#------------------------------------------------------------------------------ #$Date: 2019-05-24 05:18:40 +0300 (Fri, 24 May 2019) $ #$Revision: 215469 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021646.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_2021646 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 'C17 H13 Cl N2 O2' _chemical_formula_moiety 'C17 H13 Cl N2 O2' _chemical_formula_sum 'C17 H13 Cl N2 O2' _chemical_formula_weight 312.74 _chemical_name_systematic ; 5-(2-Chlorophenoxy)-3-methyl-1-phenyl-1H-pyrazole-4-carbaldehyde ; _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 81.013(2) _cell_angle_beta 69.861(2) _cell_angle_gamma 69.990(2) _cell_formula_units_Z 4 _cell_length_a 10.3034(4) _cell_length_b 11.4856(4) _cell_length_c 14.4725(5) _cell_measurement_reflns_used 7620 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.522 _cell_measurement_theta_min 1.500 _cell_volume 1509.47(10) _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 0.0418 _diffrn_reflns_av_unetI/netI 0.0342 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 35720 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.549 _diffrn_reflns_theta_min 1.500 _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 0.261 _exptl_absorpt_correction_T_max 0.967 _exptl_absorpt_correction_T_min 0.902 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.376 _exptl_crystal_description block _exptl_crystal_F_000 648 _exptl_crystal_size_max 0.190 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.130 _refine_diff_density_max 0.200 _refine_diff_density_min -0.256 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 425 _refine_ls_number_reflns 6296 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0422 _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^)+(0.0353P)^2^+0.7109P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0893 _refine_ls_wR_factor_ref 0.1122 _reflns_number_gt 4051 _reflns_number_total 6296 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ky3177sup1.cif _cod_data_source_block II _cod_database_code 2021646 _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 0.952 _shelx_estimated_absorpt_t_max 0.967 _shelx_hkl_file ; -1 0 0 394.96 8.50 -1 0 0 346.97 8.80 -1 0 0 406.86 8.00 1 0 0 403.26 8.00 1 0 0 342.57 8.70 -2 0 0 924.41 18.90 -2 0 0 910.31 19.90 -2 0 0 908.51 21.30 -2 0 0 907.91 20.80 -2 0 0 892.61 20.10 -2 0 0 1020.90 19.00 2 0 0 892.11 19.90 2 0 0 921.31 18.90 2 0 0 920.91 20.60 2 0 0 932.91 18.90 2 0 0 767.72 20.00 2 0 0 916.51 20.80 -3 0 0 162.58 4.30 -3 0 0 173.78 4.90 -3 0 0 172.48 4.70 -3 0 0 169.78 4.40 -3 0 0 173.28 4.40 -3 0 0 173.08 4.50 3 0 0 170.68 4.80 3 0 0 172.58 4.30 3 0 0 160.68 4.40 3 0 0 170.08 4.30 3 0 0 174.28 4.30 3 0 0 171.58 4.80 -4 0 0 8.90 1.20 -4 0 0 11.30 1.20 -4 0 0 10.50 0.80 -4 0 0 11.50 1.00 -4 0 0 11.40 1.00 -4 0 0 10.70 1.00 4 0 0 10.60 0.70 4 0 0 9.00 0.90 4 0 0 12.20 1.40 4 0 0 11.10 1.10 4 0 0 11.70 1.20 4 0 0 12.10 1.20 -5 0 0 160.68 5.40 -5 0 0 170.68 5.00 -5 0 0 161.28 4.80 -5 0 0 171.08 4.90 -5 0 0 167.48 4.60 5 0 0 171.68 4.90 5 0 0 164.38 5.40 5 0 0 172.88 5.00 -6 0 0 43.40 2.70 -6 0 0 44.30 2.30 -6 0 0 40.00 1.90 6 0 0 41.40 2.20 6 0 0 40.00 2.20 6 0 0 43.20 2.60 -7 0 0 5.00 1.50 -7 0 0 7.90 1.50 -7 0 0 7.30 1.00 7 0 0 9.50 1.60 7 0 0 6.90 1.30 7 0 0 7.00 1.30 -8 0 0 0.00 1.30 -8 0 0 0.50 1.50 -8 0 0 2.90 0.90 8 0 0 2.00 1.00 8 0 0 1.10 1.50 8 0 0 1.90 1.20 -9 0 0 8.80 1.80 -9 0 0 8.40 1.10 9 0 0 7.90 2.10 9 0 0 13.20 2.10 9 0 0 11.60 1.90 -10 0 0 0.10 1.20 10 0 0 0.30 1.50 10 0 0 0.30 1.90 10 0 0 -0.90 1.30 -11 0 0 -0.70 1.70 11 0 0 0.40 1.50 11 0 0 -1.00 1.40 11 0 0 -1.00 1.00 -12 0 0 0.80 2.00 12 0 0 1.10 1.70 12 0 0 2.70 1.50 12 0 0 -1.10 2.30 12 -1 0 -1.30 1.60 12 -1 0 -2.30 2.00 12 -1 0 1.90 1.50 -12 1 0 1.90 2.10 11 -1 0 2.50 1.40 11 -1 0 -2.00 1.80 11 -1 0 2.20 1.70 -11 1 0 -0.20 2.00 10 -1 0 15.10 2.30 10 -1 0 20.50 2.50 10 -1 0 16.20 2.80 -10 1 0 23.40 3.00 9 -1 0 12.90 2.40 9 -1 0 10.80 1.90 9 -1 0 16.50 2.10 -9 1 0 17.20 2.50 -9 1 0 14.10 1.70 8 -1 0 47.50 3.60 8 -1 0 50.39 2.90 8 -1 0 51.09 3.20 -8 1 0 43.90 2.50 -8 1 0 49.00 3.30 -8 1 0 37.40 3.20 7 -1 0 9.20 1.40 7 -1 0 11.80 1.60 7 -1 0 10.10 1.90 -7 1 0 8.80 1.60 -7 1 0 6.80 1.40 -7 1 0 9.20 1.20 6 -1 0 1.90 1.00 6 -1 0 1.90 0.50 6 -1 0 0.80 1.00 6 -1 0 1.00 1.20 -6 1 0 -0.50 0.80 -6 1 0 1.70 0.80 -6 1 0 1.40 0.90 5 -1 0 0.20 0.70 5 -1 0 -0.60 0.50 5 -1 0 0.40 0.40 5 -1 0 -0.80 0.50 -5 1 0 0.60 0.60 -5 1 0 -1.20 0.60 -5 1 0 -0.80 0.80 4 -1 0 180.48 5.40 4 -1 0 185.78 5.20 4 -1 0 192.28 5.60 4 -1 0 194.08 5.10 4 -1 0 182.18 5.00 4 -1 0 184.98 5.10 -4 1 0 186.18 5.20 -4 1 0 180.68 5.10 -4 1 0 184.38 5.20 -4 1 0 188.78 5.40 -4 1 0 178.48 5.60 -4 1 0 189.68 5.10 3 -1 0 36.30 1.70 3 -1 0 34.60 1.50 3 -1 0 34.90 1.60 3 -1 0 36.90 1.60 3 -1 0 34.60 1.80 3 -1 0 37.80 1.50 -3 1 0 37.10 1.60 -3 1 0 37.80 1.80 -3 1 0 36.00 1.60 -3 1 0 36.60 1.60 -3 1 0 34.30 1.60 -3 1 0 33.20 1.60 2 -1 0 88.49 2.50 2 -1 0 86.29 2.60 2 -1 0 85.89 2.70 2 -1 0 84.19 2.50 2 -1 0 88.49 2.70 2 -1 0 86.99 2.60 -2 1 0 90.19 2.80 -2 1 0 85.49 2.60 -2 1 0 90.29 2.50 -2 1 0 88.59 2.60 -2 1 0 84.39 2.50 -2 1 0 88.19 2.50 1 -1 0 36.00 1.30 1 -1 0 34.90 1.10 1 -1 0 37.20 1.20 1 -1 0 36.60 1.30 1 -1 0 34.40 1.20 -1 1 0 35.70 1.20 -1 1 0 34.90 1.20 -1 1 0 33.90 1.20 -1 1 0 35.70 1.30 -1 1 0 36.10 1.30 -1 1 0 34.40 1.10 0 -1 0 -1.80 0.10 0 -1 0 -1.70 0.10 0 1 0 -1.70 0.10 0 1 0 -1.70 0.10 -1 -1 0 148.09 4.20 -1 -1 0 191.28 4.30 -1 -1 0 179.38 4.20 -1 -1 0 188.48 4.00 1 1 0 189.58 3.90 1 1 0 189.78 4.10 -2 -1 0 1.60 0.40 -2 -1 0 2.50 0.50 -2 -1 0 1.80 0.40 -2 -1 0 1.80 0.40 2 1 0 2.40 0.40 2 1 0 2.30 0.40 2 1 0 1.70 0.40 2 1 0 1.80 0.40 -3 -1 0 46.30 1.70 -3 -1 0 42.50 1.20 -3 -1 0 41.90 1.70 -3 -1 0 45.90 1.80 -3 -1 0 45.70 1.80 3 1 0 44.50 1.70 3 1 0 45.60 1.70 3 1 0 45.30 2.00 3 1 0 43.60 1.60 3 1 0 46.10 1.70 -4 -1 0 0.80 0.70 -4 -1 0 0.80 0.30 -4 -1 0 0.60 0.50 -4 -1 0 0.90 0.60 -4 -1 0 0.50 0.60 4 1 0 0.00 0.70 4 1 0 0.90 0.60 4 1 0 1.30 0.50 4 1 0 1.10 0.40 4 1 0 0.10 0.50 -5 -1 0 0.80 0.70 -5 -1 0 0.40 0.60 -5 -1 0 0.80 0.70 -5 -1 0 0.10 0.30 5 1 0 0.30 0.60 5 1 0 0.00 0.50 5 1 0 0.40 0.50 5 1 0 0.90 0.90 -6 -1 0 5.80 1.10 -6 -1 0 4.50 0.60 -6 -1 0 4.80 1.30 6 1 0 4.10 0.90 6 1 0 4.00 1.00 6 1 0 5.60 1.20 -7 -1 0 237.68 6.20 -7 -1 0 236.58 7.70 -7 -1 0 230.08 6.90 7 1 0 242.28 7.00 7 1 0 240.68 7.10 7 1 0 240.68 