#------------------------------------------------------------------------------ #$Date: 2019-05-24 05:18:40 +0300 (Fri, 24 May 2019) $ #$Revision: 215469 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021651.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_2021651 loop_ _publ_author_name 'Kiran Kumar, Haruvegowda' 'Yathirajan, Hemmige S.' 'Manju, Nagaraj' 'Kalluraya, Balakrishna' 'Rathore, Ravindranath S.' 'Glidewell, Christopher' _publ_section_title ; Conversion of substituted 5-aryloxypyrazolecarbaldehydes into reduced 3,4'-bipyrazoles: synthesis and characterization, and the structures of four precursors and two products, and their supramolecular assembly in zero, one and two dimensions ; _journal_coeditor_code KY3177 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229619006752 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac 'C31 H25 N7 O2' _chemical_formula_moiety 'C31 H25 N7 O2' _chemical_formula_sum 'C31 H25 N7 O2' _chemical_formula_weight 527.58 _chemical_name_systematic (3RS)-2-Acetyl-5-(4-azidophenyl)-3'-methyl-5'-(naphthalen-2-yloxy)-1'-phenyl-3,4-dihydro-1'H,2H-[3,4'-bipyrazole] _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 105.323(3) _cell_angle_beta 93.505(3) _cell_angle_gamma 117.460(3) _cell_formula_units_Z 2 _cell_length_a 10.4911(11) _cell_length_b 11.2048(12) _cell_length_c 13.5943(17) _cell_measurement_reflns_used 5566 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.036 _cell_measurement_theta_min 2.170 _cell_volume 1335.9(3) _computing_cell_refinement ; SAINT (Bruker, 2015) ; _computing_data_collection ; APEX2 (Bruker, 2015) ; _computing_data_reduction ; SAINT (Bruker, 2015) ; _computing_molecular_graphics ; PLATON (Spek, 2009) ; _computing_publication_material ; SHELXL2014 (Sheldrick, 2015b) and PLATON (Spek, 2009) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 296(2) _diffrn_detector_area_resol_mean 0.3333 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Bruker 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 0.0384 _diffrn_reflns_av_unetI/netI 0.0547 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 16901 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.549 _diffrn_reflns_theta_min 2.170 _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 0.086 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_correction_T_min 0.926 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2015) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.312 _exptl_crystal_description block _exptl_crystal_F_000 552 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.250 _refine_diff_density_min -0.245 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 363 _refine_ls_number_reflns 5470 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.014 _refine_ls_R_factor_all 0.1190 _refine_ls_R_factor_gt 0.0547 _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^)+(0.0878P)^2^+0.1031P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1379 _refine_ls_wR_factor_ref 0.1776 _reflns_number_gt 2883 _reflns_number_total 5470 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ky3177sup1.cif _cod_data_source_block X _cod_database_code 2021651 _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 0.987 _shelx_estimated_absorpt_t_max 0.990 _shelx_hkl_file ; -1 0 0 111.09 3.30 -1 0 0 108.49 2.10 -2 0 0 479.45 8.50 -2 0 0 499.85 8.60 2 0 0 508.05 8.60 2 0 0 496.15 8.50 2 0 0 498.95 13.70 -3 0 0 85.89 2.40 -3 0 0 90.59 2.50 3 0 0 89.89 2.40 3 0 0 88.09 2.40 3 0 0 89.49 3.60 -4 0 0 117.59 3.20 -4 0 0 118.49 3.30 4 0 0 125.39 4.90 4 0 0 119.89 3.10 4 0 0 123.79 3.20 -5 0 0 34.50 1.90 -5 0 0 35.90 1.90 5 0 0 35.10 1.70 5 0 0 35.40 1.80 5 0 0 37.60 2.60 -6 0 0 54.69 2.50 -6 0 0 54.49 2.50 6 0 0 54.09 2.30 6 0 0 56.69 2.40 6 0 0 56.99 3.60 -7 0 0 55.29 2.70 -7 0 0 53.29 2.70 7 0 0 56.59 3.80 7 0 0 56.09 2.60 -8 0 0 43.20 2.60 -8 0 0 37.40 2.60 8 0 0 41.90 3.60 8 0 0 39.20 2.30 -9 0 0 25.00 2.40 -10 0 0 1.40 1.40 -11 0 0 0.10 1.30 11 0 0 1.10 1.80 -11 1 0 0.30 1.10 -10 1 0 1.10 1.10 9 -1 0 2.30 1.10 -9 1 0 4.50 1.20 8 -1 0 105.29 3.30 8 -1 0 102.79 6.10 -8 1 0 100.19 3.50 -8 1 0 100.79 3.40 7 -1 0 56.29 4.10 7 -1 0 54.29 2.20 7 -1 0 54.99 2.10 -7 1 0 54.19 2.40 -7 1 0 55.99 2.40 6 -1 0 14.60 2.10 6 -1 0 13.40 1.10 6 -1 0 14.40 1.10 -6 1 0 13.70 1.30 -6 1 0 12.40 1.30 5 -1 0 14.00 1.90 5 -1 0 11.10 0.90 5 -1 0 12.10 0.90 -5 1 0 7.40 0.90 -5 1 0 9.60 1.00 4 -1 0 76.79 3.90 4 -1 0 75.99 2.00 4 -1 0 75.29 1.90 -4 1 0 72.09 2.00 3 -1 0 316.37 5.50 3 -1 0 306.37 5.40 3 -1 0 308.97 9.90 2 -1 0 980.80 15.90 2 -1 0 931.01 15.70 -2 1 0 952.00 15.60 1 -1 0 194.38 3.30 0 -1 0 6.20 0.50 0 1 0 6.40 0.50 -1 -1 0 278.47 5.30 -1 -1 0 270.67 5.20 1 1 0 268.57 5.20 1 1 0 276.37 5.30 -2 -1 0 23.40 1.10 -2 -1 0 21.60 1.40 -2 -1 0 19.70 1.30 2 1 0 18.30 1.30 2 1 0 26.80 1.20 2 1 0 18.40 1.20 -3 -1 0 111.49 3.20 -3 -1 0 108.09 3.20 3 1 0 115.99 3.30 3 1 0 117.09 3.90 -4 -1 0 14.40 1.60 -4 -1 0 17.90 1.50 4 1 0 17.30 1.50 4 1 0 16.90 1.60 4 1 0 17.00 1.50 -5 -1 0 -2.00 0.80 5 1 0 0.70 0.50 5 1 0 -1.70 0.80 5 1 0 0.70 0.80 -6 -1 0 16.90 2.00 -6 -1 0 18.60 2.00 6 1 0 17.70 2.10 6 1 0 17.60 1.80 -7 -1 0 59.49 3.00 -7 -1 0 55.89 3.20 7 1 0 55.19 2.90 7 1 0 53.59 3.10 -8 -1 0 0.10 1.20 8 1 0 -0.30 1.00 -9 -1 0 0.80 1.30 -10 -1 0 11.20 2.10 10 1 0 10.20 2.60 -11 2 0 2.10 1.00 10 -2 0 0.90 1.10 -10 2 0 1.20 0.90 9 -2 0 47.30 4.60 -9 2 0 46.50 2.10 -9 2 0 44.90 2.10 8 -2 0 3.30 0.70 8 -2 0 1.40 1.00 8 -2 0 2.40 0.60 -8 2 0 2.00 0.70 -8 2 0 2.70 0.80 7 -2 0 0.30 0.40 7 -2 0 0.20 0.70 7 -2 0 0.00 0.40 -7 2 0 -0.70 0.50 -7 2 0 0.60 0.60 6 -2 0 17.10 2.50 6 -2 0 18.00 0.90 6 -2 0 18.50 1.00 -6 