#------------------------------------------------------------------------------ #$Date: 2019-05-24 05:18:40 +0300 (Fri, 24 May 2019) $ #$Revision: 215469 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021649.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_2021649 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 'C16 H19 N3 O' _chemical_formula_moiety 'C16 H19 N3 O' _chemical_formula_sum 'C16 H19 N3 O' _chemical_formula_weight 269.34 _chemical_name_systematic ; 3-Methyl-1-phenyl-5-(piperidin-1-yl)-1H-pyrazole-4-carbaldehyde ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014 _cell_angle_alpha 90 _cell_angle_beta 97.777(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.9432(7) _cell_length_b 16.0546(14) _cell_length_c 10.1155(8) _cell_measurement_reflns_used 3504 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.090 _cell_measurement_theta_min 2.396 _cell_volume 1439.0(2) _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 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 0.0466 _diffrn_reflns_av_unetI/netI 0.0304 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 27358 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.548 _diffrn_reflns_theta_min 2.396 _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 0.080 _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_correction_T_min 0.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.243 _exptl_crystal_description block _exptl_crystal_F_000 576 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.292 _refine_diff_density_min -0.178 _refine_ls_extinction_coef 0.011(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2014 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 183 _refine_ls_number_reflns 3000 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0466 _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^)+(0.0563P)^2^+0.4589P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1117 _refine_ls_wR_factor_ref 0.1405 _reflns_number_gt 1869 _reflns_number_total 3000 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ky3177sup1.cif _cod_data_source_block VI _cod_database_code 2021649 _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 0.992 _shelx_hkl_file ; -1 0 0 -9.90 0.90 2 0 0 8127.39 165.28 -2 0 0 7941.41 169.98 -2 0 0 8184.68 167.38 -2 0 0 8351.46 168.58 2 0 0 7726.53 170.48 -2 0 0 7833.62 167.48 3 0 0 -0.40 0.60 -3 0 0 0.40 1.40 3 0 0 -0.40 1.60 3 0 0 0.10 1.20 3 0 0 1.10 1.60 -3 0 0 0.20 1.30 -3 0 0 0.50 2.60 -3 0 0 0.20 1.70 -4 0 0 6.30 1.90 -4 0 0 6.20 1.90 4 0 0 7.60 2.20 4 0 0 7.20 1.70 4 0 0 4.00 2.10 -4 0 0 4.20 2.30 -4 0 0 7.90 3.70 5 0 0 -0.60 0.70 5 0 0 -0.40 2.00 -5 0 0 1.00 1.80 5 0 0 -2.10 1.30 5 0 0 -1.20 1.60 -5 0 0 0.80 1.70 -5 0 0 2.30 2.40 -5 0 0 -1.80 3.70 6 0 0 19.50 3.50 6 0 0 22.40 2.20 -6 0 0 13.30 5.20 -6 0 0 16.70 2.90 -6 0 0 19.40 3.10 6 0 0 19.60 2.00 -6 0 0 12.90 3.60 -7 0 0 1.50 5.20 -7 0 0 -3.20 3.00 7 0 0 1.30 2.90 7 0 0 -1.50 3.00 -8 0 0 530.05 24.30 8 0 0 496.95 16.10 8 0 0 528.85 15.70 -8 0 0 505.25 18.50 -9 0 0 0.30 3.50 -9 0 0 -5.80 5.80 9 0 0 -0.80 3.20 -10 0 0 4.60 3.60 -10 0 0 1.30 6.50 -11 0 0 9.70 8.00 0 -1 0 -4.40 0.40 0 -1 0 -4.80 0.30 0 -1 0 -4.60 0.30 0 -1 0 -4.30 0.50 0 -1 0 -4.60 0.20 0 -1 0 -4.40 0.30 0 1 0 -4.20 0.50 0 1 0 -4.30 0.30 0 1 0 -4.50 0.10 0 1 0 -4.80 0.10 0 1 0 -3.80 0.50 0 1 0 -4.10 0.40 -1 -1 0 1099.79 25.20 -1 -1 0 876.31 23.40 1 -1 0 995.90 22.40 -1 -1 0 903.91 23.60 -1 -1 0 1153.08 23.60 1 1 0 1112.39 24.70 -1 1 0 1118.39 22.50 1 1 0 1127.49 23.90 -1 1 0 1012.70 22.50 -1 1 0 981.80 22.40 1 1 0 1140.69 23.90 2 -1 0 9778.32 202.98 -2 -1 0 9380.36 198.98 2 -1 0 9295.47 199.78 -2 -1 0 9432.16 199.38 2 -1 0 9812.82 200.18 -2 -1 0 9751.82 199.18 -2 -1 0 9539.05 201.58 2 1 0 9799.22 198.88 2 1 0 9109.59 200.98 -2 1 0 9999.00 202.28 -2 1 0 9498.45 201.28 -2 1 0 9668.33 201.98 2 1 0 9602.44 201.48 -2 1 0 9997.70 204.68 2 1 0 9573.24 199.48 3 -1 0 4284.07 84.79 3 -1 0 4172.08 85.89 -3 -1 0 4099.99 91.09 -3 -1 0 4136.39 88.39 3 -1 0 3982.80 85.19 -3 -1 0 4144.59 87.89 -3 -1 0 4165.48 87.29 3 1 0 3671.13 86.39 -3 1 0 4176.98 86.39 3 1 0 4079.79 87.89 3 1 0 4151.08 90.89 -3 1 0 4150.38 85.69 -3 1 0 4079.99 89.79 -3 1 0 4096.29 85.69 3 1 0 4094.49 87.39 -3 1 0 4074.09 85.79 3 1 0 4262.47 87.59 -4 -1 0 20.10 3.00 4 -1 0 21.50 2.70 -4 -1 0 18.30 2.90 4 -1 0 18.80 2.40 -4 -1 0 15.00 4.50 -4 -1 0 18.20 3.50 4 -1 0 18.90 1.50 4 -1 0 17.50 1.30 -4 1 0 18.40 2.30 4 1 0 19.90 3.20 -4 1 0 18.70 4.10 4 1 0 15.70 3.10 -4 1 0 22.90 