#------------------------------------------------------------------------------ #$Date: 2023-06-29 17:26:13 +0200 (Thu, 29 Jun 2023) $ #$Revision: 284684 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022777.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_2022777 loop_ _publ_author_name 'Ghichi, Nadir' 'Djedouani, Amel' 'Hannachid, Douniazed' 'Elhadi, Said Mohamed' 'Benboudiaf, Ali' 'Merazig, Hocine' 'Ouksel, Louiza' 'Hellal, Abdelkader' 'Stoeckli-Evans, Helen' _publ_section_title ; Synthesis and crystal structures of two 1H-benzo[d]imidazole derivatives: DFT and anticorrosion studies, and Hirshfeld surface analysis ; _journal_coeditor_code WV3012 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C Structural Chemistry' _journal_page_first 292 _journal_page_last 304 _journal_paper_doi 10.1107/S2053229623005545 _journal_volume 79 _journal_year 2023 _chemical_formula_iupac 'C30 H24 N2 O2, C2 H6 O' _chemical_formula_moiety 'C30 H24 N2 O2, C2 H6 O' _chemical_formula_sum 'C32 H30 N2 O3' _chemical_formula_weight 490.58 _chemical_name_systematic '2-(4-Methoxynaphthalen-1-yl)-1-[(4-methoxynaphthalen-1-yl)methyl]-1H-benzo[d]imidazole ethanol monosolvate' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 69.0290(10) _cell_angle_beta 82.8710(10) _cell_angle_gamma 67.5150(10) _cell_formula_units_Z 2 _cell_length_a 10.7065(3) _cell_length_b 10.9434(3) _cell_length_c 12.8256(4) _cell_measurement_reflns_used 6273 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.53 _cell_measurement_theta_min 2.24 _cell_volume 1296.37(7) _computing_cell_refinement ; SAINT (Bruker, 2012) ; _computing_data_collection ; APEX2 (Bruker, 2012) ; _computing_data_reduction ; SAINT (Bruker, 2012) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2020) ; _computing_publication_material ; PLATON (Spek, 2020), SHELXL2018 (Sheldrick, 2015b) and publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_unetI/netI 0.0210 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 20872 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.247 _diffrn_reflns_theta_min 3.517 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.257 _exptl_crystal_description block _exptl_crystal_F_000 520 _exptl_crystal_size_max 0.030 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.010 _refine_diff_density_max 0.310 _refine_diff_density_min -0.256 _refine_ls_extinction_coef 0.029(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; (SHELXL2018; Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 358 _refine_ls_number_reflns 4611 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 1.092 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0539 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+0.1721P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1507 _refine_ls_wR_factor_ref 0.1616 _reflns_number_gt 3587 _reflns_number_total 4611 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wv3012sup1.cif _cod_data_source_block II _cod_database_code 2022777 _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 0.998 _shelx_estimated_absorpt_t_max 0.999 _shelx_hkl_file ; 2 0 0 107.69 2.60 -3 0 0 21.80 1.10 -3 0 0 20.20 0.60 -3 0 0 18.60 0.60 3 0 0 21.10 0.70 3 0 0 21.70 1.00 3 0 0 21.20 0.60 3 0 0 20.40 0.60 -4 0 0 586.44 13.90 -4 0 0 598.94 13.80 -4 0 0 582.94 13.60 -4 0 0 591.14 13.60 4 0 0 596.84 13.60 4 0 0 586.84 13.60 4 0 0 609.54 13.80 4 0 0 601.04 13.40 -5 0 0 79.79 2.70 -5 0 0 82.29 2.30 -5 0 0 82.69 2.30 -5 0 0 83.99 2.50 5 0 0 81.69 2.20 5 0 0 83.59 2.50 5 0 0 82.49 2.20 5 0 0 82.39 2.10 -6 0 0 185.38 5.20 -6 0 0 187.78 4.70 -6 0 0 183.38 5.00 -6 0 0 189.38 4.70 6 0 0 195.68 4.70 6 0 0 189.58 4.50 6 0 0 186.78 4.70 -7 0 0 48.70 2.30 -7 0 0 48.60 2.00 -7 0 0 51.29 1.80 -7 0 0 49.50 1.70 7 0 0 52.39 1.70 7 0 0 50.39 1.60 7 0 0 51.09 1.70 -8 0 0 113.09 3.20 -8 0 0 111.09 3.20 -8 0 0 113.39 3.90 8 0 0 108.79 3.00 8 0 0 112.59 3.20 8 0 0 110.29 3.20 -9 0 0 -1.60 0.60 -9 0 0 0.40 0.70 -9 0 0 1.70 1.20 9 0 0 -0.40 0.70 9 0 0 0.60 0.60 -10 0 0 0.20 0.70 -10 0 0 1.10 1.20 -10 0 0 -0.10 0.80 10 0 0 0.40 0.70 -11 0 0 7.90 1.20 -11 0 0 10.70 1.90 -11 0 0 6.20 1.00 11 0 0 6.60 1.00 -12 0 0 6.50 1.10 -12 0 0 5.70 1.20 -12 0 0 5.30 1.60 12 0 0 7.70 1.20 12 -1 0 1.30 0.90 -12 1 0 3.20 1.80 -12 1 0 -0.10 1.10 -12 1 0 1.90 1.00 11 -1 0 4.00 0.90 -11 1 0 1.80 0.90 -11 1 0 1.60 1.30 -11 1 0 1.40 1.00 10 -1 0 5.50 0.90 -10 1 0 8.50 1.70 -10 1 0 7.00 1.00 -10 1 0 7.60 1.10 9 -1 0 21.70 1.40 -9 1 0 24.10 2.10 -9 1 0 24.00 1.60 -9 1 0 19.00 1.80 -9 1 0 23.00 1.50 8 -1 0 -0.10 0.50 8 -1 0 -0.40 0.50 -8 1 0 0.00 1.00 -8 1 0 -0.50 0.50 -8 1 0 0.60 0.80 -8 1 0 0.40 0.60 7 -1 0 7.50 0.70 7 -1 0 9.00 0.80 7 -1 0 7.80 0.60 -7 1 0 8.10 0.80 -7 1 0 8.60 0.80 -7 1 0 10.30 1.30 -7 1 0 8.20 1.10 6 -1 0 7.40 0.60 6 -1 0 7.40 0.60 6 -1 0 8.50 0.70 -6 1 0 8.10 1.10 -6 1 0 7.50 0.70 -6 1 0 6.90 0.60 -6 1 0 8.90 1.00 5 -1 0 1.40 0.40 5 -1 0 0.30 0.30 5 -1 0 0.90 0.40 -5 1 0 0.50 0.40 -5 1 0 0.10 0.50 -5 1 0 0.30 0.40 -5 1 0 -0.10 0.70 4 -1 0 161.88 3.90 4 -1 0 155.28 3.80 4 -1 0 158.28 3.70 -4 1 0 156.78 3.90 -4 1 0 162.68 4.20 -4 1 0 155.38 3.90 -4 1 0 152.48 4.30 3 -1 0 1.10 0.20 3 -1 0 1.10 0.20 3 -1 0 0.60 0.30 3 -1 0 1.10 0.30 -3 1 0 1.20 0.20 -3 1 0 0.40 0.30 -3 1 0 0.80 0.30 -3 1 0 1.10 0.20 -3 1 0 0.00 0.20 -3 1 0 0.80 0.20 -3 1 0 0.50 0.50 -3 -1 0 155.18 3.90 -3 -1 0 152.38 3.60 3 1 0 154.28 3.60 3 1 0 156.78 3.70 3 1 0 156.78 3.80 3 1 0 155.38 3.70 -4 -1 0 13.30 1.00 -4 -1 0 12.60 0.70 -4 -1 0 10.80 0.50 -4 -1 0 14.60 0.70 4 1 0 12.40 0.50 4 1 0 9.50 0.60 4 1 0 12.00 0.80 4 1 0 12.80 0.50 4 1 0 12.60 0.70 -5 -1 0 50.29 1.50 -5 -1 0 48.40 1.50 -5 -1 0 46.50 1.30 -5 -1 0 45.90 1.90 5 1 0 49.30 1.40 5 1 0 47.90 1.50 5 1 0 49.00 1.70 5 1 0 49.50 1.50 5 1 0 49.20 1.50 -6 -1 0 226.88 5.50 -6 -1 0 226.88 5.60 -6 -1 0 220.98 6.00 6 1 0 233.38 5.80 6 1 0 226.98 5.50 6 1 0 221.98 5.50 6 1 0 229.78 5.40 -7 -1 0 101.19 2.80 -7 -1 0 95.99 3.30 -7 -1 0 98.49 2.80 7 1 0 101.29 2.80 7 1 0 99.09 2.80 7 1 0 101.19 2.70 -8 -1 0 2.20 0.60 -8 -1 0 2.60 0.60 -8 -1 0 0.40 0.90 8 1 0 2.50 0.50 8 1 0 2.80 0.60 8 1 0 3.20 0.60 -9 -1 0 122.09 4.40 -9 -1 0 129.89 3.70 -9 -1 0 129.29 3.70 9 1 0 126.69 3.60 9 1 0 125.99 3.60 -10 -1 0 43.60 2.70 -10 -1 0 46.30 2.10 -10 -1 0 50.69 2.20 10 1 0 45.70 2.00 -11 -1 0 0.20 1.20 -11 -1 0 0.30 0.70 -11 -1 0 -0.50 0.80 11 1 0 0.30 0.80 -12 -1 0 8.20 1.30 -12 -1 0 8.20 1.20 -12 -1 0 9.80 1.90 12 1 0 11.30 1.30 -13 -1 0 13.40 2.30 -13 -1 0 11.40 1.60 13 1 0 12.50 1.50 11 -2 0 2.20 0.90 -11 2 0 1.20 0.80 -11 2 0 2.10 1.10 -11 2 0 2.20 1.50 -11 2 0 2.30 1.20 10 -2 0 3.00 0.80 -10 2 0 2.70 1.10 -10 2 0 1.70 0.90 -10 2 0 2.50 0.80 -10 2 0 2.90 1.30 9 -2 0 8.50 1.00 -9 2 0 6.60 1.10 -9 2 0 6.60 1.20 -9 2 0 9.10 1.60 -9 2 0 9.50 1.00 8 -2 0 2.90 0.90 8 -2 0 3.80 0.70 -8 2 0 5.00 0.80 -8 2 0 3.60 1.00 -8 2 0 4.20 0.90 -8 2 0 3.10 1.20 7 -2 0 2.30 0.60 7 -2 0 2.00 0.60 -7 2 0 3.30 0.70 -7 2 0 2.00 0.60 -7 2 0 0.60 0.80 -7 2 0 1.70 1.00 6 -2 0 12.90 0.90 6 -2 0 11.80 0.90 -6 2 0 12.90 1.10 -6 2 0 11.20 0.90 -6 2 0 12.60 1.40 -6 2 0 12.10 1.20 5 -2 0 1.80 0.40 5 -2 0 2.60 0.50 -5 2 0 2.00 0.50 -5 2 0 2.30 0.50 -5 2 0 1.60 0.70 -5 2 0 2.60 0.70 4 -2 0 682.83 15.60 4 -2 0 675.83 15.60 -4 2 0 676.23 16.00 -4 2 0 680.93 15.60 -4 2 0 685.23 15.60 -4 2 0 676.93 16.00 3 -2 0 742.03 17.10 3 -2 0 765.62 17.10 -3 2 0 742.03 17.10 -3 2 0 753.12 17.10 -3 2 0 747.23 17.00 -3 2 0 749.23 17.40 2 -2 0 39.80 1.10 2 -2 0 41.00 1.20 2 -2 0 40.80 1.10 -2 2 0 39.70 1.40 -2 2 0 35.00 1.20 -2 2 0 39.30 1.10 -1 2 0 1294.57 29.50 -3 -2 0 