#------------------------------------------------------------------------------ #$Date: 2021-07-24 08:13:05 +0300 (Sat, 24 Jul 2021) $ #$Revision: 267732 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243878.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_2243878 loop_ _publ_author_name 'Atio\(glu, Zeliha' 'Akkurt, Mehmet' 'Shikhaliyev, Namiq Q.' 'Askerova, Ulviyya F.' 'Niyazova, Aytan A.' 'Mlowe, Sixberth' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of (2Z)-N,N-dimethyl-2-(pentafluorophenyl)-2-(2-phenylhydrazin-1-ylidene)acetamide ; _journal_coeditor_code HB7979 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 829 _journal_page_last 833 _journal_paper_doi 10.1107/S2056989021007349 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac 'C16 H12 F5 N3 O' _chemical_formula_moiety 'C16 H12 F5 N3 O' _chemical_formula_sum 'C16 H12 F5 N3 O' _chemical_formula_weight 357.29 _chemical_name_systematic (2Z)-N,N-Dimethyl-2-(pentafluorophenyl)-2-(2-phenylhydrazin-1-ylidene)acetamide _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 116.5260(10) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 19.0048(6) _cell_length_b 11.5216(4) _cell_length_c 17.2227(6) _cell_measurement_reflns_used 9937 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 30.51 _cell_measurement_theta_min 2.95 _cell_volume 3374.2(2) _computing_cell_refinement ; SAINT (Bruker, 2007) ; _computing_data_collection ; APEX3 (Bruker, 2007) ; _computing_data_reduction ; SAINT (Bruker, 2007) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2016/6 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS (Sheldrick, 2008) ; _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.981 _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 0.0254 _diffrn_reflns_av_unetI/netI 0.0176 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 20072 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.998 _diffrn_reflns_theta_min 2.953 _exptl_absorpt_coefficient_mu 0.128 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.407 _exptl_crystal_description prism _exptl_crystal_F_000 1456 _exptl_crystal_size_max 0.860 _exptl_crystal_size_mid 0.760 _exptl_crystal_size_min 0.320 _refine_diff_density_max 0.272 _refine_diff_density_min -0.158 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 232 _refine_ls_number_reflns 3619 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.079 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0436 _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^)+(0.0660P)^2^+1.0984P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1256 _refine_ls_wR_factor_ref 0.1294 _reflns_number_gt 3075 _reflns_number_total 3619 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb7979sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2243878 _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 0.898 _shelx_estimated_absorpt_t_max 0.960 _shelx_hkl_file ; -4 0 0 58.39 2.70 4 0 0 69.29 3.40 -4 0 0 62.99 2.80 -4 0 0 65.29 3.80 6 0 0 191.98 6.80 6 0 0 198.78 6.70 -6 0 0 189.38 6.60 -6 0 0 203.38 6.40 -6 0 0 200.08 7.30 -8 0 0 3008.80 66.99 8 0 0 2900.61 66.99 8 0 0 2902.31 67.79 -8 0 0 2989.20 67.89 -10 0 0 2642.14 60.69 -10 0 0 2655.73 61.89 10 0 0 2564.94 61.79 12 0 0 4574.24 105.09 -12 0 0 4541.85 103.39 -14 0 0 751.82 21.80 14 0 0 742.93 23.40 -14 0 0 758.32 23.40 -16 0 0 546.55 18.30 16 0 0 548.65 19.90 -16 0 0 542.85 19.70 18 0 0 8.40 5.00 -18 0 0 14.40 5.80 -18 0 0 3.60 4.00 20 0 0 156.98 12.40 -20 0 0 199.78 13.00 -22 0 0 19.80 6.40 22 0 0 12.50 6.80 -5 -1 0 1048.50 24.40 -5 -1 0 1005.10 25.00 5 -1 0 1048.10 25.30 -5 -1 0 1063.89 25.00 5 -1 0 1052.99 25.10 5 -1 0 1062.79 24.10 5 1 0 1039.80 25.60 5 1 0 1060.09 24.10 -5 1 0 1066.09 24.20 -5 1 0 1002.10 25.70 5 1 0 1053.59 25.20 7 -1 0 3225.08 75.49 -7 -1 0 3330.07 74.89 -7 -1 0 3290.97 75.19 7 -1 0 3331.57 75.59 7 -1 0 3284.07 74.19 -7 1 0 3396.26 74.49 7 1 0 3293.17 74.29 7 1 0 3388.36 75.89 -7 1 0 3346.77 76.39 -7 1 0 3490.55 77.09 7 1 0 3306.67 74.99 -9 -1 0 474.85 14.00 9 -1 0 470.65 13.00 -9 -1 0 483.45 14.10 -9 1 0 499.25 13.40 9 1 0 452.75 15.10 -9 1 0 478.05 15.50 9 1 0 461.65 13.10 -11 -1 0 97.49 6.70 11 -1 0 107.59 6.90 -11 -1 0 108.79 6.40 -11 1 0 100.79 8.30 11 1 0 107.99 6.90 -11 1 0 105.19 5.80 11 1 0 101.39 6.50 13 -1 0 457.15 16.10 -13 -1 0 470.35 15.40 -13 1 0 464.45 14.50 -13 1 0 446.86 17.30 13 1 0 459.85 16.20 15 -1 0 62.29 6.90 -15 -1 0 67.49 7.30 -15 -1 0 53.89 6.50 -15 1 0 65.49 8.40 -15 1 0 65.69 5.80 15 1 0 60.79 7.00 17 -1 0 56.99 7.70 -17 -1 0 53.39 8.10 -17 -1 0 55.69 7.30 -17 1 0 51.19 7.00 17 1 0 70.19 8.20 -17 1 0 45.90 7.70 19 -1 0 416.86 18.50 -19 -1 0 459.05 17.90 -19 1 0 407.96 16.80 -19 1 0 416.16 19.40 19 1 0 421.66 18.80 21 -1 0 7.70 5.80 -21 -1 0 13.80 5.90 21 1 0 4.60 5.60 -21 1 0 27.40 7.30 -21 1 0 20.20 10.90 -23 1 0 121.89 12.90 6 -2 0 82.29 5.00 6 -2 0 80.69 4.10 6 -2 0 82.39 3.20 -6 -2 0 80.39 4.40 -6 -2 0 77.69 3.10 6 2 0 86.69 4.50 -6 2 0 84.39 5.80 6 2 0 81.79 4.30 -6 2 0 75.89 4.00 -6 2 0 84.89 3.20 6 2 0 83.69 3.10 8 -2 0 1990.40 44.60 8 -2 0 1806.72 47.80 -8 -2 0 1926.21 47.70 -8 -2 0 2004.40 44.80 -8 2 0 2031.00 48.20 -8 2 0 2007.20 44.80 8 2 0 1952.80 47.10 8 2 0 1964.30 44.30 10 -2 0 1169.48 28.90 -10 -2 0 1204.98 29.40 -10 -2 0 1192.58 30.90 10 -2 0 1185.08 31.10 10 2 0 1226.68 31.70 -10 2 0 1242.68 29.40 -10 2 0 1214.68 32.80 -12 -2 0 425.56 14.20 -12 -2 0 403.46 12.90 12 -2 0 416.56 14.60 12 2 0 417.26 14.80 12 2 0 396.86 12.00 -12 2 0 404.66 12.60 -12 2 0 398.36 16.40 -14 -2 0 18.30 4.40 -14 -2 0 16.50 3.80 14 -2 0 18.00 4.50 -14 2 0 16.70 3.30 14 2 0 12.30 4.10 -14 2 0 11.40 6.00 -16 -2 0 48.50 6.60 16 -2 0 37.90 6.20 -16 -2 0 50.59 6.80 -16 2 0 54.99 8.90 16 2 0 48.50 6.90 -16 2 0 41.20 5.50 18 -2 0 45.00 7.00 -18 -2 0 54.89 7.80 18 2 0 40.70 7.40 -18 2 0 36.70 8.00 -18 2 0 40.60 6.00 20 -2 0 235.18 14.40 -20 -2 0 235.98 14.40 -20 2 0 255.97 17.20 20 2 0 225.18 14.90 -20 2 0 239.08 12.50 22 -2 0 17.10 6.60 -22 -2 0 22.00 7.00 -22 2 0 25.00 10.60 -22 2 0 41.90 9.40 22 2 0 16.10 6.60 1 -3 0 19.10 2.50 -1 -3 0 14.40 1.50 -1 -3 0 13.10 2.00 -1 -3 0 18.10 1.70 1 -3 0 12.60 1.40 1 3 0 17.40 1.60 1 3 0 22.80 2.70 1 3 0 18.60 2.20 -1 3 0 20.70 1.90 -1 3 0 18.90 1.60 5 -3 0 2208.88 48.20 5 -3 0 2186.68 48.10 -5 -3 0 2212.28 50.39 -5 -3 0 2172.48 50.09 5 -3 0 2238.38 50.09 5 -3 0 2181.78 51.09 -5 3 0 2121.89 