7.60 -8 -1 0 1.20 1.50 -8 -1 0 0.20 0.50 -8 -1 0 -2.10 1.10 8 1 0 1.30 1.60 8 1 0 1.20 1.10 8 1 0 1.00 0.90 -9 -1 0 2.00 1.20 -9 -1 0 2.00 1.40 9 1 0 2.20 1.10 9 1 0 2.50 1.50 9 1 0 3.00 1.40 -10 -1 0 0.80 1.70 10 1 0 -0.40 0.90 10 1 0 -0.10 1.20 10 1 0 1.70 1.90 -11 -1 0 -0.70 1.20 11 1 0 2.80 1.60 11 1 0 -1.80 1.90 11 1 0 -1.10 1.40 -12 -1 0 -1.70 2.00 12 1 0 0.10 2.20 12 1 0 -1.80 1.30 12 1 0 2.70 1.50 11 -2 0 3.30 1.60 11 -2 0 0.60 1.60 -11 2 0 2.90 2.10 10 -2 0 -2.00 1.30 10 -2 0 1.60 1.80 10 -2 0 -0.30 1.10 -10 2 0 -1.60 1.20 9 -2 0 17.70 2.40 9 -2 0 14.60 2.30 9 -2 0 16.60 2.30 -9 2 0 17.60 2.40 -9 2 0 13.40 1.80 8 -2 0 6.00 1.40 8 -2 0 3.90 1.60 8 -2 0 7.30 1.70 -8 2 0 9.40 2.00 -8 2 0 6.20 1.30 7 -2 0 7.80 1.80 7 -2 0 8.00 1.50 7 -2 0 7.60 1.50 -7 2 0 8.10 1.60 -7 2 0 9.80 1.80 -7 2 0 9.50 1.50 6 -2 0 4.60 1.20 6 -2 0 4.10 0.80 6 -2 0 1.30 1.20 6 -2 0 3.40 1.00 -6 2 0 3.10 1.20 -6 2 0 2.40 1.30 -6 2 0 3.80 1.10 5 -2 0 13.80 1.30 5 -2 0 14.30 1.80 5 -2 0 15.70 1.70 5 -2 0 16.40 1.30 -5 2 0 15.40 1.60 -5 2 0 13.20 1.60 -5 2 0 15.00 1.70 4 -2 0 40.20 2.20 4 -2 0 38.20 1.90 4 -2 0 43.60 1.90 4 -2 0 40.40 2.10 -4 2 0 38.70 2.20 -4 2 0 41.00 2.10 -4 2 0 42.60 2.00 -4 2 0 40.90 2.00 -4 2 0 39.90 2.30 -4 2 0 42.90 2.20 3 -2 0 99.49 3.20 3 -2 0 95.19 3.10 3 -2 0 101.09 3.20 3 -2 0 95.99 3.30 3 -2 0 97.29 3.10 3 -2 0 96.09 3.20 -3 2 0 99.39 3.20 -3 2 0 97.29 3.00 -3 2 0 94.59 3.50 -3 2 0 94.49 3.10 -3 2 0 98.99 3.20 -3 2 0 93.69 3.30 2 -2 0 280.37 7.10 2 -2 0 273.57 6.50 2 -2 0 269.47 6.50 2 -2 0 288.27 7.20 2 -2 0 276.57 6.90 -2 2 0 280.77 6.60 -2 2 0 279.57 6.90 -2 2 0 274.97 7.30 -2 2 0 283.57 6.90 -2 2 0 269.17 7.20 -2 2 0 280.57 6.50 1 -2 0 26.30 1.10 1 -2 0 29.60 1.30 1 -2 0 30.10 1.30 1 -2 0 27.20 0.90 1 -2 0 29.00 1.20 1 -2 0 26.80 1.30 -1 2 0 27.70 1.20 -1 2 0 32.60 1.30 -1 2 0 28.20 1.30 -1 2 0 27.30 1.10 -1 2 0 28.80 1.10 -1 2 0 27.90 1.30 0 -2 0 1147.79 26.70 0 -2 0 1182.98 24.10 0 -2 0 1170.28 25.40 0 -2 0 1183.18 24.00 0 -2 0 1142.19 26.40 0 -2 0 1168.68 25.10 0 2 0 1188.28 24.30 0 2 0 1149.48 26.70 0 2 0 1171.68 23.80 0 2 0 1189.78 24.10 0 2 0 1183.28 25.40 0 2 0 1174.48 24.00 0 2 0 1144.19 24.90 -1 -2 0 526.15 11.60 -1 -2 0 534.35 11.20 -1 -2 0 540.45 12.40 -1 -2 0 523.95 11.10 1 2 0 526.65 11.30 1 2 0 522.45 12.40 1 2 0 528.05 11.20 1 2 0 535.95 11.60 1 2 0 535.55 11.80 1 2 0 532.25 11.10 -2 -2 0 29.10 1.10 -2 -2 0 25.00 1.00 -2 -2 0 29.40 1.00 -2 -2 0 29.10 1.20 -2 -2 0 27.60 1.20 2 2 0 26.80 1.10 2 2 0 26.60 1.00 2 2 0 29.20 1.00 2 2 0 28.00 1.10 2 2 0 29.40 1.00 2 2 0 27.00 1.30 -3 -2 0 122.49 3.30 -3 -2 0 119.69 3.50 -3 -2 0 122.49 3.10 -3 -2 0 125.79 3.70 -3 -2 0 128.29 3.40 3 2 0 124.29 3.40 3 2 0 130.39 3.50 3 2 0 122.59 3.70 3 2 0 123.49 3.30 3 2 0 125.79 3.50 -4 -2 0 314.37 7.50 -4 -2 0 310.37 8.10 -4 -2 0 311.27 7.50 -4 -2 0 310.97 8.00 4 2 0 322.37 8.20 4 2 0 319.07 8.00 4 2 0 299.17 7.40 4 2 0 316.07 7.40 -5 -2 0 87.39 3.00 -5 -2 0 88.59 3.40 -5 -2 0 86.19 2.20 -5 -2 0 88.79 3.10 5 2 0 88.89 3.10 5 2 0 91.09 3.10 5 2 0 83.09 3.50 5 2 0 84.59 3.20 -6 -2 0 0.90 0.70 -6 -2 0 0.40 0.60 -6 -2 0 0.40 0.30 -6 -2 0 -0.80 0.90 6 2 0 -0.40 0.70 6 2 0 0.10 0.50 6 2 0 -0.80 0.70 -7 -2 0 6.50 0.50 -7 -2 0 4.90 1.10 -7 -2 0 6.80 1.30 7 2 0 5.40 1.10 7 2 0 7.20 1.20 7 2 0 7.10 1.40 -8 -2 0 11.30 1.80 -8 -2 0 8.90 1.90 8 2 0 9.30 1.50 8 2 0 10.70 1.60 8 2 0 11.40 2.10 -9 -2 0 4.10 1.80 -9 -2 0 3.90 1.30 9 2 0 0.70 1.70 9 2 0 3.40 1.30 9 2 0 1.40 1.10 -10 -2 0 3.20 1.40 10 2 0 4.00 1.60 10 2 0 4.30 1.50 10 2 0 4.10 1.60 -11 -2 0 4.90 2.00 11 2 0 0.60 2.00 11 2 0 1.70 1.40 11 2 0 -0.50 1.30 -12 -2 0 -1.90 1.70 12 2 0 -0.20 2.20 12 2 0 0.70 1.20 12 2 0 0.00 1.40 11 -3 0 -1.10 1.70 11 -3 0 2.60 2.00 -11 3 0 -0.60 1.40 10 -3 0 2.80 1.90 10 -3 0 1.10 1.70 -10 3 0 6.20 2.00 9 -3 0 -0.70 1.00 9 -3 0 -0.80 1.00 -9 3 0 -0.70 1.10 -9 3 0 -3.90 1.50 8 -3 0 20.60 2.50 8 -3 0 26.20 2.70 -8 3 0 25.40 2.50 -8 3 0 26.80 2.60 7 -3 0 -0.60 0.90 7 -3 0 0.20 0.90 -7 3 0 0.40 1.10 -7 3 0 -1.20 0.90 6 -3 0 4.80 1.20 6 -3 0 4.80 1.40 -6 3 0 6.00 1.40 -6 3 0 5.40 1.20 -6 3 0 5.60 1.40 5 -3 0 13.00 1.40 5 -3 0 12.20 1.50 -5 3 0 9.20 1.40 -5 3 0 10.40 1.50 -5 3 0 11.50 1.50 4 -3 0 3.50 0.70 4 -3 0 3.30 0.80 4 -3 0 3.20 0.80 -4 3 0 3.20 1.00 -4 3 0 2.60 1.10 -4 3 0 1.90 0.80 3 -3 0 -0.20 0.70 3 -3 0 0.10 0.70 3 -3 0 -0.30 0.40 3 -3 0 0.60 0.70 3 -3 0 -0.90 0.50 -3 3 0 -0.60 0.80 -3 3 0 -0.10 0.60 -3 3 0 0.10 0.70 -3 3 0 -0.30 0.60 -3 3 0 0.80 0.50 -3 3 0 -0.20 0.70 2 -3 0 296.37 7.20 2 -3 0 304.27 6.90 2 -3 0 303.87 7.80 2 -3 0 307.17 8.00 2 -3 0 293.87 7.60 2 -3 0 298.47 7.20 -2 3 0 298.57 7.10 -2 3 0 299.97 7.90 -2 3 0 306.37 7.60 -2 3 0 301.17 8.10 -2 3 0 297.27 7.50 -2 3 0 302.77 7.40 1 -3 0 121.89 3.00 1 -3 0 119.49 3.60 1 -3 0 122.99 3.30 1 -3 0 127.99 3.80 1 -3 0 120.89 2.90 1 -3 0 127.79 3.40 1 -3 0 122.69 3.50 -1 3 0 124.19 3.90 -1 3 0 120.59 3.30 -1 3 0 127.09 3.60 -1 3 0 122.29 3.50 -1 3 0 121.39 3.30 -1 3 0 121.49 3.50 -1 3 0 124.69 3.00 0 -3 0 0.00 0.40 0 -3 0 0.10 0.30 0 -3 0 0.40 0.40 0 -3 0 0.40 0.30 0 -3 0 1.20 0.50 0 -3 0 -0.20 0.50 0 3 0 -0.30 0.30 0 3 0 -0.10 0.30 0 3 0 0.50 0.40 0 3 0 0.20 0.30 0 3 0 -0.50 0.40 0 3 0 0.30 0.50 0 3 0 -0.10 0.20 -1 -3 0 494.95 11.70 -1 -3 0 549.54 12.70 -1 -3 0 498.35 11.30 -1 -3 0 534.85 11.50 1 3 0 523.45 11.70 1 3 0 520.35 11.50 1 3 0 543.05 11.30 1 3 0 523.55 12.70 1 3 0 583.94 11.60 -2 -3 0 1.80 0.40 -2 -3 0 2.00 0.60 -2 -3 0 -0.40 0.60 -2 -3 0 1.30 0.40 2 3 0 0.70 0.40 -3 -3 0 390.06 9.40 -3 -3 0 388.96 8.90 -3 -3 0 381.16 8.70 -3 -3 0 378.76 9.20 -3 -3 0 387.36 9.20 3 3 0 385.96 8.80 3 3 0 388.96 9.30 3 3 0 385.86 9.40 3 3 0 399.66 8.70 3 3 0 389.26 9.10 3 3 0 391.56 9.20 -4 -3 0 394.86 9.20 -4 -3 0 389.86 9.20 -4 -3 0 391.46 9.70 -4 -3 0 388.96 9.70 -4 -3 0 396.36 9.00 4 3 0 386.16 9.10 4 3 0 391.16 9.80 4 3 0 390.66 9.00 4 3 0 394.96 9.50 4 3 0 389.36 9.50 -5 -3 0 26.20 0.90 -5 -3 0 23.70 1.50 -5 -3 0 22.90 1.50 -5 -3 0 24.00 1.70 5 3 0 26.30 2.00 5 3 0 24.10 1.50 5 3 0 27.30 1.50 -6 -3 0 0.50 0.90 -6 -3 0 0.00 0.80 -6 -3 0 1.10 0.80 6 3 0 0.10 0.70 6 3 0 1.10 1.10 6 3 0 0.50 0.80 -7 -3 0 26.00 2.10 -7 -3 0 26.60 2.10 7 3 0 21.60 2.00 7 3 0 26.10 2.30 7 3 0 25.90 2.10 -8 -3 0 44.80 3.20 -8 -3 0 39.60 2.50 8 3 0 45.60 2.80 8 3 0 37.30 3.00 8 3 0 38.90 2.50 -9 -3 0 27.70 3.10 -9 -3 0 24.20 2.60 9 3 0 26.40 2.80 9 3 0 28.00 2.50 9 3 0 23.50 2.20 -10 -3 0 -0.40 1.50 10 3 0 0.70 