#------------------------------------------------------------------------------ #$Date: 2019-11-30 07:35:07 +0200 (Sat, 30 Nov 2019) $ #$Revision: 244827 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/32/2243208.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_2243208 loop_ _publ_author_name 'Sedykh, Alexander E.' 'Kurth, Dirk G.' 'M\"uller-Buschbaum, Klaus' _publ_section_title ; The crystal structure of the triclinic polymorph of 1,4-bis([2,2':6',2''-terpyridin]-4'-yl)benzene ; _journal_coeditor_code SU5525 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 1947 _journal_page_last 1951 _journal_paper_doi 10.1107/S2056989019015810 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac 'C36 H24 N6' _chemical_formula_moiety 'C36 H24 N6' _chemical_formula_sum 'C36 H24 N6' _chemical_formula_weight 540.61 _chemical_name_systematic ; 1,4-Bis([2,2':6',2''-terpyridin]-4'-yl)benzene ; _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 _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 100.050(7) _cell_angle_beta 102.247(6) _cell_angle_gamma 104.314(7) _cell_formula_units_Z 1 _cell_length_a 7.312(2) _cell_length_b 8.847(3) _cell_length_c 11.039(3) _cell_measurement_reflns_used 3259 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.09 _cell_measurement_theta_min 2.45 _cell_volume 656.5(3) _computing_cell_refinement ; SAINT (Bruker, 2017) ; _computing_data_collection ; APEX3 (Bruker, 2017) ; _computing_data_reduction ; SAINT (Bruker, 2017) ; _computing_molecular_graphics ; shelXle (H\"ubschle et al., 2011) and Mercury (Macrae et al., 2008) ; _computing_publication_material ; SHELXL (Sheldrick, 2015b), PLATON (Spek, 2009) and publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker X8 APEXII' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'multi-layer mirror' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_unetI/netI 0.0545 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 10437 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 27.196 _diffrn_reflns_theta_min 1.944 _diffrn_source 'rotating-anode (Nonius FR-591)' _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_T_max 0.9583 _exptl_absorpt_correction_T_min 0.7641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2017) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.368 _exptl_crystal_description plate _exptl_crystal_F_000 282 _exptl_crystal_size_max 0.530 _exptl_crystal_size_mid 0.296 _exptl_crystal_size_min 0.234 _refine_diff_density_max 0.265 _refine_diff_density_min -0.223 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 190 _refine_ls_number_reflns 2918 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.090 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0465 _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^)+(0.0552P)^2^+0.1381P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1188 _refine_ls_wR_factor_ref 0.1334 _reflns_number_gt 1953 _reflns_number_total 2918 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file su5525sup1.cif _cod_data_source_block I _cod_original_cell_volume 656.4(3) _cod_database_code 2243208 _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 0.957 _shelx_estimated_absorpt_t_max 0.981 _shelx_hkl_file ; -1 0 0 2.80 0.40 -1 0 0 2.90 0.80 -1 0 0 2.30 0.40 1 0 0 3.20 0.30 1 0 0 1.30 0.70 1 0 0 2.40 0.40 -2 0 0 247.48 10.80 -2 0 0 223.48 10.80 -2 0 0 245.78 11.50 2 0 0 230.78 11.40 2 0 0 217.68 10.70 2 0 0 249.18 10.70 -3 0 0 28.10 2.80 -3 0 0 25.90 3.10 -3 0 0 27.90 1.90 -3 0 0 23.30 1.80 3 0 0 28.30 1.60 -4 0 0 17.20 1.60 -4 0 0 17.50 2.70 -4 0 0 16.30 1.70 -4 0 0 13.90 2.70 -5 0 0 139.59 7.00 -5 0 0 130.29 8.30 -5 0 0 136.79 8.60 -5 0 0 138.89 6.90 -6 0 0 3.20 3.10 -6 0 0 2.70 2.30 -6 0 0 1.00 1.20 -6 0 0 1.80 1.40 -7 0 0 5.70 1.80 -7 0 0 4.70 1.60 -7 0 0 2.50 2.90 -7 0 0 0.90 3.60 -8 0 0 96.29 8.30 -8 0 0 95.49 9.50 -8 1 0 0.10 1.60 -8 1 0 1.40 2.80 -8 1 0 2.00 4.20 -8 1 0 1.30 1.60 -7 1 0 36.90 3.00 -7 1 0 34.60 3.60 -7 1 0 39.00 5.20 -7 1 0 30.70 3.20 -7 1 0 26.40 5.10 -6 1 0 7.00 1.50 -6 1 0 3.70 2.80 -6 1 0 8.20 1.50 -6 1 0 7.10 2.00 -6 1 0 4.10 3.00 -5 1 0 13.90 1.70 -5 1 0 15.90 3.40 -5 1 0 14.70 1.70 -5 1 0 16.80 2.10 -4 1 0 345.77 16.60 -4 1 0 341.07 15.20 -4 1 0 298.17 15.00 -4 1 0 318.67 15.10 3 -1 0 122.09 5.30 3 -1 0 121.19 5.40 -3 1 0 105.29 6.70 -3 1 0 106.89 5.60 -3 1 0 117.69 5.80 -3 1 0 118.99 5.80 2 -1 0 8418.86 391.36 2 -1 0 9205.98 391.76 -2 1 0 8676.73 391.56 -2 1 0 8905.11 391.96 -2 1 0 8514.75 391.46 -2 1 0 8834.82 391.66 1 -1 0 145.89 7.40 1 -1 0 136.59 7.40 1 -1 0 155.88 7.40 -1 1 0 146.59 7.40 -1 1 0 147.49 7.40 -1 1 0 147.19 7.40 -1 1 0 144.19 8.00 0 -1 0 654.53 30.80 0 -1 0 681.33 30.50 0 -1 0 690.73 30.50 0 -1 0 672.23 30.50 0 -1 0 697.83 30.50 0 1 0 669.43 30.50 0 1 0 701.13 30.50 0 1 0 673.43 30.50 0 1 0 646.04 30.40 0 1 0 676.23 30.80 0 1 0 681.23 30.50 -1 -1 0 574.44 25.60 -1 -1 0 554.24 25.50 -1 -1 0 606.44 25.40 -1 -1 0 562.44 25.70 1 1 0 572.44 25.40 1 1 0 549.25 25.50 1 1 0 562.44 25.70 1 1 0 548.45 25.50 1 1 0 530.35 25.50 -2 -1 0 0.40 1.00 -2 -1 0 0.50 0.60 -2 -1 0 -0.60 0.90 -2 -1 0 1.00 0.60 -2 -1 0 0.50 0.90 2 1 0 0.20 0.80 2 1 0 0.60 0.50 2 1 0 1.20 0.90 2 1 0 1.30 0.60 -3 -1 0 52.79 3.10 -3 -1 0 54.59 4.20 -3 -1 0 57.59 3.20 -3 -1 0 50.79 4.20 -3 -1 0 49.80 3.40 3 1 0 50.49 3.90 