#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:30:28 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227277 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/58/4035865.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4035865 loop_ _publ_author_name 'Bookser, Brett C.' 'Weinhouse, Michael I.' 'Burns, Aaron C.' 'Valiere, Andrew N.' 'Valdez, Lino J.' 'Stanczak, Pawel' 'Na, Jim' 'Rheingold, Arnold L.' 'Moore, Curtis E.' 'Dyck, Brian' _publ_section_title ; Solvent-Controlled, Site-Selective N-Alkylation Reactions of Azolo-Fused Ring Heterocycles at N1-, N2-, and N3-Positions, Including Pyrazolo[3,4- d]pyrimidines, Purines, [1,2,3]Triazolo[4,5]pyridines, and Related Deaza-Compounds. ; _journal_issue 12 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 6334 _journal_page_last 6353 _journal_paper_doi 10.1021/acs.joc.8b00540 _journal_volume 83 _journal_year 2018 _chemical_formula_moiety 'C6 H5 Cl N4' _chemical_formula_sum 'C6 H5 Cl N4' _chemical_formula_weight 168.59 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2016-09-07 _audit_creation_method ; Olex2 1.2-beta (compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221) ; _cell_angle_alpha 90 _cell_angle_beta 96.91(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 3.816(10) _cell_length_b 13.38(3) _cell_length_c 14.05(3) _cell_measurement_reflns_used 2086 _cell_measurement_temperature 100 _cell_measurement_theta_max 25.608 _cell_measurement_theta_min 2.961 _cell_volume 712(3) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_collection 'APEX2 v2013.6-2 (Bruker, 2013)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2008)' _diffrn_ambient_temperature 100 _diffrn_detector 'Bruker APEX-II CCD' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD Area Detector' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.979 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker APEX II Ultra' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'Double Bounce Multilayer Mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_unetI/netI 0.0291 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.979 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 4943 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.979 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.419 _diffrn_reflns_theta_min 2.110 _diffrn_source 'Micro Focus Rotating Anode' _diffrn_source_type 'Bruker TXS' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.466 _exptl_absorpt_correction_T_max 0.2590 _exptl_absorpt_correction_T_min 0.2332 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0533 before and 0.0391 after correction. The Ratio of minimum to maximum transmission is 0.9004. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.573 _exptl_crystal_description needle _exptl_crystal_F_000 344 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.242 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.048 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 101 _refine_ls_number_reflns 1297 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0289 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.2638P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.0683 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1127 _reflns_number_total 1297 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; dart172.res created by SHELXL-2014/7 TITL dart172_a.res in P2(1)/c CELL 0.71073 3.8164 13.376 14.0473 90 96.91 90 ZERR 4 0.0098 0.0292 0.0299 0 0.042 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N UNIT 24 20 4 16 L.S. 4 PLAN -19 0 0 SIZE 0.04 0.08 0.3 TEMP -173.15 HTAB BOND $H CONF fmap 2 acta MORE -1 REM REM REM WGHT 0.030800 0.263800 FVAR 0.30553 CL1 3 0.668902 0.959393 0.374845 11.00000 0.02026 0.01553 = 0.02547 0.00339 0.00234 -0.00186 N1 4 0.142267 0.620125 0.344340 11.00000 0.01507 0.01655 = 0.01403 0.00025 -0.00043 0.00117 C1 1 0.007808 0.517517 0.352151 11.00000 0.01804 0.01638 = 0.02423 -0.00134 -0.00023 -0.00193 AFIX 137 H1A 2 -0.135124 0.499044 0.292058 11.00000 -1.50000 H1B 2 -0.137698 0.514142 0.404986 11.00000 -1.50000 H1C 2 0.206849 0.471144 0.364604 11.00000 -1.50000 AFIX 0 C2 1 0.325726 0.677799 0.414824 11.00000 0.01041 0.01657 = 0.01493 -0.00115 0.00077 0.00324 N3 4 0.425888 0.651490 0.507535 11.00000 0.01722 0.01839 = 0.01481 0.00104 0.00224 0.00108 C4 1 0.601631 0.725976 0.557972 11.00000 0.01726 0.01969 = 0.01447 -0.00108 0.00055 0.00187 AFIX 43 H4 2 0.678416 0.713841 0.623816 11.00000 -1.20000 AFIX 0 C5 1 0.681049 0.821335 0.520268 11.00000 0.01431 0.01777 = 0.01979 -0.00338 0.00042 0.00128 AFIX 43 H5 2 0.807069 0.869488 0.560664 11.00000 -1.20000 AFIX 0 N6 4 0.093384 0.673122 0.259772 11.00000 0.01843 0.02074 = 0.01532 0.00248 -0.00015 0.00069 N7 4 0.238075 0.763453 0.273107 11.00000 0.01798 0.02019 = 0.01536 0.00120 0.00020 0.00067 C8 1 0.386252 0.768929 0.368169 11.00000 0.01269 0.01515 = 0.01564 0.00130 0.00287 0.00316 C9 1 0.574392 0.843860 0.424601 11.00000 0.01119 0.01362 = 0.02071 0.00181 0.00479 0.00128 HKLF 4 REM dart172_a.res in P2(1)/c REM R1 = 0.0289 for 1127 Fo > 4sig(Fo) and 0.0362 for all 1297 data REM 101 parameters refined using 0 restraints END WGHT 0.0305 0.2639 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y+1, -z+1 HTAB C1 N3_$1 REM Highest difference peak 0.242, deepest hole -0.248, 1-sigma level 0.048 Q1 1 0.3006 0.7369 0.4027 11.00000 0.05 0.24 Q2 1 0.5225 0.8063 0.3815 11.00000 0.05 0.22 Q3 1 0.4757 0.7124 0.3870 11.00000 0.05 0.21 