51.59 5 3 0 2137.49 50.29 5 3 0 2158.88 50.29 -5 3 0 2165.28 50.09 7 -3 0 1136.19 26.50 -7 -3 0 1128.09 25.80 7 -3 0 1184.58 26.70 7 -3 0 1155.58 28.70 7 3 0 1177.28 25.70 -9 -3 0 1532.75 35.50 -9 -3 0 1568.74 38.80 9 -3 0 1536.05 35.90 9 -3 0 1574.14 38.50 9 3 0 1534.05 39.00 -9 3 0 1553.44 40.70 -9 3 0 1620.04 36.40 9 3 0 1591.94 35.30 11 -3 0 2.60 1.70 -11 -3 0 -4.30 2.50 -11 -3 0 -2.70 1.90 11 -3 0 0.90 2.70 11 3 0 0.30 1.50 -11 3 0 1.10 1.60 11 3 0 -0.40 2.10 -11 3 0 3.00 5.10 -13 -3 0 10.40 3.80 13 -3 0 19.10 4.00 -13 -3 0 23.00 3.50 13 3 0 18.50 2.80 -13 3 0 20.80 7.10 -13 3 0 20.30 3.10 -15 -3 0 226.68 11.60 -15 -3 0 245.08 9.40 15 -3 0 236.58 11.80 15 3 0 247.08 12.70 -15 3 0 240.08 14.30 -15 3 0 237.08 9.40 17 -3 0 46.20 6.90 17 3 0 44.10 7.20 -17 3 0 38.80 8.50 -17 3 0 41.00 5.30 19 -3 0 901.71 29.40 -19 -3 0 939.01 25.00 -19 -3 0 865.91 28.70 -19 3 0 874.01 31.50 -19 3 0 868.11 25.70 19 3 0 904.31 30.30 21 -3 0 350.06 17.70 -21 -3 0 364.96 18.40 -21 3 0 397.66 21.70 21 3 0 342.77 18.50 2 -4 0 58.69 3.20 -2 -4 0 47.00 2.40 -2 -4 0 49.70 3.20 -2 -4 0 52.49 3.60 2 -4 0 49.40 2.70 2 -4 0 50.79 3.70 2 4 0 47.30 3.00 -2 4 0 53.89 2.50 2 4 0 51.39 3.20 2 4 0 45.80 3.30 -2 4 0 48.00 2.90 4 -4 0 2489.55 54.19 4 -4 0 2462.85 56.19 -4 -4 0 2474.85 56.59 4 4 0 2493.35 53.99 4 4 0 2451.75 53.69 4 4 0 2407.96 56.39 -4 4 0 2443.16 54.29 -4 4 0 2444.36 57.99 6 -4 0 1027.00 26.00 6 -4 0 1009.50 23.20 -6 -4 0 1038.80 26.40 6 -4 0 1029.10 23.40 6 4 0 1019.30 26.10 -6 4 0 1008.90 28.20 -8 -4 0 711.73 20.00 8 -4 0 696.63 16.80 8 -4 0 684.43 16.70 8 -4 0 693.63 19.50 8 4 0 690.33 20.00 -8 4 0 739.13 22.40 -10 -4 0 332.67 12.40 10 -4 0 329.87 9.10 10 -4 0 326.07 9.30 10 -4 0 315.07 11.70 10 4 0 315.97 12.30 -10 4 0 331.87 15.10 -12 -4 0 98.49 3.60 -12 -4 0 94.79 3.80 12 -4 0 95.49 6.90 12 -4 0 99.79 4.80 12 -4 0 96.89 4.70 -12 -4 0 105.79 7.70 12 4 0 101.49 7.50 -12 4 0 103.69 10.80 -14 -4 0 17.00 2.20 14 -4 0 21.20 4.80 -14 -4 0 16.80 2.10 -14 -4 0 11.30 4.20 14 -4 0 12.80 2.70 14 4 0 6.10 4.40 -14 4 0 12.00 6.90 -16 -4 0 50.49 3.90 16 -4 0 51.39 5.50 16 -4 0 56.09 10.20 16 4 0 58.89 7.70 -16 4 0 48.20 8.50 18 -4 0 31.10 4.60 18 -4 0 31.00 6.60 -18 -4 0 29.10 6.90 -18 4 0 23.10 8.10 18 4 0 31.90 7.20 20 -4 0 590.74 18.90 20 -4 0 596.64 23.20 -20 -4 0 588.34 23.10 20 4 0 625.64 24.70 -20 4 0 630.74 26.70 -22 -4 0 47.50 9.10 22 -4 0 39.30 5.60 22 -4 0 45.80 8.20 -22 4 0 49.50 10.90 22 4 0 40.80 8.40 1 -5 0 203.08 6.70 -1 -5 0 203.28 7.40 -1 -5 0 189.88 7.20 1 -5 0 212.68 7.40 -1 -5 0 197.08 6.60 1 -5 0 178.58 7.10 -1 5 0 201.68 6.60 1 5 0 179.28 6.90 -1 5 0 207.48 8.50 1 5 0 201.68 7.60 -5 -5 0 273.47 13.90 5 -5 0 315.87 11.40 5 -5 0 319.77 8.10 -5 5 0 310.77 14.30 -5 5 0 316.97 8.10 5 5 0 307.47 10.40 5 5 0 299.67 7.30 7 -5 0 14.30 2.70 7 -5 0 18.80 1.80 -7 -5 0 18.80 3.70 7 -5 0 20.60 1.60 -7 5 0 15.20 5.40 7 5 0 14.70 3.00 9 -5 0 111.69 3.90 -9 -5 0 101.89 7.00 9 -5 0 109.99 6.50 9 -5 0 109.29 3.90 9 5 0 116.49 7.00 -9 5 0 110.59 10.10 11 -5 0 524.15 16.80 -11 -5 0 509.85 17.50 11 -5 0 517.45 13.20 11 -5 0 509.25 13.10 11 5 0 504.15 17.70 -11 5 0 512.15 20.60 13 -5 0 17.50 2.30 13 -5 0 16.40 2.40 -13 -5 0 12.80 4.80 13 -5 0 14.40 4.10 -13 5 0 7.90 6.90 13 5 0 4.30 4.60 15 -5 0 13.80 2.60 15 -5 0 4.00 4.00 15 5 0 1.60 4.00 -15 5 0 19.10 7.90 -17 -5 0 1.70 4.40 17 -5 0 1.70 4.10 17 5 0 -3.50 3.70 -17 5 0 -2.40 6.60 19 -5 0 9.20 5.80 19 -5 0 15.70 3.40 -19 -5 0 14.50 5.80 19 5 0 22.30 6.70 -19 5 0 15.60 7.80 21 -5 0 36.70 7.90 21 -5 0 35.50 4.50 -21 -5 0 44.00 8.30 21 5 0 54.79 9.40 -21 5 0 54.09 11.30 23 -5 0 19.90 6.80 23 5 0 17.40 7.10 -23 5 0 44.90 10.30 2 -6 0 1037.70 25.00 2 -6 0 1052.29 26.80 -2 -6 0 1028.80 26.80 -2 -6 0 1048.10 26.40 2 6 0 1038.50 26.10 -2 6 0 1037.60 24.90 -2 6 0 1060.39 28.10 -4 -6 0 1719.53 41.90 4 -6 0 1692.33 41.50 4 -6 0 1746.33 39.30 4 6 0 1725.13 42.00 -4 6 0 1811.22 44.30 -4 6 0 1713.03 39.30 4 6 0 1706.03 39.00 4 6 0 1725.93 39.80 6 -6 0 117.09 6.20 6 -6 0 125.79 4.40 -6 -6 0 105.59 6.70 -6 6 0 112.29 4.10 -6 6 0 126.39 9.50 6 6 0 123.59 6.60 -8 -6 0 13.20 3.80 8 -6 0 15.00 3.30 8 -6 0 14.90 2.00 8 -6 0 14.60 1.50 -8 6 0 16.80 6.80 8 6 0 12.80 3.50 10 -6 0 390.76 10.20 10 -6 0 402.36 10.20 -10 -6 0 405.76 15.50 10 -6 0 393.56 14.40 -10 6 0 423.86 19.00 10 6 0 418.06 15.40 -12 -6 0 861.11 26.50 12 -6 0 858.81 20.40 12 -6 0 839.42 20.40 12 -6 0 886.61 25.70 -12 6 0 883.91 30.10 12 6 0 871.91 26.90 14 -6 0 320.37 13.90 14 -6 0 314.97 9.30 -14 -6 0 325.57 15.80 14 -6 0 315.57 9.00 14 6 0 323.17 16.20 16 -6 0 122.29 9.60 -16 -6 0 119.39 10.00 16 -6 0 119.79 5.10 16 -6 0 118.69 5.00 -16 6 0 123.99 13.70 16 6 0 117.29 9.90 -18 -6 0 4.70 4.80 18 -6 0 4.10 4.70 18 -6 0 12.00 2.40 -18 6 0 19.10 7.90 18 6 0 9.40 5.00 20 -6 0 -3.50 4.70 20 -6 0 0.80 1.90 -20 -6 0 4.00 5.80 20 6 0 7.80 5.80 -20 6 0 8.90 7.50 22 -6 0 -4.30 6.20 22 6 0 0.90 5.90 -22 6 0 6.00 8.20 1 -7 0 174.68 7.70 -1 -7 0 168.98 7.60 1 -7 0 185.08 7.10 -1 -7 0 165.18 7.60 1 7 0 180.88 8.50 -3 -7 0 603.64 17.50 3 -7 0 607.24 15.50 -3 -7 0 583.14 17.50 3 -7 0 580.64 17.30 3 7 0 597.74 16.60 -3 7 0 594.04 15.30 3 7 0 553.34 15.10 -3 7 0 603.54 19.70 -5 -7 0 49.30 5.60 5 -7 0 53.39 4.60 5 -7 0 58.69 3.60 5 7 0 55.39 2.60 -5 7 0 54.09 2.90 -5 7 0 58.19 8.50 5 7 0 57.99 3.80 -7 -7 0 25.50 5.00 7 -7 0 32.40 2.70 7 -7 0 27.70 2.10 7 -7 0 32.30 4.60 -7 7 0 44.60 8.00 7 7 0 25.40 4.00 -9 -7 0 -6.60 4.20 9 -7 0 12.80 4.10 9 -7 0 4.90 1.90 9 -7 0 5.00 1.40 -9 7 0 0.40 7.10 9 7 0 7.50 3.70 -11 -7 0 124.39 10.30 11 -7 0 133.79 9.20 -11 7 0 135.79 13.60 11 7 0 134.59 9.80 -13 -7 0 38.20 6.60 13 -7 0 42.40 6.50 13 7 0 48.20 7.40 -13 7 0 57.19 10.70 15 -7 0 5.70 4.20 -15 -7 0 2.40 4.30 -15 7 0 4.00 7.10 15 7 0 13.40 5.20 17 -7 0 -3.00 4.20 -17 -7 0 -0.30 4.30 17 7 0 -2.00 3.80 -17 7 0 -2.50 6.90 19 -7 0 11.20 6.10 -19 -7 0 6.30 5.70 19 7 0 21.50 6.80 -19 7 0 19.40 8.80 -21 -7 0 12.10 11.40 21 -7 0 -5.30 4.30 21 7 0 0.90 6.10 -21 7 0 7.10 8.30 0 -8 0 9.20 2.70 2 -8 0 152.48 7.60 -2 -8 0 143.99 7.60 -2 -8 0 146.69 7.70 2 -8 0 143.79 6.80 -2 8 0 149.19 10.40 2 8 0 140.89 8.30 -4 -8 0 594.94 18.10 4 -8 0 573.14 17.70 4 -8 0 581.54 15.40 -4 8 0 566.64 15.20 4 8 0 572.94 18.00 4 8 0 568.24 16.30 -4 8 0 605.34 21.10 4 8 0 528.05 14.80 6 -8 0 303.57 11.90 6 -8 0 319.77 9.10 -6 -8 0 300.97 12.60 -6 8 0 310.27 9.80 6 8 0 309.47 12.20 -6 8 0 292.77 15.90 6 8 