1.20 10 3 0 0.80 1.50 10 3 0 0.20 1.00 -11 -3 0 -2.20 1.40 11 3 0 -0.10 1.00 11 3 0 0.60 2.20 11 3 0 0.30 1.30 -12 -3 0 0.90 1.40 12 3 0 2.20 1.50 12 3 0 1.40 1.30 12 3 0 1.20 2.40 10 -4 0 -0.40 1.80 10 -4 0 -0.60 1.20 -10 4 0 -3.60 1.60 9 -4 0 3.60 1.50 9 -4 0 0.20 1.70 -9 4 0 0.90 1.50 -9 4 0 2.40 1.60 8 -4 0 0.50 1.10 8 -4 0 1.20 1.20 -8 4 0 1.30 1.80 -8 4 0 1.00 1.40 7 -4 0 2.10 1.50 7 -4 0 3.30 1.50 -7 4 0 2.70 1.80 -7 4 0 2.70 1.30 6 -4 0 14.70 1.80 6 -4 0 16.60 1.80 -6 4 0 12.20 1.80 -6 4 0 15.90 2.20 5 -4 0 1.50 0.90 5 -4 0 1.60 1.10 -5 4 0 2.90 1.10 -5 4 0 2.10 1.20 4 -4 0 34.50 2.20 4 -4 0 35.20 1.60 4 -4 0 35.70 2.10 -4 4 0 35.50 2.40 -4 4 0 34.40 2.30 -4 4 0 33.50 2.50 3 -4 0 15.30 1.00 3 -4 0 17.30 1.40 3 -4 0 13.00 1.30 -3 4 0 15.30 1.50 -3 4 0 14.20 1.40 -3 4 0 16.30 1.50 -3 4 0 16.00 1.60 2 -4 0 19.10 1.40 2 -4 0 17.50 1.30 2 -4 0 17.40 0.90 2 -4 0 18.30 1.50 2 -4 0 17.30 1.30 2 -4 0 20.60 1.60 -2 4 0 19.20 1.30 -2 4 0 17.90 1.20 -2 4 0 17.90 1.40 -2 4 0 20.10 1.80 1 -4 0 32.90 1.20 1 -4 0 32.70 1.80 1 -4 0 33.90 1.60 1 -4 0 30.20 1.50 1 -4 0 31.30 1.20 1 -4 0 34.00 1.70 1 -4 0 33.60 1.50 -1 4 0 31.60 1.50 -1 4 0 33.20 1.70 -1 4 0 31.80 1.20 -1 4 0 33.40 1.80 -1 4 0 32.40 1.90 -1 4 0 30.90 1.60 0 -4 0 125.49 3.50 0 -4 0 124.29 3.20 0 -4 0 124.09 4.00 0 -4 0 123.79 3.40 0 -4 0 129.49 3.60 0 -4 0 124.09 3.70 0 4 0 120.89 3.60 0 4 0 123.79 3.40 0 4 0 123.49 4.10 0 4 0 121.89 3.40 0 4 0 120.49 3.60 0 4 0 125.99 3.20 0 4 0 121.49 3.00 -1 -4 0 0.40 0.40 -1 -4 0 0.60 0.40 -1 -4 0 0.00 0.50 -1 -4 0 0.50 0.40 1 4 0 0.30 0.60 1 4 0 -0.10 0.40 1 4 0 0.00 0.40 1 4 0 0.80 0.40 1 4 0 0.00 0.40 1 4 0 -0.10 0.40 -2 -4 0 9.70 0.80 -2 -4 0 9.30 0.90 -2 -4 0 11.30 0.40 -2 -4 0 9.60 1.00 -2 -4 0 9.20 1.00 2 4 0 8.30 0.90 2 4 0 10.40 1.10 2 4 0 10.60 0.90 2 4 0 10.60 0.90 2 4 0 9.60 0.80 2 4 0 9.00 0.80 -3 -4 0 6.40 0.80 -3 -4 0 6.20 0.80 -3 -4 0 6.80 0.80 -3 -4 0 7.00 1.00 -3 -4 0 5.80 0.60 3 4 0 4.60 0.80 3 4 0 6.90 0.80 3 4 0 6.60 0.50 3 4 0 7.00 0.90 3 4 0 6.00 0.80 3 4 0 6.50 0.80 -4 -4 0 19.10 1.30 -4 -4 0 18.60 1.10 -4 -4 0 18.10 1.30 -4 -4 0 17.40 1.20 -4 -4 0 16.60 1.20 -4 -4 0 19.50 1.00 4 4 0 19.70 1.40 4 4 0 18.80 1.10 4 4 0 19.10 1.00 4 4 0 20.30 1.50 4 4 0 18.20 1.30 -5 -4 0 273.57 7.00 -5 -4 0 278.57 6.60 -5 -4 0 287.57 7.30 -5 -4 0 274.87 6.80 -5 -4 0 280.37 7.40 5 4 0 270.57 7.10 5 4 0 275.07 7.80 5 4 0 277.07 7.20 -6 -4 0 16.10 1.60 -6 -4 0 17.00 0.70 -6 -4 0 14.70 1.40 -6 -4 0 18.00 1.80 6 4 0 15.90 1.60 6 4 0 14.90 1.30 6 4 0 20.40 2.20 -7 -4 0 6.50 1.10 -7 -4 0 8.70 1.30 7 4 0 7.50 1.60 7 4 0 6.40 1.20 7 4 0 6.00 1.20 -8 -4 0 22.40 2.60 -8 -4 0 25.10 2.10 8 4 0 22.30 2.20 8 4 0 23.30 2.00 8 4 0 25.20 3.00 -9 -4 0 3.60 1.60 -9 -4 0 7.00 1.80 9 4 0 9.70 1.80 9 4 0 6.20 1.80 9 4 0 5.50 1.40 -10 -4 0 0.50 1.10 10 4 0 2.00 1.40 10 4 0 0.10 1.20 10 4 0 1.30 1.50 -11 -4 0 3.80 1.60 11 4 0 2.30 1.50 11 4 0 2.00 2.20 11 4 0 6.20 1.60 -12 -4 0 6.70 1.90 12 4 0 3.20 2.60 12 4 0 10.40 2.10 12 4 0 12.80 2.20 10 -5 0 -1.70 1.70 10 -5 0 -3.10 1.60 -10 5 0 1.30 2.20 9 -5 0 -0.90 1.50 9 -5 0 -1.60 1.60 -9 5 0 -2.00 1.30 -9 5 0 3.60 1.80 8 -5 0 -1.40 1.10 8 -5 0 0.40 1.50 -8 5 0 -0.80 1.30 -8 5 0 -0.80 1.20 7 -5 0 18.20 1.60 7 -5 0 11.80 2.20 7 -5 0 17.00 2.20 -7 5 0 15.00 2.30 -7 5 0 17.20 2.40 6 -5 0 12.70 1.40 6 -5 0 13.00 2.00 6 -5 0 12.50 2.10 -6 5 0 15.30 2.40 -6 5 0 10.60 1.90 5 -5 0 41.30 1.90 5 -5 0 45.00 2.80 5 -5 0 43.80 2.70 -5 5 0 45.80 3.30 -5 5 0 44.50 2.90 4 -5 0 102.19 3.00 4 -5 0 94.59 4.00 4 -5 0 99.59 3.80 -4 5 0 94.29 3.90 -4 5 0 94.79 4.40 3 -5 0 126.89 4.50 3 -5 0 116.99 3.30 3 -5 0 116.79 4.00 -3 5 0 118.19 4.70 -3 5 0 111.89 4.10 2 -5 0 6.70 1.20 2 -5 0 7.90 0.80 2 -5 0 6.30 1.00 2 -5 0 6.30 1.00 2 -5 0 6.70 0.80 -2 5 0 5.80 1.10 -2 5 0 7.30 1.20 1 -5 0 47.50 2.00 1 -5 0 47.70 2.20 1 -5 0 46.60 1.60 1 -5 0 46.30 2.00 1 -5 0 44.70 2.10 1 -5 0 45.90 1.50 -1 5 0 44.50 2.50 -1 5 0 47.10 2.00 -1 5 0 44.60 2.20 -1 5 0 44.30 1.60 0 -5 0 6.90 0.80 0 -5 0 5.80 1.00 0 -5 0 6.70 1.00 0 -5 0 7.60 0.90 0 5 0 6.90 1.00 0 5 0 6.80 1.00 0 5 0 5.50 0.60 0 5 0 8.50 1.00 0 5 0 7.20 0.70 0 5 0 7.00 1.10 0 5 0 6.10 0.80 -1 -5 0 271.87 6.80 -1 -5 0 270.67 6.50 -1 -5 0 275.57 6.60 -1 -5 0 263.87 6.30 -1 -5 0 273.87 7.50 1 5 0 265.87 7.60 1 5 0 267.97 7.00 1 5 0 272.97 6.50 1 5 0 263.57 6.60 1 5 0 271.37 6.50 1 5 0 260.77 6.80 -2 -5 0 160.08 4.40 -2 -5 0 159.48 4.40 -2 -5 0 166.88 4.60 -2 -5 0 159.68 4.90 2 5 0 162.48 4.40 2 5 0 163.78 4.30 2 5 0 159.18 4.60 2 5 0 153.28 4.90 2 5 0 162.48 4.30 2 5 0 158.88 4.70 -3 -5 0 116.69 3.70 -3 -5 0 109.99 3.30 -3 -5 0 115.09 3.60 -3 -5 0 113.79 3.60 -3 -5 0 114.49 2.80 3 5 0 110.49 3.50 3 5 0 108.69 3.60 3 5 0 105.79 3.20 3 5 0 104.69 3.40 3 5 0 112.19 3.70 3 5 0 107.99 3.40 -4 -5 0 63.09 2.10 -4 -5 0 66.09 2.10 -4 -5 0 62.19 2.60 -4 -5 0 61.09 2.40 -4 -5 0 64.79 2.50 4 5 0 62.19 2.40 4 5 0 63.29 2.90 4 5 0 61.29 1.90 4 5 0 69.19 2.70 -5 -5 0 5.90 0.90 -5 -5 0 6.40 0.90 -5 -5 0 6.50 0.80 -5 -5 0 7.50 0.80 -5 -5 0 7.40 1.30 5 5 0 6.10 0.70 5 5 0 5.90 1.00 5 5 0 6.60 1.30 -6 -5 0 25.20 1.80 -6 -5 0 23.60 1.70 -6 -5 0 21.70 1.80 -6 -5 0 23.60 1.40 -6 -5 0 21.30 1.10 6 5 0 22.90 2.00 6 5 0 24.20 1.50 6 5 0 22.40 1.70 -7 -5 0 11.50 1.50 -7 -5 0 13.90 0.50 -7 -5 0 10.70 1.60 -7 -5 0 16.40 1.30 7 5 0 10.90 1.60 7 5 0 14.00 1.80 -8 -5 0 3.50 0.90 -8 -5 0 3.90 1.30 -8 -5 0 3.60 1.10 8 5 0 3.50 1.10 8 5 0 3.80 1.00 8 5 0 3.30 1.80 -9 -5 0 48.20 2.80 -9 -5 0 47.60 3.40 -9 -5 0 48.00 3.00 9 5 0 52.09 3.20 9 5 0 54.19 3.70 9 5 0 49.10 2.90 -10 -5 0 0.70 1.50 -10 -5 0 2.50 1.20 10 5 0 3.40 1.50 10 5 0 0.60 1.40 10 5 0 2.60 1.50 -11 -5 0 0.00 1.60 -11 -5 0 0.50 1.10 11 5 0 0.70 1.40 11 5 0 -1.30 1.20 11 5 0 -0.20 1.60 -12 -5 0 0.30 1.40 -12 -5 0 -1.50 1.00 12 5 0 1.20 1.60 12 5 0 -4.30 2.00 12 5 0 0.10 1.40 9 -6 0 0.90 2.00 9 -6 0 0.00 1.40 -9 6 0 -0.60 1.70 -9 6 0 1.20 2.20 8 -6 0 -0.80 1.60 8 -6 0 -1.60 1.60 -8 6 0 1.40 1.60 -8 6 0 -1.70 1.50 7 -6 0 1.80 1.70 7 -6 0 -0.20 1.60 -7 6 0 4.60 2.10 -7 6 0 0.80 1.10 6 -6 0 1.80 1.20 6 -6 0 2.20 0.80 6 -6 0 4.20 1.40 -6 6 0 2.30 1.40 -6 6 0 5.00 1.80 5 -6 0 -1.80 1.20 5 -6 0 -0.20 0.60 5 -6 0 0.10 1.30 -5 6 0 0.60 1.40 -5 6 0 1.90 1.70 4 -6 0 126.49 4.80 4 -6 0 129.79 5.20 4 -6 0 124.39 3.70 -4 6 0 129.79 4.90 -4 6 0 127.99 5.40 3 -6 0 5.30 0.70 3 -6 0 5.90 1.20 3 -6 0 6.20 0.80 3 -6 0 5.40 1.40 -3 6 0 8.20 1.70 -3 6 0 5.30 1.50 2 -6 0 0.40 0.70 