Q4 1 0.2805 0.6446 0.3785 11.00000 0.05 0.21 Q5 1 -0.2447 0.5162 0.3232 11.00000 0.05 0.21 Q6 1 0.2684 0.7838 0.3291 11.00000 0.05 0.20 Q7 1 0.3815 0.8193 0.3960 11.00000 0.05 0.19 Q8 1 0.1807 0.6547 0.3856 11.00000 0.05 0.19 Q9 1 0.1461 0.8158 0.2418 11.00000 0.05 0.18 Q10 1 0.0762 0.5816 0.3550 11.00000 0.05 0.18 Q11 1 -0.0853 0.6550 0.2042 11.00000 0.05 0.18 Q12 1 0.2541 0.5963 0.5279 11.00000 0.05 0.17 Q13 1 0.7030 0.7645 0.5165 11.00000 0.05 0.17 Q14 1 0.0978 0.6411 0.3051 11.00000 0.05 0.16 Q15 1 0.3604 0.6586 0.4573 11.00000 0.05 0.16 Q16 1 0.0666 0.7315 0.2715 11.00000 0.05 0.15 Q17 1 0.5795 0.6880 0.5197 11.00000 0.05 0.14 Q18 1 0.3892 0.6615 0.5414 11.00000 0.05 0.14 Q19 1 0.1965 0.4674 0.4175 11.00000 0.05 0.14 REM The information below was added by Olex2. REM REM R1 = 0.0289 for 1127 Fo > 4sig(Fo) and 0.0362 for all 5105 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.24, deepest hole -0.25 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0362 REM R1_gt = 0.0289 REM wR_ref = 0.0683 REM GOOF = 1.059 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 5105 REM Reflections_gt = 1127 REM Parameters = n/a REM Hole = -0.25 REM Peak = 0.24 REM Flack = n/a ; _cod_data_source_file jo8b00540_si_007.cif _cod_data_source_block dart172 _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas ; _cod_database_code 4035865 _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_max 0.982 _shelx_estimated_absorpt_t_min 0.873 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C4(H4), C5(H5) 2.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C) ; _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn Cl1 Cl 0.66890(11) 0.95939(3) 0.37485(3) 0.02045(15) Uani 1 1 d . N1 N 0.1423(3) 0.62012(11) 0.34434(10) 0.0154(3) Uani 1 1 d . C1 C 0.0078(5) 0.51752(13) 0.35215(13) 0.0198(4) Uani 1 1 d . H1A H -0.1351 0.4990 0.2921 0.030 Uiso 1 1 calc GR H1B H -0.1377 0.5141 0.4050 0.030 Uiso 1 1 calc GR H1C H 0.2068 0.4711 0.3646 0.030 Uiso 1 1 calc GR C2 C 0.3257(4) 0.67780(13) 0.41482(12) 0.0140(4) Uani 1 1 d . N3 N 0.4259(4) 0.65149(11) 0.50753(10) 0.0168(3) Uani 1 1 d . C4 C 0.6016(4) 0.72598(13) 0.55797(13) 0.0173(4) Uani 1 1 d . H4 H 0.6784 0.7138 0.6238 0.021 Uiso 1 1 calc R C5 C 0.6810(4) 0.82133(13) 0.52027(12) 0.0174(4) Uani 1 1 d . H5 H 0.8071 0.8695 0.5607 0.021 Uiso 1 1 calc R N6 N 0.0934(4) 0.67312(11) 0.25977(10) 0.0183(3) Uani 1 1 d . N7 N 0.2381(4) 0.76345(11) 0.27311(11) 0.0180(4) Uani 1 1 d . C8 C 0.3863(4) 0.76893(12) 0.36817(12) 0.0144(4) Uani 1 1 d . C9 C 0.5744(4) 0.84386(12) 0.42460(12) 0.0149(4) Uani 1 1 d . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0203(2) 0.0155(2) 0.0255(3) 0.00339(18) 0.00234(17) -0.00186(18) N1 0.0151(7) 0.0166(8) 0.0140(8) 0.0002(6) -0.0004(6) 0.0012(6) C1 0.0180(9) 0.0164(10) 0.0242(10) -0.0013(8) -0.0002(7) -0.0019(8) C2 0.0104(8) 0.0166(9) 0.0149(9) -0.0012(7) 0.0008(6) 0.0032(7) N3 0.0172(7) 0.0184(8) 0.0148(8) 0.0010(6) 0.0022(6) 0.0011(6) C4 0.0173(9) 0.0197(10) 0.0145(9) -0.0011(7) 0.0005(7) 0.0019(7) C5 0.0143(8) 0.0178(9) 0.0198(10) -0.0034(7) 0.0004(7) 0.0013(7) N6 0.0184(7) 0.0207(8) 0.0153(8) 0.0025(6) -0.0002(6) 0.0007(7) N7 0.0180(7) 0.0202(8) 0.0154(8) 0.0012(6) 0.0002(6) 0.0007(7) C8 0.0127(8) 0.0151(9) 0.0156(9) 0.0013(7) 0.0029(7) 0.0032(7) C9 0.0112(8) 0.0136(9) 0.0207(10) 0.0018(7) 0.0048(7) 0.0013(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' Cl Cl 0.1484 0.1585 '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 C2 N1 C1 128.25(17) N6 N1 C1 122.10(15) N6 N1 C2 109.6(2) N1 C1 H1A 109.5 N1 C1 H1B 109.5 N1 C1 H1C 109.5 H1A C1 H1B 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 N1 C2 C8 104.3(2) N3 C2 N1 127.14(19) N3 C2 C8 128.59(16) C4 N3 C2 112.07(18) N3 C4 H4 117.4 N3 C4 C5 125.3(2) C5 C4 H4 117.4 C4 C5 H5 119.9 C9 C5 C4 120.13(16) C9 C5 H5 119.9 N7 N6 N1 109.56(16) N6 N7 C8 107.28(14) C2 C8 C9 116.7(2) N7 C8 C2 109.24(17) N7 C8 C9 134.05(17) C5 C9 Cl1 121.79(14) C5 C9 C8 117.19(19) C8 C9 Cl1 121.01(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cl1 C9 1.751(3) N1 C1 1.474(4) N1 C2 1.378(3) N1 N6 1.377(3) C1 H1A 0.9800 C1 H1B 0.9800 C1 H1C 0.9800 C2 N3 1.359(3) C2 C8 1.416(3) N3 C4 1.353(3) C4 H4 0.9500 C4 C5 1.428(4) C5 H5 0.9500 C5 C9 1.390(4) N6 N7 1.332(3) N7 C8 1.388(3) C8 C9 1.418(3) 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 N1 C2 N3 C4 -179.78(16) N1 C2 C8 N7 0.38(18) N1 C2 C8 C9 -179.88(14) N1 N6 N7 C8 0.44(17) C1 N1 C2 N3 0.7(3) C1 N1 C2 C8 -179.76(15) C1 N1 N6 N7 179.47(14) C2 N1 N6 N7 -0.21(18) C2 N3 C4 C5 -0.8(2) C2 C8 C9 Cl1 179.47(12) C2 C8 C9 C5 -0.2(2) N3 C2 C8 N7 179.89(15) N3 C2 C8 C9 -0.4(3) N3 C4 C5 C9 0.3(3) C4 C5 C9 Cl1 -179.45(13) C4 C5 C9 C8 0.2(2) N6 N1 C2 N3 -179.63(15) N6 N1 C2 C8 -0.11(17) N6 N7 C8 C2 -0.51(18) N6 N7 C8 C9 179.81(18) N7 C8 C9 Cl1 -0.9(3) N7 C8 C9 C5 179.48(17) C8 C2 N3 C4 0.8(2) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma -1 0 0 238.78 4.05 1 0 0 235.36 4.09 1 0 0 244.88 4.12 1 0 0 238.54 3.89 -1 0 0 246.44 3.91 -1 0 0 237.41 4.03 -2 0 0 28.42 1.04 2 0 0 28.55 0.89 2 0 0 26.53 1.16 2 0 0 31.32 1.22 -2 0 0 30.06 1.09 -2 0 0 27.37 0.88 -3 0 0 132.78 2.89 -3 0 0 126.78 2.89 3 0 0 127.81 3.36 3 0 0 128.86 3.31 4 0 0 46.85 2.25 0 -1 0 0 0.07 0 1 0 0.04 0.06 0 1 0 0.05 0.06 1 -1 0 80.49 1.83 1 -1 0 80.39 1.72 -1 -1 0 80.08 1.41 1 -1 0 81.14 1.83 -1 -1 0 81.85 1.43 -1 1 0 81.14 1.8 1 1 0 82.64 1.58 1 1 0 79.1 1.57 -1 1 0 82.71 1.74 -1 1 0 81.61 1.82 2 -1 0 60.55 1.85 -2 -1 0 63.33 1.43 -2 -1 