2 0 18.90 1.10 -6 2 0 19.70 1.10 5 -2 0 -0.10 0.20 5 -2 0 -0.20 0.50 5 -2 0 -0.40 0.30 -5 2 0 -0.60 0.30 -5 2 0 -0.10 0.30 4 -2 0 6.60 0.40 4 -2 0 6.60 0.40 -4 2 0 6.10 0.50 -4 2 0 5.80 0.40 3 -2 0 244.28 4.20 3 -2 0 244.18 4.10 -3 2 0 261.77 4.20 -3 2 0 240.88 4.10 2 -2 0 820.62 13.70 2 -2 0 866.81 13.80 -2 2 0 848.52 13.70 1 -2 0 120.09 2.70 1 -2 0 121.39 2.20 1 -2 0 121.59 2.70 -1 2 0 121.39 2.70 -1 2 0 119.79 2.70 0 -2 0 805.42 13.40 0 -2 0 801.72 13.50 0 2 0 754.42 13.20 0 2 0 767.92 13.40 0 2 0 769.82 13.40 -1 -2 0 487.65 9.20 -1 -2 0 500.45 9.40 1 2 0 500.65 9.40 1 2 0 489.65 9.20 -2 -2 0 641.44 17.30 -2 -2 0 641.94 12.00 -2 -2 0 633.14 12.00 2 2 0 659.33 12.10 2 2 0 641.14 11.90 -3 -2 0 63.89 2.70 -3 -2 0 62.29 2.70 3 2 0 63.99 2.70 -4 -2 0 21.60 2.10 -4 -2 0 22.40 1.90 4 2 0 24.80 1.80 4 2 0 21.20 1.90 -5 -2 0 22.90 2.10 -5 -2 0 25.40 2.20 5 2 0 27.40 2.20 -6 -2 0 10.70 1.70 -6 -2 0 10.60 1.70 6 2 0 10.10 1.70 -7 -2 0 15.70 2.10 -7 -2 0 16.70 2.20 7 2 0 13.60 1.90 -8 -2 0 -0.80 1.50 8 2 0 2.10 1.40 -9 -2 0 1.00 1.40 9 2 0 0.40 1.70 -10 -2 0 -0.10 1.60 10 2 0 1.50 2.10 11 -3 0 0.80 1.20 10 -3 0 0.40 0.90 -10 3 0 0.80 0.50 9 -3 0 3.00 0.40 9 -3 0 1.70 1.10 9 -3 0 2.60 0.40 -9 3 0 3.30 0.60 -9 3 0 2.50 0.60 8 -3 0 4.90 1.50 8 -3 0 6.10 0.50 8 -3 0 5.40 0.50 -8 3 0 5.00 0.70 -8 3 0 4.90 0.60 7 -3 0 32.00 0.80 7 -3 0 33.60 3.80 7 -3 0 30.90 0.80 -7 3 0 31.40 1.00 -7 3 0 32.60 1.00 6 -3 0 5.00 1.20 6 -3 0 8.10 0.30 6 -3 0 7.80 0.30 -6 3 0 8.40 0.40 -6 3 0 7.60 0.50 5 -3 0 88.19 1.60 5 -3 0 91.49 5.30 5 -3 0 89.79 1.60 -5 3 0 87.89 1.70 -5 3 0 89.49 1.70 4 -3 0 292.97 5.10 4 -3 0 297.67 5.10 -4 3 0 292.27 5.10 -4 3 0 301.97 5.10 3 -3 0 37.00 1.20 3 -3 0 35.70 1.20 -3 3 0 35.50 1.20 2 -3 0 925.31 15.70 2 -3 0 917.41 15.70 -2 3 0 937.91 15.70 -2 3 0 948.61 15.70 1 -3 0 91.39 1.90 1 -3 0 95.79 2.60 1 -3 0 94.49 2.70 -1 3 0 90.89 2.70 -1 3 0 95.59 2.70 -1 3 0 90.19 1.90 0 -3 0 118.39 3.30 0 -3 0 120.99 3.30 0 3 0 117.39 3.30 0 3 0 118.79 3.30 0 3 0 113.49 2.80 -1 -3 0 4.30 1.00 -1 -3 0 5.50 0.90 1 3 0 4.70 0.90 1 3 0 4.30 0.70 1 3 0 5.20 1.00 -2 -3 0 18.90 1.60 -2 -3 0 21.10 1.80 2 3 0 19.20 1.60 2 3 0 19.10 1.80 -3 -3 0 1.90 1.10 -3 -3 0 1.20 0.90 3 3 0 1.10 0.80 -4 -3 0 25.40 2.30 -4 -3 0 29.70 2.40 4 3 0 29.00 2.40 -5 -3 0 4.20 1.40 -5 -3 0 2.20 1.30 5 3 0 3.50 1.30 -6 -3 0 0.30 1.40 -6 -3 0 0.90 1.50 6 3 0 -0.20 1.20 6 3 0 -0.70 0.90 -7 -3 0 0.80 1.70 7 3 0 0.60 1.30 7 3 0 -0.80 1.20 -8 -3 0 -1.20 1.50 8 3 0 0.00 1.50 -9 -3 0 -1.00 1.50 9 3 0 3.30 2.10 11 -4 0 -0.10 1.00 10 -4 0 40.20 5.10 9 -4 0 6.10 1.70 8 -4 0 14.30 3.10 7 -4 0 -0.30 0.70 6 -4 0 24.00 3.30 -6 4 0 20.80 0.50 5 -4 0 33.40 1.10 5 -4 0 33.20 3.40 5 -4 0 31.40 1.00 -5 4 0 32.60 1.10 -5 4 0 33.00 1.10 4 -4 0 508.85 9.00 4 -4 0 507.05 9.10 -4 4 0 527.05 9.00 3 -4 0 28.90 1.40 3 -4 0 32.10 1.40 -3 4 0 32.20 1.50 -3 4 0 28.50 1.40 2 -4 0 443.06 8.70 2 -4 0 450.65 7.90 2 -4 0 452.95 8.80 -2 4 0 470.25 8.80 -2 4 0 453.45 8.80 1 -4 0 34.60 1.90 1 -4 0 34.60 1.80 -1 4 0 35.30 1.20 -1 4 0 33.70 1.70 -1 4 0 33.90 1.80 0 -4 0 0.00 0.70 0 -4 0 0.70 0.80 0 4 0 0.40 0.70 0 4 0 1.20 0.50 0 4 0 0.30 0.80 -1 -4 0 16.00 1.70 -1 -4 0 18.20 1.80 1 4 0 18.60 1.70 1 4 0 15.70 1.80 1 4 0 17.20 1.50 -2 -4 0 31.80 2.10 -2 -4 0 30.00 2.10 2 4 0 27.70 1.90 2 4 0 27.00 2.10 2 4 0 27.20 2.00 -3 -4 0 18.20 2.10 -3 -4 0 15.90 1.10 -3 -4 0 15.90 1.30 -3 -4 0 15.40 2.10 3 4 0 15.20 2.10 3 4 0 16.90 2.20 -4 -4 0 1.60 1.20 -4 -4 0 1.00 1.20 4 4 0 0.40 1.00 4 4 0 0.80 1.20 -5 -4 0 4.10 1.60 -5 -4 0 6.40 1.70 5 4 0 3.50 1.60 5 4 0 1.10 1.40 -6 -4 0 0.60 1.50 6 4 0 -0.70 1.30 6 4 0 1.40 1.40 -7 -4 0 -0.50 1.40 7 4 0 -1.20 1.30 7 4 0 1.80 1.60 -8 -4 0 -1.60 1.40 8 4 0 1.10 1.80 9 4 0 1.00 1.90 12 -5 0 1.10 1.40 11 -5 0 1.80 1.40 10 -5 0 2.70 1.50 9 -5 0 2.50 1.30 8 -5 0 5.30 1.60 7 -5 0 4.20 1.50 6 -5 0 192.68 3.80 6 -5 0 193.28 3.80 6 -5 0 183.88 9.50 -6 5 0 195.48 3.80 -6 5 0 195.58 3.90 5 -5 0 35.50 1.40 5 -5 0 35.60 1.50 -5 5 0 36.40 1.50 4 -5 0 22.50 1.40 4 -5 0 23.90 1.30 -4 5 0 22.90 1.40 -4 5 0 22.60 1.50 3 -5 0 38.90 1.30 3 -5 0 39.60 1.90 3 -5 0 40.80 1.90 -3 5 0 39.30 2.00 -3 5 0 41.60 2.00 2 -5 0 6.60 0.50 2 -5 0 6.20 1.10 2 -5 0 6.80 1.10 -2 5 0 5.60 1.10 -2 5 0 6.70 1.20 1 -5 0 45.80 2.30 1 -5 0 43.30 2.20 -1 5 0 45.80 1.50 -1 5 0 44.30 2.40 -1 5 0 42.90 2.40 0 -5 0 0.00 0.60 0 -5 0 0.10 0.90 0 5 0 0.50 1.00 0 5 0 -0.30 0.80 0 5 0 0.20 0.50 -1 -5 0 43.30 2.70 -1 -5 0 47.20 2.80 1 5 0 46.60 2.90 1 5 0 47.20 2.70 1 5 0 47.10 2.30 -2 -5 0 97.59 4.20 -2 -5 0 92.79 4.00 2 5 0 93.99 4.20 2 5 0 96.29 3.70 -3 -5 0 0.00 0.30 -3 -5 0 -1.10 0.60 -3 -5 0 0.30 1.20 3 5 0 0.10 0.80 3 5 0 -0.30 1.20 -4 -5 0 -0.80 1.40 4 5 0 -0.20 1.10 4 5 0 0.50 1.50 -5 -5 0 41.60 3.50 5 5 0 35.80 3.40 5 5 0 32.40 3.40 -6 -5 0 5.70 1.90 6 5 0 6.10 1.90 6 5 0 3.80 1.70 -7 -5 0 1.00 1.70 7 5 0 2.00 1.80 -8 -5 0 0.30 1.80 8 5 0 3.10 2.20 13 -6 0 -0.70 1.40 12 -6 0 23.50 5.00 11 -6 0 5.80 2.10 10 -6 0 3.80 1.70 9 -6 0 0.20 1.00 8 -6 0 0.20 1.00 7 -6 0 6.00 0.60 7 -6 0 5.20 0.60 7 -6 0 3.60 1.50 -7 6 0 6.00 0.80 6 -6 0 23.70 3.90 6 -6 0 27.80 1.30 6 -6 0 29.20 1.40 -6 6 0 29.70 1.50 5 -6 0 11.20 1.10 5 -6 0 10.90 1.20 -5 6 0 8.80 1.20 -5 6 0 9.80 1.20 4 -6 0 11.80 1.20 4 -6 0 10.80 0.90 4 -6 0 12.40 1.30 -4 6 0 10.60 1.40 -4 6 0 12.20 1.30 3 -6 0 7.40 1.10 3 -6 0 6.90 0.50 3 -6 0 5.40 1.10 -3 6 0 7.30 1.20 -3 6 0 4.60 1.10 2 -6 0 14.30 1.60 2 -6 0 13.90 1.60 -2 6 0 14.10 1.50 -2 6 0 14.80 0.80 -2 6 0 13.20 1.70 1 -6 0 13.90 1.80 -1 6 0 18.50 1.90 -1 6 0 16.00 1.70 -1 6 0 16.20 1.10 0 -6 0 16.60 2.10 0 6 0 17.10 2.20 0 6 0 19.90 2.10 0 6 0 18.10 1.50 -1 -6 0 3.00 1.20 1 6 0 3.80 0.90 1 6 0 4.60 1.40 -2 -6 0 0.80 0.70 -2 -6 0 1.60 1.40 2 6 0 -0.80 1.30 2 6 0 0.60 0.90 -3 -6 0 21.40 2.50 -3 -6 0 19.40 2.50 -3 -6 0 22.50 1.80 3 6 0 25.20 2.60 3 6 0 22.70 3.00 -4 -6 0 -1.80 0.90 4 6 0 -0.20 1.30 4 6 0 -2.50 1.40 -5 -6 0 0.30 1.60 5 6 0 2.40 1.60 5 6 0 4.70 2.00 -6 -6 0 0.70 1.90 6 6 0 4.50 2.10 6 6 0 2.00 1.70 -7 -6 0 3.40 2.10 7 6 0 2.50 2.00 13 -7 0 2.40 1.80 12 -7 0 1.60 1.70 11 -7 0 9.90 2.60 10 -7 0 -0.30 1.20 9 -7 0 1.50 1.30 8 -7 0 3.00 0.50 8 -7 0 3.60 0.50 8 -7 0 0.60 1.30 -8 7 0 3.10 0.60 7 -7 0 23.10 3.90 7 -7 0 19.30 1.20 7 -7 0 23.10 1.30 -7 7 0 21.90 1.40 6 -7 0 1.00 0.60 6 -7 0 0.20 0.90 6 -7 0 0.70 0.70 -6 7 0 0.20 0.80 -6 7 0 -0.10 0.70 5 -7 0 1.90 0.70 -5 7 0 2.60 1.00 -5 7 0 1.50 0.80 4 -7 0 -0.70 0.60 4 -7 0 0.10 0.30 -4 7 0 -0.60 0.80 -4 7 0 1.20 0.90 3 -7 0 73.39 3.20 -3 7 0 69.49 3.30 -3 7 0 74.29 3.30 2 -7 0 92.39 3.90 -2 7 0 96.49 2.30 -2 7 0 101.09 4.00 -2 7 0 97.69 4.10 1 -7 0 -0.20 1.00 -1 7 0 1.10 0.60 -1 7 0 1.10 1.30 0 -7 0 19.40 2.40 0 7 0 20.10 1.70 0 7 0 18.90 2.60 -1 -7 0 16.30 2.80 -1 -7 0 13.50 2.20 1 7 0 16.40 2.40 1 7 0 18.20 1.90 -2 -7 0 1.20 1.30 -2 -7 0 0.30 0.70 2 7 0 0.60 0.90 2 7 0 -0.90 1.20 -3 -7 0 -1.80 1.50 3 7 0 -2.10 1.50 3 7 0 -0.40 1.10 -4 -7 0 -1.30 1.50 4 7 0 0.60 1.30 4 7 0 -0.50 1.60 -5 -7 0 18.10 3.10 5 7 0 15.10 2.50 5 7 0 11.40 2.50 -6 -7 0 1.90 2.00 6 7 0 2.10 2.10 6 7 0 2.90 2.00 13 -8 0 0.90 1.70 12 -8 0 0.20 1.30 11 -8 0 0.50 1.50 10 -8 0 7.70 2.40 9 -8 0 0.90 1.40 -9 8 0 3.60 0.60 -9 8 0 2.50 0.50 8 -8 0 2.50 0.60 8 -8 0 0.60 1.50 -8 8 0 2.60 0.80 7 -8 0 -0.60 1.30 7 -8 0 1.40 0.70 -7 8 0 1.50 1.00 -7 8 0 2.40 0.90 6 -8 0 0.60 0.50 6 -8 0 1.70 0.80 6 -8 0 -0.80 1.10 -6 8 0 0.60 0.90 -6 8 0 1.80 1.00 5 -8 0 -0.20 0.30 5 -8 0 -0.10 0.80 -5 8 0 1.10 1.10 -5 8 0 0.80 1.10 4 -8 0 25.00 2.20 -4 8 0 25.60 2.30 -4 8 0 26.60 2.30 3 -8 0 14.90 2.00 -3 8 0 9.50 1.70 -3 8 0 9.40 1.70 2 -8 0 4.90 1.50 -2 8 0 4.80 1.70 -2 8 0 5.50 0.80 1 -8 0 6.00 1.70 -1 8 0 4.60 1.80 -1 8 0 2.70 0.70 0 -8 0 14.00 2.80 0 -8 0 12.50 2.20 0 8 0 11.40 2.30 0 8 0 14.20 1.60 -1 -8 0 -0.30 1.50 -1 -8 0 -0.10 0.80 1 8 0 -0.70 1.70 1 8 0 1.40 0.90 -2 -8 0 -0.30 1.60 -2 -8 0 0.40 0.80 2 8 0 -0.40 1.70 2 8 0 0.80 1.10 -3 -8 0 3.40 2.10 3 8 0 4.70 1.50 3 8 0 3.00 2.10 -4 -8 0 -0.20 1.80 4 8 0 2.00 2.20 4 8 0 -1.00 1.20 -5 -8 0 1.90 2.20 5 8 0 1.90 1.70 5 8 0 -3.70 1.70 13 -9 0 0.50 1.60 12 -9 0 1.90 1.80 11 -9 0 4.70 2.20 10 -9 0 4.80 2.10 9 -9 0 2.10 1.40 -9 9 0 4.50 0.90 8 -9 0 2.00 1.90 -8 9 0 3.80 1.10 7 -9 0 24.40 1.90 7 -9 0 21.70 1.60 7 -9 0 20.80 4.50 -7 9 0 25.10 2.10 -7 9 0 22.30 2.20 6 -9 0 2.00 1.50 6 -9 0 5.50 1.20 6 -9 0 3.60 0.60 -6 9 0 5.10 1.40 -6 9 0 4.90 1.50 5 -9 0 7.70 2.30 5 -9 0 15.30 1.90 -5 9 0 13.80 1.90 -5 9 0 11.20 1.80 4 -9 0 2.80 1.40 4 -9 0 5.30 1.40 -4 9 0 5.90 1.70 -4 9 0 7.30 1.70 3 -9 0 4.00 1.50 3 -9 0 3.40 1.50 -3 9 0 3.80 1.40 2 -9 0 1.00 1.10 2 -9 0 1.40 1.20 -2 9 0 0.30 0.40 -2 9 0 1.40 1.70 1 -9 0 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117.69 4.20 1 5 -3 102.19 4.10 -1 -5 3 121.19 4.30 -1 -5 3 106.19 4.00 0 5 -3 42.10 2.70 0 5 -3 47.50 2.60 0 -5 3 47.80 2.60 0 -5 3 49.99 2.60 -1 5 -3 1.80 1.10 -1 5 -3 3.50 1.00 -1 5 -3 2.30 0.40 1 -5 3 4.80 1.10 1 -5 3 3.70 1.00 -2 5 -3 193.28 4.90 -2 5 -3 196.18 5.10 -2 5 -3 191.28 3.70 2 -5 3 193.28 5.00 2 -5 3 198.78 3.70 2 -5 3 192.38 4.90 -3 5 -3 0.40 0.80 -3 5 -3 1.90 0.80 3 -5 3 2.20 0.70 3 -5 3 1.70 0.70 3 -5 3 2.00 0.40 -4 5 -3 52.39 1.80 -4 5 -3 51.69 2.00 4 -5 3 53.19 1.90 4 -5 3 51.29 2.00 4 -5 3 54.79 1.90 -5 5 -3 18.10 0.90 -5 5 -3 18.00 1.00 5 -5 3 18.40 0.90 5 -5 3 17.90 1.60 5 -5 3 18.20 0.90 6 -5 3 69.69 3.20 7 -5 3 0.80 0.90 8 -5 3 16.70 2.30 9 -5 3 11.40 1.90 10 -5 3 -0.40 1.10 10 -5 3 0.60 1.10 11 -5 3 2.70 1.60 12 -5 3 -1.50 1.20 -9 -4 3 7.20 2.30 -8 -4 3 -0.70 1.50 7 4 -3 -0.60 1.40 -7 -4 3 1.50 1.60 6 4 -3 18.90 2.60 -6 -4 3 23.60 2.90 -6 -4 3 19.10 2.30 5 4 -3 1.20 1.40 -5 -4 3 2.30 1.50 -5 -4 3 3.90 1.60 -5 -4 3 2.10 0.90 4 4 -3 83.99 3.90 -4 -4 3 89.29 4.10 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2 -3 52.69 2.60 3 2 -3 54.19 4.00 3 2 -3 49.60 2.30 -3 -2 3 51.59 2.50 -3 -2 3 49.70 3.70 -3 -2 3 51.49 2.50 2 2 -3 348.57 11.90 2 2 -3 344.47 7.20 2 2 -3 353.96 7.60 -2 -2 3 343.17 12.00 -2 -2 3 352.36 7.50 -2 -2 3 351.36 7.40 1 2 -3 35.30 1.80 1 2 -3 34.60 1.60 1 2 -3 42.10 3.40 -1 -2 3 36.80 1.80 -1 -2 3 38.00 1.70 -1 -2 3 44.90 3.50 0 2 -3 184.08 4.20 0 2 -3 181.38 3.90 0 2 -3 167.38 3.80 0 -2 3 170.28 3.80 0 -2 3 173.78 4.10 0 -2 3 180.88 4.00 0 -2 3 174.08 7.10 -1 2 -3 102.59 2.70 -1 2 -3 106.69 2.50 -1 2 -3 104.19 2.70 1 -2 3 102.29 2.60 1 -2 3 101.99 2.70 1 -2 3 101.29 2.50 -2 2 -3 177.88 3.60 -2 2 -3 178.78 4.30 -2 2 -3 173.38 3.80 2 -2 3 178.18 4.20 2 -2 3 182.18 3.60 2 -2 3 175.58 3.70 -3 2 -3 0.10 0.30 -3 2 -3 0.10 0.40 3 -2 3 0.20 0.30 3 -2 3 -0.40 0.50 3 -2 3 0.50 0.30 -4 2 -3 0.10 0.10 -4 2 -3 0.30 0.40 4 -2 3 0.60 0.30 4 -2 3 0.10 0.50 4 -2 3 0.60 0.30 -5 2 -3 100.49 2.60 5 -2 3 97.59 2.40 5 -2 3 100.79 4.10 5 -2 3 96.69 2.50 -6 2 -3 9.20 1.10 6 -2 3 9.80 0.80 6 -2 3 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2.20 1.70 6 8 -4 1.50 2.30 -6 -8 4 -0.30 1.90 5 8 -4 1.50 1.50 5 8 -4 -1.80 1.90 -5 -8 4 -0.80 1.90 4 8 -4 5.10 2.40 -4 -8 4 6.90 2.50 3 8 -4 22.60 3.10 -3 -8 4 21.30 2.90 2 8 -4 -1.90 1.70 -2 -8 4 -1.40 1.60 1 8 -4 12.50 2.50 -1 -8 4 11.10 2.40 0 8 -4 17.50 2.60 0 8 -4 15.50 1.40 0 -8 4 16.60 2.40 -1 8 -4 3.40 0.50 -1 8 -4 4.60 1.50 -1 8 -4 4.30 0.60 1 -8 4 4.80 1.50 -2 8 -4 1.00 1.40 -2 8 -4 0.00 1.20 2 -8 4 0.70 1.20 -3 8 -4 101.99 4.10 -3 8 -4 102.79 4.30 3 -8 4 101.79 4.00 -4 8 -4 0.70 1.10 -4 8 -4 3.10 1.30 4 -8 4 2.30 1.10 -5 