3.00 -4 1 0 23.20 2.30 4 1 0 21.60 3.70 -5 -1 0 219.18 8.40 -5 -1 0 212.68 10.00 5 -1 0 218.78 7.70 -5 -1 0 228.28 9.10 5 -1 0 235.48 8.30 -5 -1 0 233.28 12.90 -5 1 0 230.88 8.90 -5 1 0 231.28 7.20 -5 1 0 219.48 7.40 5 1 0 236.48 9.10 5 1 0 238.48 8.70 -5 1 0 234.88 12.10 5 1 0 219.78 9.40 -6 -1 0 564.54 22.40 -6 -1 0 569.44 18.80 -6 -1 0 555.84 16.70 6 -1 0 560.24 15.00 6 -1 0 568.34 15.60 -6 1 0 548.95 14.50 -6 1 0 562.84 21.50 6 1 0 540.25 16.40 6 1 0 564.64 15.40 6 1 0 510.25 16.90 6 1 0 528.85 14.60 -6 1 0 552.44 14.20 -6 1 0 564.74 17.10 -7 -1 0 7.60 2.90 -7 -1 0 7.40 4.20 -7 -1 0 -0.20 5.10 7 -1 0 6.70 3.00 7 -1 0 12.00 3.10 7 1 0 5.70 2.30 7 1 0 5.20 2.10 7 1 0 -3.40 2.10 7 1 0 8.50 3.70 -7 1 0 7.00 2.00 -7 1 0 8.30 3.40 -7 1 0 10.50 2.10 -7 1 0 7.10 5.70 8 -1 0 2.70 3.00 -8 -1 0 3.20 4.20 -8 -1 0 6.50 6.90 8 -1 0 2.80 3.00 -8 1 0 3.90 3.60 8 1 0 10.30 4.10 8 1 0 0.60 2.70 -8 1 0 1.60 6.00 9 -1 0 -1.20 2.40 -9 -1 0 -4.00 5.90 -9 -1 0 6.80 4.30 -9 1 0 4.00 3.10 -9 1 0 -1.60 6.10 9 1 0 -1.30 3.60 -10 -1 0 8.70 7.30 -10 -1 0 6.40 4.20 -10 1 0 2.80 7.80 10 1 0 7.50 3.90 -11 -1 0 6.90 7.90 0 -2 0 3056.49 62.19 0 -2 0 3014.90 66.29 0 -2 0 3105.99 76.59 0 -2 0 2466.65 61.89 0 2 0 3117.09 62.39 0 2 0 2794.32 62.19 0 2 0 2901.71 62.49 1 -2 0 1609.34 36.20 -1 -2 0 1687.43 38.50 -1 -2 0 1698.93 39.60 -1 -2 0 1678.63 37.60 1 -2 0 1740.63 47.00 -1 -2 0 1684.73 37.90 1 -2 0 1645.74 36.30 -1 -2 0 1670.63 37.30 1 2 0 1676.43 38.50 -1 2 0 1679.03 36.20 -1 2 0 1667.23 46.70 1 2 0 1691.03 39.60 -1 2 0 1680.03 36.30 1 2 0 1719.33 37.80 1 2 0 1681.43 37.60 1 2 0 1682.23 37.30 -1 2 0 1680.93 36.20 2 -2 0 8157.58 183.18 -2 -2 0 8893.31 182.58 -2 -2 0 9175.08 194.68 -2 -2 0 8860.81 183.08 -2 -2 0 8692.93 183.08 2 -2 0 8935.11 183.88 -2 -2 0 8627.14 184.98 2 -2 0 8894.41 181.48 -2 2 0 8429.46 182.48 -2 2 0 8971.90 227.88 2 2 0 8405.26 182.38 -2 2 0 8980.10 187.28 2 2 0 8923.41 182.68 2 2 0 8780.12 182.98 2 2 0 8807.62 184.98 -2 2 0 8457.55 184.28 -3 -2 0 303.67 12.30 -3 -2 0 308.67 11.20 3 -2 0 297.97 8.10 -3 -2 0 316.67 10.70 -3 -2 0 312.97 10.10 3 -2 0 296.67 8.30 3 2 0 304.47 10.40 3 2 0 317.17 10.70 3 2 0 327.67 12.70 -3 2 0 307.57 8.20 3 2 0 296.47 10.50 -3 2 0 303.47 7.80 -3 2 0 306.67 8.00 -4 -2 0 305.87 12.10 -4 -2 0 338.37 10.90 -4 -2 0 323.27 14.40 4 -2 0 313.57 9.10 -4 -2 0 327.87 11.60 4 -2 0 315.67 8.80 -4 2 0 311.27 8.40 -4 2 0 305.17 8.20 -4 2 0 313.17 8.90 4 2 0 313.27 10.70 4 2 0 311.37 11.00 4 2 0 339.17 12.00 4 2 0 320.47 11.50 -4 2 0 323.57 9.60 4 2 0 340.37 14.00 5 -2 0 257.97 8.50 -5 -2 0 260.77 12.00 -5 -2 0 273.87 11.00 -5 -2 0 280.47 10.40 -5 -2 0 295.07 14.90 5 -2 0 259.57 8.20 5 2 0 298.97 14.30 -5 2 0 262.47 8.50 -5 2 0 296.87 13.20 5 2 0 264.97 9.90 -5 2 0 266.07 7.50 5 2 0 266.67 11.20 5 2 0 292.97 10.90 -5 2 0 268.77 9.40 5 2 0 269.57 10.70 -5 2 0 262.87 7.60 6 -2 0 4.90 2.20 -6 -2 0 10.20 5.90 6 -2 0 5.60 2.30 -6 -2 0 9.80 3.20 -6 -2 0 10.40 3.90 6 2 0 10.20 4.00 -6 2 0 6.70 1.50 -6 2 0 6.50 2.70 -6 2 0 7.40 1.50 6 2 0 7.70 3.30 -6 2 0 9.70 4.80 6 2 0 0.70 1.00 6 2 0 0.70 3.70 -7 -2 0 40.60 8.70 -7 -2 0 42.90 5.40 7 -2 0 51.59 4.20 7 -2 0 45.90 4.20 -7 -2 0 51.79 7.40 -7 2 0 37.90 7.60 7 2 0 48.90 4.80 -7 2 0 49.99 1.80 7 2 0 57.69 6.40 7 2 0 53.39 6.50 -7 2 0 49.30 5.10 -7 2 0 49.99 1.70 -8 -2 0 73.69 11.40 8 -2 0 67.09 4.20 -8 -2 0 67.79 8.70 8 -2 0 60.29 4.20 -8 2 0 66.79 10.40 8 2 0 69.09 7.20 -9 -2 0 -1.40 6.70 -9 -2 0 1.80 4.50 -9 2 0 3.80 6.40 9 2 0 0.40 4.10 -10 -2 0 14.50 5.60 -10 -2 0 22.30 9.10 10 2 0 8.60 4.70 -10 2 0 -3.40 5.40 -11 -2 0 3.60 4.90 -11 -2 0 5.40 8.00 -11 2 0 -14.50 7.00 0 -3 0 -0.10 1.60 0 -3 0 1.20 1.50 0 -3 0 -0.30 1.20 0 -3 0 0.10 1.30 0 -3 0 -0.10 1.50 0 -3 0 1.10 1.40 0 3 0 0.30 1.80 0 3 0 -0.30 1.80 0 3 0 0.70 1.50 0 3 0 2.00 1.90 0 3 0 -0.90 1.20 0 3 0 -1.30 1.30 -1 -3 0 2262.37 51.39 1 -3 0 2218.28 48.90 -1 -3 0 2229.18 50.89 1 -3 0 2287.77 62.19 1 -3 0 2205.28 49.20 -1 -3 0 2297.27 50.59 -1 -3 0 2305.47 53.09 -1 -3 0 2249.97 50.09 1 -3 0 2195.28 49.10 -1 3 0 2247.98 49.00 1 3 0 2238.58 50.69 1 3 0 2254.57 51.39 -1 3 0 2210.18 48.90 -1 3 0 2243.38 62.09 1 3 0 2262.97 50.49 -1 3 0 2245.98 49.20 -1 3 0 2264.97 54.39 1 3 0 2244.98 50.09 -1 3 0 2324.17 49.60 1 3 0 2250.57 53.09 -2 -3 0 3346.47 74.89 -2 -3 0 3363.56 72.49 -2 -3 0 3267.37 73.49 2 -3 0 3295.67 70.39 -2 -3 0 3377.76 77.19 -2 -3 0 3354.56 73.19 2 3 0 3290.67 72.99 -2 3 0 3413.66 91.79 2 3 0 3330.97 74.79 -2 3 0 3258.47 70.29 2 3 0 3295.97 76.99 2 3 0 3215.78 72.29 -2 3 0 3230.08 70.09 2 