2 -6 0 0.40 0.50 2 -6 0 0.50 0.50 2 -6 0 -0.50 0.70 -2 6 0 -0.20 0.80 -2 6 0 0.30 0.80 1 -6 0 5.60 1.00 1 -6 0 5.40 0.90 1 -6 0 5.60 1.00 1 -6 0 6.20 0.70 -1 6 0 7.20 1.40 -1 6 0 6.90 0.80 -1 6 0 6.70 1.00 -1 6 0 5.00 1.10 0 -6 0 6.10 0.70 0 -6 0 5.40 1.00 0 -6 0 5.00 0.70 0 6 0 5.30 0.80 0 6 0 5.30 0.70 0 6 0 5.30 0.70 0 6 0 6.40 1.10 0 6 0 4.50 1.10 -1 -6 0 19.70 1.50 -1 -6 0 20.30 1.40 -1 -6 0 19.80 1.00 -1 -6 0 21.20 1.30 1 6 0 20.40 1.80 1 6 0 21.20 1.20 1 6 0 19.30 1.80 1 6 0 21.70 1.20 1 6 0 21.90 1.40 -2 -6 0 306.17 7.70 -2 -6 0 313.57 7.80 -2 -6 0 317.47 8.60 -2 -6 0 296.67 7.50 2 6 0 302.47 7.60 2 6 0 305.17 8.70 2 6 0 309.57 7.80 2 6 0 309.77 7.60 -3 -6 0 54.09 2.50 -3 -6 0 55.99 2.50 -3 -6 0 53.59 2.40 -3 -6 0 58.39 2.60 3 6 0 52.79 2.40 3 6 0 54.09 2.30 3 6 0 54.49 2.60 3 6 0 58.09 2.60 -4 -6 0 350.96 8.20 -4 -6 0 349.96 7.80 -4 -6 0 353.16 9.20 -4 -6 0 351.36 8.50 -4 -6 0 356.36 8.80 4 6 0 339.17 8.70 4 6 0 342.27 9.30 4 6 0 345.37 8.10 4 6 0 344.77 8.60 4 6 0 349.37 9.20 -5 -6 0 12.30 1.00 -5 -6 0 13.40 1.20 -5 -6 0 14.90 1.40 -5 -6 0 17.30 1.50 -5 -6 0 14.10 1.20 5 6 0 13.10 1.70 5 6 0 14.90 0.90 5 6 0 14.90 1.30 5 6 0 12.70 1.30 -6 -6 0 1.70 0.50 -6 -6 0 1.90 0.70 -6 -6 0 2.70 1.00 -6 -6 0 0.50 0.70 6 6 0 1.60 0.50 6 6 0 2.00 1.00 6 6 0 1.30 0.90 -7 -6 0 0.80 0.70 -7 -6 0 1.10 0.40 -7 -6 0 1.30 0.90 -7 -6 0 -1.80 0.90 7 6 0 0.40 1.00 7 6 0 0.70 1.10 -8 -6 0 18.80 1.90 -8 -6 0 18.30 2.10 -8 -6 0 22.50 1.70 8 6 0 19.90 1.90 8 6 0 19.40 2.60 -9 -6 0 2.50 1.50 -9 -6 0 -1.80 0.80 9 6 0 -1.40 1.00 9 6 0 -0.40 1.20 9 6 0 1.20 1.20 -10 -6 0 1.10 1.10 -10 -6 0 1.70 1.10 10 6 0 2.20 1.40 10 6 0 3.30 1.30 10 6 0 3.70 1.70 -11 -6 0 -1.30 0.90 -11 -6 0 0.00 1.70 11 6 0 1.20 1.40 11 6 0 -2.10 2.00 11 6 0 1.90 1.60 -12 -6 0 3.50 1.60 -12 -6 0 0.40 1.20 12 6 0 -1.00 1.30 12 6 0 1.20 1.20 12 6 0 -2.30 2.10 9 -7 0 -2.20 1.20 9 -7 0 -2.10 1.90 -9 7 0 -1.10 2.20 8 -7 0 -0.90 1.70 8 -7 0 -1.80 1.90 -8 7 0 1.20 2.10 -8 7 0 -1.80 1.70 7 -7 0 16.40 2.40 7 -7 0 21.10 2.90 -7 7 0 14.50 2.40 -7 7 0 18.50 3.00 6 -7 0 50.19 3.30 6 -7 0 52.59 3.60 -6 7 0 53.09 4.30 -6 7 0 46.20 3.50 5 -7 0 7.50 1.00 5 -7 0 7.70 1.90 5 -7 0 8.00 1.20 5 -7 0 6.00 1.80 -5 7 0 5.00 1.90 -5 7 0 9.70 1.90 4 -7 0 94.89 4.50 4 -7 0 77.69 2.80 4 -7 0 84.19 2.80 4 -7 0 76.49 3.70 -4 7 0 77.59 4.40 -4 7 0 87.19 4.10 3 -7 0 18.30 1.30 3 -7 0 20.30 1.30 3 -7 0 17.10 2.10 3 -7 0 19.20 2.10 -3 7 0 22.50 2.90 -3 7 0 17.80 2.00 2 -7 0 17.70 1.70 2 -7 0 19.30 1.30 2 -7 0 15.50 1.80 2 -7 0 20.40 1.10 -2 7 0 18.80 2.20 -2 7 0 16.30 1.90 1 -7 0 0.30 0.60 1 -7 0 -0.10 0.50 1 -7 0 -0.10 1.00 1 -7 0 -0.30 1.00 -1 7 0 1.00 1.20 -1 7 0 0.60 0.70 -1 7 0 0.20 0.80 -1 7 0 0.10 0.40 0 -7 0 3.30 0.70 0 -7 0 4.10 0.80 0 7 0 4.80 1.10 0 7 0 4.90 1.20 0 7 0 5.60 0.80 0 7 0 5.50 0.90 -1 -7 0 0.80 0.70 -1 -7 0 0.90 0.40 -1 -7 0 1.50 0.70 -1 -7 0 1.40 0.80 1 7 0 0.60 0.60 1 7 0 1.30 0.60 1 7 0 2.00 0.90 1 7 0 0.90 0.80 1 7 0 0.60 0.50 -2 -7 0 3.60 0.90 -2 -7 0 4.00 0.90 -2 -7 0 4.20 1.00 2 7 0 3.60 1.00 2 7 0 3.90 1.00 2 7 0 4.00 1.20 -3 -7 0 59.49 2.00 -3 -7 0 58.39 2.70 -3 -7 0 55.19 2.60 -3 -7 0 61.09 2.90 3 7 0 59.19 2.90 3 7 0 56.69 2.80 3 7 0 52.89 2.90 3 7 0 56.99 2.60 -4 -7 0 -0.50 0.60 -4 -7 0 -0.40 0.60 -4 -7 0 0.70 0.60 -4 -7 0 0.50 0.40 4 7 0 1.00 0.70 4 7 0 -0.60 0.90 4 7 0 -1.20 0.50 4 7 0 1.10 0.90 -5 -7 0 3.20 0.60 -5 -7 0 3.10 0.80 -5 -7 0 2.80 0.90 5 7 0 2.30 0.80 5 7 0 1.90 1.00 5 7 0 3.10 0.40 5 7 0 2.90 1.30 5 7 0 1.90 0.80 -6 -7 0 14.80 1.50 -6 -7 0 13.30 1.30 -6 -7 0 14.40 1.10 6 7 0 16.80 1.90 6 7 0 14.20 1.60 6 7 0 14.60 1.70 6 7 0 15.00 1.00 -7 -7 0 0.80 0.80 -7 -7 0 2.80 0.90 -7 -7 0 2.50 0.60 7 7 0 2.00 0.60 7 7 0 1.60 1.10 7 7 0 3.20 1.10 -8 -7 0 9.00 1.70 -8 -7 0 11.40 1.40 8 7 0 9.40 1.70 8 7 0 12.20 2.00 -9 -7 0 -1.20 0.80 -9 -7 0 0.10 0.80 9 7 0 1.40 1.00 9 7 0 -2.60 1.70 -10 -7 0 25.70 2.50 -10 -7 0 21.70 2.00 10 7 0 19.60 3.20 10 7 0 27.80 2.80 10 7 0 23.50 2.30 -11 -7 0 2.80 1.70 -11 -7 0 4.50 1.30 11 7 0 2.10 1.60 11 7 0 5.90 1.60 11 7 0 7.00 2.60 -12 -7 0 0.00 1.10 -12 -7 0 2.70 1.50 12 7 0 3.50 1.40 12 7 0 -0.10 1.70 8 -8 0 1.50 1.90 8 -8 0 1.80 2.10 -8 8 0 -5.20 1.70 -8 8 0 -0.40 2.20 7 -8 0 1.10 1.50 7 -8 0 1.20 1.80 -7 8 0 -0.70 2.10 -7 8 0 1.80 2.00 6 -8 0 4.20 1.60 6 -8 0 5.70 1.60 -6 8 0 5.50 2.20 -6 8 0 8.70 2.10 5 -8 0 5.70 1.60 5 -8 0 4.10 1.80 -5 8 0 3.70 1.70 -5 8 0 4.90 2.00 4 -8 0 2.20 1.60 4 -8 0 5.20 1.40 4 -8 0 2.60 0.80 4 -8 0 2.50 0.80 -4 8 0 0.90 1.20 -4 8 0 3.20 1.50 3 -8 0 0.20 0.60 3 -8 0 0.80 1.00 3 -8 0 0.10 0.50 3 -8 0 -0.40 1.30 -3 8 0 0.00 1.50 -3 8 0 -0.90 1.00 2 -8 0 5.00 1.60 2 -8 0 6.60 1.60 2 -8 0 5.70 0.90 -2 8 0 7.30 1.60 -2 8 0 2.80 1.70 1 -8 0 27.90 2.00 1 -8 0 27.20 1.60 1 -8 0 26.60 1.80 -1 8 0 26.80 3.00 -1 8 0 31.10 1.50 -1 8 0 28.50 2.20 -1 8 0 24.90 2.20 0 -8 0 37.50 1.80 0 -8 0 36.40 2.50 0 -8 0 38.40 1.90 0 8 0 33.50 2.40 0 8 0 36.60 2.30 0 8 0 35.70 2.80 0 8 0 38.90 1.70 -1 -8 0 17.10 1.50 -1 -8 0 18.30 1.10 -1 -8 0 14.60 1.80 1 8 0 15.80 2.10 1 8 0 18.60 1.80 1 8 0 17.80 1.70 1 8 0 16.60 1.30 -2 -8 0 20.50 1.70 -2 -8 0 22.30 1.70 -2 -8 0 19.20 0.50 2 8 0 23.40 2.10 2 8 0 20.40 2.10 2 8 0 22.90 1.70 2 8 0 20.50 1.40 -3 -8 0 -0.50 0.90 -3 -8 0 -0.90 0.90 3 8 0 -0.40 0.70 3 8 0 0.40 1.00 3 8 0 0.30 1.10 3 8 0 1.10 0.80 -4 -8 0 8.70 0.80 -4 -8 0 6.10 1.30 4 8 0 6.60 1.40 4 8 0 4.50 1.30 4 8 0 7.60 1.50 4 8 0 5.90 1.40 -5 -8 0 4.60 1.10 -5 -8 0 6.40 0.70 -5 -8 0 4.70 0.80 5 8 0 5.60 1.10 5 8 0 4.40 1.20 5 8 0 5.90 1.20 5 8 0 7.10 1.30 -6 -8 0 7.60 1.50 -6 -8 0 8.80 1.00 6 8 0 8.20 1.40 6 8 0 7.30 1.60 6 8 0 9.80 1.80 -7 -8 0 25.40 1.60 -7 -8 0 23.80 2.30 -7 -8 0 23.60 1.60 7 8 0 22.90 2.30 7 8 0 22.70 2.30 7 8 0 28.10 3.00 -8 -8 0 1.20 1.30 -8 -8 0 1.20 0.90 8 8 0 1.30 1.70 8 8 0 -0.20 1.10 -9 -8 0 1.40 1.40 -9 -8 0 -1.30 0.80 9 8 0 -0.20 1.30 9 8 0 1.60 1.30 -10 -8 0 3.70 1.40 -10 -8 0 5.80 1.30 10 8 0 4.60 2.40 10 8 0 7.20 1.60 -11 -8 0 -1.50 0.90 -11 -8 0 5.40 1.90 11 8 0 0.40 1.50 11 8 0 -1.30 1.30 11 8 0 0.80 2.30 -12 -8 0 -2.00 1.00 -12 -8 0 1.10 1.80 12 8 0 -0.90 1.30 12 8 0 -1.60 2.40 7 -9 0 -1.50 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7.00 1.60 -8 -3 3 6.30 1.40 7 3 -3 5.00 1.70 7 3 -3 4.80 1.40 7 3 -3 5.70 1.30 -7 -3 3 4.80 1.10 -7 -3 3 6.00 1.50 -7 -3 3 5.30 1.10 6 3 -3 5.00 1.30 6 3 -3 5.00 1.50 6 3 -3 5.10 0.90 -6 -3 3 5.20 1.20 -6 -3 3 4.60 1.00 -6 -3 3 5.70 1.20 5 3 -3 8.60 