8 -4 7.40 1.30 -5 8 -4 7.20 1.20 5 -8 4 5.40 1.10 5 -8 4 5.80 0.80 -6 8 -4 28.80 2.10 -6 8 -4 32.20 1.80 6 -8 4 30.80 1.70 6 -8 4 27.10 1.70 -7 8 -4 15.40 1.40 -7 8 -4 15.60 1.20 7 -8 4 14.10 1.10 7 -8 4 14.20 1.10 7 -8 4 13.90 1.60 8 -8 4 13.60 1.90 9 -8 4 12.00 1.80 10 -8 4 3.90 1.30 11 -8 4 4.90 1.90 11 -8 4 8.90 1.90 12 -8 4 1.70 1.40 12 -8 4 4.90 1.70 -7 -7 4 4.50 2.30 6 7 -4 3.70 2.30 -6 -7 4 4.40 2.30 5 7 -4 0.40 1.90 -5 -7 4 2.50 2.10 4 7 -4 3.60 2.10 -4 -7 4 1.80 1.80 3 7 -4 18.60 2.70 -3 -7 4 17.80 2.60 2 7 -4 7.70 2.20 -2 -7 4 4.60 1.80 -2 -7 4 1.00 1.90 1 7 -4 0.50 1.60 -1 -7 4 0.20 1.30 0 7 -4 1.50 1.40 0 -7 4 0.10 1.20 -1 7 -4 5.00 1.60 -1 7 -4 6.10 0.80 -1 7 -4 5.70 1.50 1 -7 4 3.70 1.30 -2 7 -4 245.38 6.80 -2 7 -4 254.47 6.60 2 -7 4 241.88 6.60 -3 7 -4 23.70 2.20 -3 7 -4 26.00 2.00 3 -7 4 24.40 1.90 -4 7 -4 49.60 2.60 -4 7 -4 48.80 2.40 4 -7 4 48.80 2.40 4 -7 4 47.30 1.70 -5 7 -4 4.30 1.10 -5 7 -4 4.30 0.90 5 -7 4 4.90 1.00 5 -7 4 4.50 0.70 5 -7 4 5.00 0.90 -6 7 -4 3.40 0.90 6 -7 4 4.30 0.70 6 -7 4 3.80 0.80 6 -7 4 4.10 0.70 -7 7 -4 37.40 1.20 -7 7 -4 33.20 1.20 7 -7 4 40.10 2.50 7 -7 4 35.60 1.10 7 -7 4 35.90 1.10 8 -7 4 7.50 1.40 9 -7 4 24.90 2.60 10 -7 4 -0.40 1.00 11 -7 4 0.50 1.20 11 -7 4 -0.40 1.10 12 -7 4 0.40 1.50 12 -7 4 1.60 1.40 7 6 -4 0.00 1.90 -7 -6 4 1.00 1.80 6 6 -4 15.40 2.80 -6 -6 4 13.50 2.70 5 6 -4 7.10 2.30 -5 -6 4 8.10 2.30 4 6 -4 -1.40 1.50 -4 -6 4 -1.40 1.10 -4 -6 4 -2.10 1.50 3 6 -4 0.10 1.50 -3 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1.90 1.70 -5 -5 4 1.00 0.90 4 5 -4 -1.10 1.40 -4 -5 4 -0.50 1.00 -4 -5 4 1.80 1.60 3 5 -4 0.00 1.30 -3 -5 4 0.60 1.10 -3 -5 4 0.40 1.30 2 5 -4 280.17 7.80 -2 -5 4 286.27 7.80 -2 -5 4 275.67 11.60 -2 -5 4 273.87 7.50 1 5 -4 0.30 1.00 1 5 -4 0.30 0.90 -1 -5 4 0.20 1.20 -1 -5 4 0.40 1.00 0 5 -4 151.78 3.70 0 5 -4 147.09 4.60 0 5 -4 148.59 4.80 0 -5 4 149.19 4.80 0 -5 4 144.39 4.60 -1 5 -4 31.70 1.90 -1 5 -4 37.10 2.40 -1 5 -4 32.30 1.40 1 -5 4 34.60 2.20 1 -5 4 32.60 2.10 -2 5 -4 486.25 10.10 -2 5 -4 491.95 9.10 -2 5 -4 493.75 9.80 2 -5 4 500.15 10.00 2 -5 4 501.65 9.90 2 -5 4 501.95 9.10 -3 5 -4 16.40 1.60 -3 5 -4 14.90 1.20 -3 5 -4 15.30 1.20 3 -5 4 16.80 1.40 3 -5 4 16.60 1.20 3 -5 4 17.20 1.20 -4 5 -4 -0.20 0.50 -4 5 -4 -0.10 0.70 4 -5 4 -0.20 0.50 4 -5 4 0.60 0.50 4 -5 4 -0.20 0.40 -5 5 -4 -0.40 0.50 -5 5 -4 -0.10 0.40 5 -5 4 0.00 0.30 5 -5 4 0.10 0.60 5 -5 4 0.10 0.40 -6 5 -4 0.00 0.40 -6 5 -4 -0.30 0.30 6 -5 4 -0.40 0.20 6 -5 4 0.00 0.20 6 -5 4 -0.40 0.70 7 -5 4 22.90 2.30 8 -5 4 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278.17 6.70 0 -5 5 258.27 6.90 0 -5 5 267.07 6.90 -1 5 -5 193.28 5.60 -1 5 -5 195.68 5.20 -1 5 -5 193.38 4.50 1 -5 5 187.28 5.30 1 -5 5 187.38 5.20 -2 5 -5 100.09 3.30 -2 5 -5 105.59 3.10 -2 5 -5 105.39 3.70 2 -5 5 106.39 3.50 2 -5 5 102.19 3.50 2 -5 5 106.19 3.00 -3 5 -5 7.50 1.10 -3 5 -5 8.20 1.10 -3 5 -5 8.20 1.30 3 -5 5 8.40 1.10 3 -5 5 8.00 1.10 3 -5 5 7.50 1.00 -4 5 -5 -0.10 0.60 -4 5 -5 0.40 0.60 -4 5 -5 -0.30 0.70 4 -5 5 0.60 0.60 4 -5 5 -0.50 0.50 4 -5 5 2.00 0.70 -5 5 -5 22.10 1.60 5 -5 5 25.60 1.30 5 -5 5 24.40 2.00 5 -5 5 24.30 1.30 -6 5 -5 7.10 0.80 -6 5 -5 7.50 1.00 6 -5 5 5.90 0.70 6 -5 5 6.30 1.30 6 -5 5 6.90 0.70 -7 5 -5 15.10 0.90 -7 5 -5 14.50 0.80 7 -5 5 20.20 2.30 7 -5 5 14.20 0.50 8 -5 5 13.10 2.00 9 -5 5 -0.10 1.00 10 -5 5 0.30 1.30 11 -5 5 3.20 1.60 12 -5 5 -0.50 1.60 -9 -4 5 25.10 3.50 -8 -4 5 3.00 2.10 7 4 -5 39.90 3.60 -7 -4 5 41.40 3.70 6 4 -5 3.80 1.90 -6 -4 5 3.40 1.20 -6 -4 5 7.30 2.00 5 4 -5 19.30 2.70 -5 -4 5 23.00 2.80 4 4 -5 1.10 1.40 -4 -4 5 0.40 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4.70 3 -2 15 42.20 5.20 4 -2 15 3.90 2.50 -7 -1 15 3.50 2.30 6 1 -15 -5.50 2.60 6 1 -15 0.50 2.10 -6 -1 15 -0.20 2.10 5 1 -15 0.90 2.00 -5 -1 15 4.40 2.20 4 1 -15 1.20 1.60 -4 -1 15 -1.30 1.70 3 1 -15 -0.30 1.90 3 1 -15 -5.20 3.30 -3 -1 15 1.10 1.80 2 1 -15 -4.60 3.00 2 1 -15 4.00 2.20 -2 -1 15 2.40 1.60 -2 -1 15 1.30 1.60 1 1 -15 3.50 1.80 1 1 -15 -5.80 3.00 -1 -1 15 1.30 2.00 -1 -1 15 1.90 1.40 0 1 -15 0.30 2.60 0 1 -15 3.70 2.20 0 -1 15 0.70 1.70 0 -1 15 0.60 1.80 -1 1 -15 2.00 2.20 1 -1 15 0.00 1.90 1 -1 15 3.80 2.00 -2 1 -15 -0.20 2.00 2 -1 15 1.50 1.80 2 -1 15 -0.20 2.10 -3 1 -15 3.50 2.30 3 -1 15 -2.50 2.00 -7 0 15 0.80 2.10 6 0 -15 1.90 2.00 6 0 -15 -5.80 3.60 -6 0 15 0.70 2.00 5 0 -15 -6.70 3.50 5 0 -15 -0.40 1.70 -5 0 15 -0.10 1.40 4 0 -15 -6.50 3.40 4 0 -15 1.20 2.10 -4 0 15 0.90 1.80 3 0 -15 2.20 2.00 3 0 -15 -4.00 3.60 -3 0 15 0.50 1.40 -3 0 15 -1.20 1.70 2 0 -15 5.60 2.00 2 0 -15 -3.50 3.50 -2 0 15 5.40 2.10 -2 0 15 1.60 2.00 1 0 -15 1.10 1.60 -1 0 15 -3.50 1.60 -1 0 15 1.40 1.80 0 0 -15 1.20 2.00 0 0 -15 -4.70 3.00 0 0 15 -2.00 1.60 0 0 15 -1.40 1.30 -1 0 -15 1.10 2.20 1 0 15 -1.00 1.60 1 0 15 -1.70 1.40 -2 0 -15 0.10 2.10 2 0 15 -2.10 2.00 2 0 15 -0.30 1.70 -7 1 15 -1.60 1.90 6 -1 -15 -4.80 2.80 6 -1 -15 0.20 1.80 -6 1 15 -3.20 1.70 5 -1 -15 -7.60 3.60 5 -1 -15 0.00 1.80 -5 1 15 -0.50 1.80 4 -1 -15 -0.50 1.90 4 -1 -15 -6.90 3.50 -4 1 15 -1.80 1.70 3 -1 -15 1.20 1.90 -3 1 15 -3.20 1.60 -3 1 15 0.40 1.80 2 -1 -15 0.90 1.70 -2 1 15 2.60 2.00 -2 1 15 0.30 2.00 1 -1 -15 -5.60 3.10 1 -1 -15 4.00 2.30 -1 1 15 -0.60 1.30 -1 1 15 0.60 2.00 0 -1 -15 -3.60 3.20 0 -1 -15 2.80 2.30 0 1 15 1.60 1.90 0 1 15 -1.90 1.90 -1 -1 -15 3.00 2.40 1 1 15 -2.20 2.10 1 1 15 0.20 1.80 6 -2 -15 -8.00 3.90 6 -2 -15 -0.50 1.90 -6 2 15 0.00 1.90 5 -2 -15 -5.20 2.70 5 -2 -15 3.00 2.20 -5 2 15 2.80 2.10 4 -2 -15 0.70 2.00 4 -2 -15 -8.00 3.80 -4 2 15 -0.40 1.80 3 -2 -15 2.00 2.20 -3 2 15 1.80 2.00 -3 2 15 0.10 2.10 2 -2 -15 1.80 2.10 -2 2 15 0.90 2.00 -2 2 15 -3.40 1.60 1 -2 -15 -6.20 3.30 1 -2 -15 7.60 2.70 -1 2 15 4.00 2.30 -1 2 15 2.70 2.30 0 2 15 4.90 2.30 -6 3 15 3.30 2.20 5 -3 -15 -7.50 3.90 -5 3 15 0.30 2.00 4 -3 -15 -5.70 2.70 4 -3 -15 -0.50 2.00 -4 3 15 -1.50 1.90 3 -3 -15 2.70 1.90 -3 3 15 4.40 2.40 -3 3 15 7.60 2.60 -2 3 15 2.80 1.80 0 -8 16 0.90 2.20 -1 8 -16 3.10 2.80 1 -8 16 0.10 1.90 -2 8 -16 -1.10 2.20 2 -8 16 -0.80 1.50 -2 -7 16 -0.80 2.10 1 7 -16 0.30 2.40 -1 -7 16 0.70 1.70 0 7 -16 0.90 2.40 0 -7 16 2.90 2.10 -1 7 -16 1.60 2.40 1 -7 16 0.30 1.40 1 -7 16 2.10 1.70 -2 7 -16 1.50 2.30 2 -7 16 -1.50 1.40 -3 7 -16 -2.30 2.10 3 -7 16 -2.80 1.50 -3 -6 16 -0.20 2.10 2 6 -16 0.00 2.20 -2 -6 16 0.80 2.10 1 6 -16 6.00 2.70 -1 -6 16 1.30 2.00 0 6 -16 -1.50 2.10 0 -6 16 -1.00 1.80 -1 6 -16 1.60 2.30 1 -6 16 -2.00 1.50 1 -6 16 -1.90 1.60 -2 6 -16 0.10 2.30 2 -6 16 0.50 1.80 -3 6 -16 2.00 2.40 3 -6 16 1.80 1.80 -4 -5 16 -1.00 2.00 3 5 -16 -1.90 2.20 -3 -5 16 -1.70 1.80 2 5 -16 0.60 2.40 -2 -5 16 0.30 2.10 1 5 -16 2.40 2.40 -1 -5 16 3.40 2.20 0 5 -16 0.30 2.30 0 -5 16 2.00 1.80 0 -5 16 3.40 2.00 -1 5 -16 4.00 2.40 1 -5 16 4.10 2.10 1 -5 16 3.70 2.10 -2 5 -16 2.30 2.30 2 -5 16 2.30 2.00 2 -5 16 -1.30 1.60 -3 5 -16 -3.00 1.80 3 -5 16 -0.40 1.80 4 4 -16 -0.30 2.10 -4 -4 16 -0.10 2.10 3 4 -16 4.60 2.20 -3 -4 16 1.60 1.70 2 4 -16 -1.30 2.10 -2 -4 16 -1.10 1.70 1 4 -16 -1.10 2.00 -1 -4 16 -1.10 1.60 -1 -4 16 1.50 1.80 0 4 -16 -1.20 1.90 0 -4 16 -2.40 1.60 0 -4 16 1.40 1.70 -1 4 -16 1.70 2.30 1 -4 16 -1.70 1.50 1 -4 16 -0.80 1.80 -2 4 -16 6.50 2.50 2 -4 16 4.10 2.20 2 -4 16 4.30 2.00 -3 4 -16 6.50 2.80 3 -4 16 4.30 2.30 5 3 -16 -3.70 2.70 -5 -3 16 -2.80 1.90 4 3 -16 0.50 2.40 -4 -3 16 -0.40 2.00 3 3 -16 -2.20 3.70 3 3 -16 0.40 2.20 -3 -3 16 0.40 2.00 2 3 -16 -2.80 1.80 -2 -3 16 0.20 1.80 1 3 -16 -0.50 2.10 -1 -3 16 -0.20 1.80 -1 -3 16 3.00 1.90 0 3 -16 7.40 2.60 0 -3 16 2.30 1.90 0 -3 16 4.70 2.30 -1 3 -16 1.20 1.70 1 -3 16 -0.40 1.80 1 -3 16 -1.20 1.60 -2 3 -16 0.70 2.30 2 -3 16 -1.70 1.80 2 -3 16 -0.10 1.70 3 -3 16 3.80 2.40 5 2 -16 -4.90 3.80 5 2 -16 4.80 2.20 -5 -2 16 1.00 2.30 4 2 -16 1.50 2.30 4 2 -16 -6.20 3.50 -4 -2 16 3.60 2.20 3 2 -16 -6.60 3.40 3 2 -16 -0.10 2.10 -3 -2 16 -0.30 1.30 2 2 -16 -4.30 3.30 2 2 -16 1.30 1.70 -2 -2 16 -0.70 1.70 -2 -2 16 -1.40 1.70 1 2 -16 -1.50 1.50 -1 -2 16 -1.50 1.90 -1 -2 16 -1.00 1.20 0 2 -16 -0.30 2.10 0 -2 16 -1.10 1.60 0 -2 16 -1.90 1.70 -1 2 -16 -0.50 2.00 1 -2 16 0.80 1.70 1 -2 16 -1.60 1.80 -2 2 -16 -0.50 2.00 2 -2 16 0.10 1.80 2 -2 16 -2.10 1.90 5 1 -16 1.50 2.20 -5 -1 16 0.30 2.00 4 1 -16 0.90 2.10 -4 -1 16 -0.50 1.40 3 1 -16 2.50 2.20 -3 -1 16 -0.50 1.80 2 1 -16 -3.70 2.50 2 1 -16 0.70 2.20 -2 -1 16 -4.60 1.60 -2 -1 16 -0.30 1.80 1 1 -16 -3.70 3.30 1 1 -16 7.80 2.70 -1 -1 16 3.70 2.20 -1 -1 16 4.50 2.40 0 1 -16 1.90 2.20 0 -1 16 1.90 1.80 0 -1 16 1.10 1.80 -1 1 -16 -0.90 2.00 1 -1 16 -1.20 1.60 1 -1 16 0.60 1.90 -5 0 16 -1.60 1.90 4 0 -16 -3.10 1.70 -4 0 16 0.50 2.00 3 0 -16 -4.50 2.60 3 0 -16 0.90 2.10 -3 0 16 -1.00 1.70 -3 0 16 -1.20 1.80 2 0 -16 2.30 2.30 -2 0 16 1.30 2.20 -2 0 16 2.80 2.20 1 0 -16 -4.70 3.60 1 0 -16 -0.50 1.40 -1 0 16 -2.40 1.90 -1 0 16 -1.20 1.80 0 0 -16 1.20 2.30 0 0 16 0.80 2.00 0 0 16 1.20 2.10 -5 1 16 -2.00 1.80 -4 1 16 -1.30 1.40 3 -1 -16 -1.90 1.40 -3 1 16 -0.10 2.00 -3 1 16 -0.80 2.00 -2 1 16 -4.40 1.80 -2 1 16 1.10 1.70 -1 1 16 -1.90 1.80 -1 -5 17 0.70 2.00 0 -5 17 -0.40 1.90 1 -5 17 0.20 2.00 -2 -4 17 -1.90 2.00 1 4 -17 2.00 1.90 -1 -4 17 0.10 2.00 -1 -4 17 -1.60 1.30 0 -4 17 -0.90 1.90 0 -4 17 -0.30 1.90 1 -4 17 -0.60 1.70 -2 -3 17 1.90 2.10 -1 -3 17 -1.60 1.80 -1 -3 17 2.90 2.20 0 -3 17 0.50 1.90 -3 -2 17 0.10 2.00 2 2 -17 -4.60 3.30 -2 -2 17 -0.80 1.90 -1 -2 17 -3.40 1.70 3 1 -17 -5.60 3.80 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 25944 _shelx_res_file ; TITL bk9cgr CELL 0.71073 10.4911 11.2048 13.5943 105.323 93.505 117.460 ZERR 2.00 0.0011 0.0012 0.0017 0.003 0.003 0.003 LATT 1 SFAC C H N O UNIT 62 50 14 4 MERG 2 OMIT -2 53.1 FMAP 2 PLAN 10 SIZE 0.120 0.130 0.150 ACTA BOND $H CONF HTAB OMIT 0 0 1 L.S. 20 TEMP 23.00 WGHT 0.087800 0.103100 FVAR 0.45387 N1 3 0.665140 0.457907 0.571766 11.00000 0.04080 0.03928 = 0.04728 0.01737 0.01164 0.01988 N2 3 0.664778 0.411941 0.467562 11.00000 0.04639 0.04133 = 0.04735 0.02155 0.01636 0.02166 C3 1 0.525679 0.316134 0.421244 11.00000 0.04425 0.03645 = 0.04807 0.02184 0.01170 0.02034 C4 1 0.433085 0.296587 0.493557 11.00000 0.04152 0.03339 = 0.04759 0.01899 0.01153 0.01943 C5 1 0.525924 0.389190 0.587434 11.00000 0.04410 0.03853 = 0.04488 0.02053 0.01731 0.02386 C11 1 0.801542 0.548505 0.645023 11.00000 0.04104 0.03738 = 0.05628 0.01636 0.00812 0.01729 C12 1 0.811605 0.625557 0.744445 11.00000 0.05508 0.10181 = 0.08353 -0.02591 -0.00053 0.03675 AFIX 43 H12 2 0.727926 0.622208 0.766005 11.00000 -1.20000 AFIX 0 C13 1 0.947709 0.708962 0.813131 11.00000 0.06980 0.11986 = 0.09931 -0.03985 -0.01536 0.03699 AFIX 43 H13 2 0.953998 0.759323 0.881373 11.00000 -1.20000 AFIX 0 C14 1 1.071537 0.718224 0.782416 11.00000 0.05068 0.07862 = 0.09528 0.00227 -0.01350 0.01184 AFIX 43 H14 2 1.162430 0.776519 0.828522 11.00000 -1.20000 AFIX 0 C15 1 1.061339 0.641065 0.683096 11.00000 0.04102 0.07682 = 0.09154 0.03347 0.01149 0.01784 AFIX 43 H15 2 1.145536 0.645964 0.661508 11.00000 -1.20000 AFIX 0 C16 1 0.926515 0.555826 0.614629 11.00000 0.04369 0.06146 = 0.06081 0.02302 0.01443 0.01809 AFIX 43 H16 2 0.920289 0.502850 0.547263 11.00000 -1.20000 AFIX 0 C31 1 0.486922 0.246876 0.305523 11.00000 0.06436 0.06185 = 0.04911 0.01985 0.01158 0.03117 AFIX 137 H31A 2 0.465590 0.303635 0.272766 11.00000 -1.50000 H31B 2 0.402130 0.153709 0.286935 11.00000 -1.50000 H31C 2 0.568119 