150.78 3.70 -3 -2 0 148.09 3.60 -3 -2 0 136.39 3.60 -3 -2 0 146.09 3.50 3 2 0 149.29 3.60 3 2 0 148.19 3.50 3 2 0 147.09 3.60 3 2 0 152.58 3.60 -4 -2 0 26.90 1.20 -4 -2 0 25.70 1.00 -4 -2 0 24.90 0.90 -4 -2 0 26.70 1.00 -4 -2 0 24.80 1.00 4 2 0 27.00 0.90 4 2 0 26.40 0.90 4 2 0 27.50 1.00 4 2 0 25.60 0.90 -5 -2 0 32.00 1.50 -5 -2 0 33.00 1.20 -5 -2 0 33.90 1.10 -5 -2 0 32.10 1.20 -5 -2 0 34.40 1.10 5 2 0 33.90 1.10 5 2 0 35.70 1.20 5 2 0 34.00 1.30 5 2 0 32.80 1.20 -6 -2 0 3.50 0.50 -6 -2 0 3.60 0.40 -6 -2 0 3.30 0.50 -6 -2 0 3.00 0.80 6 2 0 3.90 0.50 6 2 0 4.10 0.50 6 2 0 3.10 0.40 6 2 0 3.80 0.60 -7 -2 0 19.20 1.10 -7 -2 0 17.40 0.70 -7 -2 0 19.40 1.50 -7 -2 0 18.20 1.10 7 2 0 17.90 1.00 7 2 0 16.10 1.00 7 2 0 18.00 1.00 7 2 0 17.40 0.90 -8 -2 0 49.99 1.80 -8 -2 0 47.90 1.90 -8 -2 0 47.80 2.30 8 2 0 47.50 1.80 8 2 0 47.60 1.70 8 2 0 48.20 1.80 -9 -2 0 1.70 0.70 -9 -2 0 0.90 1.10 -9 -2 0 1.60 0.70 9 2 0 2.60 0.70 9 2 0 2.20 0.60 9 2 0 1.60 0.70 -10 -2 0 -1.00 1.10 -10 -2 0 0.20 0.70 -10 -2 0 -0.70 0.70 10 2 0 -0.40 0.70 -11 -2 0 8.90 1.10 -11 -2 0 6.80 1.50 -11 -2 0 6.70 1.10 11 2 0 8.10 1.10 -12 -2 0 2.80 1.40 -12 -2 0 0.20 0.80 -12 -2 0 0.60 0.90 12 2 0 1.50 0.90 -13 -2 0 -0.60 1.50 -13 -2 0 -1.00 1.00 13 2 0 1.40 1.00 11 -3 0 0.20 0.80 -11 3 0 0.90 1.20 -11 3 0 -1.10 1.00 -11 3 0 -0.20 1.40 -11 3 0 1.00 0.90 10 -3 0 11.60 1.30 -10 3 0 10.30 1.80 -10 3 0 12.70 1.70 -10 3 0 10.80 1.40 -10 3 0 10.20 1.20 9 -3 0 16.60 1.30 -9 3 0 16.70 1.80 -9 3 0 15.60 1.30 -9 3 0 18.30 1.50 -9 3 0 13.90 1.90 8 -3 0 0.60 0.60 -8 3 0 0.20 1.00 -8 3 0 -0.70 0.80 -8 3 0 0.60 0.60 -8 3 0 -0.30 0.80 7 -3 0 15.80 1.20 7 -3 0 17.10 1.20 -7 3 0 19.80 1.50 -7 3 0 16.70 1.70 -7 3 0 17.40 1.70 -7 3 0 19.40 1.30 6 -3 0 70.99 2.30 6 -3 0 71.79 2.30 -6 3 0 63.69 2.80 -6 3 0 71.49 2.30 -6 3 0 66.19 2.80 -6 3 0 71.59 2.40 5 -3 0 10.50 0.90 5 -3 0 10.50 0.90 -5 3 0 12.40 1.20 -5 3 0 11.80 0.90 -5 3 0 9.70 1.10 -5 3 0 11.70 0.90 4 -3 0 74.39 2.10 4 -3 0 74.69 2.20 -4 3 0 73.29 1.80 -4 3 0 76.59 2.60 -4 3 0 71.39 2.10 -4 3 0 71.59 2.50 -4 3 0 74.59 2.20 -4 3 0 62.09 1.80 3 -3 0 501.85 11.90 3 -3 0 507.45 11.90 -3 3 0 527.35 11.90 -3 3 0 520.55 12.00 -3 3 0 509.35 11.70 -3 3 0 514.75 12.10 2 -3 0 1.40 0.40 2 -3 0 2.40 0.40 2 -3 0 1.90 0.40 -2 3 0 1.70 0.50 -2 3 0 2.30 0.40 -2 3 0 2.10 0.50 -2 3 0 1.20 0.40 -2 3 0 2.40 0.40 1 -3 0 77.29 2.10 1 -3 0 76.29 2.10 1 -3 0 77.79 2.10 -1 3 0 75.49 2.10 -1 3 0 78.79 2.10 -1 3 0 76.59 2.10 -1 3 0 78.29 2.10 -1 3 0 76.09 2.20 -1 3 0 75.99 1.90 -1 3 0 78.89 2.10 0 -3 0 79.29 2.20 0 -3 0 83.59 2.20 0 -3 0 81.59 2.20 0 3 0 82.79 2.10 0 3 0 81.39 2.30 0 3 0 83.89 2.20 0 3 0 82.59 2.20 0 3 0 81.69 2.30 -2 -3 0 350.26 8.20 -2 -3 0 358.26 8.20 -2 -3 0 352.86 8.20 2 3 0 349.57 8.30 2 3 0 354.86 8.20 2 3 0 348.67 8.20 2 3 0 347.67 8.20 2 3 0 354.26 8.20 -3 -3 0 613.24 14.00 -3 -3 0 598.54 13.90 -3 -3 0 601.34 13.80 -3 -3 0 594.34 13.90 -3 -3 0 596.14 13.90 -3 -3 0 601.34 13.80 3 3 0 600.54 13.80 3 3 0 604.64 13.80 3 3 0 604.94 13.80 3 3 0 608.54 13.90 -4 -3 0 18.70 0.80 -4 -3 0 20.70 1.00 -4 -3 0 19.60 0.80 -4 -3 0 17.70 0.90 -4 -3 0 19.20 0.90 -4 -3 0 17.80 1.00 4 3 0 19.70 0.90 4 3 0 16.60 0.90 4 3 0 17.90 0.90 4 3 0 19.10 0.90 4 3 0 19.80 1.00 -5 -3 0 29.70 1.10 -5 -3 0 27.10 1.40 -5 -3 0 28.60 1.10 -5 -3 0 27.50 1.20 -5 -3 0 29.00 0.90 -5 -3 0 28.40 1.20 5 3 0 28.70 1.10 5 3 0 27.90 1.20 5 3 0 29.60 1.20 5 3 0 29.50 1.10 -6 -3 0 158.38 4.10 -6 -3 0 153.58 4.30 -6 -3 0 152.28 3.80 -6 -3 0 152.48 4.10 -6 -3 0 153.98 3.90 6 3 0 152.28 4.00 6 3 0 154.18 4.00 6 3 0 157.68 3.90 -7 -3 0 49.60 1.60 -7 -3 0 53.69 1.90 -7 -3 0 55.19 1.60 -7 -3 0 54.39 2.20 -7 -3 0 53.39 1.90 7 3 0 54.19 1.90 7 3 0 52.79 1.80 7 3 0 54.09 1.80 -8 -3 0 5.70 1.10 -8 -3 0 7.40 0.90 -8 -3 0 5.60 0.80 -8 -3 0 6.10 0.50 8 3 0 5.70 0.70 8 3 0 5.70 0.70 8 3 0 5.40 0.80 8 3 0 6.60 0.80 -9 -3 0 1.10 1.00 -9 -3 0 0.30 0.60 -9 -3 0 -0.90 0.60 9 3 0 1.00 0.60 9 3 0 -0.70 0.60 -10 -3 0 6.20 1.00 -10 -3 0 5.10 1.00 -10 -3 0 5.30 1.30 10 3 0 6.40 1.00 -11 -3 0 3.70 1.40 -11 -3 0 4.80 1.00 -11 -3 0 3.90 1.00 11 3 0 4.10 1.00 -12 -3 0 15.10 1.50 -12 -3 0 14.20 2.00 -12 -3 0 13.80 1.50 12 3 0 16.60 1.60 -13 -3 0 1.70 1.70 -13 -3 0 -0.80 1.00 13 3 0 0.50 0.90 10 -4 0 7.00 1.20 -10 4 0 9.70 1.40 -10 4 0 9.40 1.20 -10 4 0 9.80 1.70 -10 4 0 11.40 2.10 9 -4 0 0.60 0.70 -9 4 0 -1.20 1.20 -9 4 0 0.30 1.10 -9 4 0 -1.20 0.90 -9 4 0 -0.20 0.70 8 -4 0 30.80 1.70 -8 4 0 29.50 1.70 -8 4 0 28.70 2.00 -8 4 0 30.50 2.40 -8 4 0 26.70 2.30 7 -4 0 20.30 1.50 -7 4 0 21.40 1.50 -7 4 0 24.90 2.10 -7 4 0 19.60 1.70 -7 4 0 25.20 2.10 6 -4 0 338.07 8.50 6 -4 0 340.27 8.40 -6 4 0 344.87 8.60 -6 4 0 342.67 9.10 -6 4 0 344.47 8.50 -6 4 0 346.37 9.00 5 -4 0 86.29 2.60 5 -4 0 80.79 2.60 -5 4 0 80.49 2.70 -5 4 0 83.29 3.20 -5 4 0 84.49 3.00 -5 4 0 83.49 2.60 4 -4 0 130.49 3.60 4 -4 0 136.89 3.60 -4 4 0 134.19 3.70 -4 4 0 135.59 3.90 -4 4 0 135.59 3.60 -4 4 0 132.69 3.30 3 -4 0 0.30 0.40 3 -4 0 0.60 0.40 -3 4 0 0.50 0.30 -3 4 0 -0.30 0.50 -3 4 0 0.00 0.40 -3 4 0 0.90 0.60 -3 4 0 0.30 0.50 -3 4 0 0.60 0.40 2 -4 0 208.78 5.30 2 -4 0 216.18 5.40 -2 4 0 217.28 5.40 -2 4 0 213.28 5.20 -2 4 0 216.68 5.40 -2 4 0 217.38 5.30 -2 4 0 215.98 5.50 -2 4 0 220.68 5.40 1 -4 0 512.05 11.80 1 -4 0 502.55 11.80 1 -4 0 515.55 11.80 -1 4 0 506.45 11.80 -1 4 0 504.35 11.60 -1 4 0 497.35 11.70 -1 4 0 512.15 11.90 -1 4 0 501.95 11.80 -1 4 0 508.95 11.80 -1 4 0 505.05 11.70 0 -4 0 39.30 1.40 0 -4 0 40.10 1.40 0 -4 0 38.30 1.40 0 -4 0 40.10 1.40 0 -4 0 39.20 1.40 0 4 0 41.10 1.50 0 4 0 40.10 1.30 0 4 0 39.90 1.40 0 4 0 41.60 1.50 0 4 0 40.60 1.40 0 4 0 41.30 1.50 -1 -4 0 309.67 7.20 -1 -4 0 304.17 7.20 -1 -4 0 301.77 7.20 -1 -4 0 299.97 7.30 -1 -4 0 303.97 7.20 1 4 0 298.07 7.20 1 4 0 305.87 7.20 1 4 0 302.37 7.30 1 4 0 295.17 7.10 1 4 0 296.67 7.30 1 4 0 310.47 7.30 -2 -4 0 0.80 0.40 -2 -4 0 0.70 0.40 -2 -4 0 0.80 0.40 -2 -4 0 0.40 0.40 -2 -4 0 1.00 0.40 -2 -4 0 0.20 0.30 2 4 0 0.30 0.40 2 4 0 -0.10 0.30 2 4 0 0.20 0.40 2 4 0 0.20 0.40 2 4 0 1.10 0.40 2 4 0 0.20 0.20 -3 -4 0 148.99 3.60 -3 -4 0 143.79 3.70 -3 -4 0 137.39 3.70 -3 -4 0 125.59 3.70 -3 -4 0 148.59 3.80 -3 -4 0 143.09 3.70 3 4 0 142.39 3.70 3 4 0 143.69 3.70 3 4 0 144.99 3.70 3 4 0 145.59 3.70 3 4 0 148.79 3.70 -4 -4 0 60.99 1.90 -4 -4 0 58.29 1.90 -4 -4 0 57.89 2.00 -4 -4 0 63.19 2.10 -4 -4 0 58.49 1.80 -4 -4 0 58.39 1.90 -4 -4 0 59.59 1.90 4 4 0 59.29 1.90 4 4 0 61.29 1.90 4 4 0 60.59 1.90 4 4 0 61.69 1.90 4 4 0 60.39 1.90 -5 -4 0 38.30 1.50 -5 -4 0 35.80 1.50 -5 -4 0 37.10 1.20 -5 -4 0 37.60 1.50 -5 -4 0 35.50 1.50 -5 -4 0 40.20 1.50 -5 -4 0 36.90 1.30 5 4 0 40.30 1.50 5 4 0 38.00 1.40 5 4 0 34.80 1.50 5 4 0 39.40 1.40 -6 -4 0 4.50 0.40 -6 -4 0 3.50 0.80 -6 -4 0 5.00 0.60 -6 -4 0 5.40 0.70 -6 -4 0 4.20 0.60 6 4 0 4.60 0.60 6 4 0 5.20 0.60 6 4 0 4.40 0.70 -7 -4 0 103.89 2.90 -7 -4 0 105.39 3.40 -7 -4 0 108.19 3.10 -7 -4 0 105.49 3.10 7 4 0 102.89 3.10 7 4 0 109.39 3.00 7 4 0 109.29 3.10 -8 -4 0 30.10 2.00 -8 -4 0 30.10 1.30 -8 -4 0 31.00 1.60 -8 -4 0 33.00 1.70 8 4 0 32.60 1.50 8 4 0 28.30 1.60 -9 -4 0 4.00 1.20 -9 -4 0 3.70 0.60 -9 -4 0 4.80 0.90 -9 -4 0 2.80 0.80 9 4 0 4.20 0.90 9 4 0 4.80 0.80 -10 -4 0 7.10 1.10 -10 -4 0 5.70 1.10 -10 -4 0 6.50 1.30 10 4 0 6.30 1.10 -11 -4 0 0.70 0.90 -11 -4 0 2.00 0.90 -11 -4 0 1.70 1.30 11 4 0 1.60 0.90 -12 -4 0 31.30 2.70 -12 -4 0 30.50 2.10 -12 -4 0 31.30 2.20 12 4 0 31.80 2.10 -13 -4 0 -0.30 1.00 -13 -4 0 -0.10 1.50 13 4 0 0.20 1.00 10 -5 0 0.00 0.90 -10 5 0 0.80 1.30 -10 5 0 -0.10 1.40 -10 5 0 0.40 1.00 9 -5 0 0.10 0.80 -9 5 0 1.80 1.00 -9 5 0 1.60 1.30 -9 5 0 1.70 0.90 -9 5 0 4.50 1.40 -9 5 0 2.00 0.80 8 -5 0 4.00 0.90 -8 5 0 3.80 0.90 -8 5 0 1.70 1.20 -8 5 0 1.60 0.90 -8 5 0 2.10 1.30 -8 5 0 2.50 0.80 7 -5 0 1.00 0.70 -7 5 0 0.70 0.70 -7 5 0 1.20 1.20 -7 5 0 -0.40 1.10 -7 5 0 0.30 0.80 -7 5 0 0.40 0.70 6 -5 0 51.49 2.10 -6 5 0 50.09 2.20 -6 5 0 51.69 2.60 -6 5 0 49.80 2.10 -6 5 0 53.59 2.30 -6 5 0 55.29 2.90 5 -5 0 128.89 3.90 -5 5 0 139.79 4.20 -5 5 0 136.59 4.60 -5 5 0 135.79 4.00 -5 5 0 137.69 3.90 -5 5 0 134.09 4.00 4 -5 0 16.40 1.20 4 -5 0 18.20 1.30 -4 5 0 16.00 1.30 -4 5 0 18.90 1.40 -4 5 0 14.60 0.80 -4 5 0 17.20 1.20 -4 5 0 15.80 1.30 3 -5 0 40.30 1.60 3 -5 0 40.10 1.60 -3 5 0 40.20 1.70 -3 5 0 38.50 1.40 -3 5 0 39.30 1.70 -3 5 0 40.10 1.60 -3 5 0 40.10 1.70 2 -5 0 11.70 0.90 2 -5 0 11.80 0.90 -2 5 0 11.60 0.90 -2 5 0 11.30 0.90 -2 5 0 10.70 0.90 -2 5 0 8.50 0.80 -2 5 0 10.20 0.90 1 -5 0 218.98 5.70 1 -5 0 218.28 5.70 1 -5 0 230.48 5.60 -1 5 0 231.78 5.80 -1 5 0 225.88 5.70 -1 5 0 227.48 5.60 -1 5 0 231.98 5.40 -1 5 0 226.18 5.70 0 -5 0 458.95 11.00 0 -5 0 475.55 10.90 0 -5 0 453.85 10.90 0 5 0 461.15 11.00 0 5 0 458.05 10.80 0 5 0 473.45 11.00 0 5 0 466.35 10.90 0 5 0 457.15 11.10 -1 -5 0 113.29 3.20 -1 -5 0 112.19 3.10 -1 -5 0 108.29 3.10 -1 -5 0 113.69 3.10 -1 -5 0 115.39 3.10 1 5 0 110.99 3.10 1 5 0 112.09 3.30 1 5 0 114.39 3.30 1 5 0 113.99 3.20 1 5 0 116.09 3.20 1 5 0 112.09 3.00 -2 -5 0 -0.40 0.40 -2 -5 0 -0.50 0.40 -2 -5 0 0.30 0.40 -2 -5 0 0.50 0.40 -2 -5 0 -0.10 0.50 -2 -5 0 -0.40 0.40 2 5 0 0.50 0.50 2 5 0 0.10 0.40 2 5 0 0.20 0.40 2 5 0 0.20 0.40 2 5 0 0.00 0.20 2 5 0 0.60 0.50 -3 -5 0 587.84 13.80 -3 -5 0 578.44 13.70 -3 -5 0 579.94 13.70 -3 -5 0 595.84 13.60 3 5 0 569.04 13.70 3 5 0 591.54 13.70 3 5 0 585.84 13.70 3 5 0 615.44 13.90 3 5 0 574.54 13.80 3 5 0 563.74 13.60 -4 -5 0 808.72 18.60 -4 -5 0 782.82 18.50 -4 -5 0 803.92 18.70 -4 -5 0 801.02 18.60 -4 -5 0 813.02 18.50 -4 -5 0 812.92 18.40 4 5 0 806.32 18.50 4 5 0 797.02 18.50 4 5 0 786.82 18.50 4 5 0 792.62 18.50 -5 -5 0 210.28 5.40 -5 -5 0 209.78 5.30 -5 -5 0 206.58 5.40 -5 -5 0 201.98 5.30 -5 -5 0 206.88 5.20 5 5 0 208.78 5.20 5 5 0 198.88 5.30 5 5 0 204.08 5.20 -6 -5 0 70.49 2.20 -6 -5 0 68.59 2.00 -6 -5 0 66.49 2.40 -6 -5 0 68.19 2.30 -6 -5 0 64.29 2.20 -6 -5 0 66.79 2.30 6 5 0 66.09 2.30 6 5 0 65.59 2.20 6 5 0 66.69 2.10 -7 -5 0 58.19 2.20 -7 -5 0 60.69 2.30 -7 -5 0 59.49 2.20 -7 -5 0 60.89 2.30 -7 -5 0 60.89 2.10 7 5 0 60.89 2.20 7 5 0 58.39 2.10 -8 -5 0 25.70 1.60 -8 -5 0 25.70 1.30 -8 -5 0 23.20 1.50 -8 -5 0 22.70 1.80 -8 -5 0 22.30 1.50 8 5 0 24.10 1.40 8 5 0 23.30 1.50 -9 -5 0 288.17 8.10 -9 -5 0 328.07 7.70 -9 -5 0 319.87 8.10 -9 -5 0 318.67 8.10 -9 -5 0 324.67 8.40 9 5 0 323.17 8.10 9 5 0 305.77 7.90 -10 -5 0 1.60 0.90 -10 -5 0 0.20 1.20 -10 -5 0 -0.50 0.50 -10 -5 0 0.10 0.70 -10 -5 0 0.30 0.70 10 5 0 -0.40 0.80 -11 -5 0 20.90 1.70 -11 -5 0 18.80 1.50 -11 -5 0 18.50 2.00 11 5 0 20.30 1.70 -12 -5 0 27.70 2.60 -12 -5 0 24.90 2.10 12 5 0 27.10 2.10 -13 -5 0 -1.20 1.00 -13 -5 0 -2.90 1.70 13 5 0 -1.30 1.00 9 -6 0 1.70 1.00 -9 6 0 1.20 1.40 -9 6 0 2.50 1.40 -9 6 0 3.90 1.20 8 -6 0 2.10 0.90 -8 6 0 2.00 0.80 -8 6 0 2.90 1.30 -8 6 0 5.60 1.60 -8 6 0 2.30 1.00 -8 6 0 3.30 1.10 7 -6 0 1.80 0.80 -7 6 0 3.80 1.30 -7 6 0 4.20 0.90 -7 6 0 2.70 0.90 -7 6 0 1.10 0.90 -7 6 0 2.30 1.30 6 -6 0 1.10 0.70 -6 6 0 0.70 0.70 -6 6 0 1.30 1.20 -6 6 0 0.20 0.70 -6 6 0 1.50 0.80 -6 6 0 0.20 1.00 5 -6 0 5.80 0.90 -5 6 0 6.10 1.00 -5 6 0 7.70 1.20 -5 6 0 7.00 1.10 -5 6 0 5.70 1.50 -5 6 0 6.80 1.00 4 -6 0 1.80 0.70 -4 6 0 2.70 0.70 -4 6 0 3.20 0.80 -4 6 0 2.70 0.80 -4 6 0 2.00 0.80 -4 6 0 1.90 0.50 3 -6 0 35.20 1.70 -3 6 0 34.80 1.80 -3 6 0 34.20 1.50 -3 6 0 40.20 1.90 -3 6 0 33.50 1.70 -3 6 0 36.00 1.70 2 -6 0 1.90 0.70 -2 6 0 1.20 0.60 -2 6 0 1.80 0.70 -2 6 0 1.30 0.60 -2 6 0 1.70 0.70 -2 6 0 1.90 0.60 1 -6 0 4.40 0.70 -1 6 0 6.10 0.70 -1 6 0 6.50 0.90 -1 6 0 4.20 0.70 -1 6 0 4.90 0.70 -1 6 0 4.30 0.50 0 -6 0 359.06 8.70 0 -6 0 366.46 8.80 0 6 0 351.16 8.50 0 6 0 363.26 8.80 0 6 0 362.06 8.70 0 6 0 361.16 9.00 0 6 0 360.86 8.80 -1 -6 0 9.30 0.90 -1 -6 0 9.10 0.90 -1 -6 0 7.30 0.80 1 6 0 8.20 0.70 1 6 0 8.90 0.90 1 6 0 9.40 0.90 1 6 0 7.40 0.80 1 6 0 6.50 0.80 -2 -6 0 265.47 6.70 -2 -6 0 273.17 6.90 -2 -6 0 271.67 6.80 -2 -6 0 268.67 6.80 2 6 0 268.77 6.80 2 6 0 266.17 6.60 2 6 0 271.87 6.70 2 6 0 268.37 6.90 2 6 0 274.87 6.80 -3 -6 0 2.30 0.60 -3 -6 0 1.00 0.60 -3 -6 0 2.30 0.60 -3 -6 0 1.00 0.50 -3 -6 0 1.00 0.40 -3 -6 0 1.80 0.60 3 6 0 1.30 0.60 3 6 0 1.90 0.60 3 6 0 1.30 0.50 3 6 0 1.40 0.60 3 6 0 0.50 0.30 -4 -6 0 8.30 0.80 -4 -6 0 7.60 0.70 -4 -6 0 7.90 0.80 -4 -6 0 7.20 0.80 -4 -6 0 6.10 0.80 -4 -6 0 9.60 1.00 4 6 0 8.20 0.80 4 6 0 7.50 0.80 4 6 0 6.50 0.70 4 6 0 9.90 0.90 -5 -6 0 16.10 1.20 -5 -6 0 13.20 0.90 -5 -6 0 15.70 1.20 -5 -6 0 14.60 1.20 -5 -6 0 16.30 1.20 -5 -6 0 16.70 1.20 5 6 0 14.80 1.10 5 6 0 14.80 1.20 5 6 0 14.20 1.10 -6 -6 0 60.99 1.90 -6 -6 0 61.19 2.30 -6 -6 0 58.89 2.20 -6 -6 0 59.29 2.10 -6 -6 0 62.09 2.10 -6 -6 0 61.49 2.30 6 6 0 56.09 2.20 6 6 0 62.69 2.20 6 6 0 57.39 2.00 -7 -6 0 62.79 2.40 -7 -6 0 57.59 2.20 -7 -6 0 55.79 2.30 -7 -6 0 58.69 2.10 -7 -6 0 59.99 2.20 -7 -6 0 58.19 1.80 7 6 0 56.89 2.30 7 6 0 60.19 2.20 -8 -6 0 2.10 0.70 -8 -6 0 3.30 1.00 -8 -6 0 1.90 0.80 -8 -6 0 2.30 0.80 -8 -6 0 2.80 0.80 8 6 0 4.60 0.90 8 6 0 3.50 0.80 -9 -6 0 3.60 0.90 -9 -6 0 3.50 1.00 -9 -6 0 5.40 0.80 -9 -6 0 2.60 0.90 -9 -6 0 2.10 1.20 9 6 0 2.90 0.80 9 6 0 3.30 1.00 -10 -6 0 -0.60 0.80 -10 -6 0 0.30 0.60 -10 -6 0 -2.10 1.10 -10 -6 0 -0.60 0.80 10 6 0 -1.60 0.80 10 6 0 -0.50 0.80 -11 -6 0 0.50 1.30 -11 -6 0 0.80 0.90 11 6 0 1.50 1.00 -12 -6 0 10.30 1.90 -12 -6 0 11.10 1.50 12 6 0 11.30 1.50 -13 -6 0 16.50 1.80 -13 -6 0 15.70 2.40 13 6 0 14.40 1.70 8 -7 0 1.00 1.00 -8 7 0 0.30 1.10 -8 7 0 -1.00 1.30 -8 7 0 1.30 1.30 7 -7 0 3.00 1.00 -7 7 0 3.20 1.10 -7 7 0 3.70 1.50 -7 7 0 3.90 1.00 -7 7 0 2.30 1.30 6 -7 0 8.90 1.10 -6 7 0 8.70 1.70 -6 7 0 9.60 1.50 -6 7 0 8.10 1.20 -6 7 0 6.40 1.00 -6 7 0 6.10 1.10 5 -7 0 0.40 0.70 -5 7 0 2.40 0.90 -5 7 0 0.60 0.90 -5 7 0 0.40 0.80 -5 7 0 0.60 0.70 4 -7 0 40.70 2.00 -4 7 0 42.60 2.00 -4 7 0 39.80 2.10 -4 7 0 37.00 2.10 -4 7 0 35.30 2.00 3 -7 0 2.20 0.80 -3 7 0 1.60 0.80 -3 7 0 1.70 0.70 -3 7 0 3.00 0.70 -3 7 0 2.30 0.80 -3 7 0 2.90 0.80 2 -7 0 43.00 1.90 -2 7 0 40.70 2.00 -2 7 0 39.30 1.80 -2 7 0 41.70 2.00 -2 7 0 39.70 1.70 1 -7 0 5.20 0.90 -1 7 0 4.40 0.80 -1 7 0 6.50 0.90 -1 7 0 4.70 0.50 -1 7 0 5.90 0.90 -1 7 0 5.60 0.80 0 -7 0 -0.20 0.60 0 7 0 0.20 0.60 0 7 0 1.10 0.60 0 7 0 0.80 0.60 0 7 0 0.80 0.60 0 7 0 -0.40 0.40 -1 -7 0 10.30 1.00 -1 -7 0 14.00 1.20 -1 -7 0 11.30 1.00 -1 -7 0 10.60 1.10 1 7 0 10.90 1.00 1 7 0 11.00 1.00 1 7 0 12.60 1.20 1 7 0 11.80 1.10 1 7 0 9.20 0.80 -2 -7 0 161.18 4.50 -2 -7 0 157.48 4.60 -2 -7 0 163.28 4.40 -2 -7 0 159.48 4.40 2 7 0 159.68 4.30 2 7 0 157.48 4.50 2 7 0 162.98 4.40 2 7 0 167.38 4.70 2 7 0 160.48 4.50 -3 -7 0 7.20 0.80 -3 -7 0 8.40 1.00 -3 -7 0 9.90 0.90 -3 -7 0 10.10 1.00 -3 -7 0 7.40 0.90 3 7 0 6.20 0.90 3 7 0 9.60 1.00 3 7 0 7.50 0.90 3 7 0 7.60 0.80 -4 -7 0 0.00 0.10 -4 -7 0 0.10 0.60 -4 -7 0 0.50 0.60 -4 -7 0 0.30 0.50 -4 -7 0 0.00 0.20 -4 -7 0 0.00 0.50 4 7 0 0.90 0.50 4 7 0 1.20 0.60 4 7 0 0.20 0.50 4 7 0 0.30 0.60 -5 -7 0 3.90 0.80 -5 -7 0 4.20 0.80 -5 -7 0 5.50 0.70 -5 -7 0 5.10 0.90 -5 -7 0 5.30 0.90 -5 -7 0 4.30 0.80 5 7 0 5.00 0.90 5 7 0 4.70 0.70 5 7 0 4.80 0.80 -6 -7 0 15.10 1.20 -6 -7 0 17.00 1.40 -6 -7 0 14.80 1.20 -6 -7 0 12.50 1.20 6 7 0 13.80 1.10 6 7 0 18.00 1.40 -7 -7 0 62.89 2.40 -7 -7 0 61.99 2.00 -7 -7 0 59.49 2.50 -7 -7 