#------------------------------------------------------------------------------ #$Date: 2019-11-10 08:44:35 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225932 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/58/4515832.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_4515832 loop_ _publ_author_name 'Schmitt, Daniel C.' 'Niljianskul, Nootaree' 'Sach, Neal W.' 'Trujillo, John I.' _publ_section_title ; A Parallel Approach to 7-(Hetero)arylpyrazolo[1,5- a]pyrimidin-5-ones. ; _journal_issue 5 _journal_name_full 'ACS combinatorial science' _journal_page_first 256 _journal_page_last 260 _journal_paper_doi 10.1021/acscombsci.8b00032 _journal_volume 20 _journal_year 2018 _chemical_formula_sum 'C13 H11 N3 O' _chemical_formula_weight 225.25 _space_group_crystal_system orthorhombic _space_group_IT_number 45 _space_group_name_Hall 'I 2 -2c' _space_group_name_H-M_alt 'I b a 2' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 14.7666(12) _cell_length_b 20.3760(11) _cell_length_c 7.0357(4) _cell_measurement_temperature 123(2) _cell_volume 2116.9(2) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_unetI/netI 0.0201 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 14737 _diffrn_reflns_point_group_measured_fraction_full 0.967 _diffrn_reflns_point_group_measured_fraction_max 0.967 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 72.423 _diffrn_reflns_theta_min 3.697 _exptl_absorpt_coefficient_mu 0.755 _exptl_crystal_density_diffrn 1.413 _exptl_crystal_F_000 944 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.149 _refine_diff_density_min -0.130 _refine_diff_density_rms 0.030 _refine_ls_abs_structure_details ; Flack x determined using 874 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.08(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 158 _refine_ls_number_reflns 2037 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.070 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0244 _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^)+(0.0290P)^2^+1.0222P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.0626 _reflns_Friedel_coverage 0.787 _reflns_Friedel_fraction_full 0.937 _reflns_Friedel_fraction_max 0.937 _reflns_number_gt 1995 _reflns_number_total 2037 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file co8b00032_si_002.cif _cod_data_source_block Z918 _cod_database_code 4515832 _shelx_shelxl_version_number 2014/7 _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 