1.20 5 3 -3 10.50 1.10 5 3 -3 9.50 1.30 -5 -3 3 12.10 1.30 -5 -3 3 11.10 1.20 -5 -3 3 9.80 1.00 4 3 -3 10.10 1.10 4 3 -3 11.40 1.30 4 3 -3 12.20 1.00 4 3 -3 12.30 0.60 -4 -3 3 12.00 1.10 -4 -3 3 11.30 1.10 -4 -3 3 13.00 0.80 -4 -3 3 11.00 1.10 3 3 -3 98.79 2.90 3 3 -3 102.49 2.80 3 3 -3 103.09 3.60 3 3 -3 104.89 3.20 3 3 -3 105.69 2.90 -3 -3 3 100.59 3.00 -3 -3 3 107.49 2.90 -3 -3 3 101.49 3.10 2 3 -3 2.90 0.50 2 3 -3 2.60 0.50 2 3 -3 3.00 0.50 2 3 -3 1.90 0.70 -2 -3 3 3.00 0.50 -2 -3 3 1.60 0.50 -2 -3 3 2.70 0.60 -2 -3 3 3.30 0.60 1 3 -3 25.60 1.30 1 3 -3 26.60 1.10 1 3 -3 25.00 1.10 -1 -3 3 26.20 1.20 -1 -3 3 24.90 1.10 -1 -3 3 25.60 1.10 -1 -3 3 24.70 1.30 -1 -3 3 25.20 1.00 0 3 -3 14.40 1.10 0 3 -3 15.80 0.80 0 3 -3 15.10 0.80 0 3 -3 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1.70 -4 -1 -19 -0.70 1.30 -4 -1 -19 -0.60 1.50 4 1 19 -0.20 0.90 4 1 19 0.70 1.60 -5 -1 -19 4.10 1.80 -5 -1 -19 0.40 1.20 5 1 19 2.10 1.50 -6 -1 -19 1.60 1.40 6 1 19 1.60 1.50 -3 -2 -19 -3.90 1.30 -3 -2 -19 -1.10 1.40 3 2 19 0.70 1.50 3 2 19 -0.30 1.30 -4 -2 -19 -1.70 1.10 -4 -2 -19 -0.90 1.10 4 2 19 0.90 1.40 4 2 19 0.30 1.00 -5 -2 -19 -0.50 1.20 -5 -2 -19 -2.30 1.40 5 2 19 0.60 1.30 5 2 19 1.20 1.30 -6 -2 -19 1.30 1.80 -6 -2 -19 -3.30 1.00 6 2 19 1.90 1.40 -7 -2 -19 0.00 1.30 -3 -3 -19 0.60 1.70 -3 -3 -19 5.00 1.80 3 3 19 -0.10 1.30 -4 -3 -19 -0.90 1.40 -4 -3 -19 2.30 1.40 4 3 19 1.20 1.10 4 3 19 1.70 1.40 -5 -3 -19 -2.80 1.10 -5 -3 -19 -0.10 1.30 5 3 19 0.40 1.30 5 3 19 -1.80 1.10 -6 -3 -19 1.00 1.80 -6 -3 -19 -0.40 1.30 6 3 19 0.60 1.30 -7 -3 -19 -0.50 1.30 -7 -3 -19 1.30 1.30 7 3 19 0.60 1.30 -3 -4 -19 2.90 1.60 -4 -4 -19 0.30 1.30 -4 -4 -19 2.30 1.40 4 4 19 0.50 1.30 -5 -4 -19 2.30 1.40 -5 -4 -19 3.20 1.90 5 4 19 4.70 1.70 5 4 19 1.90 1.40 -6 -4 -19 -0.40 1.70 -6 -4 -19 -1.60 1.30 6 4 19 -0.60 1.30 -7 -4 -19 0.10 1.20 -7 -4 -19 0.70 1.50 7 4 19 -0.20 1.10 7 4 19 -0.80 1.30 -4 -5 -19 0.20 1.80 -5 -5 -19 0.70 1.80 -5 -5 -19 1.50 1.70 -6 -5 -19 0.80 1.90 -6 -5 -19 -0.60 1.10 6 5 19 -1.10 1.10 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 55774 _shelx_res_file ; TITL bk5cg CELL 0.71073 10.3034 11.4856 14.4725 81.013 69.861 69.990 ZERR 4.00 0.0004 0.0004 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H N O CL UNIT 68 52 8 8 4 MERG 2 FMAP 2 OMIT -2 53.1 PLAN 10 SIZE 0.130 0.160 0.190 ACTA BOND $H CONF HTAB OMIT 0 1 0 L.S. 20 TEMP 23.00 EADP C141 C341 EADP C241 C441 WGHT 0.035300 0.710900 FVAR 0.34691 0.68157 0.53605 MOLE 1 N11 3 0.465368 0.202028 0.974848 11.00000 0.04426 0.05241 = 0.03004 0.00350 -0.01118 -0.01578 N12 3 0.486500 0.147887 1.063140 11.00000 0.05186 0.06141 = 0.03177 0.00571 -0.01554 -0.01949 C13 1 0.628285 0.112207 1.046711 11.00000 0.05151 0.05411 = 0.03877 -0.00146 -0.01738 -0.01702 C14 1 0.702679 0.143090 0.948874 11.00000 0.04572 0.05349 = 0.04227 -0.00337 -0.01175 -0.01445 C15 1 0.593943 0.199142 0.906891 11.00000 0.04869 0.04525 = 0.03254 -0.00105 -0.00766 -0.01455 C111 1 0.320755 0.248129 0.969157 11.00000 0.04220 0.04795 = 0.03561 -0.00048 -0.01287 -0.01104 C112 1 0.286354 0.331468 0.895993 11.00000 0.05380 0.10271 = 0.06686 0.03574 -0.01764 -0.01739 AFIX 43 H112 2 0.357522 0.359831 0.848305 11.00000 -1.20000 AFIX 0 C113 1 0.145098 0.372918 0.893740 11.00000 0.06359 0.14348 = 0.07845 0.05045 -0.02930 -0.01218 AFIX 43 H113 2 0.122217 0.428279 0.843241 11.00000 -1.20000 AFIX 0 C114 1 0.038861 0.334926 0.963327 11.00000 0.05005 0.11331 = 0.07215 0.01274 -0.02511 -0.01158 AFIX 43 H114 2 -0.056156 0.364052 0.961177 11.00000 -1.20000 AFIX 0 C115 1 0.073814 0.253481 1.036282 11.00000 0.04599 0.10186 = 0.06643 0.01291 -0.01292 -0.02499 AFIX 43 H115 2 0.001639 0.227065 1.084669 11.00000 -1.20000 AFIX 0 C116 1 0.213787 0.209443 1.039888 11.00000 0.04843 0.07752 = 0.04601 0.01289 -0.01331 -0.01940 AFIX 43 H116 2 0.235982 0.153445 1.090251 11.00000 -1.20000 AFIX 0 C131 1 0.690688 0.048521 1.127013 11.00000 0.06866 0.08281 = 0.04981 0.00314 -0.03069 -0.02093 AFIX 137 H13A 2 0.613356 0.042646 1.186180 11.00000 -1.50000 H13B 2 0.744738 0.095160 1.138591 11.00000 -1.50000 H13C 2 0.754123 -0.033219 1.107935 11.00000 -1.50000 AFIX 0 O151 4 0.603174 0.248260 0.814102 11.00000 0.05899 0.04586 = 0.03110 0.00183 -0.00522 -0.00879 C151 1 0.665497 0.163966 0.739366 11.00000 0.03408 0.04754 = 0.03200 0.00046 -0.01114 -0.00795 C152 1 0.731650 0.205941 0.646376 11.00000 0.03807 0.04986 = 0.03666 0.00316 -0.01120 -0.00850 CL12 5 0.741761 0.355344 0.627454 11.00000 0.06202 0.05673 = 0.06021 0.01683 -0.01063 -0.01743 C153 1 0.791463 0.127694 0.569087 11.00000 0.06348 0.07957 = 0.03614 -0.00404 -0.01163 -0.01482 AFIX 43 H153 2 0.837070 0.155410 0.506346 11.00000 -1.20000 AFIX 0 C154 1 0.783832 0.009253 0.584542 11.00000 0.07385 0.07688 = 0.05988 -0.02641 -0.02536 -0.00801 AFIX 43 H154 2 0.823564 -0.043144 0.532151 11.00000 -1.20000 AFIX 0 C155 1 0.717645 -0.032442 0.677231 11.00000 0.06678 0.05095 = 0.07462 -0.00571 -0.03598 -0.01669 AFIX 43 H155 2 0.713287 -0.113181 0.687512 11.00000 -1.20000 AFIX 0 C156 1 0.657780 0.044907 0.754906 11.00000 0.04875 0.05389 = 0.04592 0.00438 -0.01923 -0.01793 AFIX 43 H156 2 0.612348 0.016867 0.817569 11.00000 -1.20000 AFIX 0 PART 1 C141 1 0.852996 0.122118 0.909781 21.00000 0.04834 0.07162 = 0.04249 0.00837 -0.00894 -0.02140 AFIX 43 H141 2 0.911164 0.081119 0.949206 21.00000 -1.20000 AFIX 0 O141 4 0.912853 0.157105 0.822315 21.00000 0.05537 0.09841 = 0.05926 0.00444 0.00184 -0.02938 PART 2 SAME 0.01 0.02 C141 > O141 C341 1 0.864781 0.133055 0.885561 -21.00000 0.04834 0.07162 = 0.04249 0.00837 -0.00894 -0.02140 AFIX 43 H341 2 0.891956 0.166645 0.821740 -21.00000 -1.20000 AFIX 0 O341 4 0.953826 0.073593 0.932162 -21.00000 0.05854 0.13312 = 0.12767 -0.00645 -0.03945 -0.01496 PART 0 MOLE 2 N21 3 0.359910 0.306213 0.365190 11.00000 0.03343 0.04573 = 0.04461 0.00054 -0.01745 -0.01314 N22 3 0.252439 0.368251 0.322247 11.00000 0.03872 0.05497 = 0.05272 0.00447 -0.02490 -0.01568 C23 1 0.320522 0.406175 0.233831 11.00000 0.04791 0.04906 = 0.04920 -0.00004 -0.02163 -0.01719 C24 1 0.471978 0.370019 0.216471 11.00000 0.04672 0.05220 = 0.04457 -0.00100 -0.01419 -0.01915 C25 1 0.490635 0.307284 0.302238 11.00000 0.03327 0.04236 = 0.05114 -0.00622 -0.01528 -0.01184 C211 1 0.317311 0.257516 0.464276 11.00000 0.03942 0.04211 = 0.04666 -0.00042 -0.01675 -0.01502 C212 1 0.417961 0.177411 0.506570 11.00000 0.04471 