3 0 3356.86 72.99 -2 3 0 3318.37 70.09 -3 -3 0 275.07 11.40 3 -3 0 273.07 7.20 3 -3 0 268.27 8.00 -3 -3 0 260.77 10.80 -3 -3 0 274.67 10.00 3 -3 0 267.77 7.10 -3 -3 0 262.17 12.40 -3 -3 0 264.87 10.50 3 3 0 264.37 10.20 3 3 0 279.07 10.80 -3 3 0 266.47 7.50 -3 3 0 269.17 7.60 3 3 0 279.97 10.80 3 3 0 257.57 11.70 -3 3 0 270.77 8.00 -3 3 0 266.27 15.50 -4 -3 0 6.30 3.70 -4 -3 0 -1.20 3.00 -4 -3 0 4.40 2.70 4 -3 0 0.60 1.90 -4 -3 0 1.70 2.70 4 -3 0 0.10 1.60 -4 -3 0 12.80 5.10 4 3 0 4.20 3.10 -4 3 0 1.50 1.20 4 3 0 1.10 3.00 4 3 0 1.10 2.90 -4 3 0 1.40 1.40 4 3 0 2.40 3.60 -4 3 0 1.00 1.60 -4 3 0 0.60 3.10 5 -3 0 905.21 21.10 5 -3 0 874.71 20.70 -5 -3 0 917.81 25.50 -5 -3 0 899.51 26.80 -5 -3 0 867.51 29.00 5 3 0 855.11 23.80 5 3 0 885.71 25.50 -5 3 0 869.11 21.10 -5 3 0 852.11 19.70 -5 3 0 894.11 19.80 5 3 0 900.21 25.10 5 3 0 868.91 24.50 6 -3 0 8.10 2.20 -6 -3 0 14.00 6.40 6 -3 0 9.70 2.30 -6 -3 0 4.60 3.40 -6 -3 0 8.90 4.80 6 3 0 9.60 4.10 -6 3 0 9.90 4.80 -6 3 0 7.20 0.80 6 3 0 12.30 3.60 6 3 0 4.70 4.00 -6 3 0 9.20 0.90 -6 3 0 10.50 2.30 7 -3 0 229.08 7.00 -7 -3 0 203.28 12.60 7 -3 0 207.88 7.00 -7 -3 0 218.78 11.30 -7 -3 0 236.18 15.40 7 3 0 224.58 11.60 7 3 0 214.08 11.50 -7 3 0 226.68 14.00 -8 -3 0 26.30 6.80 -8 -3 0 41.80 8.90 -8 3 0 25.30 7.60 8 3 0 31.40 6.00 -9 -3 0 25.00 9.30 -9 -3 0 17.80 6.20 -9 3 0 14.80 7.20 9 3 0 19.00 5.60 -9 3 0 23.10 10.90 -10 -3 0 37.50 8.40 -10 -3 0 33.90 10.30 -10 3 0 11.50 7.10 -10 3 0 18.60 11.10 10 3 0 21.60 5.90 -11 -3 0 3.00 9.00 -11 -3 0 0.00 6.00 -11 3 0 -6.10 9.30 0 -4 0 2253.77 49.60 0 -4 0 2173.48 53.09 0 -4 0 2203.98 50.19 0 -4 0 2244.08 61.19 0 -4 0 2172.08 49.90 0 -4 0 2228.68 50.29 0 4 0 2243.48 50.19 0 4 0 2084.49 49.20 0 4 0 2182.68 60.89 0 4 0 2220.88 49.70 0 4 0 2222.88 50.29 0 4 0 2143.29 52.99 1 -4 0 7101.29 149.79 -1 -4 0 6943.91 151.58 1 -4 0 7425.26 186.28 -1 -4 0 7124.49 152.58 1 -4 0 7028.00 150.18 -1 -4 0 6725.83 151.28 -1 -4 0 7354.26 185.78 -1 -4 0 7346.67 160.38 1 -4 0 7409.96 161.88 1 -4 0 7025.30 149.99 -1 -4 0 6905.11 150.78 -1 4 0 7120.39 149.88 1 4 0 7024.00 151.38 -1 4 0 7399.16 161.88 1 4 0 6993.30 151.38 -1 4 0 6924.21 149.88 -1 4 0 7526.85 186.28 1 4 0 7114.79 152.48 1 4 0 7216.98 160.28 -1 4 0 7144.99 149.79 1 4 0 6813.52 150.78 -1 4 0 7282.37 150.58 2 -4 0 2114.19 47.30 -2 -4 0 2141.29 50.79 2 -4 0 2109.29 47.20 -2 -4 0 2141.19 51.49 -2 -4 0 2129.49 50.09 -2 -4 0 2112.29 52.19 2 -4 0 2187.48 62.59 -2 -4 0 2169.18 49.40 2 -4 0 2121.49 47.40 2 4 0 2160.08 49.50 -2 4 0 2139.29 47.10 -2 4 0 2129.59 62.29 -2 4 0 2092.99 47.40 2 4 0 2105.09 51.39 2 4 0 2170.48 50.19 -2 4 0 2091.79 54.49 2 4 0 2079.09 51.99 2 4 0 2196.38 49.99 -2 4 0 2099.09 47.00 -3 -4 0 34.20 4.90 -3 -4 0 28.60 5.30 3 -4 0 28.60 3.30 -3 -4 0 22.60 4.30 -3 -4 0 42.60 4.90 -3 -4 0 32.90 4.90 3 -4 0 25.20 2.80 -3 4 0 30.50 3.20 3 4 0 33.10 4.70 3 4 0 33.10 5.00 -3 4 0 23.60 5.00 3 4 0 30.50 5.10 3 4 0 22.80 4.50 -3 4 0 34.80 3.00 -3 4 0 28.90 3.00 4 -4 0 4086.89 87.29 -4 -4 0 3880.21 92.89 -4 -4 0 4216.98 92.59 -4 -4 0 4251.27 98.49 4 -4 0 4018.80 87.29 -4 -4 0 4220.88 91.39 -4 -4 0 4031.90 95.89 4 4 0 4154.38 91.59 -4 4 0 4005.20 86.59 -4 4 0 4059.89 87.19 -4 4 0 4125.69 118.69 -4 4 0 4128.09 86.49 4 4 0 4084.99 92.09 4 4 0 4183.78 92.09 4 4 0 4186.28 95.99 5 -4 0 42.30 4.00 -5 -4 0 55.59 6.60 5 -4 0 52.29 4.10 -5 -4 0 46.90 6.80 -5 -4 0 44.50 8.10 -5 4 0 43.40 3.60 -5 4 0 38.50 8.90 -5 4 0 50.19 2.70 -5 4 0 40.70 2.70 5 4 0 45.10 6.10 5 4 0 41.00 6.30 -6 -4 0 62.09 7.30 -6 -4 0 60.19 8.00 6 -4 0 56.79 3.90 6 -4 0 54.69 3.80 -6 -4 0 52.29 9.50 -6 4 0 49.60 3.90 -6 4 0 39.20 9.60 -6 4 0 55.39 7.30 6 4 0 55.49 6.40 6 4 0 45.60 6.40 6 4 0 39.30 6.40 -7 -4 0 202.68 13.30 -7 -4 0 240.98 16.20 7 -4 0 200.18 6.00 7 -4 0 195.08 6.00 -7 -4 0 182.58 11.30 -7 4 0 201.88 7.80 7 4 0 199.58 10.40 7 4 0 189.08 11.80 -7 4 0 192.48 13.00 -7 4 0 186.38 21.10 7 4 0 204.18 11.50 -8 -4 0 -5.30 5.20 -8 -4 0 2.70 7.30 -8 4 0 7.90 5.60 -8 4 0 4.30 5.90 8 4 0 1.40 5.00 -9 -4 0 111.59 15.20 -9 -4 0 146.39 13.40 9 4 0 140.09 10.90 -9 4 0 189.98 24.10 -9 4 0 163.58 14.50 -10 -4 0 -1.90 7.20 -10 -4 0 -5.00 5.30 -10 4 0 -2.70 6.40 10 4 0 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3 -13 0 34.80 8.60 3 -13 0 52.79 8.70 3 13 0 42.20 8.90 -3 13 0 56.59 8.50 -3 13 0 66.39 9.90 -3 13 0 44.20 10.00 -3 13 0 41.30 9.90 3 13 0 46.30 10.50 4 -13 0 67.99 10.00 4 -13 0 55.89 8.80 -4 -13 0 80.49 13.10 -4 -13 0 67.29 12.30 -4 -13 0 53.79 11.40 -4 13 0 69.69 8.90 4 13 0 74.19 12.30 4 13 0 