0.928 _shelx_estimated_absorpt_t_max 0.970 _shelx_res_file ; Z918.res created by SHELXL-2014/7 TITL Z918.res in Iba2 CELL 1.54178 14.7666 20.3760 7.0357 90.000 90.000 90.000 ZERR 8.000 0.0012 0.0011 0.0004 0.000 0.000 0.000 LATT -2 SYMM -X, -Y, Z SYMM 1/2+X, 1/2-Y, Z SYMM 1/2-X, 1/2+Y, Z SFAC C H N O UNIT 104 88 24 8 L.S. 12 ACTA BOND $H FMAP 2 PLAN 0 SIZE 0.04 0.06 0.10 WPDB -2 DFIX 1.0 N1 H1X TEMP -150 WGHT 0.029000 1.022200 FVAR 0.23994 N1 3 0.384756 0.513257 0.409553 11.00000 0.01338 0.01539 = 0.02017 -0.00018 0.00063 0.00215 H1X 2 0.424798 0.477290 0.390229 11.00000 -1.20000 N2 3 0.237449 0.550234 0.486857 11.00000 0.01304 0.01373 = 0.01530 0.00025 0.00084 0.00013 N3 3 0.152353 0.527830 0.534070 11.00000 0.01344 0.01802 = 0.01703 0.00075 0.00189 -0.00154 O1 4 0.495377 0.586580 0.336168 11.00000 0.01352 0.02076 = 0.02725 0.00294 0.00221 0.00056 C1 1 0.197864 0.722766 0.369009 11.00000 0.01659 0.01688 = 0.02004 -0.00016 -0.00008 -0.00144 AFIX 43 H1 2 0.240802 0.724351 0.268563 11.00000 -1.20000 AFIX 0 C2 1 0.138043 0.774859 0.396079 11.00000 0.02193 0.01474 = 0.02545 -0.00034 -0.00828 -0.00052 AFIX 43 H2 2 0.139718 0.811552 0.312851 11.00000 -1.20000 AFIX 0 C3 1 0.076121 0.773275 0.544088 11.00000 0.01772 0.01799 = 0.03002 -0.00788 -0.00742 0.00505 AFIX 43 H3 2 0.036233 0.809183 0.564314 11.00000 -1.20000 AFIX 0 C4 1 0.072812 0.718852 0.662524 11.00000 0.01711 0.02287 = 0.02462 -0.00637 0.00126 0.00039 AFIX 43 H4 2 0.029948 0.717516 0.763140 11.00000 -1.20000 AFIX 0 C5 1 0.131355 0.666344 0.635799 11.00000 0.01856 0.01600 = 0.01944 -0.00134 0.00067 -0.00058 AFIX 43 H5 2 0.128164 0.629219 0.717203 11.00000 -1.20000 AFIX 0 C6 1 0.194838 0.668221 0.489232 11.00000 0.01314 0.01475 = 0.01965 -0.00287 -0.00248 -0.00054 C7 1 0.262600 0.615337 0.462704 11.00000 0.01802 0.01421 = 0.01286 -0.00002 -0.00091 0.00078 C8 1 0.349823 0.627469 0.415656 11.00000 0.01648 0.01376 = 0.01896 0.00090 0.00009 -0.00036 AFIX 43 H8 2 0.368747 0.671806 0.402755 11.00000 -1.20000 AFIX 0 C9 1 0.415619 0.575983 0.384083 11.00000 0.01558 0.01912 = 0.01454 0.00169 -0.00080 0.00036 C10 1 0.297137 0.499242 0.460856 11.00000 0.01396 0.01736 = 0.01320 -0.00069 -0.00092 0.00297 C11 1 0.250709 0.442184 0.493653 11.00000 0.01742 0.01438 = 0.01721 -0.00116 -0.00164 0.00073 AFIX 43 H11 2 0.273206 0.398552 0.487739 11.00000 -1.20000 AFIX 0 C12 1 0.161628 0.462801 0.538367 11.00000 0.01755 0.01640 = 0.01279 -0.00011 -0.00175 -0.00086 C13 1 0.082573 0.420711 0.590867 11.00000 0.01832 0.02003 = 0.02171 0.00036 0.00033 -0.00276 AFIX 137 H13A 2 0.070639 0.424838 0.727363 11.00000 -1.50000 H13B 2 0.096158 0.374828 0.560354 11.00000 -1.50000 H13C 2 0.029097 0.434875 0.519299 11.00000 -1.50000 AFIX 0 HKLF 4 REM Z918.res in Iba2 REM R1 = 0.0244 for 1995 Fo > 4sig(Fo) and 0.0251 for all 2037 data REM 158 parameters refined using 2 restraints END WGHT 0.0291 1.0187 REM Highest difference peak 0.149, deepest hole -0.130, 1-sigma level 0.030 Q1 1 0.1258 0.4414 0.5582 11.00000 0.05 0.15 Q2 1 0.2725 0.4708 0.4129 11.00000 0.05 0.14 Q3 1 0.3828 0.6032 0.4428 11.00000 0.05 0.14 Q4 1 0.3136 0.6295 0.5203 11.00000 0.05 0.14 Q5 1 0.2493 0.5832 0.4869 11.00000 0.05 0.14 Q6 1 0.2775 0.5262 0.5159 11.00000 0.05 0.14 Q7 1 0.2224 0.6389 0.4620 11.00000 0.05 0.13 Q8 1 0.2094 0.6999 0.4674 11.00000 0.05 0.13 Q9 1 0.1706 0.7490 0.3997 11.00000 0.05 0.12 Q10 1 0.1144 0.5485 0.4432 11.00000 0.05 0.12 Q11 1 0.1264 0.7804 0.5081 11.00000 0.05 0.12 Q12 1 0.0874 0.6836 0.6108 11.00000 0.05 0.11 Q13 1 0.0954 0.3861 0.6745 11.00000 0.05 0.11 Q14 1 0.2091 0.4480 0.5779 11.00000 0.05 0.11 Q15 1 0.1526 0.7400 0.3652 11.00000 0.05 0.11 Q16 1 0.2861 0.4695 0.5325 11.00000 0.05 0.10 Q17 1 0.3471 0.5016 0.4802 11.00000 0.05 0.10 Q18 1 0.5295 0.5523 0.2787 11.00000 0.05 0.10 Q19 1 0.1186 0.5456 0.6247 11.00000 0.05 0.09 Q20 1 0.3523 0.6693 0.2846 11.00000 0.05 0.09 ; _shelx_res_checksum 75286 _shelx_hkl_file ; -1 0 -1 0.29 0.16 -3 0 -3 0.19 0.25 -3 0 -3 0.15 0.29 4 0 4 407.94 13.80 4 0 4 423.47 13.57 -4 0 -4 427.85 15.28 -4 0 -4 455.77 14.09 -4 0 -4 441.25 13.74 5 0 5 0.33 0.60 5 0 5 -0.48 0.29 5 0 5 0.17 0.44 5 0 5 -0.19 0.39 6 0 6 37.11 1.82 6 0 6 40.05 2.28 6 0 6 40.11 2.19 7 0 7 0.13 0.48 7 0 7 0.03 0.43 7 0 7 0.15 0.46 6 -1 7 1.81 0.50 6 -1 7 2.55 0.74 6 -1 7 1.97 0.53 5 -1 6 71.63 3.19 5 -1 6 71.18 3.25 5 -1 6 72.49 2.86 4 -1 5 15.20 1.04 4 -1 5 16.04 1.37 4 -1 5 14.22 1.25 4 -1 5 14.34 0.97 -3 1 -4 413.44 13.23 -3 1 -4 392.17 12.78 -3 1 -4 396.47 12.93 -2 1 -3 43.08 1.76 -2 1 -3 43.48 1.78 -2 1 -3 45.31 1.92 0 1 -1 -0.02 0.14 0 1 -1 -0.01 0.11 0 -1 1 -0.07 0.12 0 -1 1 0.03 0.13 1 1 0 89.38 2.75 1 1 0 87.14 2.75 -1 -1 0 85.47 2.75 -1 -1 0 88.42 2.75 2 1 1 452.21 13.95 -2 -1 -1 451.96 13.95 -3 -1 -2 178.12 5.87 -4 -1 -3 38.40 1.64 -4 -1 -3 39.84 1.86 -4 -1 -3 38.69 2.01 5 1 4 22.58 1.56 5 1 4 21.34 1.39 5 1 4 21.03 1.17 -5 -1 -4 22.46 