0.07470 = 0.05993 0.01325 -0.01678 -0.00507 AFIX 43 H212 2 0.516286 0.152399 0.470496 11.00000 -1.20000 AFIX 0 C213 1 0.370992 0.134816 0.603086 11.00000 0.06268 0.08897 = 0.07030 0.02846 -0.02789 -0.00955 AFIX 43 H213 2 0.438937 0.082128 0.632050 11.00000 -1.20000 AFIX 0 C214 1 0.227541 0.168270 0.656656 11.00000 0.07267 0.07705 = 0.05405 0.01707 -0.02041 -0.02890 AFIX 43 H214 2 0.197356 0.138274 0.721386 11.00000 -1.20000 AFIX 0 C215 1 0.128660 0.246411 0.614077 11.00000 0.04922 0.07858 = 0.05733 0.00595 -0.00986 -0.02689 AFIX 43 H215 2 0.030309 0.269321 0.650163 11.00000 -1.20000 AFIX 0 C216 1 0.172026 0.291988 0.518487 11.00000 0.04106 0.06240 = 0.05629 0.00363 -0.01922 -0.01758 AFIX 43 H216 2 0.103390 0.345899 0.490618 11.00000 -1.20000 AFIX 0 C231 1 0.236475 0.479584 0.166844 11.00000 0.06724 0.08179 = 0.06055 0.01279 -0.03614 -0.02277 AFIX 137 H23A 2 0.239285 0.563308 0.159340 11.00000 -1.50000 H23B 2 0.137368 0.479548 0.194409 11.00000 -1.50000 H23C 2 0.278665 0.443154 0.103658 11.00000 -1.50000 AFIX 0 O251 4 0.614047 0.245377 0.325367 11.00000 0.03536 0.04932 = 0.07800 0.00275 -0.02481 -0.01466 C251 1 0.697831 0.314146 0.332821 11.00000 0.03475 0.05381 = 0.03956 0.00492 -0.01340 -0.01874 C252 1 0.843987 0.253199 0.315376 11.00000 0.03339 0.05246 = 0.03576 0.00311 -0.01045 -0.01280 CL22 5 0.915232 0.100540 0.283747 11.00000 0.04882 0.06025 = 0.08248 -0.00936 -0.02614 -0.00512 C253 1 0.932335 0.314893 0.325147 11.00000 0.03705 0.07294 = 0.05377 0.00489 -0.01990 -0.01996 AFIX 43 H253 2 1.031303 0.274387 0.313100 11.00000 -1.20000 AFIX 0 C254 1 0.874446 0.435418 0.352505 11.00000 0.05473 0.06910 = 0.06448 0.00190 -0.02627 -0.03142 AFIX 43 H254 2 0.934206 0.476392 0.359315 11.00000 -1.20000 AFIX 0 C255 1 0.728663 0.496146 0.369947 11.00000 0.06494 0.05684 = 0.06990 -0.00941 -0.02628 -0.01977 AFIX 43 H255 2 0.689878 0.578176 0.388246 11.00000 -1.20000 AFIX 0 C256 1 0.639739 0.435372 0.360303 11.00000 0.03940 0.06000 = 0.06452 -0.00677 -0.01809 -0.01010 AFIX 43 H256 2 0.540836 0.476187 0.372335 11.00000 -1.20000 AFIX 0 PART 3 C241 1 0.571737 0.385711 0.123888 31.00000 0.04531 0.08117 = 0.05263 0.00377 -0.02155 -0.03128 AFIX 43 H241 2 0.539952 0.422327 0.070276 31.00000 -1.20000 AFIX 0 O241 4 0.707830 0.348043 0.115562 31.00000 0.04530 0.10905 = 0.07328 0.00339 -0.00384 -0.03201 PART 4 SAME 0.01 0.02 C241 > O241 C441 1 0.599268 0.392232 0.133534 -31.00000 0.04531 0.08117 = 0.05263 0.00377 -0.02155 -0.03128 AFIX 43 H441 2 0.691590 0.367286 0.140257 -31.00000 -1.20000 AFIX 0 O441 4 0.576697 0.446474 0.053470 -31.00000 0.10986 0.15295 = 0.06637 0.04383 -0.02031 -0.05716 PART 0 HKLF 4 REM bk5cg REM R1 = 0.0422 for 4051 Fo > 4sig(Fo) and 0.0841 for all 6296 data REM 425 parameters refined using 2 restraints END WGHT 0.0353 0.7109 REM Instructions for potential hydrogen bonds HTAB C112 O151 EQIV $1 -x+1, -y, -z+2 HTAB C156 N12_$1 HTAB C212 O251 EQIV $2 -x+1, -y+1, -z HTAB C231 O441_$2 EQIV $3 -x+1, -y+1, -z+1 HTAB C256 Cl12_$3 REM Highest difference peak 0.200, deepest hole -0.256, 1-sigma level 0.040 Q1 1 0.8423 0.0681 0.3305 11.00000 0.05 0.20 Q2 1 0.1706 0.4138 0.1616 11.00000 0.05 0.19 Q3 1 0.7118 0.1751 0.6038 11.00000 0.05 0.18 Q4 1 0.1212 0.5924 0.2292 11.00000 0.05 0.18 Q5 1 0.7582 0.2776 0.3596 11.00000 0.05 0.18 Q6 1 0.2943 0.5216 0.1059 11.00000 0.05 0.17 Q7 1 0.1276 0.5008 0.8671 11.00000 0.05 0.17 Q8 1 0.5579 0.4994 0.3205 11.00000 0.05 0.16 Q9 1 0.6528 0.1939 0.6817 11.00000 0.05 0.15 Q10 1 0.7784 0.1328 0.2963 11.00000 0.05 0.15 ; _shelx_res_checksum 57296 _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 N11 0.46537(19) 0.20203(16) 0.97485(11) 0.0428(4) Uani d 1 . . N N12 0.4865(2) 0.14789(18) 1.06314(12) 0.0481(5) Uani d 1 . . C C13 0.6283(3) 0.1122(2) 1.04671(15) 0.0471(5) Uani d 1 . . C C14 0.7027(2) 0.1431(2) 0.94887(15) 0.0478(5) Uani d 1 . . C C15 0.5939(2) 0.1991(2) 0.90689(14) 0.0436(5) Uani d 1 . . C C111 0.3208(2) 0.2481(2) 0.96916(14) 0.0427(5) Uani d 1 . . C C112 0.2864(3) 0.3315(3) 0.8960(2) 0.0814(9) Uani d 1 . . H H112 0.3575 0.3598 0.8483 0.098 Uiso calc 1 . . C C113 0.1451(3) 0.3729(4) 0.8937(2) 0.1052(13) Uani d 1 . . H H113 0.1222 0.4283 0.8432 0.126 Uiso calc 1 . . C C114 0.0389(3) 0.3349(3) 0.9633(2) 0.0826(9) Uani d 1 . . H H114 -0.0562 0.3641 0.9612 0.099 Uiso calc 1 . . C C115 0.0738(3) 0.2535(3) 1.0363(2) 0.0741(8) Uani d 1 . . H H115 0.0016 0.2271 1.0847 0.089 Uiso calc 1 . . C C116 0.2138(3) 0.2094(2) 1.03989(17) 0.0596(7) Uani d 1 . . H H116 0.2360 0.1534 1.0903 0.072 Uiso calc 1 . . C C131 0.6907(3) 0.0485(3) 1.12701(17) 0.0652(7) Uani d 1 . . H H13A 0.6134 0.0426 1.1862 0.098 Uiso calc 1 . . H H13B 0.7447 0.0952 1.1386 0.098 Uiso calc 1 . . H H13C 0.7541 -0.0332 1.1079 0.098 Uiso calc 1 . . O O151 0.60317(16) 0.24826(13) 0.81410(10) 0.0502(4) Uani d 1 . . C C151 0.6655(2) 0.1640(2) 0.73937(14) 0.0392(5) Uani d 1 . . C C152 0.7316(2) 0.2059(2) 0.64638(15) 0.0437(5) Uani d 1 . . Cl Cl12 0.74176(7) 0.35534(6) 0.62745(5) 0.0646(2) Uani d 1 . . C C153 0.7915(3) 0.1277(3) 0.56909(17) 0.0627(7) Uani d 1 . . H H153 0.8371 0.1554 0.5063 0.075 Uiso calc 1 . . C C154 0.7838(3) 0.0093(3) 0.5845(2) 0.0704(8) Uani d 1 . . H H154 0.8236 -0.0431 0.5322 0.085 Uiso calc 1 . . C C155 0.7176(3) -0.0324(2) 0.6772(2) 0.0604(7) Uani d 1 . . H H155 0.7133 -0.1132 0.6875 0.072 Uiso calc 1 . . C C156 0.6578(2) 0.0449(2) 0.75491(17) 0.0486(5) Uani d 1 . . H H156 0.6123 0.0169 0.8176 0.058 Uiso calc 1 . . C C141 0.8530(8) 0.1221(15) 0.9098(7) 0.056(2) Uani d 0.682(6) A 1 H H141 0.9112 0.0811 0.9492 0.067 Uiso calc 0.682(6) A 1 O O141 0.9129(3) 0.1571(3) 0.8223(2) 0.0759(12) Uani d 0.682(6) A 1 C C341 0.865(2) 0.133(4) 0.886(2) 0.056(2) Uani d 0.318(6) A 2 H H341 0.8920 0.1666 0.8217 0.067 Uiso calc 0.318(6) A 2 O O341 0.9538(8) 0.0736(8) 0.9322(6) 0.108(3) Uani d 0.318(6) A 2 N N21 0.35991(17) 0.30621(16) 0.36519(12) 0.0399(4) Uani d 1 . . N N22 0.25244(19) 0.36825(17) 0.32225(13) 0.0464(4) Uani d 1 . . C C23 0.3205(2) 0.4062(2) 0.23383(16) 0.0466(5) Uani d 1 . . C C24 0.4720(2) 0.3700(2) 0.21647(16) 0.0470(5) Uani d 1 . . C C25 0.4906(2) 0.30728(19) 0.30224(16) 0.0412(5) Uani d 1 . . C C211 0.3173(2) 0.25752(19) 0.46428(15) 0.0414(5) Uani d 1 . . C C212 0.4180(3) 0.1774(2) 0.50657(19) 0.0653(7) Uani d 1 . . H H212 0.5163 0.1524 0.4705 0.078 Uiso calc 1 . . C C213 0.3710(3) 0.1348(3) 0.6031(2) 