0.238740 0.282441 11.00000 -1.50000 AFIX 0 N41 3 0.169545 0.064853 0.591308 11.00000 0.03737 0.03526 = 0.05771 0.02076 0.01014 0.01456 N42 3 0.244116 0.070499 0.510320 11.00000 0.04244 0.03441 = 0.05981 0.02160 0.01619 0.01862 C43 1 0.271434 0.191960 0.472987 11.00000 0.03910 0.04013 = 0.05477 0.02359 0.01139 0.01787 AFIX 13 H43 2 0.229766 0.155670 0.397905 11.00000 -1.20000 AFIX 0 C44 1 0.179144 0.246787 0.532775 11.00000 0.04189 0.04201 = 0.07037 0.02737 0.01461 0.02051 AFIX 23 H44A 2 0.236863 0.348309 0.570248 11.00000 -1.20000 H44B 2 0.093618 0.227935 0.485831 11.00000 -1.20000 AFIX 0 C45 1 0.134745 0.163376 0.607155 11.00000 0.03238 0.03050 = 0.05411 0.01668 0.00501 0.01027 C421 1 0.292549 -0.022711 0.472568 11.00000 0.03505 0.03734 = 0.06362 0.01300 0.00845 0.01556 O421 4 0.354807 -0.014156 0.399388 11.00000 0.06292 0.05373 = 0.07719 0.02270 0.02678 0.03277 C422 1 0.266227 -0.132699 0.523877 11.00000 0.05752 0.04332 = 0.08869 0.02833 0.01485 0.02658 AFIX 137 H42A 2 0.185577 -0.222988 0.480466 11.00000 -1.50000 H42B 2 0.243184 -0.104915 0.590448 11.00000 -1.50000 H42C 2 0.353056 -0.140656 0.533588 11.00000 -1.50000 AFIX 0 C451 1 0.057629 0.186271 0.689947 11.00000 0.03697 0.04069 = 0.05294 0.01477 0.00623 0.01626 C452 1 0.018074 0.102999 0.754203 11.00000 0.05321 0.05514 = 0.06359 0.02801 0.01711 0.02797 AFIX 43 H452 2 0.039981 0.029690 0.744176 11.00000 -1.20000 AFIX 0 C453 1 -0.052864 0.126947 0.832349 11.00000 0.05710 0.06380 = 0.06615 0.03278 0.01874 0.02623 AFIX 43 H453 2 -0.079013 0.069519 0.874304 11.00000 -1.20000 AFIX 0 C454 1 -0.085707 0.236052 0.849079 11.00000 0.04710 0.06523 = 0.05283 0.01539 0.01294 0.02626 C455 1 -0.046882 0.320511 0.786272 11.00000 0.05664 0.05753 = 0.06489 0.01386 0.01318 0.03199 AFIX 43 H455 2 -0.068875 0.393818 0.796924 11.00000 -1.20000 AFIX 0 C456 1 0.024373 0.296584 0.707821 11.00000 0.05294 0.04763 = 0.06093 0.01958 0.01348 0.02546 AFIX 43 H456 2 0.050692 0.354501 0.666226 11.00000 -1.20000 AFIX 0 N451 3 -0.158403 0.253075 0.932219 11.00000 0.08094 0.09143 = 0.07120 0.02510 0.03001 0.05031 N452 3 -0.179897 0.356310 0.951975 11.00000 0.06053 0.08804 = 0.06817 0.00043 0.01385 0.02835 N453 3 -0.206695 0.444676 0.977197 11.00000 0.09730 0.09680 = 0.11087 -0.01095 0.02188 0.05107 O51 4 0.494991 0.422374 0.683631 11.00000 0.06497 0.04636 = 0.04779 0.02062 0.02241 0.03404 C51 1 0.420026 0.351664 0.827383 11.00000 0.04747 0.04316 = 0.04312 0.00962 0.00975 0.02579 AFIX 43 H51 2 0.392457 0.421254 0.843251 11.00000 -1.20000 AFIX 0 C52 1 0.481337 0.333868 0.743962 11.00000 0.04153 0.04113 = 0.03822 0.01289 0.00723 0.02014 C53 1 0.529399 0.234286 0.718524 11.00000 0.04888 0.05114 = 0.04198 0.01499 0.01302 0.02942 AFIX 43 H53 2 0.574230 0.226217 0.662077 11.00000 -1.20000 AFIX 0 C54 1 0.509003 0.149333 0.778393 11.00000 0.05468 0.04741 = 0.04642 0.01374 0.00927 0.03247 AFIX 43 H54 2 0.540207 0.082470 0.762084 11.00000 -1.20000 AFIX 0 C54A 1 0.441981 0.160353 0.864134 11.00000 0.04461 0.04443 = 0.03884 0.01181 0.00560 0.02064 C55 1 0.415075 0.069937 0.925564 11.00000 0.07011 0.06101 = 0.05377 0.02633 0.01453 0.03488 AFIX 43 H55 2 0.443412 0.000916 0.909488 11.00000 -1.20000 AFIX 0 C56 1 0.348995 0.082397 1.007011 11.00000 0.08199 0.08018 = 0.05929 0.03945 0.02532 0.04066 AFIX 43 H56 2 0.332344 0.022104 1.046272 11.00000 -1.20000 AFIX 0 C57 1 0.305627 0.185303 1.032481 11.00000 0.07767 0.09052 = 0.05379 0.03144 0.02727 0.04498 AFIX 43 H57 2 0.259684 0.192587 1.088388 11.00000 -1.20000 AFIX 0 C58 1 0.329802 0.274837 0.976516 11.00000 0.06737 0.07009 = 0.04842 0.01692 0.01937 0.03818 AFIX 43 H58 2 0.301306 0.343569 0.995028 11.00000 -1.20000 AFIX 0 C58A 1 0.397783 0.264823 0.890431 11.00000 0.04078 0.04484 = 0.03626 0.00992 0.00530 0.01874 HKLF 4 REM bk9cgr REM R1 = 0.0547 for 2883 Fo > 4sig(Fo) and 0.1190 for all 5470 data REM 363 parameters refined using 0 restraints END WGHT 0.0878 0.1031 REM Instructions for potential hydrogen bonds HTAB C12 O51 HTAB C31 O421 EQIV $1 -x+1, -y+1, -z+1 HTAB C44 N2_$1 REM Highest difference peak 0.250, deepest hole -0.245, 1-sigma level 0.044 Q1 1 0.1581 -0.1926 0.5396 11.00000 0.05 0.25 Q2 1 0.2795 -0.2012 0.4725 11.00000 0.05 0.21 Q3 1 1.0515 0.7207 0.7137 11.00000 0.05 0.20 Q4 1 0.4952 0.1473 0.2790 11.00000 0.05 0.18 Q5 1 0.8857 0.4381 0.5132 11.00000 0.05 0.17 Q6 1 0.7237 0.4085 0.3870 11.00000 0.05 0.17 Q7 1 0.5720 0.3222 0.2696 11.00000 0.05 0.17 Q8 1 0.3958 0.2332 0.2907 11.00000 0.05 0.17 Q9 1 0.3617 -0.0812 0.5988 11.00000 0.05 0.17 Q10 1 0.9510 0.7661 0.7675 11.00000 0.05 0.16 ; _shelx_res_checksum 49376 _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 N N1 0.6651(2) 0.45791(19) 0.57177(15) 0.0416(5) Uani d 1 N N2 0.6648(2) 0.41194(19) 0.46756(15) 0.0432(5) Uani d 1 C C3 0.5257(3) 0.3161(2) 0.42124(18) 0.0409(6) Uani d 1 C C4 0.4331(2) 0.2966(2) 0.49356(17) 0.0391(5) Uani d 1 C C5 0.5259(2) 0.3892(2) 0.58743(18) 0.0392(5) Uani d 1 C C11 0.8015(3) 0.5485(2) 0.64502(19) 0.0457(6) Uani d 1 C C12 0.8116(3) 0.6256(4) 0.7444(3) 0.0944(12) Uani d 1 H H12 0.7279 0.6222 0.7660 0.113 Uiso calc 1 C C13 0.9477(4) 0.7090(4) 0.8131(3) 0.1192(15) Uani d 1 H H13 0.9540 0.7593 0.8814 0.143 Uiso calc 1 C C14 1.0715(3) 0.7182(4) 0.7824(3) 0.0908(11) Uani d 1 H H14 1.1624 0.7765 0.8285 0.109 Uiso calc 1 C C15 1.0613(3) 0.6411(3) 0.6831(3) 0.0735(9) Uani d 1 H H15 1.1455 0.6460 0.6615 0.088 Uiso calc 1 C C16 0.9265(3) 0.5558(3) 0.6146(2) 0.0579(7) Uani d 1 H H16 0.9203 0.5029 0.5473 0.069 Uiso calc 1 C C31 0.4869(3) 0.2469(3) 0.30552(18) 0.0582(7) Uani d 1 H H31A 0.4656 0.3036 0.2728 0.087 Uiso calc 1 H H31B 0.4021 0.1537 0.2869 0.087 Uiso calc 1 H H31C 