0 61.19 2.30 -7 -7 0 58.09 2.30 -7 -7 0 60.59 2.50 7 7 0 61.89 2.40 7 7 0 56.69 2.40 -8 -7 0 4.40 1.00 -8 -7 0 6.40 0.90 -8 -7 0 6.10 1.00 -8 -7 0 4.70 0.90 -8 -7 0 7.80 1.10 8 7 0 4.70 0.90 8 7 0 7.50 1.10 -9 -7 0 24.20 2.00 -9 -7 0 27.10 2.00 -9 -7 0 24.50 1.90 -9 -7 0 28.10 1.90 -9 -7 0 26.30 1.60 9 7 0 29.30 1.80 9 7 0 26.40 1.90 -10 -7 0 14.60 1.50 -10 -7 0 18.20 1.80 -10 -7 0 16.80 1.30 10 7 0 15.20 1.50 10 7 0 13.80 1.30 -11 -7 0 1.50 1.30 -11 -7 0 0.10 0.90 11 7 0 0.10 1.00 -12 -7 0 5.10 1.70 -12 -7 0 6.00 1.40 12 7 0 5.90 1.40 -13 -7 0 17.00 2.50 -13 -7 0 17.10 1.80 13 7 0 13.10 1.80 7 -8 0 9.20 1.40 -7 8 0 10.70 2.10 -7 8 0 9.20 1.50 -7 8 0 10.30 1.70 6 -8 0 8.10 1.30 -6 8 0 3.80 1.60 -6 8 0 5.00 1.30 -6 8 0 4.80 1.20 -6 8 0 7.20 1.20 5 -8 0 4.90 1.10 -5 8 0 6.10 1.20 -5 8 0 4.50 1.00 -5 8 0 4.60 1.10 4 -8 0 10.40 1.20 -4 8 0 9.70 1.20 -4 8 0 10.20 1.30 -4 8 0 10.80 1.30 -4 8 0 11.00 1.30 3 -8 0 -1.00 0.70 -3 8 0 -0.30 0.70 -3 8 0 0.10 0.70 -3 8 0 -0.10 0.70 -3 8 0 -0.10 0.80 -3 8 0 1.10 0.70 2 -8 0 4.30 0.90 -2 8 0 3.60 1.00 -2 8 0 4.80 0.90 -2 8 0 4.40 1.00 -2 8 0 4.30 0.90 1 -8 0 133.59 4.20 -1 8 0 139.99 3.50 -1 8 0 139.29 4.40 -1 8 0 138.59 4.00 -1 8 0 138.29 4.30 -1 8 0 141.29 4.20 0 -8 0 25.30 1.70 0 8 0 26.00 1.80 0 8 0 28.60 1.40 0 8 0 31.00 1.70 0 8 0 29.60 1.90 0 8 0 26.50 1.60 -1 -8 0 29.00 1.70 -1 -8 0 30.80 1.80 -1 -8 0 32.90 1.60 1 8 0 33.30 1.60 1 8 0 35.60 1.90 1 8 0 33.70 1.70 1 8 0 34.00 1.80 1 8 0 34.60 2.00 -2 -8 0 156.28 4.40 -2 -8 0 147.39 4.50 -2 -8 0 155.48 4.40 2 8 0 158.68 4.80 2 8 0 153.88 4.50 2 8 0 155.78 4.30 2 8 0 156.98 4.50 2 8 0 156.58 4.50 -3 -8 0 77.49 2.90 -3 -8 0 82.09 2.80 -3 -8 0 83.39 2.90 -3 -8 0 77.79 2.80 3 8 0 75.69 2.80 3 8 0 77.79 2.70 3 8 0 80.69 2.80 3 8 0 80.29 3.00 3 8 0 75.39 2.70 -4 -8 0 0.90 0.70 -4 -8 0 -0.80 0.60 -4 -8 0 -0.10 0.60 -4 -8 0 0.70 0.70 -4 -8 0 1.20 0.70 4 8 0 -0.60 0.70 4 8 0 -0.20 0.60 4 8 0 0.00 0.60 4 8 0 0.30 0.70 -5 -8 0 44.50 2.10 -5 -8 0 42.40 1.80 -5 -8 0 42.50 2.10 -5 -8 0 43.70 2.10 5 8 0 44.60 2.00 5 8 0 45.20 2.10 5 8 0 47.20 2.20 -6 -8 0 24.00 1.70 -6 -8 0 20.90 1.60 -6 -8 0 24.60 1.40 -6 -8 0 21.90 1.70 -6 -8 0 23.20 1.70 6 8 0 21.90 1.80 6 8 0 18.90 1.60 6 8 0 18.70 1.50 -7 -8 0 38.40 1.70 -7 -8 0 43.10 2.20 -7 -8 0 42.00 2.20 -7 -8 0 46.50 2.30 -7 -8 0 48.40 2.20 7 8 0 44.30 2.30 7 8 0 47.90 2.20 -8 -8 0 34.00 1.50 -8 -8 0 33.50 2.10 -8 -8 0 35.20 1.90 -8 -8 0 32.90 1.80 -8 -8 0 31.80 2.10 8 8 0 36.30 2.20 8 8 0 37.20 2.00 -9 -8 0 12.70 1.30 -9 -8 0 14.30 1.50 -9 -8 0 15.10 1.50 9 8 0 13.60 1.30 9 8 0 11.80 1.50 -10 -8 0 7.80 1.10 -10 -8 0 10.90 1.50 -10 -8 0 8.20 1.40 10 8 0 8.70 1.40 10 8 0 6.40 1.10 -11 -8 0 -0.30 1.00 -11 -8 0 -0.30 1.10 11 8 0 -0.50 1.10 -12 -8 0 1.60 1.20 -12 -8 0 0.70 1.40 12 8 0 2.10 1.20 -13 -8 0 3.40 1.80 13 8 0 4.10 1.50 6 -9 0 -0.50 0.90 -6 9 0 -1.10 1.50 -6 9 0 0.00 1.10 5 -9 0 12.30 1.50 -5 9 0 11.20 1.50 -5 9 0 10.80 1.60 -5 9 0 14.10 2.30 4 -9 0 5.60 1.20 -4 9 0 6.90 1.30 -4 9 0 9.40 1.40 3 -9 0 1.20 0.90 -3 9 0 1.90 1.00 -3 9 0 0.80 0.90 2 -9 0 1.90 1.00 -2 9 0 1.10 0.80 -2 9 0 1.90 1.00 -2 9 0 2.60 1.00 1 -9 0 2.50 1.00 -1 9 0 0.70 0.80 -1 9 0 1.10 0.90 -1 9 0 1.40 0.90 0 -9 0 24.30 1.80 0 9 0 25.30 1.80 0 9 0 23.50 2.00 0 9 0 25.50 1.40 0 9 0 23.40 1.80 -1 -9 0 11.60 1.40 1 9 0 12.00 1.30 1 9 0 9.80 1.40 1 9 0 10.30 1.30 1 9 0 7.90 0.90 -2 -9 0 0.70 0.90 2 9 0 1.10 0.80 2 9 0 0.70 0.80 2 9 0 2.00 1.00 2 9 0 1.50 0.70 -3 -9 0 291.87 7.90 3 9 0 298.87 7.80 3 9 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5.60 1.20 1 10 0 5.90 1.30 1 10 0 5.40 0.90 1 10 0 8.00 1.20 -2 -10 0 -0.40 0.90 2 10 0 -0.40 0.90 2 10 0 -1.90 0.70 2 10 0 -1.40 0.90 -3 -10 0 0.30 0.90 3 10 0 -0.70 0.90 3 10 0 0.00 0.80 3 10 0 -0.90 0.80 -4 -10 0 2.30 1.00 4 10 0 2.10 1.00 4 10 0 2.80 0.90 -5 -10 0 9.40 1.30 5 10 0 7.10 1.20 5 10 0 6.70 1.10 -6 -10 0 44.00 2.50 6 10 0 41.50 2.40 6 10 0 47.60 2.50 -7 -10 0 1.40 1.00 7 10 0 3.40 1.10 7 10 0 1.80 1.00 -8 -10 0 1.00 0.90 8 10 0 0.30 0.90 8 10 0 2.40 1.10 -9 -10 0 0.70 0.90 9 10 0 -1.00 1.10 9 10 0 -0.50 0.90 -10 -10 0 0.40 0.90 10 10 0 -0.10 1.20 10 10 0 -0.60 1.00 11 10 0 6.70 1.60 11 10 0 3.60 1.50 12 10 0 8.00 1.70 3 -11 0 4.30 1.30 2 -11 0 0.00 1.10 -2 11 0 -0.20 1.10 1 -11 0 5.40 1.30 -1 11 0 7.90 1.40 0 -11 0 1.00 1.00 0 11 0 0.50 1.10 0 11 0 1.60 1.30 -1 -11 0 18.40 1.80 1 11 0 20.50 1.70 1 11 0 24.20 1.60 1 11 0 17.50 1.80 -2 -11 0 134.89 4.70 2 11 0 138.09 4.50 2 11 0 128.99 4.80 2 11 0 139.29 4.10 -3 -11 0 -1.80 1.00 3 11 0 -0.90 0.80 3 11 0 -1.20 0.90 -4 -11 0 -1.60 0.90 4 11 0 -0.30 0.90 4 11 0 0.40 0.80 -5 -11 0 -1.50 0.90 5 11 0 -1.30 0.90 5 11 0 -1.90 0.80 -6 -11 0 22.60 1.90 6 11 0 21.20 1.90 6 11 0 29.00 2.30 -7 -11 0 11.40 1.50 7 11 0 12.50 1.60 7 11 0 9.00 1.40 -8 -11 0 3.10 1.20 8 11 0 2.40 1.30 8 11 0 2.10 1.10 -9 -11 0 2.60 1.10 9 11 0 2.80 1.30 9 11 0 1.70 1.20 -10 -11 0 -0.10 1.00 10 11 0 -1.40 1.00 10 11 0 1.60 1.30 11 11 0 4.70 1.40 11 11 0 7.30 1.70 0 -12 0 1.10 1.20 0 12 0 5.40 1.40 -1 -12 0 0.30 1.20 1 12 0 1.70 1.20 -2 -12 0 41.60 2.70 2 12 0 38.70 2.80 2 12 0 41.20 2.20 2 12 0 42.50 2.50 -3 -12 0 52.79 3.00 3 12 0 45.90 2.70 3 12 0 50.89 2.60 -4 -12 0 0.50 1.20 4 12 0 -0.90 0.90 4 12 0 -0.40 1.00 -5 -12 0 0.30 1.10 5 12 0 0.50 1.00 5 12 0 3.00 1.20 -6 -12 0 2.60 1.20 6 12 0 3.20 1.20 6 12 0 1.20 1.20 -7 -12 0 3.20 1.30 7 12 0 3.20 1.30 7 12 0 1.70 1.10 -8 -12 0 2.40 1.30 8 12 0 3.40 1.20 8 12 0 4.80 1.40 -9 -12 0 -1.30 1.10 9 12 0 -1.20 1.10 9 12 0 -1.40 1.20 -10 -12 0 1.00 1.50 10 12 0 0.10 1.30 10 12 0 0.70 1.40 -3 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5.60 0.70 -7 4 -4 6.30 1.40 7 -4 4 5.00 0.80 -8 4 -4 0.10 1.10 -8 4 -4 0.90 0.80 -8 4 -4 1.40 0.70 -8 4 -4 0.70 1.20 -8 4 -4 0.10 0.50 8 -4 4 -0.20 0.60 -9 4 -4 6.70 1.70 -9 4 -4 8.00 1.00 -9 4 -4 6.40 1.10 -9 4 -4 7.40 1.70 9 -4 4 6.30 0.90 12 3 -4 3.30 1.20 -12 -3 4 5.70 1.80 11 3 -4 2.80 1.10 -11 -3 4 1.00 1.10 -11 -3 4 3.10 1.60 10 3 -4 5.10 1.20 -10 -3 4 3.70 0.90 -10 -3 4 3.20 1.40 -10 -3 4 3.00 1.10 9 3 -4 -0.70 0.80 -9 -3 4 1.10 0.90 -9 -3 4 0.90 0.50 -9 -3 4 1.80 1.00 -9 -3 4 0.70 1.20 -9 -3 4 2.40 0.80 8 3 -4 277.07 7.30 8 3 -4 259.77 6.50 -8 -3 4 286.47 7.20 -8 -3 4 280.67 6.80 -8 -3 4 267.77 7.30 -8 -3 4 274.47 7.30 7 3 -4 6.70 0.60 7 3 -4 6.80 1.00 7 3 -4 6.40 0.70 -7 -3 4 6.30 0.90 -7 -3 4 7.80 1.10 -7 -3 4 7.50 1.00 -7 -3 4 6.00 0.70 6 3 -4 0.20 0.50 6 3 -4 0.40 0.60 -6 -3 4 0.20 0.40 -6 -3 4 0.20 0.60 -6 -3 4 1.20 0.60 -6 -3 4 -0.20 0.60 5 3 -4 13.00 1.00 5 3 -4 12.60 1.00 5 3 -4 14.50 1.10 -5 -3 4 13.80 1.10 -5 -3 4 14.70 1.00 -5 -3 4 10.80 1.00 -5 -3 4 15.90 1.20 4 3 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15.60 1.30 -2 -8 5 11.70 1.40 1 8 -5 2.80 0.80 1 8 -5 2.30 1.00 -1 -8 5 4.10 1.10 0 8 -5 0.80 0.90 0 -8 5 2.00 1.00 -1 8 -5 0.10 0.90 1 -8 5 0.30 0.90 -2 8 -5 5.10 1.60 -2 8 -5 4.10 1.10 2 -8 5 5.70 1.20 -3 8 -5 3.90 1.10 -3 8 -5 3.40 1.50 3 -8 5 3.80 1.00 -4 8 -5 6.80 1.30 -4 8 -5 5.30 1.70 4 -8 5 6.50 1.20 11 7 -5 -1.10 1.20 -11 -7 5 0.80 1.20 -11 -7 5 0.70 1.40 10 7 -5 11.70 1.70 -10 -7 5 11.20 1.70 -10 -7 5 11.80 1.60 9 7 -5 -0.80 1.10 -9 -7 5 -1.50 1.00 -9 -7 5 0.10 1.00 8 7 -5 50.49 2.80 -8 -7 5 56.89 2.60 -8 -7 5 54.59 2.80 7 7 -5 85.69 3.40 -7 -7 5 94.89 3.60 6 7 -5 53.69 2.70 -6 -7 5 60.89 2.80 5 7 -5 -0.80 0.80 -5 -7 5 0.00 0.90 4 7 -5 8.00 1.20 4 7 -5 6.00 1.10 -4 -7 5 5.00 1.20 3 7 -5 158.08 4.60 3 7 -5 149.69 4.70 -3 -7 5 152.68 4.80 2 7 -5 47.80 2.40 2 7 -5 46.20 2.10 2 7 -5 46.40 2.20 -2 -7 5 46.20 2.30 1 7 -5 80.19 3.00 1 7 -5 81.59 2.70 1 7 -5 80.59 3.10 -1 -7 