0.0796(9) Uani d 1 . . H H213 0.4389 0.0821 0.6320 0.096 Uiso calc 1 . . C C214 0.2275(3) 0.1683(3) 0.65666(19) 0.0686(7) Uani d 1 . . H H214 0.1974 0.1383 0.7214 0.082 Uiso calc 1 . . C C215 0.1287(3) 0.2464(3) 0.61408(18) 0.0627(7) Uani d 1 . . H H215 0.0303 0.2693 0.6502 0.075 Uiso calc 1 . . C C216 0.1720(2) 0.2920(2) 0.51849(17) 0.0525(6) Uani d 1 . . H H216 0.1034 0.3459 0.4906 0.063 Uiso calc 1 . . C C231 0.2365(3) 0.4796(3) 0.16684(19) 0.0674(7) Uani d 1 . . H H23A 0.2393 0.5633 0.1593 0.101 Uiso calc 1 . . H H23B 0.1374 0.4795 0.1944 0.101 Uiso calc 1 . . H H23C 0.2787 0.4432 0.1037 0.101 Uiso calc 1 . . O O251 0.61405(15) 0.24538(14) 0.32537(12) 0.0525(4) Uani d 1 . . C C251 0.6978(2) 0.3141(2) 0.33282(15) 0.0417(5) Uani d 1 . . C C252 0.8440(2) 0.2532(2) 0.31538(14) 0.0414(5) Uani d 1 . . Cl Cl22 0.91523(7) 0.10054(6) 0.28375(5) 0.06481(19) Uani d 1 . . C C253 0.9323(2) 0.3149(2) 0.32515(16) 0.0532(6) Uani d 1 . . H H253 1.0313 0.2744 0.3131 0.064 Uiso calc 1 . . C C254 0.8744(3) 0.4354(2) 0.35251(18) 0.0579(6) Uani d 1 . . H H254 0.9342 0.4764 0.3593 0.070 Uiso calc 1 . . C C255 0.7287(3) 0.4961(2) 0.36995(19) 0.0615(7) Uani d 1 . . H H255 0.6899 0.5782 0.3882 0.074 Uiso calc 1 . . C C256 0.6397(3) 0.4354(2) 0.36030(18) 0.0551(6) Uani d 1 . . H H256 0.5408 0.4762 0.3723 0.066 Uiso calc 1 . . C C241 0.5717(19) 0.386(3) 0.1239(9) 0.056(2) Uani d 0.536(5) B 3 H H241 0.5400 0.4223 0.0703 0.067 Uiso calc 0.536(5) B 3 O O241 0.7078(4) 0.3480(4) 0.1156(3) 0.0786(15) Uani d 0.536(5) B 3 C C441 0.599(2) 0.392(3) 0.1335(10) 0.056(2) Uani d 0.464(5) B 4 H H441 0.6916 0.3673 0.1403 0.067 Uiso calc 0.464(5) B 4 O O441 0.5767(6) 0.4465(6) 0.0535(4) 0.113(2) Uani d 0.464(5) B 4 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 N11 0.0443(10) 0.0524(11) 0.0300(9) -0.0158(9) -0.0112(8) 0.0035(8) N12 0.0519(12) 0.0614(12) 0.0318(9) -0.0195(10) -0.0155(8) 0.0057(8) C13 0.0515(14) 0.0541(14) 0.0388(12) -0.0170(11) -0.0174(10) -0.0015(10) C14 0.0457(13) 0.0535(14) 0.0423(12) -0.0145(11) -0.0118(10) -0.0034(10) C15 0.0487(13) 0.0452(13) 0.0325(11) -0.0145(10) -0.0077(10) -0.0011(9) C111 0.0422(12) 0.0479(13) 0.0356(11) -0.0110(10) -0.0129(9) -0.0005(9) C112 0.0538(16) 0.103(2) 0.0669(18) -0.0174(16) -0.0176(14) 0.0357(16) C113 0.064(2) 0.143(3) 0.078(2) -0.012(2) -0.0293(17) 0.050(2) C114 0.0500(16) 0.113(3) 0.0722(19) -0.0116(16) -0.0251(15) 0.0127(18) C115 0.0460(15) 0.102(2) 0.0664(17) -0.0250(15) -0.0129(13) 0.0129(16) C116 0.0484(14) 0.0775(18) 0.0460(13) -0.0194(13) -0.0133(11) 0.0129(12) C131 0.0687(17) 0.0828(19) 0.0498(14) -0.0209(15) -0.0307(13) 0.0031(13) O151 0.0590(10) 0.0459(9) 0.0311(7) -0.0088(7) -0.0052(7) 0.0018(6) C151 0.0341(11) 0.0475(13) 0.0320(10) -0.0079(9) -0.0111(9) 0.0005(9) C152 0.0381(12) 0.0499(13) 0.0367(11) -0.0085(10) -0.0112(9) 0.0032(9) Cl12 0.0620(4) 0.0567(4) 0.0602(4) -0.0174(3) -0.0106(3) 0.0168(3) C153 0.0635(16) 0.080(2) 0.0361(13) -0.0148(14) -0.0116(11) -0.0040(12) C154 0.0738(19) 0.077(2) 0.0599(17) -0.0080(15) -0.0254(14) -0.0264(15) C155 0.0668(17) 0.0510(15) 0.0746(18) -0.0167(13) -0.0360(14) -0.0057(13) C156 0.0488(13) 0.0539(14) 0.0459(12) -0.0179(11) -0.0192(11) 0.0044(11) C141 0.048(2) 0.072(4) 0.042(6) -0.021(2) -0.009(3) 0.008(4) O141 0.0554(18) 0.098(2) 0.059(2) -0.0294(16) 0.0018(14) 0.0044(16) C341 0.048(2) 0.072(4) 0.042(6) -0.021(2) -0.009(3) 0.008(4) O341 0.059(5) 0.133(7) 0.128(7) -0.015(4) -0.039(4) -0.006(5) N21 0.0334(9) 0.0457(10) 0.0446(10) -0.0131(8) -0.0175(8) 0.0005(8) N22 0.0387(10) 0.0550(12) 0.0527(11) -0.0157(9) -0.0249(9) 0.0045(9) C23 0.0479(13) 0.0491(13) 0.0492(13) -0.0172(11) -0.0216(11) 0.0000(10) C24 0.0467(13) 0.0522(14) 0.0446(12) -0.0192(11) -0.0142(10) -0.0010(10) C25 0.0333(11) 0.0424(12) 0.0511(12) -0.0118(9) -0.0153(10) -0.0062(10) C211 0.0394(12) 0.0421(12) 0.0467(12) -0.0150(10) -0.0168(10) -0.0004(9) C212 0.0447(14) 0.0747(18) 0.0599(15) -0.0051(13) -0.0168(12) 0.0132(13) C213 0.0627(18) 0.089(2) 0.0703(18) -0.0095(16) -0.0279(15) 0.0285(16) C214 0.0727(19) 0.0770(19) 0.0540(15) -0.0289(15) -0.0204(14) 0.0171(13) C215 0.0492(15) 0.0786(19) 0.0573(15) -0.0269(14) -0.0099(12) 0.0060(13) C216 0.0411(13) 0.0624(15) 0.0563(14) -0.0176(11) -0.0192(11) 0.0036(11) C231 0.0672(17) 0.0818(19) 0.0606(16) -0.0228(15) -0.0361(14) 0.0128(14) O251 0.0354(8) 0.0493(9) 0.0780(11) -0.0147(7) -0.0248(8) 0.0028(8) C251 0.0347(11) 0.0538(14) 0.0396(11) -0.0187(10) -0.0134(9) 0.0049(10) C252 0.0334(11) 0.0525(13) 0.0358(11) -0.0128(10) -0.0105(9) 0.0031(9) Cl22 0.0488(4) 0.0603(4) 0.0825(5) -0.0051(3) -0.0261(3) -0.0094(3) C253 0.0371(12) 0.0729(18) 0.0538(14) -0.0200(12) -0.0199(11) 0.0049(12) C254 0.0547(15) 0.0691(18) 0.0645(16) -0.0314(14) -0.0263(13) 0.0019(13) C255 0.0649(17) 0.0568(16) 0.0699(17) -0.0198(13) -0.0263(13) -0.0094(13) C256 0.0394(13) 0.0600(16) 0.0645(15) -0.0101(11) -0.0181(11) -0.0068(12) C241 0.045(6) 0.081(3) 0.053(3) -0.031(5) -0.022(3) 0.004(3) O241 0.045(2) 0.109(3) 0.073(2) -0.032(2) -0.0038(18) 0.003(2) C441 0.045(6) 0.081(3) 0.053(3) -0.031(5) -0.022(3) 0.004(3) O441 0.110(4) 0.153(5) 0.066(3) -0.057(4) -0.020(3) 0.044(3) 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' Cl Cl 0.1484 0.1585 '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 C15 N11 N12 109.92(17) C15 N11 C111 131.34(17) N12 N11 C111 118.73(16) C13 N12 N11 105.69(16) N12 C13 C14 111.49(19) N12 C13 C131 120.3(2) C14 C13 C131 128.3(2) C15 C14 C141 130.6(4) C15 C14 C13 104.06(19) C141 C14 C13 125.3(4) C15 C14 C341 119.0(8) C13 C14 C341 136.8(8) N11 C15 O151 121.68(19) N11 C15 C14 108.84(18) O151 C15 C14 129.5(2) C112 C111 C116 119.5(2) C112 C111 N11 121.6(2) C116 C111 N11 118.93(18) C111 C112 C113 119.3(3) C111 C112 H112 120.4 C113 C112 H112 120.4 C114 C113 C112 121.5(3) C114 C113 H113 119.2 C112 C113 H113 119.2 C113 C114 C115 118.7(3) C113 C114 H114 120.7 C115 C114 H114 120.7 C114 C115 C116 121.1(3) C114 C115 H115 119.4 C116 C115 H115 119.4 C111 C116 C115 119.9(2) C111 C116 H116 120.1 C115 C116 H116 120.1 C13 C131 H13A 109.5 C13 C131 H13B 109.5 H13A C131 H13B 109.5 C13 C131 H13C 109.5 H13A C131 H13C 109.5 H13B C131 H13C 109.5 C15 O151 C151 116.19(16) C156 C151 C152 120.2(2) C156 C151 O151 122.55(18) C152 C151 O151 117.18(19) C151 C152 C153 119.7(2) C151 C152 Cl12 119.99(17) C153 C152 Cl12 120.30(18) C154 C153 C152 120.1(2) C154 C153 H153 120.0 C152 C153 H153 