0.5681 0.2387 0.2824 0.087 Uiso calc 1 N N41 0.1695(2) 0.06485(19) 0.59131(15) 0.0437(5) Uani d 1 N N42 0.2441(2) 0.07050(19) 0.51032(15) 0.0441(5) Uani d 1 C C43 0.2714(2) 0.1920(2) 0.47299(19) 0.0436(6) Uani d 1 H H43 0.2298 0.1557 0.3979 0.052 Uiso calc 1 C C44 0.1791(3) 0.2468(3) 0.5328(2) 0.0494(6) Uani d 1 H H44A 0.2369 0.3483 0.5702 0.059 Uiso calc 1 H H44B 0.0936 0.2279 0.4858 0.059 Uiso calc 1 C C45 0.1347(2) 0.1634(2) 0.60715(18) 0.0409(6) Uani d 1 C C421 0.2925(3) -0.0227(2) 0.4726(2) 0.0473(6) Uani d 1 O O421 0.3548(2) -0.01416(18) 0.39939(15) 0.0622(5) Uani d 1 C C422 0.2662(3) -0.1327(3) 0.5239(2) 0.0611(7) Uani d 1 H H42A 0.1856 -0.2230 0.4805 0.092 Uiso calc 1 H H42B 0.2432 -0.1049 0.5904 0.092 Uiso calc 1 H H42C 0.3531 -0.1407 0.5336 0.092 Uiso calc 1 C C451 0.0576(2) 0.1863(2) 0.68995(19) 0.0451(6) Uani d 1 C C452 0.0181(3) 0.1030(3) 0.7542(2) 0.0547(7) Uani d 1 H H452 0.0400 0.0297 0.7442 0.066 Uiso calc 1 C C453 -0.0529(3) 0.1269(3) 0.8323(2) 0.0611(7) Uani d 1 H H453 -0.0790 0.0695 0.8743 0.073 Uiso calc 1 C C454 -0.0857(3) 0.2361(3) 0.8491(2) 0.0565(7) Uani d 1 C C455 -0.0469(3) 0.3205(3) 0.7863(2) 0.0595(7) Uani d 1 H H455 -0.0689 0.3938 0.7969 0.071 Uiso calc 1 C C456 0.0244(3) 0.2966(3) 0.7078(2) 0.0532(7) Uani d 1 H H456 0.0507 0.3545 0.6662 0.064 Uiso calc 1 N N451 -0.1584(3) 0.2531(3) 0.9322(2) 0.0777(7) Uani d 1 N N452 -0.1799(3) 0.3563(4) 0.9520(2) 0.0815(8) Uani d 1 N N453 -0.2067(3) 0.4447(4) 0.9772(3) 0.1105(12) Uani d 1 O O51 0.49499(18) 0.42237(16) 0.68363(12) 0.0487(4) Uani d 1 C C51 0.4200(2) 0.3517(2) 0.82738(17) 0.0442(6) Uani d 1 H H51 0.3925 0.4213 0.8433 0.053 Uiso calc 1 C C52 0.4813(2) 0.3339(2) 0.74396(17) 0.0406(6) Uani d 1 C C53 0.5294(2) 0.2343(2) 0.71852(17) 0.0453(6) Uani d 1 H H53 0.5742 0.2262 0.6621 0.054 Uiso calc 1 C C54 0.5090(3) 0.1493(3) 0.77839(18) 0.0469(6) Uani d 1 H H54 0.5402 0.0825 0.7621 0.056 Uiso calc 1 C C54A 0.4420(3) 0.1604(2) 0.86413(18) 0.0438(6) Uani d 1 C C55 0.4151(3) 0.0699(3) 0.9256(2) 0.0589(7) Uani d 1 H H55 0.4434 0.0009 0.9095 0.071 Uiso calc 1 C C56 0.3490(3) 0.0824(3) 1.0070(2) 0.0694(8) Uani d 1 H H56 0.3323 0.0221 1.0463 0.083 Uiso calc 1 C C57 0.3056(3) 0.1853(3) 1.0325(2) 0.0702(8) Uani d 1 H H57 0.2597 0.1926 1.0884 0.084 Uiso calc 1 C C58 0.3298(3) 0.2748(3) 0.9765(2) 0.0605(7) Uani d 1 H H58 0.3013 0.3436 0.9950 0.073 Uiso calc 1 C C58A 0.3978(2) 0.2648(2) 0.89043(17) 0.0426(6) Uani d 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1 0.0408(12) 0.0393(11) 0.0473(12) 0.0199(10) 0.0116(9) 0.0174(9) N2 0.0464(12) 0.0413(11) 0.0473(12) 0.0217(10) 0.0164(10) 0.0215(9) C3 0.0443(14) 0.0364(13) 0.0481(14) 0.0203(12) 0.0117(12) 0.0218(11) C4 0.0415(13) 0.0334(12) 0.0476(14) 0.0194(11) 0.0115(11) 0.0190(11) C5 0.0441(14) 0.0385(13) 0.0449(14) 0.0239(12) 0.0173(11) 0.0205(11) C11 0.0410(14) 0.0374(13) 0.0563(16) 0.0173(11) 0.0081(12) 0.0164(12) C12 0.0551(19) 0.102(3) 0.084(2) 0.0367(19) -0.0005(17) -0.026(2) C13 0.070(2) 0.120(3) 0.099(3) 0.037(2) -0.015(2) -0.040(2) C14 0.051(2) 0.079(2) 0.095(3) 0.0118(17) -0.0135(18) 0.002(2) C15 0.0410(16) 0.077(2) 0.092(2) 0.0178(15) 0.0115(16) 0.0335(19) C16 0.0437(16) 0.0615(17) 0.0608(17) 0.0181(14) 0.0144(13) 0.0230(14) C31 0.0644(17) 0.0618(17) 0.0491(16) 0.0312(15) 0.0116(13) 0.0198(13) N41 0.0374(11) 0.0353(11) 0.0577(13) 0.0146(9) 0.0101(9) 0.0208(9) N42 0.0424(11) 0.0344(11) 0.0598(13) 0.0186(9) 0.0162(10) 0.0216(9) C43 0.0391(13) 0.0401(13) 0.0548(15) 0.0179(11) 0.0114(11) 0.0236(11) C44 0.0419(14) 0.0420(14) 0.0704(17) 0.0205(12) 0.0146(12) 0.0274(13) C45 0.0324(12) 0.0305(12) 0.0541(15) 0.0103(10) 0.0050(11) 0.0167(11) C421 0.0350(13) 0.0373(14) 0.0636(17) 0.0156(11) 0.0085(12) 0.0130(12) O421 0.0629(12) 0.0537(11) 0.0772(13) 0.0328(10) 0.0268(11) 0.0227(10) C422 0.0575(16) 0.0433(15) 0.089(2) 0.0266(13) 0.0149(15) 0.0283(14) C451 0.0370(13) 0.0407(14) 0.0529(15) 0.0163(11) 0.0062(11) 0.0148(12) C452 0.0532(16) 0.0551(16) 0.0636(18) 0.0280(14) 0.0171(14) 0.0280(14) C453 0.0571(17) 0.0638(18) 0.0662(19) 0.0262(15) 0.0187(14) 0.0328(15) C454 0.0471(15) 0.0652(18) 0.0528(16) 0.0263(14) 0.0129(13) 0.0154(14) C455 0.0566(17) 0.0575(17) 0.0649(18) 0.0320(15) 0.0132(14) 0.0139(15) C456 0.0529(16) 0.0476(15) 0.0609(17) 0.0255(13) 0.0135(13) 0.0196(13) N451 0.0809(18) 0.091(2) 0.0712(17) 0.0503(17) 0.0300(14) 0.0251(15) N452 0.0605(16) 0.088(2) 0.0682(18) 0.0283(16) 0.0139(13) 0.0004(16) N453 0.097(2) 0.097(2) 0.111(3) 0.051(2) 0.0219(18) -0.0110(19) O51 0.0650(11) 0.0464(10) 0.0478(10) 0.0340(9) 0.0224(8) 0.0206(8) C51 0.0475(14) 0.0432(14) 0.0431(14) 0.0258(12) 0.0098(11) 0.0096(11) C52 0.0415(13) 0.0411(13) 0.0382(13) 0.0201(11) 0.0072(11) 0.0129(11) C53 0.0489(14) 0.0511(15) 0.0420(14) 0.0294(13) 0.0130(11) 0.0150(12) C54 0.0547(15) 0.0474(15) 0.0464(15) 0.0325(13) 0.0093(12) 0.0137(12) C54A 0.0446(14) 0.0444(14) 0.0388(13) 0.0206(12) 0.0056(11) 0.0118(11) C55 0.0701(18) 0.0610(17) 0.0538(17) 0.0349(15) 0.0145(14) 0.0263(14) C56 0.082(2) 0.080(2) 0.0593(18) 0.0407(18) 0.0253(16) 0.0394(16) C57 0.078(2) 0.091(2) 0.0538(17) 0.0450(19) 0.0273(15) 0.0314(17) C58 0.0674(18) 0.0701(19) 0.0484(16) 0.0382(16) 0.0194(14) 0.0169(14) C58A 0.0408(13) 0.0448(14) 0.0363(13) 0.0187(11) 0.0053(11) 0.0099(11) 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 109.79(18) C5 N1 C11 130.2(2) N2 N1 C11 119.39(18) C3 N2 N1 105.52(18) N2 C3 C4 111.9(2) N2 C3 C31 119.0(2) C4 C3 C31 129.1(2) C5 C4 C3 104.0(2) C5 C4 C43 128.0(2) C3 C4 C43 128.0(2) N1 C5 O51 121.4(2) N1 C5 C4 108.9(2) O51 C5 C4 129.7(2) C12 C11 C16 119.3(2) C12 C11 N1 122.4(2) C16 C11 N1 118.3(2) C11 C12 C13 119.5(3) C11 C12 H12 120.2 