0 305.57 8.60 6 8 0 306.57 8.10 8 -8 0 1966.50 45.90 8 -8 0 2078.69 45.90 8 -8 0 2057.19 50.89 -8 -8 0 2078.59 52.09 -8 8 0 2030.60 55.49 8 8 0 2089.59 51.79 10 -8 0 179.18 10.20 -10 -8 0 168.48 11.30 10 8 0 177.68 10.50 -10 8 0 162.38 14.30 -12 -8 0 77.19 8.60 12 -8 0 77.89 9.50 -12 8 0 90.39 12.40 12 8 0 67.89 8.30 14 -8 0 57.29 7.30 -14 -8 0 50.69 7.60 14 8 0 65.09 8.70 -14 8 0 65.19 11.50 -16 -8 0 -0.30 4.40 16 -8 0 -3.00 3.90 16 8 0 -2.00 4.30 -16 8 0 -1.80 6.90 18 -8 0 18.90 6.10 -18 -8 0 37.30 7.70 18 8 0 24.10 6.70 -18 8 0 22.40 10.00 20 -8 0 5.00 5.30 -20 8 0 10.30 8.70 -1 -9 0 771.32 23.10 -1 -9 0 767.22 22.10 1 -9 0 782.92 22.90 1 -9 0 780.52 21.40 -1 9 0 807.42 24.90 1 9 0 791.82 23.70 3 -9 0 11.40 3.30 -3 -9 0 12.40 3.90 -3 -9 0 11.10 3.90 3 -9 0 13.80 3.10 3 9 0 13.60 4.30 -3 9 0 8.70 6.10 5 -9 0 29.00 4.70 5 -9 0 34.90 3.90 -5 -9 0 29.50 5.50 5 9 0 41.00 2.80 5 9 0 27.70 4.50 5 9 0 38.50 4.30 -5 9 0 32.40 2.90 -5 9 0 36.70 8.90 7 -9 0 6.00 2.10 7 -9 0 -2.50 3.40 -7 9 0 7.80 2.40 -7 9 0 -14.60 6.90 7 9 0 4.90 3.50 -9 -9 0 504.75 19.90 9 -9 0 570.54 19.30 9 9 0 599.54 21.90 -9 9 0 581.64 24.20 11 -9 0 101.49 8.60 -11 -9 0 89.59 9.60 -11 9 0 113.49 13.70 11 9 0 95.29 8.90 -13 -9 0 11.00 5.70 13 -9 0 14.10 4.90 13 9 0 -1.60 4.30 -13 9 0 -0.50 7.50 15 -9 0 2.90 4.20 -15 -9 0 -2.50 4.70 -15 9 0 1.50 7.90 15 9 0 -5.60 4.10 -17 -9 0 0.90 5.40 17 -9 0 1.40 4.80 -17 9 0 7.30 8.70 17 9 0 2.00 4.90 19 -9 0 2.00 4.70 -19 -9 0 4.80 9.30 0 -10 0 33.20 5.30 0 -10 0 33.90 5.00 0 10 0 33.10 6.60 -2 -10 0 36.00 5.50 2 -10 0 22.40 4.50 -2 -10 0 29.00 5.30 2 -10 0 26.00 4.30 -2 10 0 41.40 7.60 2 10 0 29.70 5.80 -4 -10 0 96.49 7.80 4 -10 0 82.99 7.40 4 10 0 86.29 6.90 -4 10 0 89.89 11.00 4 10 0 88.69 7.70 6 -10 0 26.70 5.50 -6 -10 0 19.50 5.60 6 -10 0 37.70 3.70 6 10 0 23.60 4.80 -6 10 0 33.30 3.00 6 10 0 43.20 3.40 -6 10 0 19.70 8.10 8 -10 0 550.34 14.40 8 -10 0 586.64 14.50 -8 10 0 593.94 31.40 8 10 0 579.24 20.60 10 -10 0 13.90 4.80 -10 -10 0 -1.70 5.30 -10 10 0 1.00 7.60 10 10 0 -1.40 4.50 -12 -10 0 62.09 9.00 12 -10 0 53.19 7.50 12 10 0 39.50 6.90 -12 10 0 45.30 10.00 -14 -10 0 3.50 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4.40 4.50 -17 1 -3 9.30 4.50 -19 -1 -3 27.50 6.80 19 -1 3 21.50 6.50 -19 -1 -3 37.00 6.60 -19 1 -3 35.10 8.10 -19 1 -3 23.60 6.20 19 1 3 16.90 5.80 -21 -1 -3 175.78 14.00 21 -1 3 177.08 13.50 21 1 3 185.28 14.00 -21 1 -3 193.58 13.40 -22 -2 3 23.70 6.80 22 -2 -3 13.30 5.80 22 2 -3 20.90 6.60 -22 2 3 33.50 5.60 -22 2 3 27.70 8.10 -20 -2 3 5.80 5.30 20 -2 -3 4.70 5.70 -20 2 3 8.20 3.60 20 2 -3 0.40 5.40 -20 2 3 -0.30 6.20 18 -2 -3 1576.94 42.80 -18 -2 3 1489.55 39.40 -18 -2 3 1539.65 40.90 -18 2 3 1512.95 38.40 18 2 -3 1546.95 43.20 -18 2 3 1492.15 43.60 16 -2 -3 30.20 6.00 -16 -2 3 24.20 5.30 16 2 -3 31.70 5.90 -16 2 3 14.80 6.70 -14 -2 3 82.79 6.60 14 -2 -3 84.29 6.80 -14 -2 3 82.39 6.40 -14 -2 3 73.19 4.70 14 2 -3 79.09 6.90 -14 2 3 88.89 9.30 -14 2 3 72.59 4.70 -12 -2 3 315.97 9.40 -12 -2 3 322.37 11.60 12 -2 -3 335.37 12.20 -12 -2 3 322.17 10.70 12 -2 -3 322.07 9.60 -12 2 3 329.97 13.40 12 2 -3 325.07 12.40 -12 2 3 330.07 9.70 -10 -2 3 2668.53 64.19 -10 -2 3 2658.13 60.39 10 -2 -3 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5.90 -23 -3 3 8.40 6.10 23 -3 -3 9.10 5.30 23 3 -3 3.70 5.70 -23 3 3 10.10 7.80 -23 3 3 7.00 3.60 21 -3 -3 25.00 6.90 -21 -3 3 27.20 6.50 -21 3 3 38.30 9.30 -21 3 3 28.10 4.50 21 3 -3 33.50 7.20 -19 -3 3 359.46 16.30 19 -3 -3 368.56 17.30 -19 3 3 359.36 27.10 19 3 -3 378.96 17.70 -19 3 3 364.46 12.80 -17 -3 3 40.40 6.50 17 -3 -3 36.60 11.70 -17 -3 3 39.60 5.20 -17 3 3 29.20 8.10 17 3 -3 30.40 6.90 -15 -3 3 160.78 7.50 15 -3 -3 153.88 6.70 15 -3 -3 160.68 9.50 -15 -3 3 154.18 5.80 -15 -3 3 160.38 9.30 -15 3 3 169.98 12.80 15 3 -3 159.28 9.90 -15 3 3 158.08 6.50 -13 -3 3 27.20 4.60 -13 -3 3 31.60 4.30 13 -3 -3 37.20 5.00 13 -3 -3 40.60 5.10 -13 -3 3 30.20 2.40 13 3 -3 33.90 5.20 -13 3 3 32.20 2.80 -13 3 3 32.70 6.40 11 -3 -3 766.42 18.20 -11 -3 3 769.12 18.30 11 -3 -3 772.82 21.80 -11 -3 3 765.22 19.00 -11 -3 3 779.02 21.70 -11 3 3 770.02 23.10 -11 3 3 777.92 18.40 11 3 -3 729.43 22.00 -9 -3 3 106.09 3.70 -9 -3 3 109.39 4.10 9 -3 -3 115.19 3.50 -9 -3 3 112.79 6.70 9 -3 -3 110.39 6.20 -9 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3 3 -2.30 4.50 -17 3 -3 -0.10 5.80 19 -3 3 -1.70 4.60 -19 -3 -3 -1.60 4.80 19 -3 3 -0.50 3.90 -19 3 -3 2.30 6.90 19 3 3 5.20 4.70 -21 -3 -3 92.39 12.40 21 -3 3 93.59 10.70 21 -3 3 84.79 9.10 21 3 3 97.39 11.50 24 -4 -3 -2.30 3.60 24 -4 -3 -5.80 5.10 -24 -4 3 15.60 7.50 -24 4 3 4.80 8.10 24 4 -3 -2.80 5.80 -22 -4 3 12.00 5.60 22 -4 -3 3.60 2.80 22 -4 -3 6.20 5.20 22 4 -3 7.40 6.00 -22 4 3 18.50 8.40 20 -4 -3 1.40 4.90 -20 -4 3 0.80 4.50 20 4 -3 3.80 5.10 -20 4 3 1.80 7.40 18 -4 -3 16.80 6.20 -18 -4 3 17.30 5.80 18 4 -3 15.60 5.70 -18 4 3 14.60 3.00 -18 4 3 21.40 9.60 -16 -4 3 48.70 3.10 16 -4 -3 38.40 3.60 -16 -4 3 31.70 5.60 -16 -4 3 48.00 2.40 16 -4 -3 34.30 6.00 16 4 -3 23.60 5.30 -16 4 3 29.10 7.70 -16 4 3 36.50 3.20 14 -4 -3 304.27 12.90 14 -4 -3 314.87 8.80 -14 -4 3 303.57 8.70 -14 -4 3 323.07 13.30 -14 -4 3 312.27 8.30 -14 4 3 346.27 16.50 -14 4 3 312.77 8.90 14 4 -3 325.97 13.90 12 -4 -3 707.43 21.50 12 -4 -3 726.23 16.90 -12 -4 3 745.03 22.00 12 4 -3 721.43 22.20 -12 4 3 738.73 24.00 10 -4 -3 138.69 7.20 -10 -4 3 137.79 8.00 10 4 -3 152.48 7.80 -10 4 3 149.59 9.50 8 -4 -3 318.27 10.80 -8 -4 3 296.37 11.20 -8 4 3 313.67 12.30 8 4 -3 325.07 11.10 -6 -4 3 847.12 19.70 -6 -4 3 863.81 23.50 6 -4 -3 835.62 22.80 6 4 -3 836.32 19.40 -6 4 3 824.82 24.10 6 4 -3 855.51 22.00 4 -4 -3 3443.06 74.99 -4 -4 3 3374.86 77.29 4 -4 -3 3413.66 76.99 -4 -4 3 3496.15 76.39 4 4 -3 3389.46 75.99 4 4 -3 3348.36 76.89 -4 4 3 3489.35 78.89 4 4 -3 3401.66 76.79 -4 4 3 3436.36 74.89 -2 -4 3 5052.09 113.99 0 -4 -3 1850.51 42.60 0 -4 -3 1847.72 42.90 0 -4 3 1837.72 44.30 0 -4 -3 1859.01 43.10 0 -4 3 1850.11 42.60 0 -4 3 1873.81 42.70 0 4 3 1968.60 43.50 0 4 3 1852.61 42.70 0 4 -3 1852.91 42.70 0 4 -3 1878.51 42.70 0 4 -3 1849.91 44.30 0 4 3 1770.92 42.80 2 -4 3 4912.11 107.09 -2 4 -3 4817.62 107.29 -2 4 -3 4802.22 109.89 -4 -4 -3 875.51 23.30 4 -4 3 867.41 21.50 -4 -4 -3 850.71 20.60 4 -4 3 882.31 21.90 4 4 3 884.31 22.60 -4 4 -3 867.31 21.70 4 4 3 858.41 21.00 -4 4 -3 906.11 23.30 6 -4 3 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6.40 -20 4 -3 16.90 8.40 -23 -5 3 8.70 6.30 23 -5 -3 6.10 5.40 -23 5 3 16.90 9.80 23 5 -3 8.80 6.50 -21 -5 3 7.00 5.10 21 -5 -3 6.90 1.90 21 -5 -3 4.80 5.40 21 5 -3 9.00 6.10 -21 5 3 12.70 8.50 19 -5 -3 135.59 11.10 -19 -5 3 145.49 11.10 19 -5 -3 138.79 5.20 19 5 -3 149.69 11.80 -19 5 3 151.78 14.70 -17 -5 3 568.54 20.50 17 -5 -3 537.75 13.60 17 -5 -3 566.34 20.60 17 -5 -3 516.25 13.50 -17 5 3 587.54 24.20 17 5 -3 563.44 21.50 -15 -5 3 27.90 5.80 15 -5 -3 19.40 4.60 -15 5 3 24.10 7.40 15 5 -3 22.30 5.10 13 -5 -3 27.20 5.10 -13 -5 3 7.80 4.50 13 5 -3 9.80 4.10 -13 5 3 23.80 7.20 11 -5 -3 679.93 20.60 -11 -5 3 698.53 21.20 -11 5 3 702.13 23.40 11 5 -3 686.73 21.30 -9 -5 3 1133.59 30.70 9 -5 -3 1172.28 30.40 9 5 -3 1195.68 30.90 -9 5 3 1173.98 32.30 7 -5 -3 518.45 15.50 -7 -5 3 534.75 16.00 -7 -5 3 515.05 12.30 7 5 -3 522.45 15.60 7 5 -3 520.25 12.00 -7 5 3 515.95 17.00 -5 -5 3 2233.18 54.09 5 -5 -3 2217.78 49.30 -5 -5 3 2288.37 50.69 -5 5 3 2282.27 53.49 5 5 -3 2152.08 50.29 -5 5 3 2253.17 49.30 -3 -5 3 555.44 15.10 3 -5 -3 507.95 15.80 -3 -5 3 540.85 14.60 -3 -5 3 519.85 15.70 3 -5 -3 514.45 13.10 -3 5 3 515.25 15.10 3 5 -3 497.05 14.20 -3 5 3 509.95 13.00 -1 -5 3 840.82 21.30 1 -5 -3 846.82 21.70 -1 -5 3 859.11 21.40 1 -5 -3 840.22 21.00 1 5 -3 859.41 21.50 -1 5 3 874.11 21.60 -1 5 3 820.32 21.10 1 5 -3 855.21 22.60 -1 5 3 808.92 20.70 -3 -5 -3 1748.43 38.80 3 -5 3 1676.33 39.80 3 -5 3 1697.93 39.20 3 5 3 1665.43 38.80 -3 5 -3 1674.13 39.50 -3 5 -3 1670.53 43.30 -5 -5 -3 654.83 15.80 5 -5 3 650.33 17.90 5 -5 3 658.83 16.80 -5 -5 -3 637.34 18.90 5 5 3 668.13 18.60 -5 5 -3 647.84 21.20 -5 5 -3 638.64 17.00 5 5 3 616.34 16.00 7 -5 3 1389.06 32.80 7 -5 3 1367.96 34.10 -7 -5 -3 1354.66 31.20 -7 -5 -3 1393.66 35.70 7 -5 3 1353.86 32.90 -7 5 -3 1432.56 38.50 7 5 3 1357.86 35.10 7 5 3 1296.87 31.70 9 -5 3 4.90 2.10 -9 -5 -3 -2.30 3.00 -9 -5 -3 5.80 1.30 9 -5 3 15.50 3.40 -9 5 -3 -3.60 5.20 9 5 3 15.40 4.10 9 5 3 8.60 2.50 11 -5 3 195.88 9.60 -11 -5 -3 188.18 10.80 11 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6 3 52.89 3.30 4 6 3 46.00 2.90 -4 6 -3 50.69 3.40 4 6 3 48.80 4.50 6 -6 3 6.30 2.30 6 -6 3 6.50 1.90 -6 -6 -3 3.00 3.10 6 -6 3 6.40 2.40 6 6 3 5.60 1.40 -6 6 -3 1.80 4.90 6 6 3 5.80 2.90 6 6 3 6.40 1.70 8 -6 3 73.69 4.40 8 -6 3 72.49 5.50 -8 -6 -3 50.49 6.60 8 6 3 58.59 5.90 8 6 3 62.99 3.50 -8 6 -3 76.59 10.00 -10 -6 -3 66.59 8.30 10 -6 3 94.09 7.10 10 -6 3 94.99 5.40 -10 6 -3 86.99 11.40 10 6 3 90.99 7.70 -12 -6 -3 125.29 11.90 12 -6 3 152.48 8.10 12 -6 3 145.49 9.20 12 6 3 134.19 10.00 -14 -6 -3 360.56 16.70 14 -6 3 347.37 11.90 -14 6 -3 343.67 19.10 14 6 3 355.06 16.30 16 -6 3 -1.90 3.90 16 -6 3 4.90 2.60 -16 -6 -3 5.10 4.60 16 6 3 -1.00 4.40 -16 6 -3 -0.30 6.50 -18 -6 -3 27.30 7.60 18 -6 3 23.90 5.80 18 -6 3 30.30 4.60 18 6 3 23.70 6.50 -18 6 -3 32.40 9.50 20 -6 3 5.10 5.50 -20 -6 -3 19.50 10.20 20 -6 3 5.20 3.30 -20 6 -3 6.50 7.60 20 6 3 7.50 5.50 23 -7 -3 -2.30 4.90 -23 -7 3 4.70 6.30 23 7 -3 -2.20 5.20 -23 7 3 8.30 10.70 21 -7 -3 13.20 5.90 -21 -7 3 18.60 7.00 -21 7 3 25.90 11.20 21 7 -3 13.70 5.90 19 -7 -3 105.99 10.10 -19 -7 3 105.09 10.80 -19 7 3 94.39 14.30 19 7 -3 83.99 10.10 -17 -7 3 23.90 6.80 17 -7 -3 13.60 5.30 17 7 -3 12.10 5.00 -17 7 3 10.60 8.30 -15 -7 3 126.39 10.40 15 -7 -3 122.89 9.30 15 7 -3 120.89 9.70 -15 7 3 126.39 13.80 -13 -7 3 43.40 6.60 13 -7 -3 60.69 7.20 13 7 -3 54.09 7.60 -13 7 3 64.19 9.80 11 -7 -3 43.30 5.90 -11 -7 3 39.10 6.40 11 7 -3 27.70 5.80 -11 7 3 30.60 7.70 9 -7 -3 3700.63 88.39 -9 -7 3 3854.51 89.39 9 7 -3 3816.22 89.19 -9 7 3 3838.72 91.69 -7 -7 3 2153.18 51.29 7 -7 -3 2079.29 50.59 -7 -7 3 2030.70 46.50 7 7 -3 2028.40 46.70 7 7 -3 2109.59 50.99 -7 7 3 2114.19 52.99 5 -7 -3 614.64 18.20 5 -7 -3 622.34 15.40 -5 -7 3 641.14 18.80 -5 -7 3 627.54 17.50 5 7 -3 617.44 18.20 -5 7 3 613.04 15.30 5 7 -3 602.74 16.50 -5 7 3 637.64 20.10 3 -7 -3 25.30 3.30 -3 -7 3 33.50 4.10 -3 -7 3 32.00 4.50 -3 -7 3 23.90 4.10 3 -7 -3 31.70 4.10 -3 7 3 24.20 4.80 3 7 -3 28.60 4.00 -3 7 3 27.30 3.20 1 -7 -3 616.04 18.00 1 -7 -3 594.44 16.70 -1 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-3.40 4.10 -17 7 -3 9.50 7.40 17 7 3 -1.60 4.80 19 -7 3 1.30 4.60 -19 -7 -3 -0.60 4.70 19 -7 3 -6.20 2.80 19 7 3 12.30 5.80 -19 7 -3 2.40 7.60 -22 -8 3 3.20 5.60 22 -8 -3 1.30 5.30 -22 8 3 1.60 8.60 22 8 -3 -3.10 5.30 20 -8 -3 1.90 5.20 -20 -8 3 2.90 5.40 -20 8 3 4.90 8.50 20 8 -3 -0.90 4.90 18 -8 -3 36.10 7.00 -18 -8 3 45.50 8.20 18 8 -3 34.70 7.10 -18 8 3 27.50 9.30 -16 -8 3 34.20 7.50 16 -8 -3 26.90 6.10 16 8 -3 24.50 6.20 -16 8 3 38.10 10.30 -14 -8 3 114.09 9.80 14 -8 -3 120.29 9.30 14 8 -3 107.59 9.60 -14 8 3 100.49 13.30 12 -8 -3 461.85 17.10 -12 -8 3 401.16 20.60 12 8 -3 451.95 18.60 -12 8 3 470.25 24.60 -10 -8 3 2345.57 58.39 10 -8 -3 2340.57 57.39 -10 8 3 2340.97 61.39 10 8 -3 2254.87 57.99 -8 -8 3 1182.88 33.70 8 -8 -3 1227.88 33.00 -8 8 3 1181.08 36.30 8 8 -3 1256.17 33.40 -6 -8 3 338.67 13.50 6 -8 -3 328.27 9.10 6 -8 -3 324.77 12.60 6 8 -3 351.76 12.80 -6 8 3 343.07 9.10 -6 8 3 338.27 15.40 6 8 -3 328.07 10.10 4 -8 -3 162.18 6.30 -4 -8 3 166.88 8.90 4 -8 -3 155.38 8.20 -4 8 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4 22.40 9.90 -21 -5 4 21.00 6.20 21 -5 -4 21.30 6.50 -21 5 4 32.30 9.90 21 5 -4 22.10 7.40 -19 -5 4 31.30 6.80 19 -5 -4 16.00 5.50 -19 5 4 16.90 7.80 19 5 -4 15.60 5.80 17 -5 -4 39.60 6.90 -17 -5 4 50.39 7.50 17 5 -4 47.80 7.00 -17 5 4 51.99 10.70 -15 -5 4 0.80 4.00 15 -5 -4 1.50 3.40 15 5 -4 -0.30 3.60 -15 5 4 -3.00 5.80 -13 -5 4 269.27 12.40 13 -5 -4 273.47 11.80 -13 5 4 274.77 14.90 13 5 -4 264.97 12.40 11 -5 -4 1090.49 29.50 -11 -5 4 1102.79 30.10 11 5 -4 1089.39 30.10 -11 5 4 1093.19 31.60 -9 -5 4 -2.50 3.40 9 -5 -4 0.30 2.00 -9 -5 4 2.60 1.30 9 5 -4 2.90 0.80 9 5 -4 3.20 2.30 -9 5 4 6.50 3.80 -7 -5 4 2.00 3.30 -7 -5 4 5.90 1.80 7 -5 -4 4.50 2.40 7 5 -4 3.00 1.80 -7 5 4 3.10 3.20 -5 -5 4 62.79 4.20 5 -5 -4 55.39 4.80 5 -5 -4 58.49 2.60 5 5 -4 58.99 3.40 -5 5 4 56.29 2.60 -5 5 4 55.19 5.80 5 5 -4 56.39 4.40 -3 -5 4 390.46 11.60 -3 -5 4 384.56 12.20 -3 -5 4 399.46 12.10 3 -5 -4 389.16 10.60 -3 5 4 380.46 10.40 -3 5 4 381.36 12.20 3 5 -4 374.96 11.70 -1 -5 4 91.09 4.40 1 -5 -4 81.29 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7 -10 757.52 22.90 -5 -7 10 139.69 10.10 5 -7 -10 137.19 8.00 5 -7 -10 136.59 9.80 5 7 -10 128.59 9.50 5 7 -10 117.39 