3 1 0 53.79 3.00 -4 -1 0 38.30 3.80 -4 -1 0 36.80 2.60 -4 -1 0 40.30 2.70 -4 -1 0 39.10 3.80 -4 -1 0 33.70 3.10 -5 -1 0 7.90 1.50 -5 -1 0 8.00 2.30 -5 -1 0 7.90 2.90 -5 -1 0 7.00 1.40 -6 -1 0 1.10 1.30 -6 -1 0 3.80 2.40 -6 -1 0 -0.40 2.60 -6 -1 0 2.80 1.60 -7 -1 0 2.10 2.60 -7 -1 0 0.10 1.90 -7 -1 0 0.10 3.50 -8 -1 0 10.80 4.20 -8 -1 0 8.30 4.70 -9 2 0 5.60 3.40 -9 2 0 2.20 1.80 -9 2 0 2.60 4.70 -8 2 0 5.60 1.90 -8 2 0 6.50 3.50 -8 2 0 3.40 1.80 -8 2 0 5.90 4.70 -7 2 0 1.40 3.40 -7 2 0 0.80 1.50 -7 2 0 -0.10 1.80 -7 2 0 3.00 1.60 -7 2 0 1.30 2.50 -6 2 0 37.00 3.10 -6 2 0 45.80 5.70 -6 2 0 39.70 3.20 -6 2 0 36.90 3.40 -5 2 0 -1.10 1.10 -5 2 0 -0.50 2.10 -5 2 0 -2.30 1.30 -5 2 0 -0.60 1.00 -4 2 0 173.58 8.20 -4 2 0 167.68 8.10 -4 2 0 151.58 9.40 -4 2 0 162.48 8.20 3 -2 0 940.21 43.50 3 -2 0 967.30 43.70 -3 2 0 938.61 43.70 -3 2 0 962.50 43.70 -3 2 0 1022.00 43.70 2 -2 0 9549.64 411.86 2 -2 0 9999.00 412.16 2 -2 0 8376.96 411.76 -2 2 0 9297.37 412.26 -2 2 0 8951.40 411.86 -2 2 0 9152.68 414.36 -2 2 0 9180.88 412.26 1 -2 0 227.18 10.80 1 -2 0 219.78 10.90 1 -2 0 242.58 10.80 1 -2 0 213.48 11.40 -1 2 0 232.68 10.80 -1 2 0 233.68 10.90 -1 2 0 238.78 11.50 -1 2 0 226.68 10.80 -1 2 0 242.88 10.90 0 -2 0 169.68 8.10 0 -2 0 157.38 8.60 0 -2 0 179.58 8.10 0 -2 0 173.08 8.10 0 -2 0 164.38 8.10 0 2 0 166.28 7.90 0 2 0 165.88 8.10 0 2 0 168.78 8.10 0 2 0 162.88 8.60 0 2 0 168.78 8.10 0 2 0 170.28 8.00 -1 -2 0 64.39 3.50 -1 -2 0 62.29 3.50 -1 -2 0 55.99 4.50 -1 -2 0 58.49 3.50 -1 -2 0 62.79 3.60 -1 -2 0 61.39 3.40 1 2 0 62.59 3.30 1 2 0 57.79 3.40 1 2 0 61.09 3.50 1 2 0 58.39 3.50 -2 -2 0 57.99 3.50 -2 -2 0 58.39 3.90 -2 -2 0 60.69 4.10 -2 -2 0 57.99 3.70 2 2 0 57.99 3.50 2 2 0 56.79 3.70 -3 -2 0 118.89 7.10 -3 -2 0 121.29 7.20 -3 -2 0 135.59 6.50 3 2 0 119.19 6.90 3 2 0 124.89 6.40 -4 -2 0 1.90 1.20 -4 -2 0 1.50 1.80 -4 -2 0 3.10 2.10 4 2 0 2.30 1.00 -5 -2 0 44.10 3.50 -5 -2 0 40.50 4.70 -5 -2 0 40.60 4.90 -6 -2 0 316.97 17.10 -6 -2 0 301.47 15.20 -6 -2 0 317.27 16.90 -7 -2 0 36.60 5.70 -7 -2 0 51.49 6.20 -8 -2 0 94.79 9.10 -8 -2 0 84.69 8.60 -9 3 0 11.60 3.80 -9 3 0 20.90 6.30 -9 3 0 17.40 2.50 -8 3 0 17.40 2.40 -8 3 0 11.70 2.40 -8 3 0 17.00 5.10 -7 3 0 10.20 2.00 -7 3 0 12.70 4.40 -7 3 0 9.40 2.20 -7 3 0 11.10 2.10 -6 3 0 148.69 7.70 -6 3 0 125.69 7.50 -6 3 0 156.98 7.90 -6 3 0 144.89 9.90 -5 3 0 155.98 8.40 -5 3 0 168.38 10.00 -5 3 0 159.68 8.30 -5 3 0 163.48 8.20 4 -3 0 2970.20 132.99 4 -3 0 3034.50 133.29 -4 3 0 2764.92 133.39 -4 3 0 2976.10 133.19 -4 3 0 3093.89 133.39 3 -3 0 39.10 3.00 3 -3 0 37.70 2.80 -3 3 0 44.10 2.90 -3 3 0 41.60 3.00 -3 3 0 43.10 3.10 -3 3 0 36.10 4.60 2 -3 0 38.20 4.10 2 -3 0 45.00 2.80 2 -3 0 37.30 3.80 2 -3 0 43.10 2.90 -2 3 0 45.40 3.00 -2 3 0 42.90 4.20 -2 3 0 41.40 2.90 -2 3 0 41.10 2.90 -2 3 0 41.00 3.00 1 -3 0 0.10 1.00 1 -3 0 0.60 1.00 1 -3 0 1.00 1.70 1 -3 0 -0.10 1.00 1 -3 0 0.40 0.90 -1 3 0 0.40 0.80 -1 3 0 0.80 1.40 -1 3 0 0.30 0.90 -1 3 0 1.30 1.10 -1 3 0 0.50 0.90 0 -3 0 36.80 2.90 0 -3 0 35.10 3.50 0 -3 0 39.10 2.60 0 -3 0 39.70 2.80 0 -3 0 36.40 2.70 0 3 0 35.00 2.50 0 3 0 35.70 3.40 0 3 0 32.60 2.60 0 3 0 32.00 2.40 0 3 0 36.70 2.70 0 3 0 39.90 2.60 -1 -3 0 111.49 5.90 -1 -3 0 108.09 5.70 -1 -3 0 111.59 6.10 -1 -3 0 112.79 6.00 -1 -3 0 100.29 7.30 -1 -3 0 119.49 6.00 1 3 0 102.19 5.90 1 3 0 106.99 5.80 1 3 0 109.69 5.80 -2 -3 0 21.50 2.60 -2 -3 0 13.90 1.80 -2 -3 0 15.90 2.40 -2 -3 0 12.60 1.90 -2 -3 0 13.40 3.70 2 3 0 16.50 2.20 2 3 0 17.30 2.10 2 3 0 15.50 2.00 -3 -3 0 29.20 4.70 -3 -3 0 36.00 3.60 -3 -3 0 28.70 3.40 -3 -3 0 30.60 2.80 -3 -3 0 38.10 3.10 3 3 0 27.80 2.60 -4 -3 0 62.79 7.60 -4 -3 0 64.79 5.10 -4 -3 0 66.49 4.50 -4 -3 0 63.79 4.20 -4 -3 0 60.19 5.00 4 3 0 51.19 3.90 -5 -3 0 136.39 7.50 -5 -3 0 133.19 8.80 -5 -3 0 129.39 7.60 -5 -3 0 126.69 8.80 -5 -3 0 133.29 11.90 -6 -3 0 31.20 5.00 -6 -3 0 26.80 4.70 -6 -3 0 22.60 3.20 -6 -3 0 45.10 7.70 -7 -3 0 6.80 4.00 -9 4 0 4.60 5.30 -9 4 0 -0.10 2.00 -8 4 0 68.49 5.10 -8 4 0 48.80 7.30 -7 4 0 48.40 4.10 -7 4 0 45.10 6.30 -7 4 0 48.00 4.30 -7 4 0 39.10 3.90 -6 4 0 6.00 3.50 -6 4 0 15.70 2.30 -6 4 0 10.10 2.20 -6 4 0 9.90 2.30 -5 4 0 73.99 4.60 -5 4 0 72.99 4.80 -5 4 0 72.19 4.80 -5 4 0 67.19 6.20 4 -4 0 160.08 8.40 -4 4 0 154.18 8.80 -4 4 0 179.28 8.80 -4 4 0 182.68 8.70 3 -4 0 6.20 1.50 -3 4 0 8.80 1.70 -3 4 0 7.50 3.10 -3 4 0 5.40 1.60 -3 4 0 7.20 1.70 2 -4 0 28.60 3.80 2 -4 0 25.80 4.50 -2 4 0 29.00 2.90 -2 4 0 28.40 2.80 -2 4 0 31.10 4.60 -2 4 0 28.30 2.80 1 -4 0 25.20 2.70 1 -4 0 30.40 4.50 1 -4 0 26.10 2.80 1 -4 0 29.60 2.70 -1 4 0 25.50 3.50 -1 4 0 22.30 2.70 -1 4 0 26.70 2.70 -1 4 0 21.00 2.60 0 -4 0 65.89 4.00 0 -4 0 61.19 4.10 0 -4 0 54.59 5.20 0 -4 0 54.39 3.90 0 4 0 52.89 3.90 0 4 0 55.99 3.90 0 4 0 50.79 4.80 0 4 0 58.79 3.70 0 4 0 61.19 3.90 -1 -4 0 47.40 5.30 -1 -4 0 46.60 3.80 -1 -4 0 53.89 4.00 -1 -4 0 55.39 3.80 -1 -4 0 48.70 3.40 1 4 0 50.29 3.70 1 4 0 45.90 3.40 1 4 0 50.19 3.70 -2 -4 0 18.70 4.20 -2 -4 0 17.60 2.20 -2 -4 0 24.00 3.10 -2 -4 0 23.10 2.60 -2 -4 0 19.10 2.40 2 4 0 24.10 2.80 2 4 0 18.30 2.30 -3 -4 0 14.90 2.60 -3 -4 0 12.70 2.60 -3 -4 0 10.20 3.70 -3 -4 0 12.00 2.20 -3 -4 0 12.60 2.10 3 4 0 13.30 2.00 -4 -4 0 506.15 28.90 -4 -4 0 524.35 25.20 -4 -4 0 550.24 25.00 -4 -4 0 521.05 25.40 -4 -4 0 534.65 26.00 -5 -4 0 44.40 5.30 -5 -4 0 49.40 5.20 -5 -4 