52.59 10.90 -4 13 0 40.90 10.00 -4 13 0 38.30 9.90 -5 -13 0 44.60 9.90 -5 -13 0 56.69 14.30 -5 -13 0 35.10 10.60 5 -13 0 16.40 6.80 -5 13 0 43.10 10.90 -5 13 0 32.70 9.30 5 13 0 32.80 10.50 5 13 0 37.10 9.00 -6 -13 0 16.80 9.10 -6 -13 0 19.80 7.60 -6 -13 0 23.30 9.60 6 -13 0 21.20 7.10 -6 13 0 16.80 11.40 -6 13 0 18.00 9.50 6 13 0 31.70 10.50 -7 -13 0 -1.70 7.70 -7 -13 0 -4.90 10.60 7 -13 0 0.20 5.70 -7 -13 0 1.60 7.60 7 13 0 -1.70 8.40 -7 13 0 -4.10 6.20 -7 13 0 6.40 10.50 -8 -13 0 9.00 8.60 8 -13 0 -0.50 4.90 -8 -13 0 2.30 11.90 -8 13 0 5.20 9.40 8 13 0 2.30 8.80 -8 13 0 8.30 8.80 -9 -13 0 -4.50 9.80 -9 -13 0 -0.50 12.90 -9 13 0 -9.60 8.00 -9 13 0 2.90 13.30 9 13 0 -1.30 9.00 0 -14 0 185.08 17.70 0 -14 0 228.08 18.10 0 -14 0 183.18 15.10 0 14 0 196.48 14.20 0 14 0 201.28 19.20 0 14 0 179.68 17.00 -1 -14 0 68.59 12.20 -1 -14 0 78.49 13.20 1 -14 0 58.99 11.60 -1 -14 0 47.80 10.50 1 -14 0 59.79 11.40 1 14 0 39.10 9.60 -1 14 0 52.39 9.70 -1 14 0 42.00 11.10 1 14 0 59.29 12.30 -1 14 0 40.70 10.10 -2 -14 0 49.70 11.50 -2 -14 0 36.70 11.50 2 -14 0 43.60 9.70 2 -14 0 45.00 10.70 -2 -14 0 49.00 12.10 -2 14 0 53.39 8.20 2 14 0 56.79 10.20 2 14 0 48.60 9.80 -2 14 0 43.90 10.40 -2 14 0 44.80 10.30 -3 -14 0 0.30 9.70 -3 -14 0 14.40 9.30 3 -14 0 9.90 7.60 3 -14 0 6.10 7.50 -3 -14 0 5.10 9.60 3 14 0 -2.50 7.70 3 14 0 0.30 5.60 -3 14 0 -2.80 6.70 -3 14 0 14.10 6.30 -3 14 0 5.00 6.70 4 -14 0 5.30 6.80 -4 -14 0 -7.10 9.30 -4 -14 0 -3.70 5.60 4 -14 0 5.20 7.40 -4 -14 0 -19.00 8.20 -4 14 0 1.20 6.90 -4 14 0 -10.70 5.50 4 14 0 4.50 8.60 -4 14 0 -0.30 5.20 4 14 0 6.00 8.00 5 -14 0 18.90 7.10 -5 -14 0 18.40 9.50 -5 -14 0 28.90 9.80 -5 -14 0 15.00 7.80 -5 14 0 1.30 7.20 5 14 0 21.50 9.40 -5 14 0 22.80 9.10 5 14 0 12.30 10.20 -6 -14 0 14.90 10.70 -6 -14 0 1.80 6.60 -6 -14 0 -6.50 10.10 6 -14 0 -1.10 6.20 6 14 0 -8.50 8.50 -6 14 0 -1.80 9.90 -6 14 0 9.30 8.20 -7 -14 0 12.20 12.10 -7 -14 0 32.90 13.50 7 -14 0 13.70 7.10 -7 -14 0 1.90 8.60 -7 14 0 10.30 8.70 7 14 0 14.40 10.20 -7 14 0 10.10 8.70 -8 -14 0 -4.70 6.70 -8 -14 0 -5.10 11.40 -8 14 0 7.80 8.80 8 14 0 9.30 9.70 -8 14 0 8.50 11.90 0 -15 0 -7.10 8.60 0 -15 0 1.70 8.90 0 -15 0 -0.40 5.60 0 15 0 -0.20 6.90 0 15 0 1.10 9.00 0 15 0 -0.90 6.90 1 -15 0 -2.50 6.90 1 -15 0 13.70 9.60 -1 -15 0 0.90 6.00 -1 -15 0 -2.90 8.50 -1 -15 0 -1.80 9.20 1 15 0 10.40 8.10 -1 15 0 -5.00 6.90 -1 15 0 -11.80 7.90 1 15 0 -0.90 8.20 -1 15 0 -4.20 4.30 -2 -15 0 78.29 14.30 2 -15 0 94.69 13.30 -2 -15 0 78.09 14.90 2 -15 0 79.39 12.70 -2 -15 0 95.99 14.80 -2 15 0 88.39 14.70 -2 15 0 68.69 13.10 -2 15 0 101.59 11.70 2 15 0 59.29 12.60 2 15 0 95.89 13.40 -3 -15 0 11.70 10.40 3 -15 0 11.80 8.20 -3 -15 0 9.80 8.80 -3 -15 0 11.40 9.30 3 -15 0 4.20 7.70 -3 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-12 4.90 11.60 -5 3 12 5.70 11.40 5 3 -12 13.90 9.50 4 -3 -12 -1.70 8.30 -4 -3 12 33.30 12.80 4 -3 -12 22.90 12.20 -4 3 12 -21.80 9.00 -4 3 12 15.70 10.90 4 3 -12 32.10 11.80 4 3 -12 12.80 12.10 3 -3 -12 13.80 12.00 3 -3 -12 16.10 10.50 -3 -3 12 2.80 7.40 3 3 -12 12.70 9.80 -3 3 12 -18.20 8.00 3 3 -12 2.20 11.00 -3 3 12 14.10 10.70 2 -3 -12 -3.90 7.10 -2 -3 12 2.00 9.60 2 -3 -12 9.40 10.40 -2 3 12 3.10 9.80 2 3 -12 1.70 7.80 2 3 -12 9.00 9.20 -2 3 12 -8.10 9.70 1 -3 -12 -2.00 8.50 1 -3 -12 3.70 8.20 1 -3 -12 8.60 7.80 -1 -3 12 3.50 7.60 1 3 -12 13.90 8.30 1 3 -12 -11.90 7.20 -1 3 12 0.20 9.90 0 -3 -12 2.90 9.90 0 -3 -12 3.90 7.80 0 -3 -12 10.00 7.40 0 -3 12 11.10 10.50 0 3 12 -3.30 6.40 0 3 -12 6.10 7.60 1 -3 12 1.60 8.60 -1 -3 -12 16.50 11.50 -1 -3 -12 -18.30 8.30 1 3 12 6.50 7.70 -1 3 -12 0.20 8.70 -2 -3 -12 -5.00 11.60 2 -3 12 6.90 8.80 -2 -3 -12 -5.40 9.50 2 3 12 3.20 10.40 -2 3 -12 7.40 8.90 -3 -3 -12 -4.30 9.80 -3 -3 -12 -2.50 12.40 3 -3 12 27.50 11.20 -3 3 -12 7.60 8.90 3 3 12 18.40 11.70 -6 -4 12 7.90 11.50 6 -4 -12 9.80 9.40 6 -4 -12 7.40 11.50 -6 4 12 0.90 11.80 6 4 -12 3.10 11.50 -6 4 12 10.70 11.50 6 4 -12 1.40 12.70 5 -4 -12 14.10 10.50 5 -4 -12 11.80 11.20 -5 -4 12 27.40 13.30 -5 4 12 12.90 9.30 -5 4 12 14.50 13.10 5 4 -12 18.10 12.70 5 4 -12 24.00 10.40 4 -4 -12 29.30 11.80 4 -4 -12 45.40 14.30 -4 -4 12 33.70 11.50 -4 4 12 62.59 15.30 -4 4 12 20.70 14.50 4 4 -12 42.50 12.30 4 4 -12 44.10 13.30 3 -4 -12 21.90 12.50 3 -4 -12 12.50 9.00 -3 -4 12 35.10 13.60 -3 4 12 -7.60 10.10 3 4 -12 6.30 8.10 3 4 -12 -6.70 10.50 -3 4 12 40.20 11.60 2 -4 -12 36.10 12.50 2 -4 -12 63.49 13.60 -2 -4 12 35.20 13.10 -2 4 12 2.80 10.50 -2 4 12 54.79 12.90 2 4 -12 37.30 13.40 2 4 -12 26.80 9.10 1 -4 -12 