6.80 -5 7 10 145.69 7.90 3 -7 -10 463.75 16.40 -3 -7 10 442.76 16.50 3 -7 -10 431.46 15.00 3 -7 -10 437.96 15.60 3 7 -10 449.36 17.30 -1 -7 10 108.39 5.70 -1 -7 10 109.09 8.40 1 -7 -10 105.19 7.80 1 -7 -10 104.39 7.80 1 -7 -10 91.19 7.00 1 7 -10 98.19 8.90 -1 -7 -10 421.96 16.50 1 -7 10 427.76 15.70 -1 -7 -10 450.15 15.20 1 7 10 433.16 15.00 -1 7 -10 426.26 18.20 3 -7 10 12.70 4.40 -3 -7 -10 17.30 5.20 -3 -7 -10 11.70 3.70 3 -7 10 9.80 2.70 3 7 10 12.50 3.70 -5 -7 -10 42.00 6.80 5 -7 10 32.30 4.00 5 -7 10 40.80 6.00 -5 -7 -10 34.70 4.80 5 7 10 35.50 5.40 -5 7 -10 32.50 7.50 -7 -7 -10 15.00 5.30 7 -7 10 14.90 4.50 -7 -7 -10 22.40 4.60 7 -7 10 21.30 3.70 7 7 10 20.70 5.10 -7 7 -10 13.20 6.40 -9 -7 -10 8.30 5.20 9 -7 10 9.80 5.20 9 -7 10 13.80 3.40 -9 -7 -10 11.20 4.20 -9 7 -10 16.40 7.00 9 7 10 17.90 5.30 -11 -7 -10 50.59 8.70 11 -7 10 60.99 7.80 11 -7 10 52.39 6.40 11 7 10 66.99 8.60 -11 7 -10 48.10 9.90 13 -7 10 46.80 7.30 13 -7 10 52.99 6.70 -13 -7 -10 66.99 16.50 13 7 10 49.70 8.20 -13 7 -10 49.70 10.50 22 -8 -10 -6.50 6.30 -22 -8 10 -4.50 5.60 -22 8 10 -4.80 9.20 22 8 -10 0.00 5.30 -20 -8 10 9.00 6.40 20 -8 -10 6.30 5.30 -20 8 10 0.70 8.10 20 8 -10 5.80 5.60 18 -8 -10 0.50 4.10 -18 -8 10 -2.50 5.10 -18 8 10 12.20 8.20 18 8 -10 0.70 4.20 16 -8 -10 109.69 9.50 -16 -8 10 104.29 10.40 -16 -8 10 107.09 4.60 -16 -8 10 97.79 6.90 16 8 -10 108.19 9.40 -16 8 10 110.89 13.10 14 -8 -10 40.80 6.60 -14 -8 10 32.60 7.00 -14 8 10 33.30 8.30 14 8 -10 32.80 4.10 -12 -8 10 42.60 7.50 12 -8 -10 59.29 9.70 12 8 -10 52.09 6.70 -12 8 10 57.19 8.70 10 -8 -10 57.99 6.80 10 8 -10 51.39 6.40 -10 8 10 52.19 3.50 10 8 -10 54.69 6.00 -10 8 10 54.89 7.70 -10 8 10 61.29 3.30 8 -8 -10 344.07 13.80 -8 -8 10 353.26 15.40 8 8 -10 330.47 13.80 -8 8 10 349.27 11.60 8 8 -10 342.17 13.30 -8 8 10 360.16 15.50 -6 -8 10 619.04 20.80 6 -8 -10 618.64 19.50 -6 8 10 578.74 20.80 -6 8 10 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5.00 -19 7 12 9.10 7.60 19 7 -12 5.80 4.70 -17 -7 12 3.00 5.80 17 -7 -12 7.60 4.40 -17 7 12 7.30 6.40 17 7 -12 9.00 3.40 17 7 -12 6.40 4.40 15 -7 -12 19.20 4.90 -15 -7 12 33.10 7.80 15 7 -12 35.90 5.70 15 7 -12 32.00 4.80 -15 7 12 26.60 7.20 -13 -7 12 102.29 9.90 13 -7 -12 89.79 8.30 13 7 -12 111.09 7.60 -13 7 12 105.09 4.90 -13 7 12 128.69 4.40 -13 7 12 115.79 10.60 13 7 -12 96.79 7.80 11 -7 -12 139.89 8.70 -11 -7 12 138.59 10.40 11 7 -12 136.39 8.10 -11 7 12 137.09 6.10 11 7 -12 126.29 8.10 -11 7 12 125.99 10.50 -9 -7 12 11.00 5.30 9 -7 -12 11.70 3.60 -9 7 12 6.20 4.80 9 7 -12 6.90 4.10 -9 7 12 11.50 3.10 9 7 -12 6.10 3.10 7 -7 -12 406.76 14.40 7 -7 -12 412.26 16.70 -7 -7 12 413.56 16.50 7 7 -12 404.96 13.50 -7 7 12 412.76 14.50 7 7 -12 394.36 16.40 5 -7 -12 7.60 3.60 5 -7 -12 5.60 5.10 -5 -7 12 1.30 5.30 -5 7 12 6.00 4.20 5 7 -12 6.60 4.80 5 7 -12 4.50 3.30 3 -7 -12 49.50 6.00 -3 -7 12 37.60 7.00 3 -7 -12 45.60 6.60 3 7 -12 46.10 4.30 3 7 -12 67.39 8.90 1 -7 -12 12.60 5.20 1 -7 -12 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5 14 70.79 7.50 11 -5 14 48.00 8.60 11 5 14 64.99 7.70 -11 5 -14 58.39 11.00 11 5 14 37.90 9.40 -24 -6 14 50.19 9.30 24 -6 -14 48.80 10.00 24 6 -14 28.90 8.70 -22 -6 14 2.10 5.90 22 -6 -14 -4.20 4.90 -22 -6 14 -5.80 3.30 22 6 -14 -1.50 4.50 -22 6 14 -2.60 8.10 -20 -6 14 4.00 5.90 -20 -6 14 10.70 4.00 20 -6 -14 5.80 5.00 -20 6 14 11.60 7.60 20 6 -14 16.00 5.60 -18 -6 14 15.80 7.00 18 -6 -14 10.10 4.90 -18 6 14 6.20 6.40 18 6 -14 20.60 5.00 18 6 -14 12.50 5.20 -16 -6 14 1.40 5.30 16 -6 -14 -0.60 3.50 -16 6 14 0.20 4.80 16 6 -14 1.90 3.50 16 6 -14 -4.00 3.00 -16 6 14 -0.70 2.30 -14 -6 14 410.66 17.70 14 -6 -14 410.16 15.60 -14 6 14 394.46 16.70 14 6 -14 407.46 15.50 14 6 -14 398.56 14.90 -14 6 14 419.66 18.30 12 -6 -14 195.98 10.10 -12 -6 14 207.58 12.40 12 -6 -14 202.68 12.30 12 6 -14 199.78 9.60 12 6 -14 213.78 10.80 -12 6 14 208.28 8.80 -10 -6 14 132.39 10.20 10 -6 -14 131.59 7.70 10 -6 -14 137.59 10.30 10 6 -14 140.39 7.20 10 6 -14 133.29 9.40 -10 6 14 135.69 7.60 8 -6 -14 13.10 3.50 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8.10 3 3 16 46.00 8.20 -5 -3 -16 120.19 11.90 5 -3 16 128.69 11.70 5 3 16 115.79 12.20 -5 3 -16 125.69 12.60 -7 -3 -16 33.20 7.70 7 -3 16 26.40 7.40 7 3 16 26.20 8.60 7 3 16 23.00 3.70 -7 3 -16 27.70 8.40 -9 -3 -16 13.00 7.30 9 -3 16 -1.10 5.80 9 3 16 -2.90 6.10 9 3 16 0.60 4.90 -9 3 -16 3.90 8.30 -24 -4 16 11.70 6.40 -24 -4 16 4.70 5.60 24 -4 -16 11.10 5.90 -24 4 16 5.60 8.20 24 4 -16 8.30 5.50 -22 -4 16 51.79 9.80 22 -4 -16 43.50 8.00 -22 -4 16 56.69 9.20 -22 4 16 71.59 5.50 -22 4 16 38.00 9.90 22 4 -16 57.89 8.90 20 -4 -16 19.00 5.40 -20 -4 16 19.10 6.70 -20 4 16 18.60 7.10 20 4 -16 17.60 5.30 20 4 -16 13.40 6.00 -20 4 16 16.10 4.00 -18 -4 16 -2.20 5.30 18 -4 -16 10.00 4.30 18 4 -16 7.70 4.00 -18 4 16 4.20 3.70 -18 4 16 10.00 5.80 18 4 -16 7.00 5.00 -16 -4 16 8.30 5.90 16 -4 -16 10.40 4.00 16 -4 -16 10.60 5.20 16 4 -16 9.60 4.00 -16 4 16 10.50 3.80 16 4 -16 15.00 4.90 -14 -4 16 66.79 9.20 14 -4 -16 77.99 9.70 14 -4 -16 87.19 7.00 14 4 -16 93.29 8.50 14 4 -16 95.09 6.70 -14 4 16 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8.30 1.70 9 5 -16 6.20 5.20 9 5 -16 9.70 2.10 7 -5 -16 42.70 6.70 7 -5 -16 41.70 4.40 -7 -5 16 37.70 6.50 7 5 -16 27.90 6.50 -7 5 16 37.00 6.30 5 -5 -16 78.89 5.40 -5 -5 16 76.89 9.20 5 -5 -16 73.59 8.90 -5 5 16 60.39 9.50 5 5 -16 70.09 9.70 3 -5 -16 833.92 26.70 -3 -5 16 789.82 26.70 -3 5 16 825.12 22.40 3 5 -16 851.01 29.60 -3 5 16 823.82 27.90 -1 -5 16 8.90 5.60 1 -5 -16 9.50 4.70 -1 5 16 10.40 6.10 1 5 -16 10.10 5.60 -1 5 16 4.30 2.70 -1 -5 -16 99.09 9.70 1 -5 16 95.89 9.80 1 5 16 115.59 11.30 -1 5 -16 101.79 11.50 1 5 16 80.89 6.00 -3 -5 -16 7.80 5.40 3 -5 16 -1.80 4.80 3 5 16 2.60 5.80 -3 5 -16 -0.10 5.10 3 5 16 6.30 3.10 -5 -5 -16 10.50 6.10 5 -5 16 3.30 5.50 5 5 16 6.70 3.40 -5 5 -16 2.60 5.60 5 5 16 4.30 6.10 7 -5 16 29.90 7.30 -7 -5 -16 56.59 8.80 7 5 16 32.40 11.60 -7 5 -16 26.50 8.20 7 5 16 34.40 5.10 9 -5 16 61.39 11.10 9 5 16 84.09 10.10 9 5 16 44.90 10.40 24 -6 -16 49.70 8.70 -24 -6 16 55.19 10.60 24 6 -16 43.70 9.40 -24 6 16 47.30 11.80 -22 -6 16 37.10 8.40 -22 -6 16 50.19 7.30 22 -6 -16 34.00 7.30 -22 6 16 45.50 10.90 22 6 -16 52.29 8.90 -20 -6 16 1.90 6.80 20 -6 -16 1.10 4.70 20 6 -16 0.30 4.60 -20 6 16 2.00 7.10 20 6 -16 0.00 4.30 18 -6 -16 11.60 4.70 -18 -6 16 8.10 6.30 -18 6 16 10.50 6.40 18 6 -16 