1.17 6 1 5 11.66 1.33 6 1 5 11.23 1.03 6 1 5 11.65 1.28 7 1 6 8.20 1.20 7 1 6 6.66 0.93 7 1 6 8.16 1.34 8 1 7 3.26 0.52 8 1 7 2.52 0.52 8 1 7 3.32 0.64 5 -2 7 2.12 0.57 5 -2 7 3.28 0.70 3 -2 5 9.93 1.08 3 -2 5 11.37 0.91 3 -2 5 11.34 0.91 3 -2 5 11.10 1.09 -2 2 -4 343.98 10.94 -2 2 -4 326.80 10.96 -2 2 -4 349.52 11.16 -1 2 -3 228.84 7.38 -1 2 -3 227.55 7.49 -1 2 -3 237.96 7.51 3 2 1 82.95 2.85 -3 -2 -1 81.13 2.84 -3 -2 -1 80.38 2.72 -4 -2 -2 11.95 0.89 -5 -2 -3 14.63 0.87 -5 -2 -3 17.09 1.37 -5 -2 -3 16.07 1.16 6 2 4 115.61 4.65 6 2 4 124.84 4.26 6 2 4 120.95 4.52 7 2 5 11.85 1.48 7 2 5 13.42 1.12 7 2 5 13.00 1.40 8 2 6 52.56 2.60 8 2 6 54.85 2.73 9 2 7 28.68 1.28 9 2 7 31.18 1.56 9 2 7 33.86 1.60 4 -3 7 -0.71 0.42 4 -3 7 0.23 0.33 3 -3 6 67.30 2.98 3 -3 6 69.13 2.94 3 -3 6 66.25 3.01 3 -3 6 68.21 2.70 2 -3 5 135.87 4.75 2 -3 5 132.03 4.65 2 -3 5 136.69 5.00 2 -3 5 131.79 4.89 -1 3 -4 150.82 5.20 -1 3 -4 154.60 5.10 -1 3 -4 153.73 5.38 1 -3 4 153.58 5.21 0 3 -3 0.01 0.29 0 3 -3 0.10 0.16 0 3 -3 0.27 0.18 1 3 -2 79.33 2.75 1 3 -2 79.87 2.84 1 3 -2 81.33 2.60 -1 -3 2 81.95 2.68 -1 -3 2 80.00 2.87 3 3 0 6.37 0.56 3 3 0 6.34 0.54 -3 -3 0 6.01 0.54 -3 -3 0 6.52 0.54 4 3 1 390.72 12.46 -4 -3 -1 396.02 12.45 -4 -3 -1 398.80 12.32 -5 -3 -2 57.74 2.25 -5 -3 -2 64.00 2.54 6 3 3 30.53 1.47 6 3 3 31.59 1.72 6 3 3 36.22 2.64 -6 -3 -3 32.09 1.47 7 3 4 8.84 1.26 7 3 4 9.56 1.20 8 3 5 10.64 1.11 8 3 5 11.54 1.48 8 3 5 11.26 1.36 9 3 6 29.78 1.55 9 3 6 28.59 1.77 9 3 6 29.35 1.88 10 3 7 8.75 0.83 10 3 7 12.57 0.97 10 3 7 10.51 0.75 3 -4 7 36.67 1.73 2 -4 6 14.16 1.07 2 -4 6 14.88 1.16 1 -4 5 2.94 0.72 1 -4 5 4.35 0.77 1 -4 5 5.59 0.76 1 -4 5 4.43 0.68 0 4 -4 8.14 0.87 0 4 -4 10.47 0.57 0 -4 4 9.43 0.78 1 4 -3 61.03 2.43 1 4 -3 60.61 2.02 -1 -4 3 60.23 2.47 2 4 -2 98.36 3.48 2 4 -2 98.86 3.18 -2 -4 2 98.88 3.30 -2 -4 2 100.38 3.54 3 4 -1 505.30 16.03 3 4 -1 508.37 15.89 -3 -4 1 503.12 16.05 -3 -4 1 509.65 16.03 -3 -4 1 550.38 15.93 4 4 0 287.15 9.13 4 4 0 283.56 9.12 -4 -4 0 290.61 9.12 -4 -4 0 286.77 9.12 5 4 1 8.07 0.76 -5 -4 -1 7.23 0.61 -5 -4 -1 7.10 0.71 -6 -4 -2 60.71 2.42 -6 -4 -2 64.73 2.96 7 4 3 92.56 3.74 7 4 3 91.99 3.37 7 4 3 93.94 3.56 -7 -4 -3 89.13 3.43 8 4 4 3.35 0.66 8 4 4 4.35 0.95 8 4 4 3.47 0.74 9 4 5 2.66 0.72 9 4 5 2.57 0.83 10 4 6 59.50 2.73 10 4 6 51.57 2.25 10 4 6 63.00 3.22 3 -5 8 14.49 0.73 2 -5 7 19.06 1.21 1 -5 6 79.44 3.01 0 -5 5 -0.26 0.35 1 5 -4 19.44 1.31 -1 -5 4 20.09 1.15 2 5 -3 41.71 1.93 -2 -5 3 42.90 2.01 3 5 -2 396.03 12.67 3 5 -2 401.16 12.32 -3 -5 2 397.48 12.47 -3 -5 2 398.39 12.73 4 5 -1 167.43 5.45 4 5 -1 166.04 5.60 -4 -5 1 169.18 5.47 -4 -5 1 165.26 5.62 -4 -5 1 166.96 5.58 5 5 0 595.54 17.62 -5 -5 0 496.58 18.00 -5 -5 0 591.53 17.60 6 5 1 17.47 1.16 -6 -5 -1 17.39 1.03 -6 -5 -1 16.09 1.14 7 5 2 67.93 2.68 7 5 2 64.12 2.81 7 5 2 68.39 2.49 -7 -5 -2 68.01 2.72 8 5 3 35.15 1.68 8 5 3 35.71 1.84 8 5 3 33.48 1.95 8 5 3 32.91 1.43 -8 -5 -3 29.37 1.47 -8 -5 -3 31.83 1.45 9 5 4 31.49 1.91 9 5 4 30.70 1.72 9 5 4 31.15 2.08 -9 -5 -4 26.38 1.42 10 5 5 1.31 0.59 10 5 5 3.02 0.73 10 5 5 2.21 0.74 -10 -5 -5 2.17 0.44 11 5 6 28.71 1.58 11 5 6 26.71 1.32 11 5 6 27.91 1.51 2 -6 8 7.17 0.59 1 -6 7 21.91 1.33 0 -6 6 51.98 2.38 -1 -6 5 5.74 0.83 -1 -6 5 6.18 0.74 -2 -6 4 43.27 1.89 -2 -6 4 41.73 1.84 -2 -6 4 41.45 1.58 3 6 -3 15.83 1.45 -3 -6 3 14.21 1.17 -3 -6 3 14.32 0.70 4 6 -2 52.62 2.27 4 6 -2 49.94 1.89 -4 -6 2 54.51 2.09 -4 -6 2 50.09 2.30 5 6 -1 4.97 0.55 5 6 -1 5.19 0.69 -5 -6 1 4.99 0.66 -5 -6 1 5.13 0.57 -5 -6 1 4.48 0.68 6 6 0 384.29 12.03 -6 -6 0 371.21 12.00 -6 -6 0 360.51 11.97 7 6 1 0.89 0.48 7 6 1 1.03 0.35 -7 -6 -1 0.57 0.31 -7 -6 -1 0.31 0.29 8 6 2 118.92 4.05 8 6 2 117.78 4.45 8 6 2 116.40 4.11 -8 -6 -2 115.29 4.01 -8 -6 -2 112.18 4.35 -8 -6 -2 115.35 3.99 9 6 3 141.85 4.98 9 6 3 149.76 5.28 9 6 3 143.67 4.79 9 6 3 141.89 5.38 -9 -6 -3 129.33 5.11 10 6 4 220.49 7.73 -10 -6 -4 186.78 6.49 -10 -6 -4 185.01 6.74 11 6 5 21.13 1.49 11 6 5 20.93 1.59 11 6 5 21.12 1.38 -11 -6 -5 21.28 1.14 12 6 6 19.42 1.10 12 6 6 19.42 0.92 12 6 6 19.16 1.44 1 -7 8 5.18 0.52 0 -7 7 -0.09 0.35 -1 -7 6 49.01 2.34 -2 -7 5 21.82 1.37 -3 -7 4 18.67 1.14 -3 -7 4 18.20 0.93 -4 -7 3 59.78 2.46 -4 -7 3 67.56 2.48 -4 -7 3 66.40 2.41 5 7 -2 87.90 3.10 5 7 -2 85.87 3.50 -5 -7 2 89.63 3.62 -5 -7 2 87.89 3.32 6 7 -1 64.80 2.84 6 7 -1 65.14 2.64 -6 -7 1 65.03 2.85 -6 -7 1 74.69 3.22 -6 -7 1 65.39 2.68 7 7 0 298.77 9.82 7 7 0 289.86 9.61 7 7 0 309.41 10.27 7 7 0 319.86 9.80 -7 -7 0 304.58 9.68 -7 -7 0 303.35 9.67 -7 -7 0 306.47 10.22 -7 -7 0 316.41 10.25 8 7 1 1.64 0.30 8 7 1 1.49 0.57 8 7 1 1.77 0.59 8 7 1 1.71 0.42 -8 -7 -1 1.30 0.38 -8 -7 -1 1.45 0.38 9 7 2 70.50 2.77 9 7 2 68.51 3.02 9 7 2 68.50 2.97 -9 -7 -2 67.94 2.62 -9 -7 -2 67.77 2.58 10 7 3 18.62 1.11 10 7 3 18.76 1.47 10 7 3 19.84 1.65 10 7 3 21.01 1.50 -10 -7 -3 18.06 1.18 -10 -7 -3 19.42 1.13 11 7 4 11.24 1.29 11 7 4 12.72 1.39 