0 66.49 8.80 -5 -4 0 43.70 4.80 -6 -4 0 62.29 10.50 -6 -4 0 33.20 5.10 -6 -4 0 52.79 5.80 -9 5 0 78.89 6.00 -9 5 0 72.09 9.80 -8 5 0 64.79 5.50 -8 5 0 55.79 7.70 -7 5 0 57.39 5.10 -7 5 0 51.79 4.40 -7 5 0 62.29 7.90 -6 5 0 576.54 30.20 -6 5 0 598.94 27.90 -6 5 0 565.24 28.30 -6 5 0 641.74 28.30 -5 5 0 91.09 6.20 -5 5 0 99.79 6.00 -5 5 0 106.89 6.20 4 -5 0 12.70 1.90 -4 5 0 18.40 2.40 -4 5 0 14.20 2.20 -4 5 0 13.10 2.20 3 -5 0 9.10 3.10 3 -5 0 7.00 2.40 -3 5 0 7.00 1.70 -3 5 0 5.70 1.70 -3 5 0 8.20 3.20 -3 5 0 10.30 1.90 2 -5 0 0.70 2.70 2 -5 0 0.10 1.40 2 -5 0 -0.10 1.40 -2 5 0 -0.80 1.40 -2 5 0 0.90 1.50 -2 5 0 -0.90 1.50 -2 5 0 1.20 2.20 1 -5 0 75.79 5.00 1 -5 0 80.19 6.80 1 -5 0 81.99 5.20 -1 5 0 79.09 5.90 -1 5 0 74.39 5.20 -1 5 0 78.59 4.90 -1 5 0 86.19 5.10 0 -5 0 9.90 2.00 0 -5 0 7.80 1.90 0 -5 0 8.00 1.80 0 -5 0 7.70 3.10 0 5 0 8.70 1.70 0 5 0 10.30 2.00 0 5 0 11.40 2.10 -1 -5 0 4.70 2.10 -1 -5 0 4.60 1.60 -1 -5 0 5.00 2.00 -1 -5 0 3.00 2.70 1 5 0 4.40 1.70 1 5 0 3.00 1.40 1 5 0 5.30 1.60 -2 -5 0 990.30 46.40 -2 -5 0 970.10 49.00 -2 -5 0 995.40 46.70 -2 -5 0 1006.10 46.00 -2 -5 0 1079.39 46.30 2 5 0 975.90 46.30 -3 -5 0 295.97 19.10 -3 -5 0 304.87 16.30 -3 -5 0 304.67 15.90 -3 -5 0 309.07 15.50 -3 -5 0 347.57 15.80 -4 -5 0 -6.40 2.40 -4 -5 0 3.40 2.40 -4 -5 0 -1.50 4.80 -4 -5 0 0.80 2.30 -5 -5 0 0.90 2.80 -5 -5 0 5.00 5.90 -5 -5 0 1.50 2.70 -5 -5 0 0.00 2.60 -6 -5 0 18.80 3.70 -6 -5 0 25.40 4.50 -8 6 0 75.99 6.40 -8 6 0 77.69 9.50 -7 6 0 20.00 3.00 -7 6 0 11.00 3.10 -7 6 0 16.50 4.90 -6 6 0 45.90 4.30 -5 6 0 3.40 2.00 -5 6 0 2.60 2.00 -5 6 0 0.60 2.10 4 -6 0 7.30 1.90 -4 6 0 5.20 2.10 -4 6 0 9.00 2.20 -4 6 0 12.10 2.30 3 -6 0 15.20 3.80 -3 6 0 12.70 2.40 -3 6 0 11.80 2.20 -3 6 0 11.00 2.30 2 -6 0 1.80 1.60 2 -6 0 3.50 3.20 2 -6 0 1.00 1.80 -2 6 0 2.70 1.70 -2 6 0 -0.30 1.50 -2 6 0 3.00 1.80 1 -6 0 8.50 2.30 1 -6 0 9.40 2.20 1 -6 0 9.80 3.70 -1 6 0 9.30 2.10 -1 6 0 11.70 2.20 -1 6 0 10.20 2.30 0 -6 0 92.89 6.30 0 -6 0 99.49 6.50 0 -6 0 107.09 7.20 0 -6 0 104.69 8.40 0 6 0 98.89 6.10 0 6 0 85.39 6.20 -1 -6 0 128.39 7.90 -1 -6 0 149.59 8.00 -1 -6 0 132.59 10.30 -1 -6 0 127.39 8.10 1 6 0 115.79 7.70 1 6 0 131.79 7.80 -2 -6 0 424.66 21.40 -2 -6 0 433.86 24.50 -2 -6 0 437.56 21.90 2 6 0 440.26 21.40 -3 -6 0 48.90 4.80 -3 -6 0 41.60 4.10 -3 -6 0 44.70 5.30 -3 -6 0 43.90 8.20 -4 -6 0 120.29 8.80 -4 -6 0 127.29 12.80 -4 -6 0 125.99 8.10 -4 -6 0 114.79 8.30 -5 -6 0 4.10 2.90 -5 -6 0 8.90 5.60 -5 -6 0 2.00 3.50 -8 7 0 97.19 10.50 -8 7 0 90.69 7.40 -7 7 0 9.10 4.50 -7 7 0 14.90 2.90 -7 7 0 5.60 2.90 -6 7 0 2.80 2.60 -6 7 0 7.20 2.50 -5 7 0 9.60 2.90 -5 7 0 15.60 3.00 -4 7 0 13.00 3.00 -4 7 0 12.70 2.70 3 -7 0 2.00 3.20 3 -7 0 1.00 1.90 -3 7 0 0.00 2.20 -3 7 0 0.30 1.90 -3 7 0 -3.80 2.10 2 -7 0 23.60 3.20 2 -7 0 26.10 5.40 2 -7 0 28.10 3.60 -2 7 0 29.80 3.80 -2 7 0 25.90 3.30 -2 7 0 23.30 3.20 1 -7 0 6.40 4.30 1 -7 0 4.80 2.20 1 -7 0 6.30 2.30 -1 7 0 6.20 2.10 -1 7 0 9.40 2.60 0 -7 0 2011.70 90.69 0 -7 0 1959.50 88.09 0 -7 0 1937.71 88.09 0 7 0 1793.02 87.79 -1 -7 0 1.40 2.40 -1 -7 0 0.00 2.50 -1 -7 0 3.50 4.20 1 7 0 6.80 2.70 1 7 0 -0.50 3.50 -2 -7 0 18.10 3.90 -2 -7 0 18.30 5.60 -2 -7 0 20.50 3.90 2 7 0 21.70 3.70 -3 -7 0 9.20 5.00 -3 -7 0 7.10 3.00 -3 -7 0 9.10 4.20 -4 -7 0 6.50 5.40 -4 -7 0 -0.90 2.90 -4 -7 0 -7.90 3.00 -5 -7 0 37.80 5.10 -5 -7 0 33.30 5.80 -8 8 0 6.10 4.90 -8 8 0 -1.20 3.00 -7 8 0 0.20 2.90 -7 8 0 4.80 3.10 -7 8 0 4.20 4.30 -6 8 0 -1.20 2.90 -6 8 0 -0.80 2.70 -5 8 0 -2.30 2.60 -5 8 0 0.80 2.70 4 -8 0 84.89 8.40 -4 8 0 78.19 5.90 -4 8 0 58.69 5.90 3 -8 0 1.70 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-5 10 3 1.80 3.50 -4 10 3 2.90 3.40 -4 10 3 -5.00 3.40 3 -10 -3 5.40 2.90 -3 10 3 4.20 3.30 -3 10 3 -1.90 3.50 2 -10 -3 9.40 3.50 -2 10 3 10.20 3.70 1 -10 -3 126.29 9.60 -1 10 3 119.79 9.40 1 -11 4 14.90 3.60 1 -11 4 2.20 8.50 2 -11 4 12.90 7.80 -3 11 -4 3.70 3.90 -2 -10 4 -13.50 7.50 -2 -10 4 1.70 3.30 -2 -10 4 -0.80 2.90 -1 -10 4 -0.40 3.10 -1 -10 4 -13.40 7.20 -1 -10 4 0.10 2.70 0 -10 4 1.10 2.40 0 -10 4 -10.70 6.80 1 -10 4 7.40 7.90 1 -10 4 19.50 3.70 -2 10 -4 1.30 3.80 2 -10 4 4.90 6.60 -3 10 -4 10.00 5.10 -3 10 -4 5.70 3.90 -3 10 -4 11.40 3.70 3 -10 4 19.90 6.60 -4 10 -4 4.70 3.50 -4 10 -4 1.20 3.30 -4 10 -4 1.30 3.20 4 -10 4 14.40 6.10 -5 10 -4 1.10 3.40 -5 10 -4 11.90 3.60 -5 10 -4 8.40 4.40 -3 -9 4 30.90 10.50 -3 -9 4 28.50 5.00 -3 -9 4 36.50 5.40 -2 -9 4 5.40 3.30 -2 -9 4 -4.20 7.40 -2 -9 4 0.00 2.50 -1 -9 4 2.70 3.30 -1 -9 4 3.20 2.40 -1 -9 4 -8.40 6.60 0 -9 4 14.10 3.20 0 -9 4 7.70 7.40 0 -9 4 12.70 3.50 1 -9 4 -0.30 6.50 1 -9 4 4.00 2.30 -2 9 -4 1.10 3.10 -2 9 -4 1.30 3.00 -2 9 -4 -0.60 2.30 2 -9 4 -1.90 5.80 -3 9 -4 6.80 3.40 -3 9 -4 10.00 3.40 -3 9 -4 5.90 3.20 3 -9 4 14.00 5.90 -4 9 -4 -0.10 3.40 -4 9 -4 10.40 3.20 -4 9 -4 8.60 3.60 4 -9 4 13.30 5.90 -5 9 -4 -0.90 3.80 -5 9 -4 -4.60 3.10 -5 9 -4 3.20 2.70 -6 9 -4 1.40 3.50 -6 9 -4 3.30 4.10 -4 -8 4 10.70 7.40 -4 -8 4 3.00 4.00 -4 -8 4 20.50 4.20 -3 -8 4 17.20 4.00 -3 -8 4 18.10 3.90 -3 -8 4 21.50 9.00 -2 -8 4 7.60 3.30 -2 -8 4 12.10 3.40 -2 -8 4 3.10 6.40 -1 -8 4 30.60 4.20 -1 -8 4 36.50 9.30 -1 -8 4 35.70 4.20 0 -8 4 2.30 2.50 0 -8 4 1.80 6.20 0 -8 4 1.70 2.10 -1 8 -4 2.70 2.70 -1 8 -4 1.90 2.50 -1 8 -4 0.60 2.10 1 -8 4 2.60 2.80 1 -8 4 -3.60 5.00 1 -8 4 1.80 2.10 -2 8 -4 10.30 3.20 -2 8 -4 14.50 3.20 -2 8 -4 18.80 3.50 2 -8 4 16.20 6.60 2 -8 4 11.30 3.50 -3 8 -4 2.40 3.00 -3 8 -4 2.80 3.10 -3 8 -4 6.90 2.80 3 -8 4 10.00 5.40 -4 8 -4 13.10 3.80 -4 8 -4 12.70 2.90 -4 8 -4 10.20 3.90 4 -8 4 14.90 6.20 -5 8 -4 57.89 6.70 -5 8 -4 38.40 5.10 -5 8 -4 56.79 4.70 -6 8 -4 -1.20 4.30 -6 8 -4 -4.90 2.90 -7 8 -4 -1.70 3.30 -7 8 -4 -2.50 4.20 -5 -7 4 2.20 2.90 -5 -7 4 -1.50 6.40 -5 -7 4 -9.30 3.60 -4 -7 4 8.40 3.20 -4 -7 4 4.70 6.70 -4 -7 4 -2.30 3.30 -3 -7 4 48.90 9.70 -3 -7 4 52.29 5.50 -3 -7 4 45.70 5.70 -2 -7 4 29.20 4.20 -2 -7 4 31.10 7.70 -2 -7 4 27.50 3.60 -1 -7 4 7.60 2.30 -1 -7 4 8.20 2.80 -1 -7 4 13.40 6.70 0 7 -4 46.30 5.20 0 7 -4 56.99 3.90 0 -7 4 55.89 9.70 0 -7 4 54.79 5.40 0 -7 4 57.49 4.80 -1 7 -4 4.30 2.40 -1 7 -4 4.00 1.90 -1 7 -4 1.50 2.50 1 -7 4 4.40 2.40 1 -7 4 3.90 5.50 1 -7 4 5.90 2.10 -2 7 -4 39.20 4.10 -2 7 -4 32.20 4.30 -2 7 -4 40.80 4.50 2 -7 4 44.10 7.80 2 -7 4 39.20 4.60 -3 7 -4 0.40 2.20 -3 7 -4 -0.90 2.50 -3 7 -4 -2.40 2.50 3 -7 4 2.00 4.50 -4 7 -4 2.90 2.20 -4 7 -4 -0.40 3.20 -4 7 -4 2.20 2.60 4 -7 4 4.00 5.10 -5 7 -4 75.39 5.10 -5 7 -4 82.79 7.10 -5 7 -4 74.09 7.50 -6 7 -4 5.40 3.20 -6 7 -4 5.60 4.70 -7 7 -4 4.80 3.70 -7 7 -4 6.20 4.60 -6 -6 4 -4.50 3.20 -6 -6 4 6.40 7.50 -6 -6 4 2.90 2.80 -5 -6 4 -6.10 2.80 -5 -6 4 0.30 2.50 -5 -6 4 3.90 7.00 -4 -6 4 137.79 8.80 -4 -6 4 145.29 9.10 -4 -6 4 141.69 14.00 -3 -6 4 -0.60 2.40 -3 -6 4 -3.10 4.50 -3 -6 4 1.80 2.10 -2 -6 4 14.10 5.70 -2 -6 4 19.60 3.10 -2 -6 4 14.30 3.10 -2 -6 4 17.10 3.10 1 6 -4 22.70 3.10 -1 -6 4 27.30 3.40 -1 -6 4 24.50 3.50 -1 -6 4 20.90 3.10 -1 -6 4 24.40 6.30 0 6 -4 5.40 2.30 0 6 -4 7.90 1.60 0 -6 4 7.20 1.80 0 -6 4 8.40 4.50 0 -6 4 2.80 2.10 0 -6 4 7.40 2.30 -1 6 -4 0.10 1.60 -1 6 -4 1.50 2.00 1 -6 4 0.90 4.20 1 -6 4 2.80 2.00 -2 6 -4 3.80 1.90 -2 6 -4 3.20 2.20 -2 6 -4 5.40 2.30 -2 6 -4 4.90 2.30 2 -6 4 8.60 4.90 2 -6 4 2.80 2.10 -3 6 -4 130.29 8.90 -3 6 -4 145.39 8.50 -3 6 -4 132.99 9.10 -3 6 -4 146.89 7.80 3 -6 4 151.68 12.40 3 -6 4 142.29 8.40 -4 6 -4 17.70 2.50 -4 6 -4 13.60 3.70 -4 6 -4 15.50 3.20 -5 6 -4 25.50 4.00 -5 6 -4 28.60 5.10 -5 6 -4 24.10 2.60 -6 6 -4 2.70 3.90 -6 6 -4 2.30 2.90 -7 6 -4 9.70 4.70 -7 6 -4 4.70 3.20 -8 6 -4 -3.50 3.10 -7 -5 4 12.00 7.50 -7 -5 4 2.20 2.50 -7 -5 4 3.20 3.00 -6 -5 4 59.09 6.00 -6 -5 4 52.49 5.20 -6 -5 4 58.79 10.00 -5 -5 4 18.20 3.40 -5 -5 4 14.30 6.70 -5 -5 4 20.10 3.10 -4 -5 4 8.50 3.30 -4 -5 4 12.40 2.80 -4 -5 4 13.30 6.00 -4 -5 4 8.30 2.40 -3 -5 4 68.69 8.80 -3 -5 4 62.49 5.00 -3 -5 4 58.69 5.00 -3 -5 4 68.99 5.30 -2 -5 4 31.60 3.50 -2 -5 4 30.80 3.50 -2 -5 4 22.30 2.90 -2 -5 4 29.30 5.80 1 5 -4 67.79 5.10 -1 -5 4 74.89 4.90 -1 -5 4 88.09 5.50 -1 -5 4 71.19 8.30 -1 -5 4 72.49 5.30 0 5 -4 1.50 1.10 0 5 -4 2.10 1.80 0 -5 4 -0.60 1.20 0 -5 4 -0.70 1.60 0 -5 4 0.90 1.60 0 -5 4 2.00 3.70 -1 5 -4 -0.90 1.50 -1 5 -4 0.60 1.60 -1 5 -4 -3.00 1.50 1 -5 4 0.80 3.50 1 -5 4 -1.10 1.60 -2 5 -4 28.50 3.60 -2 5 -4 26.30 3.50 -2 5 -4 32.10 3.40 2 -5 4 33.60 6.10 2 -5 4 29.80 3.40 -3 5 -4 4.00 2.80 -3 5 -4 8.50 1.80 -3 5 -4 7.40 2.20 -3 5 -4 6.20 2.30 3 -5 4 8.10 2.10 3 -5 4 10.50 4.60 -4 5 -4 4.60 2.20 -4 5 -4 2.20 2.10 -4 5 -4 1.00 2.60 4 -5 4 0.30 1.70 4 -5 4 1.30 1.40 -5 5 -4 81.89 7.50 -5 5 -4 74.09 6.40 -6 5 -4 3.30 3.80 -6 5 -4 4.00 2.80 -7 5 -4 7.00 3.20 -7 5 -4 1.30 4.30 -8 5 -4 39.00 7.70 -8 5 -4 27.20 4.60 -7 -4 4 0.20 2.70 -7 -4 4 0.90 2.10 -7 -4 4 11.00 7.10 -6 -4 4 124.79 8.20 -6 -4 4 104.09 7.20 -6 -4 4 136.79 13.50 -5 -4 4 47.80 4.60 -5 -4 4 48.10 8.90 -5 -4 4 45.90 4.10 -5 -4 4 45.80 4.30 -4 -4 4 17.70 2.50 -4 -4 4 15.10 5.20 -4 -4 4 17.00 2.50 -4 -4 4 17.30 2.50 3 4 -4 4.40 1.50 -3 -4 4 5.70 1.80 -3 -4 4 5.50 1.70 -3 -4 4 4.90 3.90 -3 -4 4 2.50 1.70 2 4 -4 0.40 1.30 -2 -4 4 0.20 1.40 -2 -4 4 1.40 3.00 -2 -4 4 -0.80 1.30 -2 -4 4 0.50 1.50 1 4 -4 161.08 9.20 -1 -4 4 178.18 12.20 -1 -4 4 179.58 8.90 -1 -4 4 167.58 9.20 -1 -4 4 182.48 9.50 0 4 -4 7.40 2.30 0 4 -4 9.70 1.60 0 4 -4 4.50 1.90 0 -4 4 11.20 4.60 0 -4 4 6.50 2.00 0 -4 4 6.90 1.50 0 -4 4 7.70 2.10 -1 4 -4 58.99 4.30 -1 4 -4 59.29 4.20 -1 4 -4 54.99 4.50 1 -4 4 53.79 4.50 1 -4 4 63.59 7.80 1 -4 4 55.49 4.50 -2 4 -4 11.60 2.30 -2 4 -4 16.70 2.50 -2 4 -4 10.40 2.40 2 -4 4 13.90 2.40 2 -4 4 11.00 1.60 2 -4 4 12.00 4.00 -3 4 -4 7.70 2.60 -3 4 -4 7.00 2.20 -3 4 -4 6.40 1.80 3 -4 4 6.90 4.10 3 -4 4 7.60 1.20 -4 4 -4 53.49 4.70 -4 4 -4 54.69 4.50 -4 4 -4 50.59 5.60 4 -4 4 56.69 4.20 4 -4 4 57.39 3.20 -5 4 -4 12.70 3.90 -5 4 -4 17.00 3.20 -5 4 -4 12.70 2.70 -6 4 -4 8.30 3.00 -6 4 -4 8.40 4.30 -7 4 -4 2.00 2.80 -7 4 -4 3.60 4.80 -8 4 -4 6.30 5.00 -8 4 -4 5.00 3.50 -8 4 -4 0.50 3.10 -8 -3 4 165.18 15.80 -8 -3 4 130.69 9.90 -7 -3 4 14.10 7.00 -7 -3 4 0.70 2.30 -7 -3 4 0.50 1.80 -6 -3 4 0.30 2.10 -6 -3 4 1.30 4.70 -6 -3 4 -1.10 1.80 -6 -3 4 -1.00 1.30 -6 -3 4 -0.30 1.60 -5 -3 4 19.50 2.80 -5 -3 4 25.10 2.90 -5 -3 4 23.90 6.30 -5 -3 4 16.10 2.40 -5 -3 4 25.00 3.00 -4 -3 4 32.30 6.10 -4 -3 4 27.40 2.90 -4 -3 4 30.10 2.60 -4 -3 4 28.80 3.10 -4 -3 4 27.00 3.00 3 3 -4 5.90 1.30 -3 -3 4 6.00 0.80 -3 -3 4 5.10 1.50 -3 -3 4 4.60 3.30 -3 -3 4 6.20 1.40 -3 -3 4 4.30 1.50 2 3 -4 -0.10 0.80 2 3 -4 -1.30 1.00 -2 -3 4 1.00 2.80 -2 -3 4 -1.00 1.30 -2 -3 4 -0.90 1.30 -2 -3 4 2.30 1.20 1 3 -4 16.50 1.40 1 3 -4 14.90 1.90 -1 -3 4 14.60 2.30 -1 -3 4 17.70 2.10 -1 -3 4 13.70 2.30 -1 -3 4 14.80 