8.10 8.80 1 -4 -12 -1.50 10.40 -1 -4 12 9.90 10.20 1 -4 -12 -0.50 8.50 1 4 -12 -1.40 8.00 1 4 -12 10.40 10.60 -1 4 12 -3.00 8.90 -1 4 12 -20.40 8.20 0 -4 12 -3.20 6.70 0 -4 -12 14.10 10.50 0 -4 -12 -8.90 8.80 0 -4 -12 -22.80 8.50 0 4 -12 -5.40 9.20 0 4 12 0.90 9.40 -1 -4 -12 -1.70 10.80 -1 -4 -12 10.00 11.00 1 -4 12 6.10 9.40 -1 4 -12 6.40 10.00 1 4 12 14.70 11.20 -2 -4 -12 -8.60 12.00 2 -4 12 7.90 9.10 -2 -4 -12 16.90 9.40 -2 4 -12 4.80 9.70 2 4 12 -4.30 9.40 -3 -4 -12 -12.40 8.50 3 -4 12 19.20 9.40 -3 -4 -12 14.50 13.50 3 4 12 -19.30 9.10 -3 4 -12 1.00 8.50 -5 -5 12 10.20 10.80 5 -5 -12 9.30 13.50 5 -5 -12 11.40 11.80 5 5 -12 -7.50 9.70 -5 5 12 -0.70 10.40 -5 5 12 -16.10 11.00 5 5 -12 10.00 9.80 -4 -5 12 11.30 11.40 4 -5 -12 -14.70 5.60 4 -5 -12 -9.50 11.50 -4 5 12 22.30 10.30 4 5 -12 -3.30 7.20 4 5 -12 3.70 11.30 -4 5 12 -16.60 11.50 3 -5 -12 20.90 11.80 -3 -5 12 6.60 8.30 3 -5 -12 13.00 9.90 3 5 -12 3.20 10.00 -3 5 12 3.60 11.00 -3 5 12 -14.20 10.00 3 5 -12 -4.90 7.80 2 -5 -12 16.80 9.10 -2 -5 12 3.60 8.00 2 -5 -12 34.40 14.50 -2 5 12 13.50 11.40 2 5 -12 18.70 10.90 2 5 -12 15.30 9.60 -2 5 12 -10.60 9.70 1 -5 -12 -0.80 11.60 1 -5 -12 -13.90 9.10 -1 -5 12 -0.80 6.80 1 -5 -12 8.20 9.90 1 5 -12 11.60 8.70 1 5 -12 -0.50 6.20 -1 5 12 3.60 7.60 -1 5 12 -22.40 8.10 0 -5 12 3.30 10.50 0 -5 -12 9.40 10.70 0 -5 -12 -5.30 6.30 0 -5 -12 -4.30 10.80 0 5 -12 2.70 10.10 0 5 12 2.40 10.60 -1 -5 -12 -3.60 7.50 1 -5 12 23.30 11.20 -1 -5 -12 23.60 13.20 1 5 12 13.50 11.00 -1 5 -12 -8.20 8.50 -2 -5 -12 8.40 12.20 -2 -5 -12 4.80 12.60 2 -5 12 15.00 9.90 2 5 12 -14.50 8.90 -2 5 -12 -3.50 7.90 -3 -5 -12 4.80 9.70 5 -6 -12 -6.80 11.10 -5 -6 12 26.60 12.30 5 -6 -12 10.40 9.60 -5 6 12 33.00 13.40 5 6 -12 0.00 10.50 -5 6 12 -2.10 9.60 5 6 -12 -1.10 11.40 4 -6 -12 -7.30 11.30 -4 -6 12 12.40 10.80 4 -6 -12 -5.10 10.30 -4 6 12 14.20 11.50 4 6 -12 -13.30 8.60 4 6 -12 12.30 12.10 -4 6 12 -6.00 12.30 -3 -6 12 7.00 7.90 3 -6 -12 -0.80 10.40 3 -6 -12 8.00 12.50 -3 6 12 -4.80 9.10 -3 6 12 -23.10 10.00 3 6 -12 -4.30 10.80 3 6 -12 -7.40 8.70 2 -6 -12 -3.90 10.20 2 -6 -12 -1.70 10.80 -2 -6 12 15.70 10.90 -2 6 12 -16.70 10.10 -2 6 12 1.20 9.90 2 6 -12 3.40 7.90 2 6 -12 -2.30 8.80 1 -6 -12 -2.80 6.60 1 -6 -12 2.90 8.50 -1 -6 12 15.40 10.60 -1 6 12 -21.90 9.30 -1 6 12 16.60 11.90 1 6 -12 3.80 10.30 0 -6 -12 4.10 9.80 0 -6 12 5.30 10.70 0 -6 -12 -8.30 10.70 0 -6 -12 24.20 10.60 0 6 12 5.20 8.60 0 6 -12 1.70 10.00 -1 -6 -12 13.60 12.70 -1 -6 -12 -6.10 9.30 1 -6 12 8.20 9.60 1 6 12 11.30 11.20 -1 6 -12 6.50 10.50 -2 -6 -12 14.50 13.00 2 -6 12 8.00 10.00 -2 -6 -12 -14.30 10.80 -2 6 -12 4.90 9.30 2 6 12 24.60 12.20 -4 -7 12 18.80 12.30 4 -7 -12 3.40 9.30 4 -7 -12 3.70 10.70 -4 7 12 9.40 11.90 4 7 -12 1.60 11.90 4 7 -12 -8.90 8.10 -4 7 12 -14.10 13.00 -3 -7 12 26.80 12.50 3 -7 -12 9.60 13.10 3 -7 -12 24.70 10.70 -3 7 12 2.30 13.60 3 7 -12 7.80 12.10 3 7 -12 34.80 11.90 -3 7 12 31.90 11.10 2 -7 -12 -4.10 6.60 2 -7 -12 -5.20 7.80 -2 -7 12 8.40 10.60 2 7 -12 2.10 8.80 2 7 -12 12.20 11.10 -2 7 12 -7.90 11.60 -2 7 12 -4.30 7.40 1 -7 -12 -8.30 9.50 -1 -7 12 15.60 11.20 1 -7 -12 14.70 10.40 -1 7 12 -21.70 9.40 -1 7 12 5.60 8.60 1 7 -12 0.40 7.20 0 -7 -12 11.30 10.10 0 -7 -12 -8.00 9.10 0 -7 12 11.50 11.00 0 -7 -12 15.30 10.80 0 7 12 12.60 12.00 0 7 -12 -7.80 6.10 -1 -7 -12 -3.00 10.30 -1 -7 -12 -1.80 12.20 1 -7 12 6.70 10.30 -1 7 -12 -12.20 8.40 1 7 12 -5.90 10.20 2 -7 12 8.20 11.00 -2 -7 -12 17.20 14.10 2 7 12 8.40 10.60 -4 -8 12 29.20 11.40 4 -8 -12 -0.80 9.10 4 -8 -12 11.60 10.10 4 8 -12 -0.70 10.80 4 8 -12 3.70 9.30 -4 8 12 17.10 9.70 -4 8 12 -22.10 12.90 3 -8 -12 -2.80 8.50 3 -8 -12 8.70 11.60 -3 -8 12 2.70 10.90 3 8 -12 -15.00 7.40 -3 8 12 2.40 11.50 3 8 -12 -12.50 5.10 -3 8 12 -28.60 11.80 2 -8 -12 2.30 10.70 -2 -8 12 8.60 11.50 2 -8 -12 32.40 15.40 -2 8 12 4.20 10.10 2 8 -12 17.80 12.30 2 8 -12 -0.60 6.70 -2 8 12 33.60 13.90 -1 -8 12 15.40 11.20 1 -8 -12 3.90 13.20 1 -8 -12 0.80 8.30 1 8 -12 -0.60 7.60 -1 8 12 21.00 12.50 -1 8 12 -20.90 10.70 0 -8 -12 -5.90 10.00 0 -8 -12 -3.50 12.70 0 -8 12 2.30 10.50 0 8 -12 16.10 10.60 0 8 12 4.40 8.20 -1 -8 -12 -7.20 10.10 1 -8 12 -6.20 9.40 -1 -8 -12 12.00 11.50 1 8 12 -9.20 9.50 -1 8 -12 10.90 8.50 -2 -9 12 9.70 10.90 2 -9 -12 -17.60 10.20 2 -9 -12 -4.40 12.00 -2 9 12 -23.00 11.80 2 9 -12 -3.00 11.10 -2 9 12 10.90 9.10 -1 -9 12 3.30 10.50 1 -9 -12 7.40 10.50 1 -9 -12 -9.40 10.50 -1 9 12 -29.00 10.90 -1 9 12 4.50 12.10 1 9 -12 2.80 11.20 0 -9 12 -7.70 9.70 0 -9 -12 8.20 11.80 0 9 12 2.60 12.00 4 