11 7 4 12.44 1.25 -11 -7 -4 11.34 0.81 -11 -7 -4 12.23 0.96 12 7 5 8.51 1.02 12 7 5 7.61 0.93 12 7 5 7.33 0.91 -12 -7 -5 7.52 0.66 0 -8 8 59.80 2.17 -1 -8 7 0.55 0.41 3 8 -5 49.28 1.98 -3 -8 5 55.42 2.37 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0.54 0.36 -13 -8 -5 0.06 0.24 -1 -9 8 1.85 0.43 -2 -9 7 5.43 0.75 3 9 -6 22.03 1.11 -3 -9 6 26.34 1.49 4 9 -5 26.95 1.26 -4 -9 5 27.65 1.20 -4 -9 5 28.01 1.57 -4 -9 5 28.34 1.46 5 9 -4 144.41 4.70 5 9 -4 131.64 4.58 -5 -9 4 137.44 4.70 -5 -9 4 140.27 4.88 6 9 -3 19.26 0.95 6 9 -3 15.43 0.95 -6 -9 3 18.15 0.92 -6 -9 3 19.38 1.09 -6 -9 3 17.76 1.06 7 9 -2 129.33 4.33 7 9 -2 131.96 4.27 7 9 -2 128.73 4.62 -7 -9 2 126.55 4.50 -7 -9 2 125.09 4.29 8 9 -1 16.06 0.93 8 9 -1 14.18 1.07 -8 -9 1 15.92 0.93 -8 -9 1 16.17 1.08 -8 -9 1 15.04 0.90 9 9 0 73.46 2.48 -9 -9 0 74.06 2.88 -9 -9 0 73.92 2.80 -9 -9 0 75.58 2.96 10 9 1 14.90 1.12 10 9 1 12.68 1.15 10 9 1 15.02 1.26 10 9 1 13.17 0.76 -10 -9 -1 9.84 1.29 -10 -9 -1 14.32 1.04 -10 -9 -1 14.58 1.01 11 9 2 16.39 1.35 11 9 2 14.20 1.10 11 9 2 13.72 1.33 11 9 2 16.56 1.35 -11 -9 -2 15.89 1.14 -11 -9 -2 14.72 1.04 12 9 3 13.76 1.28 12 9 3 13.00 1.20 12 9 3 14.94 0.92 12 9 3 15.08 1.29 -12 -9 -3 14.02 0.94 -12 -9 -3 14.54 1.08 13 9 4 23.18 1.25 13 9 4 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1.28 7 13 -4 25.72 1.23 -6 -13 5 0.17 0.30 -6 -13 5 0.43 0.27 6 13 -5 0.42 0.30 6 13 -5 0.22 0.26 -5 -13 6 48.63 1.95 -4 -13 7 2.22 0.35 4 13 -7 2.68 0.32 -13 -12 -3 1.27 0.31 -13 -12 -3 1.13 0.36 13 12 3 1.48 0.47 13 12 3 0.48 0.29 13 12 3 1.18 0.27 -12 -12 -2 98.23 3.47 -12 -12 -2 97.21 3.44 12 12 2 87.45 3.41 12 12 2 99.79 3.74 12 12 2 96.15 3.52 -11 -12 -1 10.85 0.98 -11 -12 -1 10.77 1.01 -11 -12 -1 10.95 0.92 11 12 1 11.10 1.08 -10 -12 0 416.93 13.50 -10 -12 0 443.48 13.51 10 12 0 412.43 13.59 10 12 0 429.60 13.78 -9 -12 1 67.25 2.57 -9 -12 1 66.85 2.79 -9 -12 1 64.36 2.40 9 12 -1 66.46 2.35 9 12 -1 66.35 2.83 9 12 -1 68.40 2.54 -8 -12 2 139.50 4.83 -8 -12 2 149.24 5.16 8 12 -2 157.24 4.95 8 12 -2 135.34 5.16 8 12 -2 141.23 4.79 -7 -12 3 20.21 1.28 -7 -12 3 17.97 1.12 7 12 -3 19.51 1.15 7 12 -3 20.10 1.08 -6 -12 4 51.23 2.14 -6 -12 4 51.86 2.18 6 12 -4 49.72 2.07 6 12 -4 51.49 2.02 -5 -12 5 10.73 0.70 -5 -12 5 9.42 0.92 5 12 -5 10.00 0.77 -4 -12 6 33.48 1.62 -3 -12 7 17.22 0.95 3 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5.12 0.46 -13 -10 -5 14.66 0.70 13 10 5 15.43 0.88 13 10 5 12.25 0.78 -12 -10 -4 39.44 1.58 -12 -10 -4 40.09 1.71 12 10 4 44.71 2.29 12 10 4 39.31 1.92 12 10 4 37.22 2.16 -11 -10 -3 10.36 0.87 -11 -10 -3 11.18 1.02 11 10 3 10.88 1.17 11 10 3 11.08 1.25 11 10 3 10.95 0.87 11 10 3 12.13 1.20 -10 -10 -2 52.50 2.29 -10 -10 -2 51.68 2.64 10 10 2 56.55 2.56 10 10 2 57.45 2.49 10 10 2 53.50 2.57 -9 -10 -1 54.53 2.19 -9 -10 -1 53.98 2.22 -9 -10 -1 55.65 2.36 9 10 1 51.17 1.98 9 10 1 55.21 2.33 9 10 1 49.65 2.36 9 10 1 56.34 2.36 -8 -10 0 8.62 0.75 -8 -10 0 9.08 0.88 -8 -10 0 8.40 0.80 8 10 0 9.80 0.73 8 10 0 9.63 0.91 8 10 0 9.89 0.93 8 10 0 8.07 0.54 -7 -10 1 15.74 0.90 -7 -10 1 12.38 1.35 -7 -10 1 14.23 1.01 -7 -10 1 15.20 0.88 7 10 -1 15.30 1.06 7 10 -1 16.70 0.90 7 10 -1 15.71 0.82 -6 -10 2 27.18 2.14 -6 -10 2 31.39 1.52 -6 -10 2 31.40 1.33 6 10 -2 28.52 1.32 6 10 -2 32.31 1.30 -5 -10 3 9.65 0.82 -5 -10 3 9.94 0.84 5 10 -3 10.91 0.73 5 10 -3 9.74 0.69 -4 -10 4 40.51 1.69 -4 -10 4 39.10 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0.08 0.30 -11 15 0 0.26 0.54 12 -15 1 26.47 1.49 -12 15 -1 27.38 1.24 13 -15 2 1.63 0.51 -13 15 -2 2.20 0.30 -13 15 -2 1.95 0.43 6 -14 -6 37.53 1.51 6 -14 -6 38.49 1.54 -6 14 6 34.71 1.40 -6 14 6 39.13 1.97 7 -14 -5 23.51 1.22 7 -14 -5 23.13 1.31 -7 14 5 23.75 1.27 8 -14 -4 10.70 0.99 8 -14 -4 13.47 1.31 8 -14 -4 10.41 0.89 -8 14 4 10.79 1.05 9 -14 -3 100.81 3.50 9 -14 -3 107.99 4.11 9 -14 -3 103.58 3.77 -9 14 3 105.48 3.54 -9 14 3 107.50 3.98 10 -14 -2 25.49 1.35 10 -14 -2 26.63 1.73 -10 14 2 25.27 1.58 -10 14 2 25.82 1.25 11 -14 -1 66.16 2.48 11 -14 -1 69.66 2.97 -11 14 1 72.83 2.91 -11 14 1 70.94 2.44 12 -14 0 -0.01 0.53 -12 14 0 0.47 0.33 -12 14 0 -0.06 0.30 13 -14 1 11.64 0.91 13 -14 1 12.59 0.90 -13 14 -1 12.14 0.75 -13 14 -1 12.00 0.76 -14 14 -2 1.40 0.25 -14 14 -2 1.47 0.26 7 -13 -6 9.92 0.74 7 -13 -6 9.51 0.76 -7 13 6 10.79 1.09 -7 13 6 9.55 0.61 8 -13 -5 1.22 0.43 8 -13 -5 1.13 0.45 -8 13 5 1.26 0.48 -8 13 5 1.26 0.69 9 -13 -4 25.72 1.42 9 -13 -4 26.47 1.63 9 -13 -4 25.94 1.26 -9 13 4 27.40 1.53 10 -13 -3 39.15 1.54 10 -13 -3 42.74 2.17 10 -13 -3 41.92 1.88 -10 13 3 43.95 2.08 -10 13 3 41.11 1.63 11 -13 -2 9.98 0.87 11 -13 -2 10.41 1.19 -11 13 2 9.77 0.79 -11 13 2 8.57 1.07 12 -13 -1 4.88 0.78 -12 13 1 7.07 0.97 -12 13 1 6.42 0.71 -12 13 1 6.28 0.56 13 -13 0 20.77 1.36 -13 13 0 22.53 1.04 -13 13 0 22.24 1.12 14 -13 1 10.57 0.76 14 -13 1 9.61 0.72 -14 13 -1 10.63 0.69 -14 13 -1 9.74 0.65 -15 13 -2 21.74 0.83 -15 13 -2 19.33 