4.30 0 3 -4 1.40 1.50 0 3 -4 -1.70 1.40 0 3 -4 1.60 1.10 0 3 -4 2.50 1.30 0 -3 4 6.40 4.00 0 -3 4 0.90 1.30 0 -3 4 0.60 1.30 0 -3 4 0.60 1.50 0 -3 4 0.50 1.60 -1 3 -4 52.49 4.40 -1 3 -4 56.99 4.30 -1 3 -4 56.29 4.20 -1 3 -4 53.69 3.50 1 -3 4 52.29 4.30 1 -3 4 51.29 7.10 1 -3 4 55.69 4.20 1 -3 4 56.49 4.30 1 -3 4 59.09 3.40 -2 3 -4 66.69 4.50 -2 3 -4 66.19 4.80 -2 3 -4 64.99 5.30 2 -3 4 70.39 3.70 2 -3 4 67.19 7.50 2 -3 4 71.99 4.50 -3 3 -4 26.70 3.90 -3 3 -4 29.40 3.20 -3 3 -4 34.00 3.70 3 -3 4 36.20 2.00 -4 3 -4 5.90 2.10 -4 3 -4 4.80 1.80 -4 3 -4 5.10 3.10 4 -3 4 5.20 1.70 -5 3 -4 31.30 3.60 -5 3 -4 26.30 4.90 -5 3 -4 28.20 3.70 -6 3 -4 48.10 7.00 -6 3 -4 44.10 5.10 -7 3 -4 12.00 3.30 -7 3 -4 16.60 4.40 -7 3 -4 13.80 5.10 -8 3 -4 18.40 6.10 -8 3 -4 20.60 3.80 -8 3 -4 11.00 3.90 -8 -2 4 1.10 1.40 -8 -2 4 4.00 1.60 -8 -2 4 19.50 7.40 -8 -2 4 4.20 2.90 -7 -2 4 33.60 8.10 -7 -2 4 31.00 4.20 -7 -2 4 22.50 2.50 -7 -2 4 15.70 2.20 -7 -2 4 23.30 3.90 -6 -2 4 37.90 4.20 -6 -2 4 36.80 4.40 -6 -2 4 38.60 8.10 -6 -2 4 34.80 3.10 -6 -2 4 39.70 2.90 -5 -2 4 11.50 4.50 -5 -2 4 8.40 1.50 -5 -2 4 9.70 2.10 -5 -2 4 8.70 2.30 -5 -2 4 8.60 1.60 -4 -2 4 1.60 1.10 -4 -2 4 1.30 1.10 -4 -2 4 1.80 1.10 -4 -2 4 -1.50 2.40 -4 -2 4 1.10 1.40 3 2 -4 210.78 10.30 3 2 -4 208.28 10.70 -3 -2 4 224.28 10.60 -3 -2 4 216.68 10.60 -3 -2 4 218.58 10.70 -3 -2 4 218.78 13.20 2 2 -4 3.40 1.00 2 2 -4 4.50 1.20 -2 -2 4 6.40 1.10 -2 -2 4 3.90 1.50 -2 -2 4 4.80 1.00 -2 -2 4 4.30 1.40 -2 -2 4 4.30 2.80 1 2 -4 0.90 0.60 1 2 -4 0.40 2.10 1 2 -4 0.30 0.90 1 2 -4 -0.20 1.10 -1 -2 4 0.70 0.90 -1 -2 4 -1.00 1.30 -1 -2 4 -0.40 1.20 -1 -2 4 0.40 0.70 -1 -2 4 2.00 2.70 0 2 -4 54.99 3.80 0 2 -4 57.29 3.10 0 2 -4 56.09 3.80 0 2 -4 62.99 3.80 0 2 -4 53.89 5.40 0 -2 4 57.39 6.30 0 -2 4 55.29 3.60 0 -2 4 54.89 3.80 0 -2 4 53.39 3.70 -1 2 -4 107.99 6.20 -1 2 -4 96.99 5.70 -1 2 -4 107.19 6.00 1 -2 4 98.29 5.80 1 -2 4 101.19 5.80 1 -2 4 98.39 6.00 1 -2 4 96.49 7.90 -2 2 -4 0.40 1.30 -2 2 -4 1.40 1.50 -2 2 -4 0.00 2.20 2 -2 4 0.10 1.40 2 -2 4 0.10 0.60 -3 2 -4 124.59 7.90 -3 2 -4 110.49 6.80 -3 2 -4 107.19 6.40 -4 2 -4 63.69 4.80 -4 2 -4 56.69 4.40 -4 2 -4 62.09 6.30 4 -2 4 65.29 4.20 -5 2 -4 -3.00 3.00 -5 2 -4 -0.30 1.80 -5 2 -4 -1.70 1.70 -6 2 -4 -2.50 3.50 -6 2 -4 0.80 2.30 -6 2 -4 3.70 3.10 -7 2 -4 220.98 12.00 -7 2 -4 206.38 13.50 -7 2 -4 196.78 14.30 -8 2 -4 -2.20 5.30 -8 2 -4 -2.20 2.80 -8 2 -4 0.60 3.30 -8 -1 4 14.30 3.40 -8 -1 4 12.30 3.90 -8 -1 4 26.50 7.20 -7 -1 4 7.80 3.10 -7 -1 4 11.70 5.80 -7 -1 4 6.50 1.20 -7 -1 4 4.90 1.00 -7 -1 4 6.80 2.60 -6 -1 4 0.00 0.80 -6 -1 4 0.10 1.00 -6 -1 4 -0.10 1.70 -6 -1 4 -0.20 2.30 -6 -1 4 -1.40 3.50 -5 -1 4 120.99 7.20 -5 -1 4 114.69 5.70 -5 -1 4 108.39 9.40 -5 -1 4 111.49 5.80 -5 -1 4 110.09 6.70 -4 -1 4 42.00 5.20 -4 -1 4 48.70 3.40 -4 -1 4 48.90 3.00 -4 -1 4 49.10 3.00 3 1 -4 156.58 6.90 -3 -1 4 152.38 7.40 -3 -1 4 139.49 7.30 -3 -1 4 135.59 9.30 -3 -1 4 141.59 7.30 2 1 -4 12.80 2.80 2 1 -4 13.30 1.40 -2 -1 4 12.50 1.50 -2 -1 4 12.20 1.20 -2 -1 4 12.70 1.60 -2 -1 4 9.90 1.60 -2 -1 4 9.90 2.80 1 1 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11 8.60 3.00 -4 -1 11 8.10 3.40 -4 -1 11 3.00 6.10 -3 -1 11 2.90 2.70 -3 -1 11 8.20 5.30 -3 -1 11 -0.30 2.60 2 1 -11 133.89 9.20 -2 -1 11 143.49 9.00 -2 -1 11 141.39 12.50 -2 -1 11 138.29 9.00 1 1 -11 6.70 3.70 -1 -1 11 12.60 3.10 -1 -1 11 7.50 3.20 -1 -1 11 15.60 5.90 0 1 -11 -1.30 3.40 0 -1 11 -1.80 2.20 0 -1 11 0.60 2.80 -1 1 -11 4.50 4.70 -2 1 -11 1.10 4.70 -3 1 -11 40.20 7.60 -7 0 11 3.10 2.30 -7 0 11 5.70 4.50 -6 0 11 1.80 4.10 -6 0 11 -1.90 2.10 -5 0 11 10.70 7.10 -5 0 11 14.20 4.40 -5 0 11 16.40 3.30 -4 0 11 161.18 12.90 -4 0 11 137.99 10.00 -4 0 11 156.38 9.50 -3 0 11 12.40 4.80 -3 0 11 9.30 3.50 -3 0 11 11.40 3.20 2 0 -11 18.40 3.90 -2 0 11 20.90 3.80 -2 0 11 31.80 6.50 -2 0 11 21.80 3.80 1 0 -11 27.20 4.80 -1 0 11 32.10 4.10 -1 0 11 30.50 4.30 0 0 -11 0.50 4.00 0 0 11 2.50 2.30 0 0 11 -1.60 2.90 -1 0 -11 19.90 5.30 -2 0 -11 3.70 5.00 -3 0 -11 -1.60 5.40 -7 1 11 2.70 2.20 -7 1 11 8.40 4.60 -6 1 11 -0.70 2.30 -6 1 11 -3.00 3.80 -5 1 11 -2.10 2.30 -5 1 11 2.50 3.20 -4 1 11 -2.30 2.50 -4 1 11 2.10 2.90 -3 1 11 6.90 3.10 -3 1 11 10.80 3.50 2 -1 -11 21.80 4.50 -2 1 11 21.60 3.90 -2 1 11 17.60 3.60 1 -1 -11 7.30 3.60 -1 1 11 3.40 2.60 -1 1 11 6.70 3.30 0 -1 -11 -3.10 3.50 0 1 11 3.50 2.80 0 1 11 1.40 2.20 -1 -1 -11 2.00 4.40 -2 -1 -11 0.10 5.00 -3 -1 -11 -6.30 6.00 -7 2 11 1.90 2.20 -7 2 11 4.20 4.30 -6 2 11 56.49 5.20 -6 2 11 60.79 7.20 -5 2 11 1.60 3.50 -5 2 11 -1.50 2.40 -4 2 11 1.40 2.70 -4 2 11 3.30 3.40 -3 2 11 4.40 3.00 -3 2 11 3.10 2.80 -2 2 11 11.00 3.50 -2 2 11 10.60 3.30 1 -2 -11 18.80 5.00 -1 2 11 11.30 3.00 -1 2 11 15.30 3.50 0 -2 -11 0.70 4.20 0 2 11 2.10 2.20 -1 -2 -11 5.00 5.30 -2 -2 -11 58.89 8.30 -6 3 11 3.20 4.00 -6 3 11 2.30 2.50 -5 3 11 -1.10 2.50 -5 3 11 -7.80 2.90 -4 3 11 0.80 2.70 -4 3 11 -3.30 2.80 -3 3 11 1.40 2.90 -3 3 11 -1.50 2.60 -2 3 11 0.00 2.60 -2 3 11 -0.80 2.60 1 -3 -11 6.50 4.00 -1 3 11 7.50 3.40 -1 3 11 7.60 2.90 0 -3 -11 35.30 6.20 0 3 11 23.60 3.80 -1 -3 -11 34.60 6.90 -6 4 11 -0.90 2.70 -6 4 11 0.80 4.10 -5 4 11 0.80 3.60 -5 4 11 3.60 2.90 -4 4 11 0.50 3.30 -4 4 11 5.60 3.20 -3 4 11 -1.50 2.90 -3 4 11 1.70 2.90 -2 4 11 4.00 2.90 -2 4 11 -2.10 3.20 -1 4 11 3.60 2.80 0 -4 -11 215.28 14.60 -5 5 11 