5 83.39 3.10 0 7 -5 19.80 1.50 0 7 -5 16.90 1.40 0 7 -5 18.20 1.20 0 -7 5 16.20 1.50 -1 7 -5 2.10 0.80 -1 7 -5 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42.40 1.70 3 3 -5 42.00 1.70 -3 -3 5 40.30 1.70 -3 -3 5 40.80 1.70 2 3 -5 124.39 3.50 2 3 -5 124.79 3.40 2 3 -5 120.39 3.50 -2 -3 5 120.49 3.50 -2 -3 5 121.99 3.40 1 3 -5 157.48 4.30 1 3 -5 161.28 4.20 1 3 -5 165.98 4.30 -1 -3 5 161.58 4.20 -1 -3 5 163.58 4.40 -1 -3 5 159.78 4.30 0 3 -5 0.60 0.40 0 3 -5 2.20 0.50 0 3 -5 2.60 0.80 0 3 -5 1.50 0.50 0 3 -5 1.30 0.50 0 -3 5 1.30 0.50 0 -3 5 2.10 0.50 0 -3 5 2.10 0.50 -1 3 -5 145.69 3.80 -1 3 -5 141.09 3.50 -1 3 -5 142.79 3.80 -1 3 -5 139.59 4.20 1 -3 5 146.09 3.80 1 -3 5 146.79 3.80 1 -3 5 141.99 3.80 -2 3 -5 10.70 0.80 -2 3 -5 11.00 1.20 -2 3 -5 10.30 0.80 2 -3 5 10.70 0.90 2 -3 5 11.40 0.80 2 -3 5 10.30 0.80 -3 3 -5 3.70 1.00 -3 3 -5 3.50 0.60 -3 3 -5 2.90 0.60 3 -3 5 2.70 0.50 3 -3 5 3.30 0.60 -4 3 -5 28.20 2.00 -4 3 -5 29.20 1.80 -4 3 -5 30.70 1.30 -4 3 -5 29.00 1.30 4 -3 5 32.20 1.30 4 -3 5 29.30 1.20 -5 3 -5 7.40 1.40 -5 3 -5 7.10 0.70 -5 3 -5 8.40 0.80 -5 3 -5 9.20 1.40 5 -3 5 8.40 0.70 5 -3 5 8.10 0.70 -6 3 -5 70.59 3.00 -6 3 -5 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100.29 2.70 -2 2 -5 205.18 5.00 -2 2 -5 211.58 5.00 -2 2 -5 202.08 5.60 2 -2 5 194.78 5.00 2 -2 5 211.38 5.10 2 -2 5 206.68 5.00 2 -2 5 200.58 5.00 -3 2 -5 10.10 0.80 -3 2 -5 10.40 1.10 -3 2 -5 10.20 0.80 3 -2 5 9.90 0.70 3 -2 5 11.90 0.70 3 -2 5 9.60 0.70 -4 2 -5 7.00 0.60 -4 2 -5 8.30 1.10 -4 2 -5 5.90 1.00 -4 2 -5 6.80 0.60 4 -2 5 8.40 0.60 4 -2 5 6.90 0.50 -5 2 -5 250.37 6.90 -5 2 -5 243.58 5.80 -5 2 -5 246.68 6.70 -5 2 -5 239.08 5.80 5 -2 5 238.08 5.80 -6 2 -5 337.47 9.00 -6 2 -5 321.17 7.70 -6 2 -5 313.17 7.70 -6 2 -5 328.77 8.80 6 -2 5 323.57 7.70 6 -2 5 331.07 7.70 -7 2 -5 98.29 2.60 -7 2 -5 96.99 3.80 -7 2 -5 94.89 2.70 -7 2 -5 96.29 3.90 7 -2 5 91.19 2.60 -8 2 -5 2.00 0.50 -8 2 -5 2.20 0.60 -8 2 -5 1.50 1.10 -8 2 -5 1.00 1.20 8 -2 5 2.40 0.50 -9 2 -5 0.10 0.50 -9 2 -5 0.60 1.20 -9 2 -5 -1.00 1.30 -9 2 -5 1.50 0.70 9 -2 5 0.50 0.50 -10 2 -5 6.20 1.00 -10 2 -5 8.70 1.90 -10 2 -5 9.60 1.00 -10 2 -5 9.40 1.80 10 -2 5 8.20 1.00 12 1 -5 3.70 1.30 -12 -1 5 2.70 1.90 11 1 -5 1.40 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1.20 0 -1 15 2.70 1.30 0 -1 15 -0.50 1.20 -3 0 15 19.40 2.20 -2 0 15 2.10 1.40 -1 0 15 1.10 1.30 0 0 -15 -0.70 1.10 0 0 15 0.10 1.20 -1 0 -15 -0.90 1.00 1 0 15 -0.40 1.10 -2 0 -15 2.60 1.10 2 0 15 4.00 1.20 -3 0 -15 6.00 1.30 3 0 15 6.80 1.30 -4 1 15 -0.50 1.50 -3 1 15 -1.70 1.40 -2 1 15 0.50 1.40 -1 1 15 3.10 1.40 0 -1 -15 -0.50 1.00 0 1 15 -1.20 1.10 -1 -1 -15 2.10 1.10 1 1 15 -1.00 1.00 -2 -1 -15 -1.60 0.90 2 1 15 -0.20 1.00 -3 -1 -15 4.30 1.20 3 1 15 1.10 1.00 -4 -1 -15 3.10 1.00 -4 -1 -15 0.50 0.90 4 1 15 1.30 1.00 -4 2 15 0.90 1.50 -3 2 15 0.90 1.40 -2 2 15 -0.10 1.40 -1 2 15 1.30 1.40 0 -2 -15 1.70 1.20 0 2 15 0.80 1.20 -1 -2 -15 4.40 1.20 1 2 15 4.40 1.30 -2 -2 -15 0.70 1.00 2 2 15 0.30 1.00 -3 -2 -15 -0.40 0.90 3 2 15 -2.00 0.90 -4 -2 -15 1.00 1.00 -4 -2 -15 2.60 1.00 4 2 15 0.60 1.00 -5 -2 -15 -1.00 0.80 -5 -2 -15 0.10 0.90 5 2 15 0.30 0.90 4 -3 -15 1.40 1.30 -4 3 15 -1.90 1.40 -3 3 15 3.50 1.50 -2 3 15 -1.10 1.40 -1 3 15 0.30 1.30 0 -3 -15 -0.50 1.10 0 3 15 0.50 1.30 -1 -3 -15 4.50 1.20 1 3 15 5.20 1.40 -2 -3 -15 1.30 1.00 2 3 15 0.70 1.10 -3 -3 -15 13.20 1.50 3 3 15 12.90 1.60 -4 -3 -15 3.90 1.10 -4 -3 -15 1.00 1.00 4 3 15 5.30 1.30 -5 -3 -15 3.90 1.10 -5 -3 -15 1.80 0.90 5 3 15 2.90 1.10 -6 -3 -15 0.80 0.90 -6 -3 -15 -0.40 0.90 6 3 15 -1.60 0.90 4 -4 -15 0.80 1.20 -4 4 15 0.80 1.50 3 -4 -15 1.70 2.00 -3 4 15 -0.40 1.40 -2 4 15 1.40 1.40 -1 4 15 1.50 1.40 0 -4 -15 -0.40 1.10 0 4 15 -1.30 1.20 -1 -4 -15 -1.50 1.00 1 4 15 -1.30 1.20 -2 -4 -15 6.40 1.30 2 4 15 4.70 1.30 -3 -4 -15 3.70 1.10 3 4 15 3.10 1.30 -4 -4 -15 -1.20 1.00 -4 -4 -15 0.60 0.90 4 4 15 1.50 1.10 -5 -4 -15 3.30 1.20 -5 -4 -15 1.60 0.90 5 4 15 1.40 1.10 -6 -4 -15 0.40 0.90 -6 -4 -15 -0.70 1.00 6 4 15 -1.60 0.90 3 -5 -15 -0.20 1.10 -3 5 15 -1.60 1.40 -2 5 15 0.90 1.50 -1 5 15 -0.80 1.40 0 5 15 -1.70 1.20 -1 -5 -15 14.60 1.60 1 5 15 18.10 2.00 -2 -5 -15 2.80 1.10 2 5 15 0.00 1.20 -3 -5 -15 -1.30 0.90 3 5 15 0.30 1.20 -4 -5 -15 5.20 1.10 -4 -5 -15 6.70 1.60 4 5 15 4.30 1.30 -5 -5 -15 0.40 0.90 -5 -5 -15 -0.30 1.10 5 5 15 -1.40 1.00 -6 -5 -15 2.80 1.20 -6 -5 -15 2.70 1.00 6 5 15 2.40 1.20 -7 -5 -15 0.90 1.10 -7 -5 -15 2.00 0.90 7 5 15 -0.30 1.00 3 -6 -15 2.30 1.20 -3 6 15 1.60 1.60 2 -6 -15 0.70 1.30 -2 6 15 -1.30 1.40 -1 6 15 5.60 1.60 0 6 15 -2.00 1.30 -1 -6 -15 1.10 1.30 1 6 15 1.30 1.40 -2 -6 -15 15.80 1.70 2 6 15 17.90 2.00 -3 -6 -15 -0.30 0.90 3 6 15 -1.20 1.20 -4 -6 -15 0.40 1.00 4 6 15 1.60 1.20 -5 -6 -15 4.70 1.40 -5 -6 -15 5.20 1.20 5 6 15 3.70 1.30 -6 -6 -15 12.80 1.60 -6 -6 -15 13.60 1.50 6 6 15 13.00 1.60 -7 -6 -15 -1.90 1.00 -7 -6 -15 1.80 0.90 7 6 15 -1.40 1.00 2 -7 -15 1.20 1.10 -2 7 15 -1.10 1.50 -1 7 15 4.20 1.60 0 7 15 -0.80 1.40 1 7 15 15.30 2.10 -2 -7 -15 1.40 1.10 2 7 15 1.60 1.50 -3 -7 -15 5.20 1.20 3 7 15 2.30 1.40 -4 -7 -15 3.40 1.10 4 7 15 2.00 1.40 -5 -7 -15 1.80 1.00 5 7 15 -0.90 1.20 -6 -7 -15 10.30 1.40 6 7 15 9.80 1.70 -7 -7 -15 1.80 0.90 -7 -7 -15 -0.40 1.20 7 7 15 1.20 1.30 -1 8 15 -0.90 1.50 0 8 15 0.90 1.60 1 8 15 3.90 1.70 2 8 15 4.30 1.60 -3 -8 -15 8.30 1.40 3 8 15 9.80 1.90 -4 -8 -15 -0.90 1.00 4 8 15 0.30 1.30 -5 -8 -15 -1.00 0.90 5 8 15 1.70 1.40 -6 -8 -15 3.30 1.10 6 8 15 2.90 1.40 -7 -8 -15 1.10 1.00 7 8 15 -0.10 1.20 0 9 15 1.30 1.70 1 9 15 0.40 1.70 2 9 15 -1.40 1.50 3 9 15 6.00 1.80 -4 -9 -15 1.20 1.20 4 9 15 -0.10 1.50 -5 -9 -15 1.50 1.10 5 9 15 -0.30 1.40 -6 -9 -15 1.10 1.10 6 9 15 0.40 1.40 2 10 15 -1.30 1.60 3 10 15 11.70 2.00 4 10 15 0.50 1.60 5 10 15 1.30 1.60 -1 2 16 1.10 1.40 0 2 16 -0.80 1.30 -1 -2 -16 -0.30 1.10 1 2 16 -1.50 1.20 -2 -2 -16 -0.40 1.10 2 2 16 -1.10 1.10 -2 3 16 2.30 1.60 -1 3 16 -1.50 1.30 0 3 16 0.30 1.30 -1 -3 -16 0.20 1.20 1 3 16 -0.60 1.20 -2 -3 -16 -0.30 1.00 2 3 16 0.30 1.20 -3 -3 -16 5.50 1.30 3 3 16 5.90 1.40 -4 -3 -16 -0.60 1.00 4 3 16 1.80 1.20 -2 4 16 -1.30 1.40 -1 4 16 -0.10 1.40 0 4 16 -1.10 1.30 -1 -4 -16 1.00 1.10 1 4 16 -0.80 1.30 -2 -4 -16 -0.80 1.00 2 4 16 1.20 1.40 -3 -4 -16 4.50 1.20 3 4 16 1.60 1.30 -4 -4 -16 2.70 1.10 4 4 16 3.40 1.30 -1 5 16 -1.30 1.50 0 5 16 -0.40 1.40 1 5 16 1.40 1.40 -2 -5 -16 2.00 1.10 2 5 16 2.30 1.40 -3 -5 -16 0.90 1.10 3 5 16 -1.10 1.20 -4 -5 -16 0.20 1.00 4 5 16 1.30 1.30 -5 -5 -16 4.30 1.20 5 5 16 1.30 1.30 -1 6 16 2.70 1.60 0 6 16 -1.80 1.30 1 6 16 8.10 1.80 -2 -6 -16 0.70 1.10 2 6 16 1.70 1.40 -3 -6 -16 0.20 1.10 3 6 16 0.00 1.40 -4 -6 -16 3.10 1.10 4 6 16 0.80 1.40 -5 -6 -16 4.80 1.20 5 6 16 7.50 1.60 0 7 16 -2.00 1.50 1 7 16 11.60 2.00 2 7 16 12.20 2.00 -3 -7 -16 0.80 1.10 3 7 16 0.40 1.40 -4 -7 -16 1.40 1.10 4 7 16 0.00 1.40 -5 -7 -16 2.10 1.10 5 7 16 -2.10 1.20 1 8 16 1.30 1.70 2 8 16 0.90 1.60 3 8 16 -0.10 1.60 -4 -8 -16 1.90 1.10 4 8 16 0.30 1.50 ; _shelx_hkl_checksum 14988 _shelx_res_file ; TITL GLOBAL P -1 R 0.06 G:\Work_2023\009\009.res created by SHELXL-2018/3 at 16:23:06 on 15-Jun-2023 CELL 0.71073 10.70650 10.94340 12.82560 69.02900 82.87100 67.51500 ZERR 2 0.00030 0.00030 0.00040 0.00100 0.00100 0.00100 LATT 1 SFAC C H N O UNIT 64 60 4 6 SIZE 0.01 0.02 0.03 L.S. 5 FMAP 2 PLAN 20 OMIT 0 1 2 OMIT 0 3 1 OMIT 0 0 2 OMIT -1 0 2 OMIT 0 -3 1 OMIT 0 50.5 BUMP ACTA CONF BOND $H HTAB DFIX 1.40 .02 O3 C31B O3 C31A DFIX 1.50 .02 C31B C32B C31A C32A WGHT 0.096600 0.172100 EXTI 0.029242 FVAR 0.75516 O1 4 0.795040 0.577172 0.552192 11.00000 0.05633 