0 -13 2.30 11.40 -4 0 13 5.70 11.80 4 0 -13 -5.80 12.40 3 0 -13 32.20 14.10 -3 0 13 18.30 10.00 3 0 -13 -1.10 10.50 -2 0 13 23.70 12.10 2 0 -13 1.90 13.10 2 0 -13 1.90 10.40 1 0 -13 1.90 9.80 1 0 -13 -5.20 8.20 -1 0 13 -0.30 8.10 0 0 13 12.30 10.70 0 0 -13 -24.60 8.90 1 0 13 35.90 13.20 -1 0 -13 29.60 13.70 4 -1 -13 -5.00 8.20 4 -1 -13 -4.90 8.20 -4 -1 13 19.60 10.70 -4 1 13 5.70 11.60 4 1 -13 -2.80 7.80 4 1 -13 3.90 10.20 3 -1 -13 -9.40 8.90 3 -1 -13 24.60 14.30 -3 -1 13 12.60 12.50 -3 1 13 5.80 11.70 3 1 -13 32.10 14.40 3 1 -13 -12.10 5.70 2 -1 -13 6.00 9.60 -2 -1 13 14.40 11.30 2 -1 -13 7.40 10.10 2 1 -13 -1.30 7.30 2 1 -13 13.30 13.10 -2 1 13 6.60 10.80 -1 -1 13 15.70 11.70 1 -1 -13 8.30 12.50 1 -1 -13 -7.50 8.70 1 1 -13 4.70 11.90 -1 1 13 2.10 11.00 0 -1 -13 8.50 11.90 0 -1 13 4.90 10.50 0 1 -13 26.70 13.40 0 1 13 39.20 11.40 1 -1 13 8.50 10.40 -1 -1 -13 -16.30 9.70 1 1 13 5.30 7.90 -1 1 -13 12.10 11.30 4 -2 -13 6.20 13.00 -4 -2 13 -1.90 11.60 4 -2 -13 -8.80 10.40 4 2 -13 4.30 13.40 4 2 -13 -5.30 10.10 -4 2 13 8.70 11.80 -3 -2 13 18.90 10.30 3 -2 -13 27.10 10.60 3 -2 -13 15.90 11.40 3 2 -13 5.80 9.80 3 2 -13 50.69 13.70 -3 2 13 28.40 11.70 -2 -2 13 -8.60 6.70 2 -2 -13 1.90 9.80 2 -2 -13 1.90 12.60 -2 2 13 -1.50 10.80 2 2 -13 0.50 9.90 2 2 -13 5.30 11.90 1 -2 -13 0.30 9.90 1 -2 -13 3.20 9.40 1 -2 -13 -6.30 11.50 -1 -2 13 1.20 10.80 1 2 -13 29.00 11.30 -1 2 13 11.30 9.30 0 -2 -13 1.70 10.60 0 -2 13 0.30 10.60 0 -2 -13 -10.30 11.00 0 2 13 8.60 10.90 0 2 -13 3.00 10.70 -1 -2 -13 7.60 12.80 3 -3 -13 4.30 13.30 3 -3 -13 12.70 11.90 -3 -3 13 7.30 11.90 3 3 -13 22.40 9.80 3 3 -13 14.50 13.50 -3 3 13 17.50 13.00 -2 -3 13 11.40 11.30 2 -3 -13 10.40 10.00 2 -3 -13 1.90 10.60 2 3 -13 -4.20 8.70 -2 3 13 -0.40 11.00 2 3 -13 5.20 9.80 1 -3 -13 -3.50 8.50 -1 -3 13 10.90 11.60 1 -3 -13 -1.70 9.20 -1 3 13 14.80 11.50 1 3 -13 -1.80 10.90 0 -3 -13 -3.00 8.20 0 -3 13 2.20 10.40 0 -3 -13 8.70 11.90 0 3 13 1.80 8.30 0 3 -13 0.20 11.20 -3 -4 13 7.80 12.40 3 -4 -13 12.20 9.50 3 -4 -13 7.90 10.40 3 4 -13 5.50 7.50 3 4 -13 6.20 10.10 -3 4 13 -4.40 7.90 2 -4 -13 14.10 14.40 -2 -4 13 18.90 12.10 2 -4 -13 -2.90 9.20 2 4 -13 13.00 8.80 2 4 -13 -15.20 10.50 -2 4 13 13.90 10.30 -1 -4 13 50.59 15.00 1 -4 -13 17.20 14.50 1 -4 -13 21.50 11.40 1 4 -13 15.20 12.00 -1 4 13 12.10 9.60 0 -4 13 31.30 12.40 0 -4 -13 8.00 11.20 0 -4 -13 13.50 13.40 0 4 -13 7.50 11.60 0 4 13 20.80 12.50 -2 -5 13 5.00 8.70 -2 5 13 2.40 12.30 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 1523 _shelx_res_file ; TITL bk2cg CELL 0.71073 8.9432 16.0546 10.1155 90.000 97.777 90.000 ZERR 4.00 0.0007 0.0014 0.0008 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 64 76 12 4 MERG 2 FMAP 2 OMIT -2 53.1 PLAN 10 SIZE 0.100 0.150 0.200 ACTA BOND $H CONF HTAB L.S. 20 TEMP 23.00 WGHT 0.056300 0.458900 EXTI 0.010969 FVAR 0.95526 N1 3 0.351853 0.628446 0.684522 11.00000 0.04863 0.04871 = 0.04072 0.00697 0.01348 -0.00080 N2 3 0.399105 0.667231 0.574960 11.00000 0.05232 0.05961 = 0.04979 0.01693 0.01610 0.00337 C3 1 0.366388 0.614496 0.476294 11.00000 0.04770 0.06752 = 0.04298 0.01488 0.01229 0.01096 C4 1 0.303051 0.539268 0.518007 11.00000 0.04959 0.05875 = 0.03558 0.00538 0.00668 0.00920 C5 1 0.295387 0.551003 0.654073 11.00000 0.04022 0.04971 = 0.03833 0.00560 0.00589 0.00349 C11 1 0.363444 0.673697 0.806589 11.00000 0.04906 0.04182 = 0.04336 0.00650 0.00549 -0.00015 C12 1 0.237666 0.685659 0.869663 11.00000 0.05160 0.05484 = 0.05083 0.00150 0.01098 -0.00070 AFIX 43 H12 2 0.144720 0.664394 0.832378 11.00000 -1.20000 AFIX 0 C13 1 0.250139 0.729300 0.988329 11.00000 0.08086 0.05623 = 0.05084 0.00240 0.01801 0.00749 AFIX 43 H13 2 0.165601 0.737291 1.031206 11.00000 -1.20000 AFIX 0 C14 1 0.387576 0.760927 1.043054 11.00000 0.10161 0.05007 = 0.04711 0.00301 -0.00247 0.00088 AFIX 43 H14 2 0.396151 0.789696 1.123524 11.00000 -1.20000 AFIX 0 C15 1 0.511809 0.750141 0.979298 11.00000 0.07539 0.05585 = 0.06759 0.00429 -0.01504 -0.00999 AFIX 43 H15 2 0.604038 0.772660 1.015793 11.00000 -1.20000 AFIX 0 C16 1 0.501108 0.705997 0.861022 11.00000 0.05054 0.05519 = 0.06554 0.00913 0.00487 -0.00281 AFIX 43 H16 2 0.585959 0.698142 0.818517 11.00000 -1.20000 AFIX 0 C31 1 0.399100 0.636752 0.339259 11.00000 0.07872 0.10782 = 0.04833 0.02384 0.01862 0.00144 AFIX 137 H31A 2 0.444969 0.690878 0.341203 11.00000 -1.50000 H31B 2 0.306657 0.637310 0.278717 11.00000 -1.50000 H31C 2 0.466636 0.596328 0.310047 11.00000 -1.50000 AFIX 0 C41 1 0.274897 0.464452 0.441149 11.00000 0.08186 