0.70 3.50 -5 5 11 -3.80 2.70 -4 5 11 -2.40 2.80 -4 5 11 2.90 3.50 -3 5 11 2.70 3.40 -3 5 11 3.10 3.50 -2 5 11 126.49 12.40 -2 5 11 154.58 9.90 -2 -7 12 5.50 4.10 -2 -7 12 -3.00 8.90 -1 -7 12 2.60 3.60 -1 -7 12 5.00 7.80 0 -7 12 11.90 6.40 1 -7 12 13.20 7.50 -3 -6 12 -9.50 9.00 -3 -6 12 1.50 3.60 -2 -6 12 56.99 13.30 -2 -6 12 44.80 6.20 -1 -6 12 16.90 8.80 -1 -6 12 13.10 4.00 0 -6 12 7.70 6.30 1 -6 12 13.50 7.40 -2 6 -12 -6.00 4.30 2 -6 12 16.80 6.70 -4 -5 12 46.50 5.90 -4 -5 12 38.10 13.00 -3 -5 12 8.10 3.80 -3 -5 12 0.50 9.10 -2 -5 12 37.30 10.80 -2 -5 12 21.40 4.40 -1 -5 12 30.90 8.40 -1 -5 12 31.20 5.30 0 -5 12 9.30 7.00 0 -5 12 0.50 5.60 -1 5 -12 19.70 5.50 1 -5 12 34.70 9.20 -2 5 -12 5.60 5.20 -5 -4 12 40.00 5.00 -5 -4 12 7.20 10.40 -4 -4 12 1.80 3.20 -4 -4 12 -4.00 8.40 -3 -4 12 47.60 5.80 -3 -4 12 57.49 12.30 -2 -4 12 3.20 6.60 -2 -4 12 -2.80 3.10 1 4 -12 9.80 3.50 -1 -4 12 23.00 7.50 -1 -4 12 15.20 4.00 0 4 -12 0.70 3.60 0 -4 12 4.70 5.80 0 -4 12 1.60 3.50 -1 4 -12 10.60 5.10 1 -4 12 42.70 9.50 -2 4 -12 31.40 6.80 -3 4 -12 -4.90 5.30 -5 -3 12 16.50 9.90 -5 -3 12 32.70 4.60 -4 -3 12 50.79 5.70 -3 -3 12 7.70 3.40 -3 -3 12 14.40 7.90 2 3 -12 2.40 2.50 -2 -3 12 -2.40 3.00 -2 -3 12 6.00 5.80 1 3 -12 9.50 3.60 -1 -3 12 14.20 6.20 -1 -3 12 2.70 2.90 -1 -3 12 10.80 3.50 0 3 -12 -3.10 3.60 0 -3 12 13.10 6.20 0 -3 12 5.60 3.50 0 -3 12 1.60 2.60 -1 3 -12 -4.50 4.50 -2 3 -12 -9.10 4.20 -3 3 -12 -6.30 5.80 -6 -2 12 66.99 8.00 -6 -2 12 49.80 5.70 -5 -2 12 24.10 9.60 -5 -2 12 44.40 6.30 -5 -2 12 35.10 4.60 -4 -2 12 -2.10 3.50 -4 -2 12 2.10 2.90 -4 -2 12 -5.30 6.50 -3 -2 12 1.00 3.20 -3 -2 12 0.40 2.90 -3 -2 12 2.40 5.60 2 2 -12 22.50 4.20 -2 -2 12 18.10 3.90 -2 -2 12 23.60 4.10 -2 -2 12 29.00 7.20 1 2 -12 0.70 3.30 -1 -2 12 4.10 3.30 -1 -2 12 0.80 5.10 -1 -2 12 1.30 2.90 0 2 -12 22.00 5.10 0 -2 12 26.50 4.50 0 -2 12 23.60 4.30 -1 2 -12 4.00 5.00 -2 2 -12 -6.50 5.20 -3 2 -12 -5.10 5.40 -6 -1 12 3.40 2.80 -6 -1 12 -1.30 3.80 -5 -1 12 2.50 3.90 -5 -1 12 -3.30 7.40 -5 -1 12 1.70 2.80 -4 -1 12 16.90 3.90 -4 -1 12 15.30 4.40 -4 -1 12 18.10 6.40 -3 -1 12 20.00 4.30 -3 -1 12 21.10 4.10 -3 -1 12 31.40 6.90 2 1 -12 4.80 3.20 -2 -1 12 0.20 3.20 -2 -1 12 0.00 2.80 -2 -1 12 2.40 4.40 1 1 -12 9.00 4.00 -1 -1 12 10.60 3.20 -1 -1 12 12.50 3.80 0 1 -12 7.10 4.60 0 -1 12 8.70 4.10 -1 1 -12 0.90 4.40 -2 1 -12 2.20 5.30 -6 0 12 1.00 4.40 -6 0 12 1.50 2.80 -5 0 12 -1.70 3.30 -5 0 12 1.20 2.80 -4 0 12 52.39 5.60 -4 0 12 44.20 5.70 -3 0 12 43.60 5.30 -3 0 12 30.30 5.00 -3 0 12 54.69 8.00 2 0 -12 12.00 3.90 -2 0 12 8.60 3.40 -2 0 12 11.60 3.50 1 0 -12 23.30 5.20 -1 0 12 28.60 4.50 -1 0 12 23.10 3.90 0 0 -12 6.50 4.40 -1 0 -12 -0.60 4.40 -2 0 -12 21.60 7.20 -6 1 12 30.90 4.00 -6 1 12 38.30 6.40 -5 1 12 1.80 2.70 -5 1 12 0.60 3.50 -4 1 12 18.00 3.70 -4 1 12 25.30 4.60 -3 1 12 0.40 2.90 -3 1 12 0.10 2.90 2 -1 -12 48.50 6.10 -2 1 12 49.20 5.60 -2 1 12 38.00 4.90 1 -1 -12 8.40 4.00 -1 1 12 10.40 3.70 -1 1 12 4.50 2.70 0 -1 -12 1.50 4.20 -1 -1 -12 -0.50 4.50 -6 2 12 3.50 2.70 -6 2 12 6.30 4.40 -5 2 12 16.80 3.70 -5 2 12 13.60 4.50 -4 2 12 44.50 6.00 -4 2 12 47.40 5.60 -3 2 12 9.70 3.60 -3 2 12 2.10 3.10 -2 2 12 12.60 3.50 -2 2 12 11.40 3.50 1 -2 -12 8.30 4.20 -1 2 12 6.80 2.90 -1 2 12 4.80 3.50 0 -2 -12 -0.70 4.70 -1 -2 -12 32.40 7.10 -5 3 12 12.60 4.50 -5 3 12 11.30 3.30 -4 3 12 -0.20 3.00 -4 3 12 -4.10 3.30 -3 3 12 16.60 3.90 -3 3 12 23.20 4.20 -2 3 12 0.80 3.40 -2 3 12 3.60 3.00 1 -3 -12 31.50 6.20 -1 3 12 17.70 3.70 0 -3 -12 6.20 4.70 -4 4 12 11.30 3.90 -4 4 12 5.10 3.50 -3 4 12 2.30 3.00 -3 4 12 -4.90 3.20 -2 4 12 -3.20 5.30 -2 4 12 -0.60 2.90 -2 -6 13 8.50 4.20 -2 -6 13 18.60 9.20 -1 -6 13 33.80 9.80 0 -6 13 40.30 9.80 -3 -5 13 83.99 14.70 -3 -5 13 95.19 8.60 -2 -5 13 0.60 3.90 -2 -5 13 3.00 7.10 -1 -5 13 23.30 5.20 -1 -5 13 31.00 8.50 0 -5 13 11.50 7.40 -1 5 -13 0.00 5.20 1 -5 13 20.80 7.70 -4 -4 13 5.70 3.90 -4 -4 13 -2.10 8.80 -3 -4 13 -1.60 3.40 -3 -4 13 1.80 7.30 -2 -4 13 18.90 7.70 -2 -4 13 8.00 3.80 -1 -4 13 28.70 8.10 -1 -4 13 19.30 4.60 0 -4 13 43.90 10.30 -1 4 -13 -2.40 4.30 -4 -3 13 14.80 4.10 -4 -3 13 5.80 8.00 -3 -3 13 14.00 3.90 -3 -3 13 24.90 4.80 -3 -3 13 20.20 7.80 -2 -3 13 20.60 7.00 -2 -3 13 2.80 3.40 -2 -3 13 12.50 4.00 1 3 -13 6.20 3.80 -1 -3 13 17.10 7.00 -1 -3 13 7.70 3.40 -1 -3 13 2.80 3.40 0 3 -13 0.80 4.10 0 -3 13 16.90 6.40 -1 3 -13 -6.70 4.00 -5 -2 13 -7.20 9.60 -5 -2 13 -2.20 3.60 -5 -2 13 2.20 3.30 -4 -2 13 1.90 3.20 -4 -2 13 -5.00 3.60 -4 -2 13 9.50 6.70 -3 -2 13 -1.60 3.30 -3 -2 13 -0.70 3.40 -3 -2 13 16.70 5.80 2 2 -13 5.00 3.10 -2 -2 13 -5.60 2.90 -2 -2 13 3.20 3.20 -2 -2 13 11.10 5.90 1 2 -13 -0.40 3.50 -1 -2 13 -5.70 2.60 -1 -2 13 2.00 3.30 0 2 -13 3.60 4.40 -1 2 -13 33.00 6.30 -5 -1 13 0.10 3.10 -5 -1 13 2.30 4.30 -4 -1 13 -2.30 3.70 -4 -1 13 -5.40 2.90 -3 -1 13 8.90 4.10 -3 -1 13 14.30 4.40 -3 -1 13 21.50 5.70 2 1 -13 9.40 3.80 -2 -1 13 -0.10 3.10 -2 -1 13 8.70 3.60 -2 -1 13 14.20 5.60 1 1 -13 15.60 5.00 -1 -1 13 19.10 4.20 -1 -1 13 12.20 3.70 0 1 -13 9.60 5.10 -1 1 -13 1.90 4.60 -5 0 13 7.20 3.50 -5 0 13 7.10 4.40 -4 0 13 6.70 4.10 -4 0 13 3.70 3.50 -3 0 13 11.40 4.00 -3 0 13 6.10 3.60 2 0 -13 20.80 4.40 -2 0 13 27.70 4.80 -2 0 13 13.00 3.70 1 0 -13 119.99 10.20 -1 0 13 112.99 8.40 -1 0 13 130.79 9.80 0 0 -13 31.20 5.90 -5 1 13 7.50 3.40 -5 1 13 9.00 4.40 -4 1 13 62.19 6.50 -4 1 13 67.09 7.30 -3 1 13 203.58 11.80 -3 1 13 174.78 11.70 -2 1 13 21.20 4.60 -2 1 13 20.80 4.20 1 -1 -13 25.20 5.80 -1 1 13 14.40 4.70 0 -1 -13 26.20 5.80 -4 2 13 1.90 3.60 -4 2 13 3.50 3.30 -3 2 13 68.49 7.30 -3 2 13 85.99 7.60 -2 2 13 6.90 3.40 -2 2 13 3.30 3.40 1 -2 -13 33.30 6.00 -2 -3 14 64.99 7.20 -2 -3 14 52.99 6.30 1 3 -14 -0.70 4.80 -1 -3 14 16.70 6.60 -3 -2 14 14.60 4.30 -3 -2 14 8.70 4.10 2 2 -14 3.80 3.40 -2 -2 14 -4.10 3.30 -2 -2 14 4.80 4.20 -2 -2 14 19.30 6.20 1 2 -14 3.00 3.60 -3 -1 14 15.60 4.50 -3 -1 14 18.30 4.40 2 1 -14 7.40 3.50 -2 -1 14 4.00 4.10 -2 -1 14 0.50 3.