.413(3) C3 C31A 1.487(3) C4 C5 1.375(3) C4 C41 1.459(3) C5 H5 0.9300 C11 C12 1.368(3) C11 C16 1.369(3) C12 C13 1.378(3) C12 H12 0.9300 C13 C14 1.372(3) C13 H13 0.9300 C14 C15 1.363(3) C14 C141 1.505(3) C15 C16 1.377(3) C15 H15 0.9300 C16 H16 0.9300 C141 H14A 0.9600 C141 H14B 0.9600 C141 H14C 0.9600 C31A O31A 1.209(4) C31A O32A 1.319(3) O32A C32A 1.446(3) C32A H32A 0.9600 C32A H32B 0.9600 C32A H32C 0.9600 O32B C32B 1.445(5) C32B H32D 0.9600 C32B H32E 0.9600 C32B H32F 0.9600 C41 O41 1.198(2) C41 O42 1.328(2) O42 C42 1.445(2) C42 H42A 0.9600 C42 H42B 0.9600 C42 H42C 0.9600 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 C5 H5 O41 2_566 0.93 2.33 3.249(3) 168 no C12 H12 O41 2_566 0.93 2.43 3.352(3) 173 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 0.7(2) C11 N1 N2 C3 -177.91(17) N1 N2 C3 C4 -0.2(2) N1 N2 C3 C31A 178.57(18) N2 C3 C4 C5 -0.3(2) C31A C3 C4 C5 -178.9(2) N2 C3 C4 C41 -176.7(2) C31A C3 C4 C41 4.7(4) N2 N1 C5 C4 -0.9(2) C11 N1 C5 C4 177.57(18) C3 C4 C5 N1 0.7(2) C41 C4 C5 N1 177.50(18) C5 N1 C11 C12 0.3(3) N2 N1 C11 C12 178.6(2) C5 N1 C11 C16 -179.7(2) N2 N1 C11 C16 -1.4(3) C16 C11 C12 C13 0.9(4) N1 C11 C12 C13 -179.0(2) C11 C12 C13 C14 0.2(4) C12 C13 C14 C15 -1.3(4) C12 C13 C14 C141 179.7(2) C13 C14 C15 C16 1.3(4) C141 C14 C15 C16 -179.7(3) C12 C11 C16 C15 -0.9(4) N1 C11 C16 C15 179.1(2) C14 C15 C16 C11 -0.2(4) N2 C3 C31A O31A 52.4(9) C4 C3 C31A O31A -129.1(9) N2 C3 C31A O32A -121.0(5) C4 C3 C31A O32A 57.5(6) O31A C31A O32A C32A 3.6(10) C3 C31A O32A C32A 177.1(8) C5 C4 C41 O41 0.6(3) C3 C4 C41 O41 176.5(2) C5 C4 C41 O42 -178.86(19) C3 C4 C41 O42 -3.0(3) O41 C41 O42 C42 2.7(3) C4 C41 O42 C42 -177.82(18) _cod_database_fobs_code 2242738