0.05046 = 0.08073 -0.00538 0.00377 -0.02164 O2 4 -0.095604 0.729901 0.821107 11.00000 0.05209 0.05396 = 0.10254 -0.02844 -0.00929 -0.00080 N1 3 0.449262 0.194345 0.841026 11.00000 0.03952 0.04153 = 0.04965 -0.01696 0.00055 -0.01041 N2 3 0.543460 0.088732 0.715310 11.00000 0.04504 0.04913 = 0.05916 -0.02379 0.00565 -0.01562 C1 1 0.400237 0.087867 0.861698 11.00000 0.03645 0.04067 = 0.05317 -0.01193 -0.00434 -0.00808 C2 1 0.310174 0.045294 0.940763 11.00000 0.04823 0.05709 = 0.05883 -0.01472 0.00454 -0.01583 AFIX 43 H2 2 0.271852 0.089317 0.993196 11.00000 -1.20000 AFIX 0 C3 1 0.280888 -0.064204 0.937548 11.00000 0.05194 0.05960 = 0.07350 -0.00691 0.00085 -0.02497 AFIX 43 H3 2 0.221822 -0.096176 0.989567 11.00000 -1.20000 AFIX 0 C4 1 0.337428 -0.129625 0.858006 11.00000 0.05354 0.05027 = 0.08423 -0.01339 -0.01210 -0.02112 AFIX 43 H4 2 0.314703 -0.203600 0.858044 11.00000 -1.20000 AFIX 0 C5 1 0.425857 -0.086805 0.779825 11.00000 0.04952 0.04878 = 0.07503 -0.02568 -0.00602 -0.01242 AFIX 43 H5 2 0.462698 -0.130245 0.726829 11.00000 -1.20000 AFIX 0 C6 1 0.458718 0.023939 0.782380 11.00000 0.03690 0.04058 = 0.05485 -0.01443 -0.00374 -0.00862 C7 1 0.534772 0.189189 0.752563 11.00000 0.03474 0.04269 = 0.05035 -0.01644 -0.00115 -0.00746 C8 1 0.603896 0.290567 0.703836 11.00000 0.04318 0.04527 = 0.04702 -0.01771 0.00063 -0.01275 C9 1 0.529340 0.430615 0.656411 11.00000 0.04036 0.04928 = 0.06272 -0.01495 -0.00089 -0.01136 AFIX 43 H9 2 0.435537 0.460380 0.658714 11.00000 -1.20000 AFIX 0 C10 1 0.588985 0.530547 0.604645 11.00000 0.05057 0.04249 = 0.06283 -0.01067 -0.00639 -0.00939 AFIX 43 H10 2 0.535260 0.624956 0.573506 11.00000 -1.20000 AFIX 0 C11 1 0.726628 0.488801 0.600034 11.00000 0.05079 0.04709 = 0.04994 -0.01184 0.00099 -0.01879 C12 1 0.953275 0.299641 0.650768 11.00000 0.04636 0.05921 = 0.05964 -0.01698 0.00739 -0.01929 AFIX 43 H12 2 0.994730 0.364312 0.615193 11.00000 -1.20000 AFIX 0 C13 1 1.030415 0.162238 0.703294 11.00000 0.04074 0.06372 = 0.07141 -0.01817 0.00512 -0.01210 AFIX 43 H13 2 1.124085 0.134150 0.704158 11.00000 -1.20000 AFIX 0 C14 1 0.969894 0.063387 0.755788 11.00000 0.04752 0.04976 = 0.06729 -0.01350 0.00005 -0.00664 AFIX 43 H14 2 1.023558 -0.029967 0.791474 11.00000 -1.20000 AFIX 0 C15 1 0.832549 0.102729 0.755128 11.00000 0.04689 0.04511 = 0.05341 -0.01497 0.00325 -0.01353 AFIX 43 H15 2 0.793720 0.035493 0.789512 11.00000 -1.20000 AFIX 0 C16 1 0.748356 0.244635 0.702756 11.00000 0.04390 0.04544 = 0.04215 -0.01714 0.00388 -0.01309 C17 1 0.810524 0.344440 0.650054 11.00000 0.04439 0.04778 = 0.04420 -0.01549 0.00284 -0.01466 C18 1 0.716103 0.722127 0.499926 11.00000 0.07385 0.05452 = 0.08929 0.00034 -0.00193 -0.02502 AFIX 137 H18A 2 0.653487 0.756151 0.552623 11.00000 -1.50000 H18B 2 0.667131 0.732954 0.437366 11.00000 -1.50000 H18C 2 0.774556 0.774847 0.474609 11.00000 -1.50000 AFIX 0 C19 1 0.418034 0.285656 0.906771 11.00000 0.04845 0.04739 = 0.05293 -0.02080 -0.00105 -0.01248 AFIX 23 H19B 2 0.486805 0.326647 0.894256 11.00000 -1.20000 H19A 2 0.421798 0.229513 0.985259 11.00000 -1.20000 AFIX 0 C20 1 0.281034 0.402689 0.880342 11.00000 0.04375 0.04259 = 0.04869 -0.01672 0.00315 -0.01402 C21 1 0.197160 0.424373 0.798600 11.00000 0.05414 0.04822 = 0.05796 -0.02528 -0.00266 -0.01161 AFIX 43 H21 2 0.225253 0.364742 0.756752 11.00000 -1.20000 AFIX 0 C22 1 0.069653 0.533529 0.775052 11.00000 0.05183 0.05107 = 0.06458 -0.01817 -0.01138 -0.01292 AFIX 43 H22 2 0.015627 0.545888 0.717885 11.00000 -1.20000 AFIX 0 C23 1 0.025549 0.620980 0.836100 11.00000 0.04571 0.03788 = 0.06851 -0.01442 0.00349 -0.01185 C24 1 0.063675 0.689684 0.990280 11.00000 0.06292 0.04901 = 0.07129 -0.02499 0.01895 -0.02177 AFIX 43 H24 2 -0.021323 0.760820 0.976874 11.00000 -1.20000 AFIX 0 C25 1 0.142896 0.671020 1.073521 11.00000 0.09126 0.06250 = 0.06463 -0.03478 0.02021 -0.03618 AFIX 43 H25 2 0.111530 0.728456 1.117165 11.00000 -1.20000 AFIX 0 C26 1 0.271499 0.565800 1.093973 11.00000 0.08943 0.06966 = 0.05676 -0.02896 0.00575 -0.03850 AFIX 43 H26 2 0.325891 0.554375 1.150515 11.00000 -1.20000 AFIX 0 C27 1 0.317706 0.479769 1.031501 11.00000 0.06440 0.05599 = 0.05269 -0.01962 0.00144 -0.02436 AFIX 43 H27 2 0.403720 0.410497 1.045927 11.00000 -1.20000 AFIX 0 C28 1 0.237516 0.493697 0.945187 11.00000 0.05093 0.04159 = 0.04740 -0.01506 0.00675 -0.02139 C29 1 0.107932 0.603083 0.923654 11.00000 0.05116 0.03913 = 0.05373 -0.01505 0.01116 -0.01980 C30 1 -0.180310 0.755260 0.733420 11.00000 0.05558 0.06189 = 0.12033 -0.01954 -0.01959 -0.00451 AFIX 137 H30A 2 -0.200492 0.673026 0.745416 11.00000 -1.50000 H30B 2 -0.135112 0.776947 0.663545 11.00000 -1.50000 H30C 2 -0.262803 0.833016 0.731797 11.00000 -1.50000 AFIX 0 O3 4 0.629984 0.104823 0.487892 11.00000 0.10621 0.16703 = 0.08943 -0.05359 0.01949 -0.04828 AFIX 147 H3O 2 0.604169 0.125404 0.544426 11.00000 -1.50000 PART 1 AFIX 0 C31A 1 0.768063 0.083411 0.473037 10.85000 0.10345 0.09320 = 0.10383 -0.03720 0.02767 -0.02113 AFIX 23 H31A 2 0.810206 0.011400 0.438979 10.85000 -1.20000 H31B 2 0.811080 0.050081 0.545358 10.85000 -1.20000 AFIX 0 C32A 1 0.789162 0.208443 0.404724 10.85000 0.14674 0.10785 = 0.13917 -0.01122 0.01781 -0.06503 AFIX 137 H32A 2 0.745066 0.242897 0.333605 10.85000 -1.50000 H32B 2 0.884325 0.188690 0.394075 10.85000 -1.50000 H32C 2 0.752345 0.278195 0.440348 10.85000 -1.50000 PART 2 AFIX 0 C31B 1 0.721095 0.182533 0.449895 10.15000 0.10539 0.05241 = 0.21890 -0.05393 0.06853 -0.03331 AFIX 23 H31C 2 0.697732 0.249896 0.488514 10.15000 -1.20000 H31D 2 0.702879 0.235819 0.371034 10.15000 -1.20000 AFIX 0 C32B 1 0.873184 0.099305 0.465016 10.15000 0.05392 0.14795 = 0.12086 -0.04161 0.02942 -0.02091 AFIX 137 H32D 2 0.889004 0.007762 0.519770 10.15000 -1.50000 H32E 2 0.914982 0.148018 0.489595 10.15000 -1.50000 H32F 2 0.911090 0.089861 0.395180 10.15000 -1.50000 AFIX 0 HKLF 4 REM GLOBAL P -1 R 0.06 REM wR2 = 0.1616, GooF = S = 1.088, Restrained GooF = 1.092 for all data REM R1 = 0.0539 for 3587 Fo > 4sig(Fo) and 0.0697 for all 4611 data REM 358 parameters refined using 5 restraints END WGHT 0.0966 0.1721 REM Instructions for potential hydrogen bonds HTAB O3 N2 REM Highest difference peak 0.310, deepest hole -0.256, 1-sigma level 0.061 Q1 1 0.5666 0.0285 0.5189 11.00000 0.05 0.31 Q2 1 0.4505 0.2198 0.7803 11.00000 0.05 0.21 Q3 1 0.4935 0.6502 0.5842 11.00000 0.05 0.21 Q4 1 0.6560 0.5013 0.6324 11.00000 0.05 0.20 Q5 1 0.4764 0.1815 0.8260 11.00000 0.05 0.19 Q6 1 0.7777 0.7541 0.3996 11.00000 0.05 0.18 Q7 1 0.9931 -0.0198 0.7297 11.00000 0.05 0.18 Q8 1 0.4944 0.2528 0.9784 11.00000 0.05 0.18 Q9 1 0.9989 0.1012 0.6767 11.00000 0.05 0.17 Q10 1 0.9153 0.0583 0.7228 11.00000 0.05 0.17 Q11 1 0.4900 0.0620 0.7226 11.00000 0.05 0.17 Q12 1 0.5351 0.2735 0.9122 11.00000 0.05 0.17 Q13 1 0.6330 -0.0435 0.7844 11.00000 0.05 0.16 Q14 1 0.0837 0.6050 0.7915 11.00000 0.05 0.16 Q15 1 0.0437 0.5727 0.6601 11.00000 0.05 0.16 Q16 1 0.3089 0.4733 0.8901 11.00000 0.05 0.16 Q17 1 0.6143 0.3233 0.4046 11.00000 0.05 0.16 Q18 1 0.7161 -0.0760 0.8585 11.00000 0.05 0.15 Q19 1 0.6612 0.4820 0.5772 11.00000 0.05 0.15 Q20 1 0.7631 0.4184 0.6314 11.00000 0.05 0.15 ; _shelx_res_checksum 68991 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 O O1 0.79504(13) 0.57717(13) 0.55219(12) 0.0670(4) Uani d 1 . . O O2 -0.09560(13) 0.72990(14) 0.82111(14) 0.0738(4) Uani d 1 . . N N1 0.44926(13) 0.19435(13) 0.84103(11) 0.0445(3) Uani d 1 . . N N2 0.54346(14) 0.08873(15) 0.71531(12) 0.0505(4) Uani d 1 . . C C1 0.40024(15) 0.08787(16) 0.86170(14) 0.0460(4) Uani d 1 . . C