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 14039 _shelx_res_file ; TITL test_a.res in P-1 SA-246-C_19-08-19.res created by SHELXL-2018/3 at 10:02:27 on 19-Aug-2019 REM Old TITL test in P-1 REM SHELXT solution in P-1 REM R1 0.148, Rweak 0.002, Alpha 0.032, Orientation as input REM Formula found by SHELXT: C18 N3 CELL 0.71073 7.3115 8.8469 11.0388 100.050 102.247 104.314 ZERR 1.000 0.0021 0.0025 0.0030 0.007 0.006 0.007 LATT 1 SFAC C H N UNIT 36 24 6 TEMP -173.15 SIZE 0.234 0.296 0.53 L.S. 10 BOND $H LIST 4 ACTA 52 FMAP 2 PLAN 20 WGHT 0.055200 0.138100 FVAR 0.81333 N1 3 0.313144 0.571682 0.397379 11.00000 0.01677 0.02154 = 0.01603 0.00331 0.00320 0.00578 N2 3 0.445818 0.734826 0.139291 11.00000 0.02147 0.02260 = 0.01914 0.00527 0.00453 0.00597 N3 3 0.087814 0.294029 0.563361 11.00000 0.02335 0.02678 = 0.01821 0.00635 0.00644 0.00652 C1 1 0.328648 0.574101 0.278364 11.00000 0.01360 0.02229 = 0.01742 0.00351 0.00237 0.00657 C2 1 0.252332 0.437687 0.177668 11.00000 0.01620 0.02467 = 0.01290 0.00361 0.00330 0.00495 AFIX 43 H2 2 0.260141 0.444780 0.093931 11.00000 -1.20000 AFIX 0 C3 1 0.164693 0.291159 0.200713 11.00000 0.01355 0.02158 = 0.01624 0.00129 0.00208 0.00543 C4 1 0.153773 0.287872 0.324188 11.00000 0.01576 0.01977 = 0.02009 0.00444 0.00387 0.00391 AFIX 43 H4 2 0.098885 0.189236 0.344145 11.00000 -1.20000 AFIX 0 C5 1 0.224246 0.430946 0.418724 11.00000 0.01295 0.02168 = 0.01437 0.00185 0.00175 0.00476 C6 1 0.439640 0.729671 0.259448 11.00000 0.01404 0.02080 = 0.01786 0.00342 0.00336 0.00624 C7 1 0.540072 0.860083 0.363337 11.00000 0.02155 0.02407 = 0.01866 0.00168 0.00471 0.00492 AFIX 43 H7 2 0.531212 0.853493 0.446984 11.00000 -1.20000 AFIX 0 C8 1 0.652689 0.999072 0.343052 11.00000 0.02135 0.02163 = 0.02868 -0.00023 0.00295 0.00225 AFIX 43 H8 2 0.722880 1.089152 0.412386 11.00000 -1.20000 AFIX 0 C9 1 0.660991 1.004207 0.220113 11.00000 0.01908 0.02203 = 0.03078 0.00725 0.00656 0.00292 AFIX 43 H9 2 0.737656 1.097586 0.203028 11.00000 -1.20000 AFIX 0 C10 1 0.555080 0.870208 0.122135 11.00000 0.02290 0.02687 = 0.02233 0.00887 0.00659 0.00713 AFIX 43 H10 2 0.560586 0.875011 0.037631 11.00000 -1.20000 AFIX 0 C11 1 0.200841 0.430925 0.549519 11.00000 0.01556 0.02342 = 0.01714 0.00403 0.00211 0.00815 C12 1 0.292642 0.565987 0.650333 11.00000 0.02055 0.02502 = 0.01931 0.00313 0.00342 0.00798 AFIX 43 H12 2 0.370162 0.661960 0.637260 11.00000 -1.20000 AFIX 0 C13 1 0.268135 0.556914 0.770011 11.00000 0.02626 0.03441 = 0.01884 0.00176 0.00222 0.01445 AFIX 43 H13 2 0.330137 0.646686 0.840845 11.00000 -1.20000 AFIX 0 C14 1 0.153330 0.416926 0.785557 11.00000 0.02771 0.04308 = 0.01572 0.00893 0.00808 0.01689 AFIX 43 H14 2 0.134352 0.408052 0.866839 11.00000 -1.20000 AFIX 0 C15 1 0.066165 0.289327 0.679771 11.00000 0.02848 0.03439 = 0.02385 0.01229 0.00968 0.00962 AFIX 43 H15 2 -0.013662 0.192846 0.690615 11.00000 -1.20000 AFIX 0 C16 1 0.082328 0.141433 0.096986 11.00000 0.01475 0.02069 = 0.01542 0.00188 0.00538 0.00114 C17 1 0.125242 0.000684 0.113493 11.00000 0.01717 0.02644 = 0.01318 0.00296 0.00203 0.00517 AFIX 43 H17 2 0.210899 0.000508 0.191289 11.00000 -1.20000 AFIX 0 C18 1 -0.044252 0.139679 -0.017485 11.00000 0.02015 0.01998 = 0.01908 0.00403 0.00509 0.00522 AFIX 43 H18 2 -0.075227 0.234999 -0.029841 11.00000 -1.20000 AFIX 0 HKLF 4 REM test_a.res in P-1 REM wR2 = 0.133423, GooF = S = 1.09029, Restrained GooF = 1.09029 for all data REM R1 = 0.046526 for 1953 Fo > 4sig(Fo) and 0.083025 for all 2918 data REM 190 parameters refined using 0 restraints END WGHT 0.0552 0.1381 REM Highest difference peak 0.265, deepest hole -0.223, 1-sigma level 0.049 Q1 1 0.2150 0.2803 0.2742 11.00000 0.05 0.26 Q2 1 0.1894 0.4438 0.4728 11.00000 0.05 0.24 Q3 1 0.0822 0.1569 0.0155 11.00000 0.05 0.23 Q4 1 0.3923 0.7514 0.1969 11.00000 0.05 0.23 Q5 1 0.3417 0.6655 0.2583 11.00000 0.05 0.23 Q6 1 0.2759 0.4259 0.4965 11.00000 0.05 0.20 Q7 1 0.1722 0.3567 0.3682 11.00000 0.05 0.19 Q8 1 0.1743 0.4378 0.0853 11.00000 0.05 0.19 Q9 1 0.1786 0.1235 0.0952 11.00000 0.05 0.19 Q10 1 0.5425 0.9557 0.1658 11.00000 0.05 0.18 Q11 1 0.6665 0.9291 0.1667 11.00000 0.05 0.18 Q12 1 0.4183 0.8020 0.2969 11.00000 0.05 0.18 Q13 1 0.6978 0.9710 0.2821 11.00000 0.05 0.18 Q14 1 0.1255 0.2292 0.1506 11.00000 0.05 0.18 Q15 1 0.2834 0.4797 0.6051 11.00000 0.05 0.18 Q16 1 0.5337 0.7703 0.3138 11.00000 0.05 0.18 Q17 1 0.2665 0.5529 0.0857 11.00000 0.05 0.17 Q18 1 0.3263 0.6226 0.5014 11.00000 0.05 0.17 Q19 1 0.3561 0.4774 0.1161 11.00000 0.05 0.17 Q20 1 0.3258 0.5944 0.8999 11.00000 0.05 0.17 ; _shelx_res_checksum 77156 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy N N1 0.31314(19) 0.57168(16) 0.39738(13) 0.0184(3) Uani d 