120.0 C153 C154 C155 120.2(2) C153 C154 H154 119.9 C155 C154 H154 119.9 C154 C155 C156 120.2(2) C154 C155 H155 119.9 C156 C155 H155 119.9 C151 C156 C155 119.6(2) C151 C156 H156 120.2 C155 C156 H156 120.2 O141 C141 C14 122.4(5) O141 C141 H141 118.8 C14 C141 H141 118.8 O341 C341 C14 112.0(19) O341 C341 H341 124.0 C14 C341 H341 124.0 C25 N21 N22 109.99(16) C25 N21 C211 131.70(17) N22 N21 C211 118.27(16) C23 N22 N21 105.52(17) N22 C23 C24 111.66(18) N22 C23 C231 120.1(2) C24 C23 C231 128.2(2) C25 C24 C241 132.2(9) C25 C24 C23 104.14(18) C241 C24 C23 123.1(8) C25 C24 C441 120.9(9) C23 C24 C441 134.9(9) N21 C25 O251 120.89(18) N21 C25 C24 108.69(18) O251 C25 C24 130.25(19) C216 C211 C212 119.5(2) C216 C211 N21 118.85(18) C212 C211 N21 121.68(19) C211 C212 C213 119.2(2) C211 C212 H212 120.4 C213 C212 H212 120.4 C214 C213 C212 121.4(2) C214 C213 H213 119.3 C212 C213 H213 119.3 C213 C214 C215 119.0(2) C213 C214 H214 120.5 C215 C214 H214 120.5 C214 C215 C216 121.1(2) C214 C215 H215 119.5 C216 C215 H215 119.5 C215 C216 C211 119.8(2) C215 C216 H216 120.1 C211 C216 H216 120.1 C23 C231 H23A 109.5 C23 C231 H23B 109.5 H23A C231 H23B 109.5 C23 C231 H23C 109.5 H23A C231 H23C 109.5 H23B C231 H23C 109.5 C25 O251 C251 117.88(16) C252 C251 C256 120.3(2) C252 C251 O251 116.61(19) C256 C251 O251 123.02(19) C251 C252 C253 119.5(2) C251 C252 Cl22 120.09(17) C253 C252 Cl22 120.40(17) C254 C253 C252 120.1(2) C254 C253 H253 119.9 C252 C253 H253 119.9 C253 C254 C255 120.3(2) C253 C254 H254 119.8 C255 C254 H254 119.8 C254 C255 C256 119.9(2) C254 C255 H255 120.0 C256 C255 H255 120.0 C251 C256 C255 119.8(2) C251 C256 H256 120.1 C255 C256 H256 120.1 O241 C241 C24 118.2(12) O241 C241 H241 120.9 C24 C241 H241 120.9 O441 C441 C24 118.2(15) O441 C441 H441 120.9 C24 C441 H441 120.9 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N11 C15 1.344(3) N11 N12 1.385(2) N11 C111 1.428(3) N12 C13 1.319(3) C13 C14 1.414(3) C13 C131 1.492(3) C14 C15 1.375(3) C14 C141 1.400(8) C14 C341 1.58(2) C15 O151 1.357(2) C111 C112 1.368(3) C111 C116 1.370(3) C112 C113 1.378(4) C112 H112 0.9300 C113 C114 1.354(4) C113 H113 0.9300 C114 C115 1.357(4) C114 H114 0.9300 C115 C116 1.372(3) C115 H115 0.9300 C116 H116 0.9300 C131 H13A 0.9600 C131 H13B 0.9600 C131 H13C 0.9600 O151 C151 1.394(2) C151 C156 1.376(3) C151 C152 1.378(3) C152 C153 1.378(3) C152 Cl12 1.728(2) C153 C154 1.369(4) C153 H153 0.9300 C154 C155 1.374(4) C154 H154 0.9300 C155 C156 1.376(3) C155 H155 0.9300 C156 H156 0.9300 C141 O141 1.272(10) C141 H141 0.9300 C341 O341 1.271(13) C341 H341 0.9300 N21 C25 1.344(3) N21 N22 1.384(2) N21 C211 1.430(3) N22 C23 1.318(3) C23 C24 1.411(3) C23 C231 1.491(3) C24 C25 1.374(3) C24 C241 1.410(11) C24 C441 1.508(13) C25 O251 1.354(2) C211 C216 1.377(3) C211 C212 1.380(3) C212 C213 1.381(3) C212 H212 0.9300 C213 C214 1.360(4) C213 H213 0.9300 C214 C215 1.363(3) C214 H214 0.9300 C215 C216 1.377(3) C215 H215 0.9300 C216 H216 0.9300 C231 H23A 0.9600 C231 H23B 0.9600 C231 H23C 0.9600 O251 C251 1.392(2) C251 C252 1.376(3) C251 C256 1.376(3) C252 C253 1.383(3) C252 Cl22 1.721(2) C253 C254 1.368(3) C253 H253 0.9300 C254 C255 1.372(3) C254 H254 0.9300 C255 C256 1.379(3) C255 H255 0.9300 C256 H256 0.9300 C241 O241 1.286(17) C241 H241 0.9300 C441 O441 1.283(17) C441 H441 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 C156 H156 N12 2_657 0.93 2.59 3.433(3) 152 no C255 H255 Cg3 2_666 0.93 2.80 3.635(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 C15 N11 N12 C13 -0.5(2) C111 N11 N12 C13 178.80(18) N11 N12 C13 C14 0.8(3) N11 N12 C13 C131 -179.6(2) N12 C13 C14 C15 -0.8(3) C131 C13 C14 C15 179.6(2) N12 C13 C14 C141 177.3(9) C131 C13 C14 C141 -2.3(10) N12 C13 C14 C341 176(2) C131 C13 C14 C341 -3(2) N12 N11 C15 O151 -178.96(18) C111 N11 C15 O151 1.9(3) N12 N11 C15 C14 0.0(2) C111 N11 C15 C14 -179.2(2) C141 C14 C15 N11 -177.5(10) C13 C14 C15 N11 0.5(2) C341 C14 C15 N11 -177.4(18) C141 C14 C15 O151 1.3(11) C13 C14 C15 O151 179.3(2) C341 C14 C15 O151 1.4(19) C15 N11 C111 C112 -19.3(4) N12 N11 C111 C112 161.6(2) C15 N11 C111 C116 161.9(2) N12 N11 C111 C116 -17.2(3) C116 C111 C112 C113 -1.4(5) N11 C111 C112 C113 179.9(3) C111 C112 C113 C114 1.3(6) C112 C113 C114 C115 -0.4(6) C113 C114 C115 C116 -0.3(5) C112 C111 C116 C115 0.6(4) N11 C111 C116 C115 179.4(2) C114 C115 C116 C111 0.2(5) N11 C15 O151 C151 -110.9(2) C14 C15 O151 C151 70.4(3) C15 O151 C151 C156 29.1(3) C15 O151 C151 C152 -153.42(19) C156 C151 C152 C153 -0.7(3) O151 C151 C152 C153 -178.17(19) C156 C151 C152 Cl12 -179.69(16) O151 C151 C152 Cl12 2.8(3) C151 C152 C153 C154 0.6(4) Cl12 C152 C153 C154 179.7(2) C152 C153 C154 C155 -0.5(4) C153 C154 C155 C156 0.4(4) C152 C151 C156 C155 0.6(3) O151 C151 C156 C155 177.94(19) C154 C155 C156 C151 -0.5(4) C15 C14 C141 O141 1(2) C13 C14 C141 O141 -176.7(9) C341 C14 C141 O141 0(10) C15 C14 C341 O341 -176.6(18) C141 C14 C341 O341 3(9) C13 C14 C341 O341 6(4) C25 N21 N22 C23 -0.2(2) C211 N21 N22 C23 177.93(18) N21 N22 C23 C24 0.3(2) N21 N22 C23 C231 -178.8(2) N22 C23 C24 C25 -0.4(3) C231 C23 C24 C25 178.7(2) N22 C23 C24 C241 172.2(13) C231 C23 C24 C241 -8.8(14) N22 C23 C24 C441 -176.2(17) C231 C23 C24 C441 2.9(17) N22 N21 C25 O251 -175.75(17) C211 N21 C25 O251 6.5(3) N22 N21 C25 C24 0.0(2) C211 N21 C25 C24 -177.8(2) C241 C24 C25 N21 -171.4(14) C23 C24 C25 N21 0.2(2) C441 C24 C25 N21 176.8(15) C241 C24 C25 O251 3.8(14) C23 C24 C25 O251 175.4(2) C441 C24 C25 O251 -8.0(15) C25 N21 C211 C216 166.6(2) N22 N21 C211 C216 -11.1(3) C25 N21 C211 C212 -13.3(3) N22 N21 C211 C212 169.0(2) C216 C211 C212 C213 -0.9(4) N21 C211 C212 C213 178.9(2) C211 C212 C213 C214 1.3(5) C212 C213 C214 C215 -0.6(5) C213 C214 C215 C216 -0.4(4) C214 C215 C216 C211 0.6(4) C212 C211 C216 C215 0.0(4) N21 C211 C216 C215 -179.9(2) N21 C25 O251 C251 -117.7(2) C24 C25 O251 C251 67.6(3) C25 O251 C251 C252 -153.77(19) C25 O251 C251 C256 29.0(3) C256 C251 C252 C253 -0.3(3) O251 C251 C252 C253 -177.63(18) C256 C251 C252 Cl22 178.53(17) O251 C251 C252 Cl22 1.3(2) C251 C252 C253 C254 0.4(3) Cl22 C252 C253 C254 -178.51(17) C252 C253 C254 C255 -0.3(4) C253 C254 C255 C256 0.3(4) C252 C251 C256 C255 0.3(3) O251 C251 C256 C255 177.4(2) C254 C255 C256 C251 -0.3(4) C25 C24 C241 O241 -9(3) C23 C24 C241 O241 -179.1(12) C441 C24 C241 O241 35(8) C25 C24 C441 O441 177.0(16) C241 C24 C441 O441 34(8) C23 C24 C441 O441 -8(3) _cod_database_fobs_code 2021646