C2 0.31017(18) 0.0453(2) 0.94076(16) 0.0576(5) Uani d 1 . . H H2 0.271852 0.089317 0.993196 0.069 Uiso calc 1 . . C C3 0.2809(2) -0.0642(2) 0.93755(18) 0.0648(5) Uani d 1 . . H H3 0.221822 -0.096176 0.989567 0.078 Uiso calc 1 . . C C4 0.33743(19) -0.1296(2) 0.85801(19) 0.0635(5) Uani d 1 . . H H4 0.314703 -0.203600 0.858044 0.076 Uiso calc 1 . . C C5 0.42586(18) -0.08680(19) 0.77983(18) 0.0575(5) Uani d 1 . . H H5 0.462698 -0.130245 0.726829 0.069 Uiso calc 1 . . C C6 0.45872(15) 0.02394(16) 0.78238(14) 0.0459(4) Uani d 1 . . C C7 0.53477(15) 0.18919(16) 0.75256(14) 0.0443(4) Uani d 1 . . C C8 0.60390(16) 0.29057(17) 0.70384(14) 0.0456(4) Uani d 1 . . C C9 0.52934(17) 0.43062(18) 0.65641(16) 0.0534(4) Uani d 1 . . H H9 0.435537 0.460380 0.658714 0.064 Uiso calc 1 . . C C10 0.58899(18) 0.53055(18) 0.60465(16) 0.0558(5) Uani d 1 . . H H10 0.535260 0.624956 0.573506 0.067 Uiso calc 1 . . C C11 0.72663(18) 0.48880(18) 0.60003(15) 0.0503(4) Uani d 1 . . C C12 0.95327(18) 0.2996(2) 0.65077(16) 0.0566(5) Uani d 1 . . H H12 0.994730 0.364312 0.615193 0.068 Uiso calc 1 . . C C13 1.03042(18) 0.1622(2) 0.70329(17) 0.0626(5) Uani d 1 . . H H13 1.124085 0.134150 0.704158 0.075 Uiso calc 1 . . C C14 0.96989(18) 0.0634(2) 0.75579(17) 0.0602(5) Uani d 1 . . H H14 1.023558 -0.029967 0.791474 0.072 Uiso calc 1 . . C C15 0.83255(17) 0.10273(18) 0.75513(15) 0.0502(4) Uani d 1 . . H H15 0.793720 0.035493 0.789512 0.060 Uiso calc 1 . . C C16 0.74836(16) 0.24464(17) 0.70276(13) 0.0445(4) Uani d 1 . . C C17 0.81052(16) 0.34444(17) 0.65005(14) 0.0464(4) Uani d 1 . . C C18 0.7161(2) 0.7221(2) 0.4999(2) 0.0790(6) Uani d 1 . . H H18A 0.653487 0.756151 0.552623 0.118 Uiso calc 1 . . H H18B 0.667131 0.732954 0.437366 0.118 Uiso calc 1 . . H H18C 0.774556 0.774847 0.474609 0.118 Uiso calc 1 . . C C19 0.41803(17) 0.28566(18) 0.90677(15) 0.0499(4) Uani d 1 . . H H19B 0.486805 0.326647 0.894256 0.060 Uiso calc 1 . . H H19A 0.421798 0.229513 0.985259 0.060 Uiso calc 1 . . C C20 0.28103(16) 0.40269(16) 0.88034(14) 0.0454(4) Uani d 1 . . C C21 0.19716(18) 0.42437(18) 0.79860(15) 0.0532(4) Uani d 1 . . H H21 0.225253 0.364742 0.756752 0.064 Uiso calc 1 . . C C22 0.06965(18) 0.53353(19) 0.77505(17) 0.0569(5) Uani d 1 . . H H22 0.015627 0.545888 0.717885 0.068 Uiso calc 1 . . C C23 0.02555(17) 0.62098(17) 0.83610(16) 0.0531(5) Uani d 1 . . C C24 0.0637(2) 0.6897(2) 0.99028(17) 0.0610(5) Uani d 1 . . H H24 -0.021323 0.760820 0.976874 0.073 Uiso calc 1 . . C C25 0.1429(2) 0.6710(2) 1.07352(18) 0.0681(6) Uani d 1 . . H H25 0.111530 0.728456 1.117165 0.082 Uiso calc 1 . . C C26 0.2715(2) 0.5658(2) 1.09397(17) 0.0672(6) Uani d 1 . . H H26 0.325891 0.554375 1.150515 0.081 Uiso calc 1 . . C C27 0.3177(2) 0.4798(2) 1.03150(15) 0.0566(5) Uani d 1 . . H H27 0.403720 0.410497 1.045927 0.068 Uiso calc 1 . . C C28 0.23752(17) 0.49370(16) 0.94519(14) 0.0458(4) Uani d 1 . . C C29 0.10793(17) 0.60308(16) 0.92365(14) 0.0481(4) Uani d 1 . . C C30 -0.1803(2) 0.7553(2) 0.7334(2) 0.0860(7) Uani d 1 . . H H30A -0.200492 0.673026 0.745416 0.129 Uiso calc 1 . . H H30B -0.135112 0.776947 0.663545 0.129 Uiso calc 1 . . H H30C -0.262803 0.833016 0.731797 0.129 Uiso calc 1 . . O O3 0.6300(2) 0.1048(3) 0.48789(18) 0.1201(7) Uani d 1 . . H H3O 0.604169 0.125404 0.544426 0.180 Uiso calc 1 A 1 C C31A 0.7681(4) 0.0834(5) 0.4730(3) 0.1062(11) Uani d 0.85 B 1 H H31A 0.810206 0.011400 0.438979 0.127 Uiso calc 0.85 B 1 H H31B 0.811080 0.050081 0.545358 0.127 Uiso calc 0.85 B 1 C C32A 0.7892(6) 0.2084(5) 0.4047(5) 0.1359(16) Uani d 0.85 B 1 H H32A 0.745066 0.242897 0.333605 0.204 Uiso calc 0.85 B 1 H H32B 0.884325 0.188690 0.394075 0.204 Uiso calc 0.85 B 1 H H32C 0.752345 0.278195 0.440348 0.204 Uiso calc 0.85 B 1 C C31B 0.7211(17) 0.183(2) 0.450(3) 0.128(10) Uani d 0.15 B 2 H H31C 0.697732 0.249896 0.488514 0.154 Uiso calc 0.15 B 2 H H31D 0.702879 0.235819 0.371034 0.154 Uiso calc 0.15 B 2 C C32B 0.8732(17) 0.099(3) 0.465(2) 0.116(8) Uani d 0.15 B 2 H H32D 0.889004 0.007762 0.519770 0.175 Uiso calc 0.15 B 2 H H32E 0.914982 0.148018 0.489595 0.175 Uiso calc 0.15 B 2 H H32F 0.911090 0.089861 0.395180 0.175 Uiso calc 0.15 B 2 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 O1 0.0563(8) 0.0505(7) 0.0807(9) -0.0216(6) 0.0038(7) -0.0054(6) O2 0.0521(8) 0.0540(8) 0.1025(11) -0.0008(6) -0.0093(8) -0.0284(7) N1 0.0395(7) 0.0415(7) 0.0497(8) -0.0104(6) 0.0005(6) -0.0170(6) N2 0.0450(8) 0.0491(8) 0.0592(9) -0.0156(6) 0.0057(6) -0.0238(7) C1 0.0365(8) 0.0407(8) 0.0532(9) -0.0081(7) -0.0043(7) -0.0119(7) C2 0.0482(10) 0.0571(11) 0.0588(11) -0.0158(8) 0.0045(8) -0.0147(9) C3 0.0519(10) 0.0596(11) 0.0735(13) -0.0250(9) 0.0009(9) -0.0069(10) C4 0.0535(10) 0.0503(10) 0.0842(14) -0.0211(8) -0.0121(10) -0.0134(10) C5 0.0495(10) 0.0488(10) 0.0750(12) -0.0124(8) -0.0060(9) -0.0257(9) C6 0.0369(8) 0.0406(8) 0.0548(10) -0.0086(6) -0.0037(7) -0.0144(7) C7 0.0347(8) 0.0427(8) 0.0503(9) -0.0075(6) -0.0012(7) -0.0164(7) C8 0.0432(8) 0.0453(9) 0.0470(9) -0.0128(7) 0.0006(7) -0.0177(7) C9 0.0404(9) 0.0493(10) 0.0627(11) -0.0114(7) -0.0009(8) -0.0149(8) C10 0.0506(10) 0.0425(9) 0.0628(11) -0.0094(7) -0.0064(8) -0.0107(8) C11 0.0508(10) 0.0471(9) 0.0499(10) -0.0188(8) 0.0010(8) -0.0118(8) C12 0.0464(9) 0.0592(11) 0.0596(11) -0.0193(8) 0.0074(8) -0.0170(9) C13 0.0407(9) 0.0637(12) 0.0714(13) -0.0121(8) 0.0051(9) -0.0182(10) C14 0.0475(10) 0.0498(10) 0.0673(12) -0.0066(8) 0.0000(9) -0.0135(9) C15 0.0469(9) 0.0451(9) 0.0534(10) -0.0135(7) 0.0032(8) -0.0150(8) C16 0.0439(9) 0.0454(9) 0.0421(9) -0.0131(7) 0.0039(7) -0.0171(7) C17 0.0444(9) 0.0478(9) 0.0442(9) -0.0147(7) 0.0028(7) -0.0155(7) C18 0.0738(14) 0.0545(12) 0.0893(16) -0.0250(10) -0.0019(12) 0.0003(11) C19 0.0484(9) 0.0474(9) 0.0529(10) -0.0125(7) -0.0010(8) -0.0208(8) C20 0.0437(9) 0.0426(8) 0.0487(9) -0.0140(7) 0.0032(7) -0.0167(7) C21 0.0541(10) 0.0482(9) 0.0580(10) -0.0116(8) -0.0027(8) -0.0253(8) C22 0.0518(10) 0.0511(10) 0.0646(11) -0.0129(8) -0.0114(9) -0.0182(9) C23 0.0457(9) 0.0379(8) 0.0685(11) -0.0118(7) 0.0035(8) -0.0144(8) C24 0.0629(11) 0.0490(10) 0.0713(13) -0.0218(9) 0.0190(10) -0.0250(9) C25 0.0913(16) 0.0625(12) 0.0646(12) -0.0362(12) 0.0202(11) -0.0348(10) C26 0.0894(15) 0.0697(13) 0.0568(11) -0.0385(12) 0.0058(10) -0.0290(10) C27 0.0644(11) 0.0560(10) 0.0527(10) -0.0244(9) 0.0014(9) -0.0196(8) C28 0.0509(9) 0.0416(8) 0.0474(9) -0.0214(7) 0.0068(7) -0.0151(7) C29 0.0512(9) 0.0391(8) 0.0537(10) -0.0198(7) 0.0112(8) -0.0150(7) C30 0.0556(12) 0.0619(13) 0.120(2) -0.0045(10) -0.0196(13) -0.0195(13) O3 0.1062(15) 0.167(2) 0.0894(14) -0.0483(15) 0.0195(11) -0.0536(14) C31A 0.103(3) 0.093(3) 0.104(3) -0.021(2) 0.028(2) -0.037(2) C32A 0.147(5) 0.108(3) 0.139(4) -0.065(3) 0.018(3) -0.011(3) C31B 0.105(16) 0.052(11) 0.22(3) -0.033(11) 0.069(18) -0.054(15) C32B 0.054(10) 0.15(2) 0.121(17) -0.021(12) 0.029(11) -0.042(15) 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 O1 C18 . . 116.99(15) ? C23 O2 C30 . . 117.04(17) ? C7 N1 C1 . . 106.56(13) ? C7 N1 C19 . . 128.74(14) ? C1 N1 C19 . . 124.63(14) ? C7 N2 C6 . . 105.45(14) ? N1 C1 C6 . . 105.77(14) ? N1 C1 C2 . . 131.48(16) ? C6 C1 C2 . . 122.74(16) ? C3 C2 C1 . . 116.72(19) ? C3 C2 H2 . . 121.6 ? C1 C2 H2 . . 121.6 ? C2 C3 C4 . . 121.70(19) ? C2 C3 H3 . . 119.1 ? C4 C3 H3 . . 119.1 ? C5 C4 C3 . . 121.35(18) ? C5 C4 H4 . . 119.3 ? C3 C4 H4 . . 119.3 ? C4 C5 C6 . . 117.98(19) ? C4 C5 H5 . . 121.0 ? C6 C5 H5 . . 121.0 ? N2 C6 C1 . . 109.68(14) ? N2 C6 C5 . . 130.82(16) ? C1 C6 C5 . . 119.50(16) ? N2 C7 N1 . . 112.53(14) ? N2 C7 C8 . . 