0.07128 = 0.03968 -0.00090 0.00415 0.00968 AFIX 43 H41 2 0.245559 0.417870 0.485873 11.00000 -1.20000 AFIX 0 O41 4 0.285503 0.455899 0.323989 11.00000 0.12974 0.10416 = 0.03866 -0.00748 0.00680 0.02462 N51 3 0.240678 0.502652 0.749263 11.00000 0.04963 0.05092 = 0.03554 0.00410 0.00348 -0.01027 C52 1 0.131212 0.436423 0.708877 11.00000 0.06490 0.06851 = 0.05034 -0.00523 0.00386 -0.01658 AFIX 23 H52A 2 0.184221 0.385690 0.691643 11.00000 -1.20000 H52B 2 0.068150 0.452406 0.627169 11.00000 -1.20000 AFIX 0 C53 1 0.034749 0.420965 0.815816 11.00000 0.05800 0.06933 = 0.07001 -0.00120 0.01423 -0.01592 AFIX 23 H53A 2 -0.032330 0.374550 0.790018 11.00000 -1.20000 H53B 2 -0.026893 0.469744 0.825352 11.00000 -1.20000 AFIX 0 C54 1 0.128343 0.401776 0.948423 11.00000 0.06552 0.05645 = 0.06114 0.00737 0.02471 -0.00448 AFIX 23 H54A 2 0.177811 0.348334 0.943233 11.00000 -1.20000 H54B 2 0.062945 0.398191 1.017288 11.00000 -1.20000 AFIX 0 C55 1 0.246419 0.468907 0.985059 11.00000 0.06186 0.06406 = 0.04275 0.00789 0.00985 -0.00041 AFIX 23 H55A 2 0.196883 0.520368 1.004461 11.00000 -1.20000 H55B 2 0.312403 0.452285 1.064775 11.00000 -1.20000 AFIX 0 C56 1 0.338128 0.483306 0.874297 11.00000 0.05150 0.05343 = 0.04140 0.01008 0.00442 -0.00260 AFIX 23 H56A 2 0.407379 0.529142 0.897526 11.00000 -1.20000 H56B 2 0.397234 0.433925 0.862078 11.00000 -1.20000 AFIX 0 HKLF 4 REM bk2cg REM R1 = 0.0466 for 1869 Fo > 4sig(Fo) and 0.0916 for all 3000 data REM 183 parameters refined using 0 restraints END WGHT 0.0563 0.4589 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.292, deepest hole -0.178, 1-sigma level 0.036 Q1 1 0.0662 0.4939 0.7348 11.00000 0.05 0.29 Q2 1 0.2900 0.4187 0.9426 11.00000 0.05 0.28 Q3 1 0.5174 0.6470 0.3352 11.00000 0.05 0.21 Q4 1 0.3412 0.5896 0.2436 11.00000 0.05 0.16 Q5 1 0.2778 0.5284 0.9209 11.00000 0.05 0.16 Q6 1 0.2366 0.5491 0.5679 11.00000 0.05 0.16 Q7 1 0.3420 0.5306 0.6005 11.00000 0.05 0.14 Q8 1 0.1894 0.4549 0.3334 11.00000 0.05 0.13 Q9 1 0.0852 0.3820 0.7584 11.00000 0.05 0.13 Q10 1 0.2626 0.5268 0.7144 11.00000 0.05 0.12 ; _shelx_res_checksum 70982 _shelxl_version_number 2.014 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy N N1 0.35185(18) 0.62845(10) 0.68452(15) 0.0453(4) Uani d 1 N N2 0.39911(19) 0.66723(12) 0.57496(17) 0.0531(5) Uani d 1 C C3 0.3664(2) 0.61450(15) 0.4763(2) 0.0522(5) Uani d 1 C C4 0.3031(2) 0.53927(13) 0.51801(18) 0.0479(5) Uani d 1 C C5 0.2954(2) 0.55100(12) 0.65407(18) 0.0427(5) Uani d 1 C C11 0.3634(2) 0.67370(12) 0.80659(19) 0.0448(5) Uani d 1 C C12 0.2377(2) 0.68566(13) 0.8697(2) 0.0520(5) Uani d 1 H H12 0.1447 0.6644 0.8324 0.062 Uiso calc 1 C C13 0.2501(3) 0.72930(14) 0.9883(2) 0.0618(6) Uani d 1 H H13 0.1656 0.7373 1.0312 0.074 Uiso calc 1 C C14 0.3876(3) 0.76093(15) 1.0431(2) 0.0674(7) Uani d 1 H H14 0.3962 0.7897 1.1235 0.081 Uiso calc 1 C C15 0.5118(3) 0.75014(15) 0.9793(2) 0.0685(7) Uani d 1 H H15 0.6040 0.7727 1.0158 0.082 Uiso calc 1 C C16 0.5011(2) 0.70600(14) 0.8610(2) 0.0574(6) Uani d 1 H H16 0.5860 0.6981 0.8185 0.069 Uiso calc 1 C C31 0.3991(3) 0.63675(19) 0.3393(2) 0.0774(8) Uani d 1 H H31A 0.4450 0.6909 0.3412 0.116 Uiso calc 1 H H31B 0.3067 0.6373 0.2787 0.116 Uiso calc 1 H H31C 0.4666 0.5963 0.3100 0.116 Uiso calc 1 C C41 0.2749(3) 0.46445(16) 0.4411(2) 0.0646(6) Uani d 1 H H41 0.2456 0.4179 0.4859 0.078 Uiso calc 1 O O41 0.2855(2) 0.45590(13) 0.32399(16) 0.0913(6) Uani d 1 N N51 0.24068(18) 0.50265(10) 0.74926(15) 0.0456(4) Uani d 1 C C52 0.1312(3) 0.43642(16) 0.7089(2) 0.0616(6) Uani d 1 H H52A 0.1842 0.3857 0.6916 0.074 Uiso calc 1 H H52B 0.0682 0.4524 0.6272 0.074 Uiso calc 1 C C53 0.0347(3) 0.42096(16) 0.8158(2) 0.0653(6) Uani d 1 H H53A -0.0323 0.3745 0.7900 0.078 Uiso calc 1 H H53B -0.0269 0.4697 0.8254 0.078 Uiso calc 1 C C54 0.1283(3) 0.40178(14) 0.9484(2) 0.0596(6) Uani d 1 H H54A 0.1778 0.3483 0.9432 0.071 Uiso calc 1 H H54B 0.0629 0.3982 1.0173 0.071 Uiso calc 1 C C55 0.2464(2) 0.46891(15) 0.9851(2) 0.0560(6) Uani d 1 H H55A 0.1969 0.5204 1.0045 0.067 Uiso calc 1 H H55B 0.3124 0.4523 1.0648 0.067 Uiso calc 1 C C56 0.3381(2) 0.48331(13) 0.87430(19) 0.0489(5) Uani d 1 H H56A 0.4074 0.5291 0.8975 0.059 Uiso calc 1 H H56B 0.3972 0.4339 0.8621 0.059 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 0.0486(9) 0.0487(10) 0.0407(9) -0.0008(8) 0.0135(7) 0.0070(7) N2 0.0523(10) 0.0596(11) 0.0498(10) 0.0034(8) 0.0161(8) 0.0169(9) C3 0.0477(12) 0.0675(14) 0.0430(11) 0.0110(10) 0.0123(9) 0.0149(11) C4 0.0496(12) 0.0587(13) 0.0356(10) 