10.40 4.90 18 6 -16 16.20 5.30 -18 6 16 12.00 5.70 -16 -6 16 57.79 8.60 16 -6 -16 55.99 7.30 -16 6 16 74.59 9.70 16 6 -16 75.49 7.40 -16 6 16 57.39 5.50 16 6 -16 55.19 8.40 14 -6 -16 6.00 3.80 -14 -6 16 -4.00 5.50 -14 6 16 2.50 3.10 14 6 -16 -1.80 4.00 14 6 -16 0.20 2.90 -14 6 16 8.20 5.90 12 -6 -16 9.30 3.60 -12 -6 16 8.40 5.90 12 -6 -16 1.40 5.10 -12 6 16 7.20 3.50 12 6 -16 10.80 4.70 12 6 -16 9.20 3.00 10 -6 -16 131.19 7.80 10 -6 -16 129.69 10.90 -10 -6 16 132.49 10.80 -10 6 16 136.69 8.60 10 6 -16 128.99 8.50 8 -6 -16 -1.70 2.50 -8 -6 16 2.70 5.30 8 -6 -16 4.10 4.70 8 6 -16 -3.70 3.80 8 6 -16 -1.60 1.30 8 6 -16 -2.80 1.40 -8 6 16 -2.50 3.10 -6 -6 16 69.89 9.60 6 -6 -16 88.49 9.80 6 -6 -16 84.39 6.20 -6 6 16 78.99 8.50 6 6 -16 79.29 9.80 4 -6 -16 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-24 2.50 6.00 -11 -1 24 -2.10 6.40 11 1 -24 -1.10 5.30 -9 -1 24 5.60 7.10 9 -1 -24 6.70 6.30 -9 1 24 7.00 6.60 9 1 -24 6.90 6.30 7 -1 -24 -2.30 5.30 -7 -1 24 0.00 6.20 7 1 -24 3.80 5.80 -7 1 24 6.80 5.50 -16 -2 24 1.80 7.40 16 -2 -24 1.60 6.30 16 2 -24 -0.20 6.40 -16 2 24 -2.90 6.00 14 -2 -24 5.80 6.40 -14 -2 24 -0.60 7.00 14 2 -24 -6.30 5.20 -14 2 24 -9.30 5.40 12 -2 -24 6.20 6.60 -12 -2 24 -2.40 6.50 12 2 -24 5.80 6.70 -12 2 24 -1.40 5.80 -10 -2 24 6.00 6.70 10 -2 -24 3.60 6.20 -10 2 24 -3.70 9.40 10 2 -24 -1.50 6.10 -8 -2 24 1.30 6.50 8 -2 -24 2.50 6.60 -8 2 24 2.10 5.90 8 2 -24 1.10 5.20 -15 -3 24 5.70 7.60 -15 3 24 -2.50 5.70 13 -3 -24 -2.80 6.20 -13 -3 24 3.20 7.40 -13 3 24 -11.30 4.80 13 3 -24 1.80 5.80 11 -3 -24 5.20 6.40 -11 -3 24 -5.40 7.20 11 3 -24 6.30 6.20 -11 3 24 -4.80 6.80 -9 -3 24 117.79 13.80 -9 3 24 131.69 12.80 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 14301 _shelx_res_file ; TITL AA in C2/c shelx.res created by SHELXL-2018/3 at 15:49:20 on 22-Jun-2021 CELL 0.71073 19.0048 11.5216 17.2227 90.000 116.526 90.000 ZERR 8.00 0.0006 0.0004 0.0006 0.000 0.001 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O F UNIT 128 96 24 8 40 MERG 2 OMIT 0.00 54.00 ABIN DFIX 0.860 0.020 H3N N3 FMAP 2 PLAN 5 SIZE 0.320 0.760 0.860 ACTA BOND $H CONF L.S. 13 WGHT 0.066000 1.098400 FVAR 0.89880 C1 1 0.571290 0.676078 0.560902 11.00000 0.04932 0.07321 = 0.04982 -0.00963 0.02614 -0.00484 C2 1 0.628787 0.623441 0.545303 11.00000 0.05426 0.10713 = 0.06266 -0.02854 0.03637 -0.01491 C3 1 0.648669 0.510671 0.570135 11.00000 0.04256 0.10941 = 0.06683 -0.03894 0.02117 0.00555 C4 1 0.610800 0.452156 0.608941 11.00000 0.05056 0.07437 = 0.06004 -0.02060 0.00893 0.01710 C5 1 0.554290 0.505692 0.625478 11.00000 0.04181 0.05936 = 0.04775 -0.00740 0.01210 0.00511 C6 1 0.532952 0.620755 0.602358 11.00000 0.03343 0.05662 = 0.03794 -0.00644 0.01198 0.00065 C7 1 0.475801 0.682796 0.623798 11.00000 0.03274 0.04690 = 0.03630 0.00188 0.01274 0.00123 C8 1 0.491383 0.810687 0.645764 11.00000 0.03706 0.04645 = 0.04143 0.00719 0.02051 0.00117 C9 1 0.448168 1.008569 0.619483 11.00000 0.10620 0.05074 = 0.09902 0.01976 0.03373 0.01586 AFIX 137 H9A 2 0.503442 1.022817 0.652886 11.00000 -1.50000 H9B 2 0.420993 1.030799 0.652629 11.00000 -1.50000 H9C 2 0.428581 1.053157 0.566896 11.00000 -1.50000 AFIX 0 C10 1 0.364055 0.854407 0.520425 11.00000 0.06105 0.08812 = 0.05609 0.01690 0.00703 0.02069 AFIX 137 H10A 2 0.363739 0.772275 0.510888 11.00000 -1.50000 H10B 2 0.363100 0.895011 0.471289 11.00000 -1.50000 H10C 2 0.318605 0.875319 0.527986 11.00000 -1.50000 AFIX 0 C11 1 0.319182 0.604099 0.671381 11.00000 0.03155 0.04883 = 0.03710 0.00281 0.01062 -0.00398 C12 1 0.274122 0.658183 0.705410 11.00000 0.03962 0.05774 = 0.05421 0.00317 0.02107 0.00019 AFIX 43 H12 2 0.281692 0.736455 0.720011 11.00000 -1.20000 AFIX 0 C13 1 0.217930 0.595756 0.717640 11.00000 0.04458 0.08563 = 0.06600 0.01587 0.02986 0.00297 AFIX 43 H13 2 0.187876 0.632183 0.740795 11.00000 -1.20000 AFIX 0 C14 1 0.206049 0.480798 0.696009 11.00000 0.04751 0.08490 = 0.07461 0.02321 0.02503 -0.01386 AFIX 43 H14 2 0.167784 0.439171 0.703856 11.00000 -1.20000 AFIX 0 C15 1 0.251112 0.427422 0.662617 11.00000 0.06701 0.05517 = 0.07304 0.00621 0.02385 -0.01882 AFIX 43 H15 2 0.243095 0.349161 0.648076 11.00000 -1.20000 AFIX 0 C16 1 0.308136 0.487500 0.650147 11.00000 0.05270 0.05109 = 0.05328 -0.00157 0.02204 -0.00724 AFIX 43 H16 2 0.338580 0.450219 0.627863 11.00000 -1.20000 AFIX 0 N1 3 0.435283 0.885837 0.598342 11.00000 0.05314 0.05068 = 0.05296 0.01291 0.01925 0.00997 N2 3 0.422575 0.621353 0.631363 11.00000 0.03404 0.04774 = 0.04152 -0.00293 0.01523 -0.00134 N3 3 0.374061 0.672189 0.658334 11.00000 0.04056 0.04482 = 0.05395 -0.00871 0.02498 -0.00720 O1 4 0.554454 0.840092 0.705994 11.00000 0.04016 0.04866 = 0.05213 0.00370 0.01857 -0.00679 F1 5 0.552197 0.785896 0.533382 11.00000 0.09635 0.07906 = 0.08273 0.01094 0.06237 -0.00272 F2 5 0.664390 0.682333 0.506010 11.00000 0.10251 0.15032 = 0.11831 -0.03812 0.08930 -0.03310 F3 5 0.705066 0.458582 0.556676 11.00000 0.06244 0.16490 = 0.11122 -0.05521 0.04264 0.01959 F4 5 0.628943 0.340975 0.631991 11.00000 0.09198 0.08039 = 0.10782 -0.01402 0.02848 0.03921 F5 5 0.522393 0.443770 0.666827 11.00000 0.07587 0.05555 = 0.08835 0.01337 0.03889 0.01278 H3N 2 0.387517 0.738154 0.686085 11.00000 0.05366 HKLF 4 REM AA in C2/c REM wR2 = 0.1294, GooF = S = 1.079, Restrained GooF = 1.079 for all data REM R1 = 0.0436 for 3075 Fo > 4sig(Fo) and 0.0506 for all 3619 data REM 232 parameters refined using 1 restraints END WGHT 0.0660 1.0979 REM Highest difference peak 0.272, deepest hole -0.158, 1-sigma level 0.030 Q1 1 0.4822 0.7429 0.6327 11.00000 0.05 0.27 Q2 1 0.5075 0.6542 0.6190 11.00000 0.05 0.21 Q3 1 0.4808 1.0175 0.6877 11.00000 0.05 0.17 Q4 1 0.3410 0.9230 0.4895 11.00000 0.05 0.15 Q5 1 0.3243 0.5394 0.6663 11.00000 0.05 0.15 ; _shelx_res_checksum 88217 _shelx_fab_file ; 4 0 0 -0.28 0.00 6 0 0 -0.16 0.00 8 0 0 -0.19 0.00 10 0 0 0.19 0.00 12 0 0 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0.00 -4 0 2 0.75 0.00 -2 0 2 -2.98 0.00 0 0 2 -3.18 0.00 4 0 2 -0.16 0.00 -5 1 2 -0.21 0.00 -3 1 2 -0.07 0.00 3 1 2 0.29 0.00 23 1 2 0.49 0.00 0 2 2 2.20 0.00 -25 3 2 -0.58 0.00 -5 3 2 0.18 0.00 3 3 2 -0.45 0.00 21 3 2 -0.83 0.00 23 3 2 -0.88 0.00 -23 7 2 0.13 0.00 21 7 2 0.15 0.00 -19 11 2 0.10 0.00 -14 14 2 0.06 0.00 12 14 2 0.18 0.00 -11 15 2 0.17 0.00 -5 15 2 -0.08 0.00 9 15 2 -0.07 0.00 -4 16 2 -0.04 0.00 2 16 2 0.35 0.00 -25 1 3 -0.17 0.00 