0 63.4 1.46 2 -1 0 61.92 1.62 2 -1 0 62.92 1.92 -2 1 0 64.93 1.85 -2 1 0 66.12 1.8 2 1 0 62.23 1.71 2 1 0 64.2 1.76 -2 1 0 63.63 1.65 3 -1 0 0.68 0.54 3 -1 0 1.45 0.42 -3 -1 0 0.62 0.27 -3 -1 0 1.18 0.32 -3 1 0 1.13 0.51 3 1 0 0.66 0.43 3 1 0 0.84 0.52 -3 1 0 0.9 0.45 -3 1 0 1.08 0.36 4 -1 0 0.55 0.7 4 1 0 1.74 0.76 -4 1 0 0.54 0.44 0 -2 0 151.26 2.71 0 2 0 153.63 2.72 0 2 0 150.3 2.48 1 -2 0 110.33 2.36 1 -2 0 108.09 2.39 1 -2 0 109.45 2.35 1 2 0 109.68 1.77 -1 2 0 112.63 2.37 -1 2 0 107.18 2.36 -1 2 0 109.76 2.39 2 -2 0 -0.22 0.3 2 -2 0 -0.3 0.29 2 -2 0 0.05 0.4 -2 2 0 -0.31 0.32 2 2 0 0.63 0.29 2 2 0 0.08 0.25 -2 2 0 0.12 0.27 -2 2 0 -0.12 0.3 3 -2 0 24.49 1.51 3 -2 0 24.39 1.2 -3 2 0 24.66 1.38 -3 2 0 22.72 1.14 3 2 0 23.77 1.23 3 2 0 24 1.26 -3 2 0 25.76 1.33 4 -2 0 2.27 0.85 4 2 0 0.97 0.63 -4 2 0 2.25 0.67 0 -3 0 -0.01 0.3 0 3 0 -0.05 0.18 0 3 0 -0.11 0.24 1 -3 0 144.27 3.06 1 -3 0 145.89 3.01 1 -3 0 145.4 3.02 -1 3 0 143.8 3.03 -1 3 0 144.14 3.02 1 3 0 142.49 2.53 -1 3 0 147.46 3.09 2 -3 0 53.01 1.91 2 -3 0 58.53 1.84 2 -3 0 56.92 1.89 -2 3 0 54.24 1.83 -2 3 0 58.21 1.82 2 3 0 54.5 1.39 2 3 0 55.71 1.39 -2 3 0 54.94 1.89 3 -3 0 11.5 1.23 3 -3 0 11.81 0.98 -3 3 0 9.33 0.97 3 3 0 9.7 0.83 3 3 0 10.84 0.91 -3 3 0 9.95 1.06 -3 3 0 12.36 1.26 4 -3 0 17.59 1.71 -4 3 0 16.15 1.41 4 3 0 13.3 1.3 0 -4 0 100.79 2.32 0 4 0 101.74 1.98 0 4 0 102.4 2.33 0 4 0 99.36 1.99 1 -4 0 4.85 0.59 1 -4 0 5.67 0.63 1 -4 0 5.14 0.66 -1 4 0 5.75 0.67 1 4 0 4.36 0.41 -1 4 0 6.38 0.74 -1 4 0 4.59 0.59 2 -4 0 18.22 1.17 2 -4 0 18.78 1.13 2 -4 0 16.55 1.1 -2 4 0 18.59 1.1 -2 4 0 18.61 1.14 2 4 0 20.51 0.68 -2 4 0 19.64 1.19 2 4 0 19.84 0.67 3 -4 0 61.61 2.48 3 -4 0 69.15 2.3 3 4 0 64.44 1.94 3 4 0 68.07 1.93 -3 4 0 65.7 2.48 -3 4 0 67.19 2.3 -3 4 0 64.07 2.41 4 -4 0 3.4 0.96 4 4 0 2.22 0.73 -4 4 0 2.72 0.88 0 -5 0 -0.34 0.29 0 5 0 0.02 0.21 0 5 0 0.19 0.23 0 5 0 0.07 0.27 1 -5 0 120.47 3.03 1 -5 0 121.63 2.81 1 -5 0 120.3 2.75 -1 -5 0 116.23 2.52 1 5 0 122.34 2.58 -1 5 0 120.75 2.88 -1 5 0 122.02 3.03 -1 5 0 123.91 2.88 2 -5 0 20.05 1.25 2 -5 0 20.99 1.28 2 -5 0 20.23 1.19 -2 5 0 18.71 1.25 -2 5 0 19.69 1.22 -2 5 0 21.46 1.27 3 -5 0 11.8 1.25 3 -5 0 12.8 1.34 -3 5 0 13.07 1.13 3 5 0 12.61 0.81 3 5 0 11.9 0.83 -3 5 0 15.8 1.49 4 -5 0 27.47 1.97 -4 5 0 24.98 1.8 0 -6 0 188.97 4.11 0 6 0 199.01 3.66 0 6 0 196.64 3.69 0 6 0 194.43 4.17 1 -6 0 0.6 0.36 1 -6 0 0.43 0.33 -1 -6 0 0.25 0.32 1 -6 0 0.8 0.47 -1 6 0 0.21 0.31 -1 6 0 0.29 0.35 -1 6 0 0.2 0.34 1 6 0 0.31 0.24 2 -6 0 21.23 1.38 2 -6 0 22.6 1.36 2 -6 0 21.9 1.3 2 6 0 24.24 0.81 -2 6 0 22.53 1.39 -2 6 0 23.65 1.43 -2 6 0 23.22 1.37 3 -6 0 9.97 1.23 3 -6 0 9.44 1.2 -3 6 0 10.07 1.31 3 6 0 8 0.7 3 6 0 8.02 0.65 4 -6 0 2.11 0.85 -4 6 0 0.4 0.73 0 -7 0 -0.18 0.35 0 7 0 0.4 0.29 0 7 0 0.51 0.34 0 7 0 0.65 0.28 1 -7 0 178.12 4.32 1 -7 0 185.98 3.86 -1 -7 0 177.71 3.84 1 7 0 185.73 3.92 -1 7 0 184.22 4.07 -1 7 0 188.94 4.14 -1 7 0 180.12 4.36 2 -7 0 56.85 2.16 2 -7 0 52.51 2.24 -2 7 0 53.83 2.19 2 7 0 53.4 1.5 -2 7 0 55.25 2.28 3 -7 0 9.03 1.23 3 -7 0 6.51 1.09 3 7 0 6.16 0.54 3 7 0 5.55 0.57 -3 7 0 9.57 1.33 4 -7 0 5.35 1.16 -4 7 0 5.48 1.21 0 -8 0 0.23 0.39 0 8 0 0.33 0.29 0 8 0 0.21 0.29 1 -8 0 14.66 1.27 -1 -8 0 17.58 1.14 1 8 0 16.45 1.04 1 8 0 17.26 0.63 -1 8 0 16.08 1.22 -1 8 0 18.58 1.15 -1 8 0 17.44 1.17 2 -8 0 8.82 1.2 -2 8 0 10.47 1.22 2 8 0 7.64 0.67 3 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4.76 1.25 -1 13 0 6.12 1.05 1 13 0 4.49 0.74 1 13 0 4.51 0.66 2 -13 0 0.02 0.85 -2 13 0 -1.04 0.53 0 -14 0 66.19 3.1 0 14 0 73.01 2.66 1 -14 0 0.11 0.79 -1 14 0 0.53 0.61 2 -14 0 26.04 2.32 -2 14 0 31.9 2.19 0 -15 0 0.94 0.87 0 15 0 0.49 0.55 1 -15 0 2.2 1.14 -1 15 0 1.4 0.71 0 16 0 20.21 1.62 4 0 -1 0.1 0.57 3 0 -1 0.15 0.38 -3 0 1 0.18 0.32 3 0 -1 -0.45 0.26 3 0 -1 -0.43 0.41 -3 0 1 0.5 0.34 2 0 -1 0.08 0.29 -2 0 1 0.03 0.25 2 0 -1 -0.13 0.22 2 0 -1 -0.23 0.31 -2 0 1 0.15 0.25 1 0 -1 -0.4 0.19 -1 0 1 0.29 0.22 -1 0 1 -0.15 0.19 1 0 -1 -0.39 0.22 1 0 -1 0.21 0.25 0 0 -1 -0.02 0.06 0 0 1 0 0.05 -1 0 -1 0.21 0.23 1 0 1 -0.09 0.23 1 0 1 0.25 0.25 -1 0 -1 -0.15 0.16 -1 0 -1 -0.11 0.2 -2 0 -1 -0.01 0.18 2 0 1 0.08 0.29 2 0 1 -0.37 0.29 -2 0 -1 0.1 0.27 -2 0 -1 -0.13 0.25 3 0 1 0.04 0.5 3 0 1 -0.13 0.36 -3 0 -1 0.49 0.38 -3 0 -1 -0.05 0.35 4 0 1 -0.05 0.63 4 -1 -1 2.6 0.84 4 1 -1 3.58 0.88 -4 1 1 5.05 0.73 -3 -1 1 58.41 1.44 3 -1 -1 55.79 2.12 3 -1 -1 56.99 2.81 -3 -1 1 55.55 1.42 3 -1 -1 59.31 1.75 3 1 -1 59.36 1.31 3 1 -1 58.18 2.03 -3 1 1 56.64 1.9 -3 1 1 57.36 1.88 3 1 -1 56.4 1.98 2 -1 -1 91.12 2.39 2 -1 -1 92.14 2.4 -2 -1 1 92.01 1.9 2 -1 -1 94.2 2.2 -2 -1 1 94.89 1.92 -2 1 1 96.68 2.21 2 1 -1 97.16 2.25 -2 1 1 90.23 2.26 2 1 -1 91.75 1.85 -2 1 1 98.2 2.36 2 1 -1 91.59 2.22 1 -1 -1 29.49 0.99 -1 -1 1 29.76 0.67 -1 -1 1 29.42 0.68 1 -1 -1 28.54 0.94 1 -1 -1 30.43 1.01 -1 1 1 31.12 0.95 -1 1 1 29.52 0.98 1 1 -1 27.65 0.78 1 1 -1 30.46 0.8 -1 1 1 29.13 0.97 0 -1 -1 11.29 0.42 0 -1 -1 11.02 0.36 0 1 1 11.32 0.42 0 1 1 11.73 0.37 0 1 -1 11.19 0.37 -1 -1 -1 592.4 8.96 1 -1 1 574.38 9.4 1 -1 1 570.6 9.33 -1 -1 -1 575.78 8.98 1 -1 1 588.45 9.22 1 1 1 587.75 9.1 1 1 1 583.32 9.1 -1 1 -1 589.78 9.23 -1 1 -1 586.45 9.36 -1 1 -1 578.66 9.37 2 -1 1 5.07 0.69 2 -1 1 5.78 0.65 -2 -1 -1 6.19 0.51 -2 -1 -1 5.2 0.44 2 1 1 5.45 0.62 2 1 1 5.88 0.6 -2 1 -1 6.13 0.54 -2 1 -1 5.48 0.63 -2 1 -1 6.46 0.67 -3 -1 -1 9.1 0.61 -3 -1 -1 8.46 0.57 3 -1 1 10.25 1.13 3 1 1 9.89 0.96 3 1 1 9.19 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