C13 C12 H12 120.2 C14 C13 C12 121.1(3) C14 C13 H13 119.4 C12 C13 H13 119.4 C13 C14 C15 119.3(3) C13 C14 H14 120.4 C15 C14 H14 120.4 C14 C15 C16 120.2(3) C14 C15 H15 119.9 C16 C15 H15 119.9 C11 C16 C15 120.6(3) C11 C16 H16 119.7 C15 C16 H16 119.7 C3 C31 H31A 109.5 C3 C31 H31B 109.5 H31A C31 H31B 109.5 C3 C31 H31C 109.5 H31A C31 H31C 109.5 H31B C31 H31C 109.5 C45 N41 N42 108.22(19) C421 N42 N41 122.79(19) C421 N42 C43 123.8(2) N41 N42 C43 113.33(17) N42 C43 C4 111.61(17) N42 C43 C44 100.55(18) C4 C43 C44 116.11(19) N42 C43 H43 109.4 C4 C43 H43 109.4 C44 C43 H43 109.4 C45 C44 C43 103.33(18) C45 C44 H44A 111.1 C43 C44 H44A 111.1 C45 C44 H44B 111.1 C43 C44 H44B 111.1 H44A C44 H44B 109.1 N41 C45 C451 121.0(2) N41 C45 C44 113.7(2) C451 C45 C44 125.3(2) O421 C421 N42 119.7(2) O421 C421 C422 122.9(2) N42 C421 C422 117.4(2) C421 C422 H42A 109.5 C421 C422 H42B 109.5 H42A C422 H42B 109.5 C421 C422 H42C 109.5 H42A C422 H42C 109.5 H42B C422 H42C 109.5 C452 C451 C456 118.0(2) C452 C451 C45 121.9(2) C456 C451 C45 120.1(2) C453 C452 C451 121.1(2) C453 C452 H452 119.4 C451 C452 H452 119.4 C452 C453 C454 120.4(3) C452 C453 H453 119.8 C454 C453 H453 119.8 C455 C454 C453 119.4(2) C455 C454 N451 124.3(3) C453 C454 N451 116.3(3) C456 C455 C454 120.2(2) C456 C455 H455 119.9 C454 C455 H455 119.9 C455 C456 C451 120.8(3) C455 C456 H456 119.6 C451 C456 H456 119.6 N452 N451 C454 116.6(3) N453 N452 N451 173.0(4) C5 O51 C52 118.44(16) C52 C51 C58A 120.1(2) C52 C51 H51 119.9 C58A C51 H51 119.9 C51 C52 C53 122.4(2) C51 C52 O51 116.1(2) C53 C52 O51 121.5(2) C54 C53 C52 118.4(2) C54 C53 H53 120.8 C52 C53 H53 120.8 C53 C54 C54A 121.6(2) C53 C54 H54 119.2 C54A C54 H54 119.2 C54 C54A C58A 119.1(2) C54 C54A C55 122.6(2) C58A C54A C55 118.3(2) C56 C55 C54A 121.2(3) C56 C55 H55 119.4 C54A C55 H55 119.4 C55 C56 C57 120.3(3) C55 C56 H56 119.8 C57 C56 H56 119.8 C58 C57 C56 120.7(3) C58 C57 H57 119.7 C56 C57 H57 119.7 C57 C58 C58A 120.8(3) C57 C58 H58 119.6 C58A C58 H58 119.6 C51 C58A C58 122.9(2) C51 C58A C54A 118.3(2) C58 C58A C54A 118.8(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C5 1.363(3) N1 N2 1.373(2) N1 C11 1.422(3) N2 C3 1.328(3) C3 C4 1.411(3) C3 C31 1.493(3) C4 C5 1.368(3) C4 C43 1.505(3) C5 O51 1.364(2) C11 C12 1.366(4) C11 C16 1.372(3) C12 C13 1.389(4) C12 H12 0.9300 C13 C14 1.356(5) C13 H13 0.9300 C14 C15 1.365(4) C14 H14 0.9300 C15 C16 1.379(4) C15 H15 0.9300 C16 H16 0.9300 C31 H31A 0.9600 C31 H31B 0.9600 C31 H31C 0.9600 N41 C45 1.286(3) N41 N42 1.387(3) N42 C421 1.360(3) N42 C43 1.488(3) C43 C44 1.535(3) C43 H43 0.9800 C44 C45 1.506(3) C44 H44A 0.9700 C44 H44B 0.9700 C45 C451 1.462(3) C421 O421 1.224(3) C421 C422 1.499(4) C422 H42A 0.9600 C422 H42B 0.9600 C422 H42C 0.9600 C451 C452 1.387(3) C451 C456 1.399(3) C452 C453 1.373(3) C452 H452 0.9300 C453 C454 1.384(4) C453 H453 0.9300 C454 C455 1.380(4) C454 N451 1.422(3) C455 C456 1.378(3) C455 H455 0.9300 C456 H456 0.9300 N451 N452 1.243(4) N452 N453 1.125(4) O51 C52 1.411(3) C51 C52 1.352(3) C51 C58A 1.411(3) C51 H51 0.9300 C52 C53 1.398(3) C53 C54 1.363(3) C53 H53 0.9300 C54 C54A 1.404(3) C54 H54 0.9300 C54A C58A 1.419(3) C54A C55 1.420(3) C55 C56 1.352(3) C55 H55 0.9300 C56 C57 1.396(4) C56 H56 0.9300 C57 C58 1.357(4) C57 H57 0.9300 C58 C58A 1.413(3) C58 H58 0.9300 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C44 H44A N2 2_666 0.97 2.60 3.397(4) 139 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 0.0(2) C11 N1 N2 C3 172.04(18) N1 N2 C3 C4 -0.5(2) N1 N2 C3 C31 178.74(18) N2 C3 C4 C5 0.8(2) C31 C3 C4 C5 -178.4(2) N2 C3 C4 C43 -175.98(19) C31 C3 C4 C43 4.9(4) N2 N1 C5 O51 -175.81(17) C11 N1 C5 O51 13.3(3) N2 N1 C5 C4 0.5(2) C11 N1 C5 C4 -170.4(2) C3 C4 C5 N1 -0.7(2) C43 C4 C5 N1 176.04(19) C3 C4 C5 O51 175.1(2) C43 C4 C5 O51 -8.1(4) C5 N1 C11 C12 -26.2(4) N2 N1 C11 C12 163.7(3) C5 N1 C11 C16 152.5(2) N2 N1 C11 C16 -17.6(3) C16 C11 C12 C13 -0.5(5) N1 C11 C12 C13 178.2(3) C11 C12 C13 C14 1.8(7) C12 C13 C14 C15 -1.8(7) C13 C14 C15 C16 0.6(5) C12 C11 C16 C15 -0.7(4) N1 C11 C16 C15 -179.4(2) C14 C15 C16 C11 0.6(5) C45 N41 N42 C421 -178.16(19) C45 N41 N42 C43 4.6(2) C421 N42 C43 C4 -62.2(3) N41 N42 C43 C4 115.0(2) C421 N42 C43 C44 174.0(2) N41 N42 C43 C44 -8.7(2) C5 C4 C43 N42 -71.3(3) C3 C4 C43 N42 104.7(2) C5 C4 C43 C44 43.1(3) C3 C4 C43 C44 -140.9(2) N42 C43 C44 C45 8.9(2) C4 C43 C44 C45 -111.7(2) N42 N41 C45 C451 -178.57(18) N42 N41 C45 C44 2.2(2) C43 C44 C45 N41 -7.5(2) C43 C44 C45 C451 173.2(2) N41 N42 C421 O421 178.4(2) C43 N42 C421 O421 -4.6(3) N41 N42 C421 C422 -1.6(3) C43 N42 C421 C422 175.4(2) N41 C45 C451 C452 -0.4(3) C44 C45 C451 C452 178.8(2) N41 C45 C451 C456 178.2(2) C44 C45 C451 C456 -2.6(3) C456 C451 C452 C453 0.6(4) C45 C451 C452 C453 179.3(2) C451 C452 C453 C454 -0.4(4) C452 C453 C454 C455 0.2(4) C452 C453 C454 N451 -179.6(2) C453 C454 C455 C456 -0.2(4) N451 C454 C455 C456 179.6(2) C454 C455 C456 C451 0.4(4) C452 C451 C456 C455 -0.7(4) C45 C451 C456 C455 -179.3(2) C455 C454 N451 N452 -4.2(4) C453 C454 N451 N452 175.6(2) N1 C5 O51 C52 -100.0(2) C4 C5 O51 C52 84.6(3) C58A C51 C52 C53 -2.2(3) C58A C51 C52 O51 178.06(19) C5 O51 C52 C51 -166.12(19) C5 O51 C52 C53 14.2(3) C51 C52 C53 C54 2.2(3) O51 C52 C53 C54 -178.1(2) C52 C53 C54 C54A -0.2(3) C53 C54 C54A C58A -1.6(3) C53 C54 C54A C55 177.8(2) C54 C54A C55 C56 -179.3(2) C58A C54A C55 C56 0.1(4) C54A C55 C56 C57 0.0(4) C55 C56 C57 C58 -0.4(4) C56 C57 C58 C58A 0.8(4) C52 C51 C58A C58 -177.8(2) C52 C51 C58A C54A 0.3(3) C57 C58 C58A C51 177.4(2) C57 C58 C58A C54A -0.7(4) C54 C54A C58A C51 1.5(3) C55 C54A C58A C51 -177.9(2) C54 C54A C58A C58 179.7(2) C55 C54A C58A C58 0.3(3) _cod_database_fobs_code 2021651