1 1 3 0.54 0.00 3 1 3 0.18 0.00 -24 2 3 -0.53 0.00 -2 2 3 -0.17 0.00 2 2 3 -0.29 0.00 22 4 3 0.74 0.00 1 5 3 0.04 0.00 -24 6 3 0.02 0.00 -18 12 3 -0.03 0.00 -14 14 3 0.02 0.00 -4 16 3 -0.20 0.00 4 16 3 0.41 0.00 -26 0 4 -0.11 0.00 -4 0 4 -0.40 0.00 -2 0 4 1.42 0.00 0 0 4 0.32 0.00 2 0 4 0.11 0.00 -25 1 4 -0.27 0.00 -1 1 4 0.16 0.00 1 1 4 -0.05 0.00 -24 2 4 0.13 0.00 0 2 4 -0.24 0.00 22 2 4 -0.10 0.00 -5 3 4 -0.40 0.00 3 3 4 0.27 0.00 -22 4 4 -0.09 0.00 -25 5 4 -0.10 0.00 21 5 4 -0.33 0.00 -3 15 4 0.25 0.00 -4 16 4 0.18 0.00 -5 1 5 1.00 0.00 -3 1 5 -0.27 0.00 -26 2 5 0.31 0.00 -8 2 5 -0.08 0.00 -6 2 5 -0.35 0.00 -4 2 5 -0.09 0.00 -7 3 5 0.12 0.00 21 3 5 0.12 0.00 -3 5 5 0.40 0.00 19 7 5 0.23 0.00 15 11 5 0.15 0.00 -6 14 5 -0.05 0.00 -7 15 5 -0.28 0.00 -5 15 5 -0.08 0.00 -6 16 5 0.33 0.00 -6 0 6 0.89 0.00 -2 0 6 0.21 0.00 0 0 6 0.27 0.00 2 0 6 0.22 0.00 -8 2 6 0.40 0.00 4 2 6 -0.15 0.00 -7 3 6 0.06 0.00 3 3 6 0.01 0.00 18 4 6 -0.17 0.00 20 4 6 -0.17 0.00 17 5 6 -0.12 0.00 7 9 6 -0.05 0.00 11 13 6 -0.15 0.00 -7 15 6 0.06 0.00 -4 16 6 0.02 0.00 -2 16 6 -0.02 0.00 3 1 7 -0.19 0.00 19 3 7 -0.17 0.00 18 4 7 -0.05 0.00 17 5 7 0.06 0.00 12 12 7 -0.04 0.00 -17 13 7 0.23 0.00 -9 13 7 0.03 0.00 -11 15 7 -0.06 0.00 -27 1 8 -0.13 0.00 -6 2 8 0.40 0.00 -19 5 8 0.09 0.00 16 6 8 0.09 0.00 16 8 8 -0.13 0.00 15 9 8 -0.03 0.00 -9 13 8 -0.39 0.00 9 13 8 0.14 0.00 16 4 9 0.05 0.00 17 5 9 -0.05 0.00 -23 9 9 0.23 0.00 -14 14 9 -0.02 0.00 -8 14 9 0.01 0.00 -5 15 9 -0.06 0.00 1 15 9 -0.11 0.00 -27 1 10 0.01 0.00 17 3 10 -0.01 0.00 -18 6 10 -0.04 0.00 12 8 10 -0.06 0.00 14 8 10 0.14 0.00 13 9 10 0.04 0.00 -10 14 10 -0.06 0.00 -5 15 10 0.03 0.00 -27 1 11 0.06 0.00 12 8 11 0.04 0.00 -12 12 11 0.20 0.00 -11 13 11 -0.10 0.00 5 13 11 0.01 0.00 -10 14 11 -0.13 0.00 -8 14 11 0.07 0.00 2 14 11 0.00 0.00 -25 3 12 -0.04 0.00 15 3 12 0.05 0.00 10 8 12 0.05 0.00 -18 12 12 0.03 0.00 6 12 12 -0.03 0.00 -10 14 12 -0.07 0.00 -8 14 12 -0.09 0.00 13 5 13 -0.04 0.00 11 7 13 0.05 0.00 -15 11 13 0.15 0.00 -11 13 13 -0.02 0.00 -8 14 13 -0.06 0.00 -4 14 13 -0.02 0.00 -27 1 14 -0.03 0.00 -15 11 14 0.06 0.00 5 11 14 -0.07 0.00 -14 12 14 0.03 0.00 -13 13 14 0.16 0.00 -1 13 14 -0.09 0.00 10 6 15 0.06 0.00 9 7 15 0.12 0.00 8 8 15 -0.10 0.00 -20 10 15 0.07 0.00 -14 12 15 0.15 0.00 -5 13 15 0.04 0.00 -4 0 16 0.09 0.00 -25 5 16 0.09 0.00 -21 9 16 0.07 0.00 5 9 16 0.05 0.00 -17 11 16 -0.13 0.00 -15 11 16 0.10 0.00 1 11 16 -0.04 0.00 -2 12 16 -0.21 0.00 -19 9 17 0.09 0.00 -18 10 17 -0.14 0.00 -1 11 17 -0.10 0.00 -10 12 17 0.11 0.00 -8 12 17 0.05 0.00 -25 3 18 -0.07 0.00 -19 9 18 -0.11 0.00 -13 11 18 0.06 0.00 -5 11 18 -0.05 0.00 -25 1 19 0.11 0.00 6 2 19 0.00 0.00 -23 5 19 -0.04 0.00 -21 7 19 0.02 0.00 -1 9 19 -0.02 0.00 -4 10 19 -0.01 0.00 -24 2 20 0.00 0.00 -18 8 20 0.04 0.00 -15 9 20 -0.02 0.00 2 2 21 0.05 0.00 -21 5 21 -0.05 0.00 -22 0 22 -0.06 0.00 0 2 22 -0.16 0.00 -21 3 22 -0.06 0.00 -19 5 22 0.12 0.00 -4 6 22 0.03 0.00 -15 7 22 -0.13 0.00 -7 7 22 0.00 0.00 -20 2 23 -0.10 0.00 -19 3 23 -0.11 0.00 -18 4 23 0.08 0.00 -12 6 23 0.02 0.00 -10 6 23 0.00 0.00 -18 0 24 0.05 0.00 -6 0 24 0.17 0.00 -12 4 24 0.05 0.00 -10 4 24 0.08 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 130819) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.228 0.750 63 1 ' ' 2 1.000 0.271 0.250 63 1 ' ' 3 1.000 0.728 0.750 63 1 ' ' 4 0.500 0.771 0.250 63 1 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 2 0 0 2.396 1 1 0 2.135 3 1 0 4.007 0 2 0 3.537 2 2 0 4.273 4 2 0 5.963 3 3 0 6.417 0 4 0 7.087 3 5 0 9.583 -7 1 1 8.104 -1 1 1 2.212 1 1 1 2.779 -2 2 1 4.144 1 3 1 5.728 3 3 1 6.872 -4 4 1 8.336 -1 5 1 8.972 1 5 1 9.131 -4 0 2 4.319 -2 0 2 2.659 0 0 2 2.644 4 0 2 6.435 -5 1 2 5.650 -3 1 2 3.815 3 1 2 5.621 0 2 2 4.417 -5 3 2 7.559 3 3 2 7.537 1 1 3 4.957 3 1 3 6.683 -2 2 3 5.052 2 2 3 6.527 1 5 3 10.024 -4 0 4 5.324 -2 0 4 4.734 0 0 4 5.293 2 0 4 6.722 -1 1 4 5.188 1 1 4 6.188 0 2 4 6.371 -5 3 4 8.002 3 3 4 9.309 -5 1 5 6.893 -3 1 5 6.215 -8 2 5 9.604 -6 2 5 8.112 -4 2 5 7.147 -7 3 5 9.666 -6 0 6 8.000 -2 0 6 7.204 0 0 6 7.953 2 0 6 9.290 -8 2 6 10.014 -7 3 6 10.145 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL shelx C 2/c R = 0.05 CELL 0.71073 19.0048 11.5216 17.2227 90.000 116.526 90.000 SPGR C2/c ) ; _shelx_fab_checksum 16055 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.57129(9) 0.67608(14) 0.56090(9) 0.0560(4) Uani d 1 . . C C2 0.62879(10) 0.6234(2) 0.54530(11) 0.0709(5) Uani d 1 . . C C3 0.64867(9) 0.5107(2) 0.57013(12) 0.0741(6) Uani d 1 . . C C4 0.61080(9) 0.45216(16) 0.60894(11) 0.0675(5) Uani d 1 . . C C5 0.55429(8) 0.50569(13) 0.62548(9) 0.0526(3) Uani d 1 . . C C6 0.53295(7) 0.62075(12) 0.60236(8) 0.0441(3) Uani d 1 . . C C7 0.47580(7) 0.68280(11) 0.62380(7) 0.0396(3) Uani d 1 . . C C8 0.49138(7) 0.81069(11) 0.64576(8) 0.0405(3) Uani d 1 . . C C9 0.44817(14) 1.00857(16) 0.61948(15) 0.0898(6) Uani d 1 . . H H9A 0.503442 1.022817 0.652886 0.135 Uiso calc 1 . . H H9B 0.420993 1.030799 0.652629 0.135 Uiso calc 1 . . H H9C 0.428581 1.053157 0.566896 0.135 Uiso calc 1 . . C C10 0.36406(10) 0.85441(17) 0.52042(11) 0.0755(5) Uani d 1 . . H H10A 0.363739 0.772275 0.510888 0.113 Uiso calc 1 . . H H10B 0.363100 0.895011 0.471289 0.113 Uiso calc 1 . . H H10C 0.318605 0.875319 0.527986 0.113 Uiso calc 1 . . C C11 0.31918(7) 0.60410(11) 0.67138(7) 0.0409(3) Uani d 1 . . C C12 0.27412(8) 0.65818(13) 0.70541(9) 0.0505(3) Uani d 1 . . H H12 0.281692 0.736455 0.720011 0.061 Uiso calc 1 . . C C13 0.21793(9) 0.59576(16) 0.71764(11) 0.0635(4) Uani d 1 . . H H13 0.187876 0.632183 0.740795 0.076 Uiso calc 1 . . C C14 0.20605(9) 0.48080(17) 0.69601(11) 0.0698(5) Uani d 1 . . H H14 0.167784 0.439171 0.703856 0.084 Uiso calc 1 . . C C15 0.25111(10) 0.42742(15) 0.66262(11) 0.0678(4) Uani d 1 . . H H15 0.243095 0.349161 0.648076 0.081 Uiso calc 1 . . C C16 0.30814(9) 0.48750(13) 0.65015(9) 0.0530(3) Uani d 1 . . H H16 0.338580 0.450219 0.627863 0.064 Uiso calc 1 . . N N1 0.43528(7) 0.88584(11) 0.59834(8) 0.0539(3) Uani d 1 . . N N2 0.42258(6) 0.62135(9) 0.63136(6) 0.0417(3) Uani d 1 . . N N3 0.37406(6) 0.67219(10) 0.65833(7) 0.0450(3) Uani d 1 . . O O1 0.55445(5) 0.84009(8) 0.70599(6) 0.0477(2) Uani d 1 . . F F1 0.55220(7) 0.78590(9) 0.53338(7) 0.0777(3) Uani d 1 . . F F2 0.66439(8) 0.68233(13) 0.50601(9) 0.1088(5) Uani d 1 . . F F3 0.70507(6) 0.45858(14) 0.55668(9) 0.1114(5) Uani