0.0092(10) 0.0067(8) 0.0054(9) C5 0.0402(10) 0.0497(12) 0.0383(10) 0.0035(9) 0.0059(8) 0.0056(8) C11 0.0491(12) 0.0418(11) 0.0434(11) -0.0002(9) 0.0055(9) 0.0065(9) C12 0.0516(12) 0.0548(13) 0.0508(12) -0.0007(10) 0.0110(10) 0.0015(10) C13 0.0809(17) 0.0562(14) 0.0508(13) 0.0075(12) 0.0180(12) 0.0024(11) C14 0.102(2) 0.0501(14) 0.0471(13) 0.0009(13) -0.0025(13) 0.0030(10) C15 0.0754(17) 0.0559(14) 0.0676(16) -0.0100(13) -0.0150(13) 0.0043(12) C16 0.0505(13) 0.0552(14) 0.0655(14) -0.0028(10) 0.0049(10) 0.0091(11) C31 0.0787(17) 0.108(2) 0.0483(14) 0.0014(15) 0.0186(12) 0.0238(14) C41 0.0819(16) 0.0713(16) 0.0397(12) 0.0097(13) 0.0041(11) -0.0009(11) O41 0.1297(16) 0.1042(15) 0.0387(10) 0.0246(12) 0.0068(9) -0.0075(9) N51 0.0496(9) 0.0509(10) 0.0355(8) -0.0103(8) 0.0035(7) 0.0041(7) C52 0.0649(14) 0.0685(15) 0.0503(13) -0.0166(12) 0.0039(11) -0.0052(11) C53 0.0580(13) 0.0693(16) 0.0700(15) -0.0159(12) 0.0142(11) -0.0012(12) C54 0.0655(14) 0.0564(14) 0.0611(14) -0.0045(11) 0.0247(11) 0.0074(11) C55 0.0619(13) 0.0641(14) 0.0427(12) -0.0004(11) 0.0098(10) 0.0079(10) C56 0.0515(11) 0.0534(12) 0.0414(11) -0.0026(10) 0.0044(9) 0.0101(9) 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 111.91(16) C5 N1 C11 130.03(15) N2 N1 C11 118.02(16) C3 N2 N1 104.94(17) N2 C3 C4 112.29(17) N2 C3 C31 119.9(2) C4 C3 C31 127.8(2) C5 C4 C3 104.59(18) C5 C4 C41 128.1(2) C3 C4 C41 126.73(19) N1 C5 N51 120.83(16) N1 C5 C4 106.22(16) N51 C5 C4 132.91(19) C12 C11 C16 120.2(2) C12 C11 N1 120.24(18) C16 C11 N1 119.60(18) C11 C12 C13 119.8(2) C11 C12 H12 120.1 C13 C12 H12 120.1 C14 C13 C12 120.0(2) C14 C13 H13 120.0 C12 C13 H13 120.0 C15 C14 C13 120.1(2) C15 C14 H14 119.9 C13 C14 H14 119.9 C14 C15 C16 120.5(2) C14 C15 H15 119.8 C16 C15 H15 119.8 C11 C16 C15 119.4(2) C11 C16 H16 120.3 C15 C16 H16 120.3 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 O41 C41 C4 126.5(2) O41 C41 H41 116.7 C4 C41 H41 116.7 C5 N51 C52 120.08(16) C5 N51 C56 119.72(15) C52 N51 C56 112.51(16) N51 C52 C53 110.39(18) N51 C52 H52A 109.6 C53 C52 H52A 109.6 N51 C52 H52B 109.6 C53 C52 H52B 109.6 H52A C52 H52B 108.1 C52 C53 C54 111.81(19) C52 C53 H53A 109.3 C54 C53 H53A 109.3 C52 C53 H53B 109.3 C54 C53 H53B 109.3 H53A C53 H53B 107.9 C53 C54 C55 110.77(18) C53 C54 H54A 109.5 C55 C54 H54A 109.5 C53 C54 H54B 109.5 C55 C54 H54B 109.5 H54A C54 H54B 108.1 C56 C55 C54 111.16(18) C56 C55 H55A 109.4 C54 C55 H55A 109.4 C56 C55 H55B 109.4 C54 C55 H55B 109.4 H55A C55 H55B 108.0 N51 C56 C55 110.90(17) N51 C56 H56A 109.5 C55 C56 H56A 109.5 N51 C56 H56B 109.5 C55 C56 H56B 109.5 H56A C56 H56B 108.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C5 1.361(3) N1 N2 1.386(2) N1 C11 1.424(2) N2 C3 1.311(3) C3 C4 1.422(3) C3 C31 1.498(3) C4 C5 1.400(3) C4 C41 1.434(3) C5 N51 1.377(2) C11 C12 1.380(3) C11 C16 1.380(3) C12 C13 1.381(3) C12 H12 0.9300 C13 C14 1.375(3) C13 H13 0.9300 C14 C15 1.369(4) C14 H14 0.9300 C15 C16 1.383(3) C15 H15 0.9300 C16 H16 0.9300 C31 H31A 0.9600 C31 H31B 0.9600 C31 H31C 0.9600 C41 O41 1.209(3) C41 H41 0.9300 N51 C52 1.465(3) N51 C56 1.469(2) C52 C53 1.493(3) C52 H52A 0.9700 C52 H52B 0.9700 C53 C54 1.514(3) C53 H53A 0.9700 C53 H53B 0.9700 C54 C55 1.519(3) C54 H54A 0.9700 C54 H54B 0.9700 C55 C56 1.493(3) C55 H55A 0.9700 C55 H55B 0.9700 C56 H56A 0.9700 C56 H56B 0.9700 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 C15 H15 Cg1 4_676 0.93 2.97 3.848(3) 159 no C52 H52A Cg2 2_546 0.97 2.96 3.761(3) 140 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 2.2(2) C11 N1 N2 C3 -175.79(16) N1 N2 C3 C4 -2.3(2) N1 N2 C3 C31 178.66(18) N2 C3 C4 C5 1.5(2) C31 C3 C4 C5 -179.5(2) N2 C3 C4 C41 -170.3(2) C31 C3 C4 C41 8.7(3) N2 N1 C5 N51 -179.19(16) C11 N1 C5 N51 -1.5(3) N2 N1 C5 C4 -1.3(2) C11 N1 C5 C4 176.41(18) C3 C4 C5 N1 -0.1(2) C41 C4 C5 N1 171.6(2) C3 C4 C5 N51 177.5(2) C41 C4 C5 N51 -10.8(4) C5 N1 C11 C12 -53.6(3) N2 N1 C11 C12 124.00(19) C5 N1 C11 C16 126.9(2) N2 N1 C11 C16 -55.6(2) C16 C11 C12 C13 -0.7(3) N1 C11 C12 C13 179.70(19) C11 C12 C13 C14 0.2(3) C12 C13 C14 C15 0.8(3) C13 C14 C15 C16 -1.3(4) C12 C11 C16 C15 0.2(3) N1 C11 C16 C15 179.78(18) C14 C15 C16 C11 0.8(3) C5 C4 C41 O41 -178.4(2) C3 C4 C41 O41 -8.4(4) N1 C5 N51 C52 156.64(19) C4 C5 N51 C52 -20.6(3) N1 C5 N51 C56 -56.2(3) C4 C5 N51 C56 126.5(2) C5 N51 C52 C53 -152.67(19) C56 N51 C52 C53 58.0(3) N51 C52 C53 C54 -55.2(3) C52 C53 C54 C55 52.9(3) C53 C54 C55 C56 -52.5(3) C5 N51 C56 C55 152.27(18) C52 N51 C56 C55 -58.3(2) C54 C55 C56 N51 54.9(2) _cod_database_fobs_code 2021649