125.10(15) ? N1 C7 C8 . . 122.33(14) ? C9 C8 C16 . . 119.00(16) ? C9 C8 C7 . . 119.83(15) ? C16 C8 C7 . . 121.16(14) ? C8 C9 C10 . . 122.43(16) ? C8 C9 H9 . . 118.8 ? C10 C9 H9 . . 118.8 ? C11 C10 C9 . . 119.65(16) ? C11 C10 H10 . . 120.2 ? C9 C10 H10 . . 120.2 ? O1 C11 C10 . . 124.48(16) ? O1 C11 C17 . . 114.74(15) ? C10 C11 C17 . . 120.76(16) ? C13 C12 C17 . . 120.42(17) ? C13 C12 H12 . . 119.8 ? C17 C12 H12 . . 119.8 ? C12 C13 C14 . . 120.54(17) ? C12 C13 H13 . . 119.7 ? C14 C13 H13 . . 119.7 ? C15 C14 C13 . . 120.51(17) ? C15 C14 H14 . . 119.7 ? C13 C14 H14 . . 119.7 ? C14 C15 C16 . . 120.89(17) ? C14 C15 H15 . . 119.6 ? C16 C15 H15 . . 119.6 ? C15 C16 C17 . . 118.26(15) ? C15 C16 C8 . . 122.42(15) ? C17 C16 C8 . . 119.30(15) ? C12 C17 C16 . . 119.37(15) ? C12 C17 C11 . . 121.78(16) ? C16 C17 C11 . . 118.83(15) ? O1 C18 H18A . . 109.5 ? O1 C18 H18B . . 109.5 ? H18A C18 H18B . . 109.5 ? O1 C18 H18C . . 109.5 ? H18A C18 H18C . . 109.5 ? H18B C18 H18C . . 109.5 ? N1 C19 C20 . . 113.88(14) ? N1 C19 H19B . . 108.8 ? C20 C19 H19B . . 108.8 ? N1 C19 H19A . . 108.8 ? C20 C19 H19A . . 108.8 ? H19B C19 H19A . . 107.7 ? C21 C20 C28 . . 118.77(15) ? C21 C20 C19 . . 123.07(15) ? C28 C20 C19 . . 118.15(14) ? C20 C21 C22 . . 122.50(16) ? C20 C21 H21 . . 118.7 ? C22 C21 H21 . . 118.7 ? C23 C22 C21 . . 119.84(17) ? C23 C22 H22 . . 120.1 ? C21 C22 H22 . . 120.1 ? C22 C23 O2 . . 125.12(18) ? C22 C23 C29 . . 120.45(15) ? O2 C23 C29 . . 114.43(16) ? C25 C24 C29 . . 121.13(18) ? C25 C24 H24 . . 119.4 ? C29 C24 H24 . . 119.4 ? C24 C25 C26 . . 120.22(18) ? C24 C25 H25 . . 119.9 ? C26 C25 H25 . . 119.9 ? C27 C26 C25 . . 120.4(2) ? C27 C26 H26 . . 119.8 ? C25 C26 H26 . . 119.8 ? C26 C27 C28 . . 121.36(18) ? C26 C27 H27 . . 119.3 ? C28 C27 H27 . . 119.3 ? C27 C28 C29 . . 117.73(15) ? C27 C28 C20 . . 122.86(16) ? C29 C28 C20 . . 119.41(15) ? C24 C29 C28 . . 119.18(17) ? C24 C29 C23 . . 121.80(16) ? C28 C29 C23 . . 119.02(15) ? O2 C30 H30A . . 109.5 ? O2 C30 H30B . . 109.5 ? H30A C30 H30B . . 109.5 ? O2 C30 H30C . . 109.5 ? H30A C30 H30C . . 109.5 ? H30B C30 H30C . . 109.5 ? C31A O3 H3O . . 109.5 ? O3 C31A C32A . . 112.0(4) ? O3 C31A H31A . . 109.2 ? C32A C31A H31A . . 109.2 ? O3 C31A H31B . . 109.2 ? C32A C31A H31B . . 109.2 ? H31A C31A H31B . . 107.9 ? C31A C32A H32A . . 109.5 ? C31A C32A H32B . . 109.5 ? H32A C32A H32B . . 109.5 ? C31A C32A H32C . . 109.5 ? H32A C32A H32C . . 109.5 ? H32B C32A H32C . . 109.5 ? O3 C31B C32B . . 118.1(18) ? O3 C31B H31C . . 107.8 ? C32B C31B H31C . . 107.8 ? O3 C31B H31D . . 107.8 ? C32B C31B H31D . . 107.8 ? H31C C31B H31D . . 107.1 ? C31B C32B H32D . . 109.5 ? C31B C32B H32E . . 109.5 ? H32D C32B H32E . . 109.5 ? C31B C32B H32F . . 109.5 ? H32D C32B H32F . . 109.5 ? H32E C32B H32F . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C11 . 1.362(2) ? O1 C18 . 1.426(2) ? O2 C23 . 1.362(2) ? O2 C30 . 1.415(3) ? N1 C7 . 1.370(2) ? N1 C1 . 1.384(2) ? N1 C19 . 1.449(2) ? N2 C7 . 1.316(2) ? N2 C6 . 1.388(2) ? C1 C6 . 1.390(2) ? C1 C2 . 1.392(3) ? C2 C3 . 1.364(3) ? C2 H2 . 0.9300 ? C3 C4 . 1.399(3) ? C3 H3 . 0.9300 ? C4 C5 . 1.374(3) ? C4 H4 . 0.9300 ? C5 C6 . 1.397(2) ? C5 H5 . 0.9300 ? C7 C8 . 1.479(2) ? C8 C9 . 1.369(2) ? C8 C16 . 1.432(2) ? C9 C10 . 1.398(3) ? C9 H9 . 0.9300 ? C10 C11 . 1.366(3) ? C10 H10 . 0.9300 ? C11 C17 . 1.431(2) ? C12 C13 . 1.364(3) ? C12 C17 . 1.415(2) ? C12 H12 . 0.9300 ? C13 C14 . 1.396(3) ? C13 H13 . 0.9300 ? C14 C15 . 1.365(3) ? C14 H14 . 0.9300 ? C15 C16 . 1.417(2) ? C15 H15 . 0.9300 ? C16 C17 . 1.417(2) ? C18 H18A . 0.9600 ? C18 H18B . 0.9600 ? C18 H18C . 0.9600 ? C19 C20 . 1.511(2) ? C19 H19B . 0.9700 ? C19 H19A . 0.9700 ? C20 C21 . 1.362(2) ? C20 C28 . 1.429(2) ? C21 C22 . 1.407(2) ? C21 H21 . 0.9300 ? C22 C23 . 1.360(3) ? C22 H22 . 0.9300 ? C23 C29 . 1.426(3) ? C24 C25 . 1.355(3) ? C24 C29 . 1.410(3) ? C24 H24 . 0.9300 ? C25 C26 . 1.397(3) ? C25 H25 . 0.9300 ? C26 C27 . 1.363(3) ? C26 H26 . 0.9300 ? C27 C28 . 1.415(2) ? C27 H27 . 0.9300 ? C28 C29 . 1.422(2) ? C30 H30A . 0.9600 ? C30 H30B . 0.9600 ? C30 H30C . 0.9600 ? O3 C31A . 1.405(4) ? O3 C31B . 1.460(15) ? O3 H3O . 0.8200 ? C31A C32A . 1.421(5) ? C31A H31A . 0.9700 ? C31A H31B . 0.9700 ? C32A H32A . 0.9600 ? C32A H32B . 0.9600 ? C32A H32C . 0.9600 ? C31B C32B . 1.528(17) ? C31B H31C . 0.9700 ? C31B H31D . 0.9700 ? C32B H32D . 0.9600 ? C32B H32E . 0.9600 ? C32B H32F . 0.9600 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O3 H3O N2 . 0.82 2.15 2.913(3) 156 yes C21 H21 Cg1 1_555 0.93 2.95 3.575(2) 126 yes C19 H19A Cg2 2_657 0.97 2.85 3.600(2) 135 yes C26 H26 Cg3 2_667 0.93 2.82 3.626(2) 146 yes C25 H25 Cg4 2_667 0.93 2.66 3.528(2) 155 yes 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C7 N1 C1 C6 . . . . -0.64(16) ? C19 N1 C1 C6 . . . . -177.79(14) ? C7 N1 C1 C2 . . . . -179.66(17) ? C19 N1 C1 C2 . . . . 3.2(3) ? N1 C1 C2 C3 . . . . 178.97(17) ? C6 C1 C2 C3 . . . . 0.1(2) ? C1 C2 C3 C4 . . . . -0.6(3) ? C2 C3 C4 C5 . . . . 0.4(3) ? C3 C4 C5 C6 . . . . 0.4(3) ? C7 N2 C6 C1 . . . . -0.65(17) ? C7 N2 C6 C5 . . . . 178.45(18) ? N1 C1 C6 N2 . . . . 0.80(17) ? C2 C1 C6 N2 . . . . 179.93(15) ? N1 C1 C6 C5 . . . . -178.41(15) ? C2 C1 C6 C5 . . . . 0.7(2) ? C4 C5 C6 N2 . . . . -179.98(17) ? C4 C5 C6 C1 . . . . -1.0(2) ? C6 N2 C7 N1 . . . . 0.24(17) ? C6 N2 C7 C8 . . . . -177.54(15) ? C1 N1 C7 N2 . . . . 0.26(17) ? C19 N1 C7 N2 . . . . 177.25(15) ? C1 N1 C7 C8 . . . . 178.10(14) ? C19 N1 C7 C8 . . . . -4.9(2) ? N2 C7 C8 C9 . . . . 115.26(19) ? N1 C7 C8 C9 . . . . -62.3(2) ? N2 C7 C8 C16 . . . . -63.2(2) ? N1 C7 C8 C16 . . . . 119.24(17) ? C16 C8 C9 C10 . . . . 1.4(3) ? C7 C8 C9 C10 . . . . -177.08(16) ? C8 C9 C10 C11 . . . . 0.3(3) ? C18 O1 C11 C10 . . . . -2.5(3) ? C18 O1 C11 C17 . . . . 179.27(18) ? C9 C10 C11 O1 . . . . -179.70(17) ? C9 C10 C11 C17 . . . . -1.6(3) ? C17 C12 C13 C14 . . . . 0.9(3) ? C12 C13 C14 C15 . . . . 0.1(3) ? C13 C14 C15 C16 . . . . -0.9(3) ? C14 C15 C16 C17 . . . . 0.6(3) ? C14 C15 C16 C8 . . . . -177.73(17) ? C9 C8 C16 C15 . . . . 176.64(16) ? C7 C8 C16 C15 . . . . -4.9(2) ? C9 C8 C16 C17 . . . . -1.7(2) ? C7 C8 C16 C17 . . . . 176.74(15) ? C13 C12 C17 C16 . . . . -1.1(3) ? C13 C12 C17 C11 . . . . 177.17(18) ? C15 C16 C17 C12 . . . . 0.4(2) ? C8 C16 C17 C12 . . . . 178.80(15) ? C15 C16 C17 C11 . . . . -177.99(15) ? C8 C16 C17 C11 . . . . 0.4(2) ? O1 C11 C17 C12 . . . . 1.2(3) ? C10 C11 C17 C12 . . . . -177.09(17) ? O1 C11 C17 C16 . . . . 179.51(15) ? C10 C11 C17 C16 . . . . 1.2(3) ? C7 N1 C19 C20 . . . . 104.57(18) ? C1 N1 C19 C20 . . . . -78.93(19) ? N1 C19 C20 C21 . . . . -2.9(2) ? N1 C19 C20 C28 . . . . 176.49(14) ? C28 C20 C21 C22 . . . . 0.4(3) ? C19 C20 C21 C22 . . . . 179.81(17) ? C20 C21 C22 C23 . . . . -0.9(3) ? C21 C22 C23 O2 . . . . -179.97(17) ? C21 C22 C23 C29 . . . . 0.2(3) ? C30 O2 C23 C22 . . . . -1.5(3) ? C30 O2 C23 C29 . . . . 178.36(17) ? C29 C24 C25 C26 . . . . 0.8(3) ? C24 C25 C26 C27 . . . . -0.9(3) ? C25 C26 C27 C28 . . . . -0.3(3) ? C26 C27 C28 C29 . . . . 1.6(3) ? C26 C27 C28 C20 . . . . -178.04(17) ? C21 C20 C28 C27 . . . . -179.76(16) ? C19 C20 C28 C27 . . . . 0.8(2) ? C21 C20 C28 C29 . . . . 0.6(2) ? C19 C20 C28 C29 . . . . -178.78(14) ? C25 C24 C29 C28 . . . . 0.5(3) ? C25 C24 C29 C23 . . . . 179.72(17) ? C27 C28 C29 C24 . . . . -1.7(2) ? C20 C28 C29 C24 . . . . 177.94(15) ? C27 C28 C29 C23 . . . . 179.13(15) ? C20 C28 C29 C23 . . . . -1.2(2) ? C22 C23 C29 C24 . . . . -178.34(17) ? O2 C23 C29 C24 . . . . 1.8(2) ? C22 C23 C29 C28 . . . . 0.8(2) ? O2 C23 C29 C28 . . . . -179.01(14) ? _cod_database_fobs_code 2022777