d 1 . . F F4 0.62894(7) 0.34098(10) 0.63199(9) 0.0994(4) Uani d 1 . . F F5 0.52239(6) 0.44377(8) 0.66683(7) 0.0724(3) Uani d 1 . . H H3N 0.3875(9) 0.7382(12) 0.6861(10) 0.054(4) Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.0493(8) 0.0732(10) 0.0498(7) -0.0048(7) 0.0261(6) -0.0096(7) C2 0.0543(9) 0.1071(15) 0.0627(9) -0.0149(9) 0.0364(8) -0.0285(9) C3 0.0426(8) 0.1094(15) 0.0668(10) 0.0056(9) 0.0212(7) -0.0389(10) C4 0.0506(8) 0.0744(11) 0.0600(9) 0.0171(7) 0.0089(7) -0.0206(8) C5 0.0418(7) 0.0594(8) 0.0477(7) 0.0051(6) 0.0121(6) -0.0074(6) C6 0.0334(6) 0.0566(7) 0.0379(6) 0.0006(5) 0.0120(5) -0.0064(5) C7 0.0327(6) 0.0469(7) 0.0363(6) 0.0012(5) 0.0127(4) 0.0019(5) C8 0.0371(6) 0.0464(7) 0.0414(6) 0.0012(5) 0.0205(5) 0.0072(5) C9 0.1062(16) 0.0507(9) 0.0990(15) 0.0159(10) 0.0337(12) 0.0198(9) C10 0.0611(10) 0.0881(12) 0.0561(9) 0.0207(9) 0.0070(7) 0.0169(8) C11 0.0315(6) 0.0488(7) 0.0371(6) -0.0040(5) 0.0106(5) 0.0028(5) C12 0.0396(6) 0.0577(8) 0.0542(7) 0.0002(6) 0.0211(6) 0.0032(6) C13 0.0446(7) 0.0856(11) 0.0660(9) 0.0030(7) 0.0299(7) 0.0159(8) C14 0.0475(8) 0.0849(12) 0.0746(10) -0.0139(8) 0.0250(7) 0.0232(9) C15 0.0670(10) 0.0552(9) 0.0730(10) -0.0188(7) 0.0239(8) 0.0062(7) C16 0.0527(8) 0.0511(8) 0.0533(7) -0.0072(6) 0.0220(6) -0.0016(6) N1 0.0531(7) 0.0507(7) 0.0530(7) 0.0100(5) 0.0193(5) 0.0129(5) N2 0.0340(5) 0.0477(6) 0.0415(5) -0.0013(4) 0.0152(4) -0.0029(4) N3 0.0406(6) 0.0448(6) 0.0540(6) -0.0072(4) 0.0250(5) -0.0087(5) O1 0.0402(5) 0.0487(5) 0.0521(5) -0.0068(4) 0.0186(4) 0.0037(4) F1 0.0964(8) 0.0791(7) 0.0827(7) -0.0027(6) 0.0624(6) 0.0109(5) F2 0.1025(9) 0.1503(12) 0.1183(10) -0.0331(8) 0.0893(8) -0.0381(9) F3 0.0624(7) 0.1649(13) 0.1112(9) 0.0196(7) 0.0426(6) -0.0552(9) F4 0.0920(8) 0.0804(8) 0.1078(9) 0.0392(6) 0.0285(7) -0.0140(6) F5 0.0759(6) 0.0556(5) 0.0884(7) 0.0128(4) 0.0389(5) 0.0134(5) 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' F F 0.0171 0.0103 '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 F1 C1 C2 . . 117.32(15) ? F1 C1 C6 . . 119.67(13) ? C2 C1 C6 . . 123.01(17) ? F2 C2 C3 . . 120.62(16) ? F2 C2 C1 . . 120.0(2) ? C3 C2 C1 . . 119.34(17) ? F3 C3 C4 . . 120.3(2) ? F3 C3 C2 . . 120.2(2) ? C4 C3 C2 . . 119.47(14) ? F4 C4 C3 . . 119.80(16) ? F4 C4 C5 . . 119.29(18) ? C3 C4 C5 . . 120.90(17) ? F5 C5 C4 . . 117.09(14) ? F5 C5 C6 . . 121.33(12) ? C4 C5 C6 . . 121.55(15) ? C1 C6 C5 . . 115.69(13) ? C1 C6 C7 . . 121.43(13) ? C5 C6 C7 . . 122.82(12) ? N2 C7 C6 . . 117.21(12) ? N2 C7 C8 . . 125.67(11) ? C6 C7 C8 . . 116.65(10) ? O1 C8 N1 . . 123.28(12) ? O1 C8 C7 . . 119.03(11) ? N1 C8 C7 . . 117.68(11) ? N1 C9 H9A . . 109.5 ? N1 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? N1 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? N1 C10 H10A . . 109.5 ? N1 C10 H10B . . 109.5 ? H10A C10 H10B . . 109.5 ? N1 C10 H10C . . 109.5 ? H10A C10 H10C . . 109.5 ? H10B C10 H10C . . 109.5 ? C12 C11 C16 . . 119.99(12) ? C12 C11 N3 . . 117.50(12) ? C16 C11 N3 . . 122.50(12) ? C13 C12 C11 . . 119.85(14) ? C13 C12 H12 . . 120.1 ? C11 C12 H12 . . 120.1 ? C14 C13 C12 . . 120.56(16) ? C14 C13 H13 . . 119.7 ? C12 C13 H13 . . 119.7 ? C13 C14 C15 . . 119.37(14) ? C13 C14 H14 . . 120.3 ? C15 C14 H14 . . 120.3 ? C14 C15 C16 . . 121.37(16) ? C14 C15 H15 . . 119.3 ? C16 C15 H15 . . 119.3 ? C15 C16 C11 . . 118.85(15) ? C15 C16 H16 . . 120.6 ? C11 C16 H16 . . 120.6 ? C8 N1 C9 . . 118.65(14) ? C8 N1 C10 . . 124.09(13) ? C9 N1 C10 . . 116.99(14) ? C7 N2 N3 . . 119.24(11) ? N2 N3 C11 . . 119.22(11) ? N2 N3 H3N . . 119.5(10) ? C11 N3 H3N . . 117.2(11) ? 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 C1 F1 . 1.3430(19) ? C1 C2 . 1.377(2) ? C1 C6 . 1.383(2) ? C2 F2 . 1.336(2) ? C2 C3 . 1.367(3) ? C3 F3 . 1.3359(18) ? C3 C4 . 1.360(3) ? C4 F4 . 1.340(2) ? C4 C5 . 1.374(2) ? C5 F5 . 1.3301(18) ? C5 C6 . 1.392(2) ? C6 C7 . 1.4783(17) ? C7 N2 . 1.2880(16) ? C7 C8 . 1.5172(18) ? C8 O1 . 1.2317(15) ? C8 N1 . 1.3325(16) ? C9 N1 . 1.453(2) ? C9 H9A . 0.9600 ? C9 H9B . 0.9600 ? C9 H9C . 0.9600 ? C10 N1 . 1.463(2) ? C10 H10A . 0.9600 ? C10 H10B . 0.9600 ? C10 H10C . 0.9600 ? C11 C12 . 1.3832(19) ? C11 C16 . 1.3835(19) ? C11 N3 . 1.4011(16) ? C12 C13 . 1.380(2) ? C12 H12 . 0.9300 ? C13 C14 . 1.367(3) ? C13 H13 . 0.9300 ? C14 C15 . 1.372(3) ? C14 H14 . 0.9300 ? C15 C16 . 1.381(2) ? C15 H15 . 0.9300 ? C16 H16 . 0.9300 ? N2 N3 . 1.3385(14) ? N3 H3N . 0.873(13) ? 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 N3 H3N O1 2_656 0.874(14) 2.054(15) 2.8658(15) 154.2(14) yes C9 H9A O1 . 0.960 2.33 2.717(2) 103 no C10 H10A N2 . 0.96 2.55 3.194(2) 124 no C14 H14 O1 3_445 0.93 2.45 3.377(2) 172 yes C10 H10B Cg2 7_566 0.96 2.77 3.4685(19) 130 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 F1 C1 C2 F2 . . . . 1.5(2) ? C6 C1 C2 F2 . . . . -179.03(14) ? F1 C1 C2 C3 . . . . -178.29(14) ? C6 C1 C2 C3 . . . . 1.2(2) ? F2 C2 C3 F3 . . . . 1.2(2) ? C1 C2 C3 F3 . . . . -179.06(14) ? F2 C2 C3 C4 . . . . -179.10(15) ? C1 C2 C3 C4 . . . . 0.7(2) ? F3 C3 C4 F4 . . . . -1.5(2) ? C2 C3 C4 F4 . . . . 178.76(14) ? F3 C3 C4 C5 . . . . 178.08(13) ? C2 C3 C4 C5 . . . . -1.7(2) ? F4 C4 C5 F5 . . . . 2.3(2) ? C3 C4 C5 F5 . . . . -177.31(13) ? F4 C4 C5 C6 . . . . -179.60(13) ? C3 C4 C5 C6 . . . . 0.8(2) ? F1 C1 C6 C5 . . . . 177.51(12) ? C2 C1 C6 C5 . . . . -2.0(2) ? F1 C1 C6 C7 . . . . -5.2(2) ? C2 C1 C6 C7 . . . . 175.37(13) ? F5 C5 C6 C1 . . . . 179.00(12) ? C4 C5 C6 C1 . . . . 0.95(19) ? F5 C5 C6 C7 . . . . 1.72(19) ? C4 C5 C6 C7 . . . . -176.33(12) ? C1 C6 C7 N2 . . . . 154.68(12) ? C5 C6 C7 N2 . . . . -28.19(17) ? C1 C6 C7 C8 . . . . -32.65(16) ? C5 C6 C7 C8 . . . . 144.48(12) ? N2 C7 C8 O1 . . . . 114.61(14) ? C6 C7 C8 O1 . . . . -57.36(15) ? N2 C7 C8 N1 . . . . -65.23(16) ? C6 C7 C8 N1 . . . . 122.80(12) ? C16 C11 C12 C13 . . . . -0.4(2) ? N3 C11 C12 C13 . . . . 178.48(12) ? C11 C12 C13 C14 . . . . -0.3(2) ? C12 C13 C14 C15 . . . . 0.6(2) ? C13 C14 C15 C16 . . . . -0.2(3) ? C14 C15 C16 C11 . . . . -0.5(2) ? C12 C11 C16 C15 . . . . 0.7(2) ? N3 C11 C16 C15 . . . . -178.03(13) ? O1 C8 N1 C9 . . . . -1.2(2) ? C7 C8 N1 C9 . . . . 178.61(14) ? O1 C8 N1 C10 . . . . 172.55(14) ? C7 C8 N1 C10 . . . . -7.6(2) ? C6 C7 N2 N3 . . . . 174.02(10) ? C8 C7 N2 N3 . . . . 2.09(18) ? C7 N2 N3 C11 . . . . -176.33(11) ? C12 C11 N3 N2 . . . . 175.29(11) ? C16 C11 N3 N2 . . . . -5.90(18) ? _cod_database_fobs_code 2243878