1 N N2 0.4458(2) 0.73483(17) 0.13929(13) 0.0213(3) Uani d 1 N N3 0.0878(2) 0.29403(17) 0.56336(13) 0.0227(4) Uani d 1 C C1 0.3286(2) 0.5741(2) 0.27836(16) 0.0180(4) Uani d 1 C C2 0.2523(2) 0.4377(2) 0.17767(16) 0.0183(4) Uani d 1 H H2 0.260141 0.444780 0.093931 0.022 Uiso calc 1 C C3 0.1647(2) 0.2912(2) 0.20071(15) 0.0178(4) Uani d 1 C C4 0.1538(2) 0.2879(2) 0.32419(16) 0.0190(4) Uani d 1 H H4 0.098885 0.189236 0.344145 0.023 Uiso calc 1 C C5 0.2242(2) 0.4309(2) 0.41872(15) 0.0170(4) Uani d 1 C C6 0.4396(2) 0.7297(2) 0.25945(15) 0.0177(4) Uani d 1 C C7 0.5401(2) 0.8601(2) 0.36334(16) 0.0223(4) Uani d 1 H H7 0.531212 0.853493 0.446984 0.027 Uiso calc 1 C C8 0.6527(2) 0.9991(2) 0.34305(18) 0.0261(4) Uani d 1 H H8 0.722880 1.089152 0.412386 0.031 Uiso calc 1 C C9 0.6610(2) 1.0042(2) 0.22011(17) 0.0245(4) Uani d 1 H H9 0.737656 1.097586 0.203028 0.029 Uiso calc 1 C C10 0.5551(2) 0.8702(2) 0.12213(17) 0.0236(4) Uani d 1 H H10 0.560586 0.875011 0.037631 0.028 Uiso calc 1 C C11 0.2008(2) 0.4309(2) 0.54952(15) 0.0187(4) Uani d 1 C C12 0.2926(2) 0.5660(2) 0.65033(16) 0.0220(4) Uani d 1 H H12 0.370162 0.661960 0.637260 0.026 Uiso calc 1 C C13 0.2681(3) 0.5569(2) 0.77001(17) 0.0267(4) Uani d 1 H H13 0.330137 0.646686 0.840845 0.032 Uiso calc 1 C C14 0.1533(3) 0.4169(2) 0.78556(17) 0.0270(4) Uani d 1 H H14 0.134352 0.408052 0.866839 0.032 Uiso calc 1 C C15 0.0662(3) 0.2893(2) 0.67977(17) 0.0277(4) Uani d 1 H H15 -0.013662 0.192846 0.690615 0.033 Uiso calc 1 C C16 0.0823(2) 0.14143(19) 0.09699(15) 0.0178(4) Uani d 1 C C17 0.1252(2) 0.0007(2) 0.11349(16) 0.0197(4) Uani d 1 H H17 0.210899 0.000508 0.191289 0.024 Uiso calc 1 C C18 -0.0443(2) 0.1397(2) -0.01748(15) 0.0200(4) Uani d 1 H H18 -0.075227 0.234999 -0.029841 0.024 Uiso calc 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1 0.0168(7) 0.0215(8) 0.0160(8) 0.0058(6) 0.0032(6) 0.0033(6) N2 0.0215(7) 0.0226(8) 0.0191(8) 0.0060(6) 0.0045(6) 0.0053(6) N3 0.0234(8) 0.0268(8) 0.0182(8) 0.0065(6) 0.0064(6) 0.0063(6) C1 0.0136(8) 0.0223(9) 0.0174(9) 0.0066(7) 0.0024(7) 0.0035(7) C2 0.0162(8) 0.0247(9) 0.0129(9) 0.0049(7) 0.0033(7) 0.0036(7) C3 0.0136(8) 0.0216(9) 0.0162(9) 0.0054(7) 0.0021(7) 0.0013(7) C4 0.0158(8) 0.0198(9) 0.0201(9) 0.0039(7) 0.0039(7) 0.0044(7) C5 0.0129(8) 0.0217(9) 0.0144(9) 0.0048(7) 0.0017(6) 0.0018(7) C6 0.0140(8) 0.0208(9) 0.0179(9) 0.0062(7) 0.0034(7) 0.0034(7) C7 0.0216(9) 0.0241(9) 0.0187(9) 0.0049(7) 0.0047(7) 0.0017(7) C8 0.0213(9) 0.0216(10) 0.0287(11) 0.0023(7) 0.0029(8) -0.0002(8) C9 0.0191(8) 0.0220(9) 0.0308(11) 0.0029(7) 0.0066(8) 0.0072(8) C10 0.0229(9) 0.0269(10) 0.0223(10) 0.0071(8) 0.0066(7) 0.0089(8) C11 0.0156(8) 0.0234(9) 0.0171(9) 0.0081(7) 0.0021(7) 0.0040(7) C12 0.0205(9) 0.0250(10) 0.0193(9) 0.0080(7) 0.0034(7) 0.0031(8) C13 0.0263(9) 0.0344(11) 0.0188(10) 0.0144(8) 0.0022(8) 0.0018(8) C14 0.0277(9) 0.0431(12) 0.0157(9) 0.0169(9) 0.0081(8) 0.0089(8) C15 0.0285(10) 0.0344(11) 0.0238(10) 0.0096(8) 0.0097(8) 0.0123(9) C16 0.0148(8) 0.0207(9) 0.0154(9) 0.0011(7) 0.0054(7) 0.0019(7) C17 0.0172(8) 0.0264(9) 0.0132(9) 0.0052(7) 0.0020(6) 0.0030(7) C18 0.0201(8) 0.0200(9) 0.0191(9) 0.0052(7) 0.0051(7) 0.0040(7) 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' 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 C5 N1 C1 . 117.93(14) C10 N2 C6 . 117.38(14) C15 N3 C11 . 117.47(15) N1 C1 C2 . 122.49(15) N1 C1 C6 . 116.71(14) C2 C1 C6 . 120.75(15) C3 C2 C1 . 119.43(15) C3 C2 H2 . 120.3 C1 C2 H2 . 120.3 C4 C3 C2 . 118.00(15) C4 C3 C16 . 120.29(15) C2 C3 C16 . 121.70(15) C3 C4 C5 . 119.28(16) C3 C4 H4 . 120.4 C5 C4 H4 . 120.4 N1 C5 C4 . 122.72(15) N1 C5 C11 . 117.46(14) C4 C5 C11 . 119.82(15) N2 C6 C7 . 122.30(16) N2 C6 C1 . 116.79(14) C7 C6 C1 . 120.83(15) C8 C7 C6 . 119.20(16) C8 C7 H7 . 120.4 C6 C7 H7 . 120.4 C9 C8 C7 . 118.65(16) C9 C8 H8 . 120.7 C7 C8 H8 . 120.7 C8 C9 C10 . 118.53(16) C8 C9 H9 . 120.7 C10 C9 H9 . 120.7 N2 C10 C9 . 123.93(17) N2 C10 H10 . 118.0 C9 C10 H10 . 118.0 N3 C11 C12 . 122.76(16) N3 C11 C5 . 115.99(14) C12 C11 C5 . 121.25(15) C13 C12 C11 . 118.34(17) C13 C12 H12 . 120.8 C11 C12 H12 . 120.8 C14 C13 C12 . 119.44(17) C14 C13 H13 . 120.3 C12 C13 H13 . 120.3 C13 C14 C15 . 118.26(17) C13 C14 H14 . 120.9 C15 C14 H14 . 120.9 N3 C15 C14 . 123.72(18) N3 C15 H15 . 118.1 C14 C15 H15 . 118.1 C17 C16 C18 . 119.01(15) C17 C16 C3 . 120.93(15) C18 C16 C3 . 120.04(15) C18 C17 C16 2 120.68(16) C18 C17 H17 2 119.7 C16 C17 H17 . 119.7 C17 C18 C16 2 120.31(16) C17 C18 H18 2 119.8 C16 C18 H18 . 119.8 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance N1 C5 . 1.340(2) N1 C1 . 1.346(2) N2 C10 . 1.334(2) N2 C6 . 1.345(2) N3 C15 . 1.334(2) N3 C11 . 1.340(2) C1 C2 . 1.393(2) C1 C6 . 1.489(2) C2 C3 . 1.389(2) C2 H2 . 0.9500 C3 C4 . 1.387(2) C3 C16 . 1.487(2) C4 C5 . 1.395(2) C4 H4 . 0.9500 C5 C11 . 1.490(2) C6 C7 . 1.396(2) C7 C8 . 1.383(2) C7 H7 . 0.9500 C8 C9 . 1.379(3) C8 H8 . 0.9500 C9 C10 . 1.385(2) C9 H9 . 0.9500 C10 H10 . 0.9500 C11 C12 . 1.393(2) C12 C13 . 1.384(2) C12 H12 . 0.9500 C13 C14 . 1.374(3) C13 H13 . 0.9500 C14 C15 . 1.383(3) C14 H14 . 0.9500 C15 H15 . 0.9500 C16 C17 . 1.389(2) C16 C18 . 1.394(2) C17 C18 2 1.388(2) C17 H17 . 0.9500 C18 H18 . 0.9500 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 C17 H17 Cg2 1_545 0.96 2.99 3.682(2) 131 _cod_database_fobs_code 2243208