0.88 8 -12 -6 13.04 0.84 8 -12 -6 15.07 0.88 -8 12 6 14.77 1.21 -8 12 6 13.75 0.70 -9 12 5 3.08 0.88 10 -12 -4 24.25 1.53 10 -12 -4 20.79 1.28 10 -12 -4 22.01 1.11 -10 12 4 21.88 1.39 11 -12 -3 34.04 1.59 11 -12 -3 34.46 1.89 -11 12 3 31.08 1.74 -11 12 3 32.52 1.36 12 -12 -2 97.12 3.80 12 -12 -2 93.41 3.37 -12 12 2 95.04 3.63 -12 12 2 99.16 3.35 13 -12 -1 0.94 0.55 -13 12 1 0.53 0.47 -13 12 1 0.63 0.35 -13 12 1 0.68 0.30 14 -12 0 8.23 0.93 -14 12 0 8.28 0.62 -14 12 0 8.48 0.68 15 -12 1 3.81 0.56 -15 12 -1 5.10 0.47 -15 12 -1 4.94 0.47 9 -11 -6 0.84 0.33 9 -11 -6 1.04 0.35 -9 11 6 0.92 0.32 -9 11 6 0.74 0.50 10 -11 -5 28.40 1.38 10 -11 -5 27.65 1.27 -10 11 5 25.97 1.36 11 -11 -4 78.75 3.16 11 -11 -4 79.67 2.91 11 -11 -4 74.97 2.89 -11 11 4 78.95 3.03 12 -11 -3 2.88 0.50 12 -11 -3 3.23 0.73 -12 11 3 3.55 0.51 13 -11 -2 10.38 0.92 13 -11 -2 8.98 1.11 -13 11 2 11.07 0.78 14 -11 -1 9.18 1.12 -14 11 1 10.17 0.93 -14 11 1 9.53 0.54 -14 11 1 10.94 0.75 15 -11 0 1.57 0.50 -15 11 0 0.92 0.26 -15 11 0 0.79 0.29 -16 11 -1 43.52 1.51 -16 11 -1 45.60 1.58 10 -10 -6 7.21 0.60 10 -10 -6 6.45 0.62 -10 10 6 6.02 0.43 -10 10 6 7.19 0.88 11 -10 -5 70.40 2.60 11 -10 -5 69.89 2.44 12 -10 -4 48.99 2.47 12 -10 -4 38.61 2.01 -12 10 4 46.11 2.32 13 -10 -3 4.37 0.81 13 -10 -3 3.64 0.61 -13 10 3 3.88 0.49 14 -10 -2 3.67 0.91 14 -10 -2 3.17 0.41 -14 10 2 3.53 0.51 15 -10 -1 26.33 1.47 -15 10 1 27.06 1.34 -15 10 1 26.91 1.18 16 -10 0 0.81 0.36 -16 10 0 0.53 0.16 -16 10 0 0.61 0.26 11 -9 -6 1.43 0.26 11 -9 -6 2.23 0.44 -11 9 6 1.78 0.49 -11 9 6 1.28 0.23 12 -9 -5 3.29 0.46 12 -9 -5 2.35 0.49 -12 9 5 2.81 0.47 13 -9 -4 23.70 1.16 13 -9 -4 20.52 1.34 14 -9 -3 3.30 0.70 14 -9 -3 2.71 0.42 -14 9 3 2.92 0.42 15 -9 -2 1.30 0.26 15 -9 -2 1.89 0.58 -15 9 2 1.60 0.33 16 -9 -1 30.88 1.47 -16 9 1 26.72 1.47 -16 9 1 31.85 1.21 17 -9 0 6.42 0.48 -17 9 0 5.30 0.42 13 -8 -5 0.71 0.31 -13 8 5 0.46 0.31 14 -8 -4 23.88 1.32 14 -8 -4 26.16 1.15 15 -8 -3 30.03 1.23 15 -8 -3 28.14 1.52 -15 8 3 34.26 1.22 16 -8 -2 5.85 0.79 -16 8 2 4.68 0.43 -16 8 2 5.16 0.60 17 -8 -1 13.00 0.80 -17 8 1 12.55 0.60 14 -7 -5 2.10 0.32 -14 7 5 1.66 0.30 -14 7 5 2.11 0.40 15 -7 -4 6.46 0.51 15 -7 -4 5.09 0.70 16 -7 -3 5.50 0.67 -17 7 2 3.31 0.32 2 -24 -2 19.54 0.95 -2 24 2 21.22 0.98 3 -24 -1 7.02 0.71 -3 24 1 7.40 0.59 -3 24 1 7.49 0.44 4 -24 0 -0.10 0.28 -4 24 0 0.22 0.22 -5 24 -1 7.95 0.46 2 -23 -3 0.85 0.25 -2 23 3 1.14 0.34 3 -23 -2 2.65 0.46 3 -23 -2 2.70 0.54 -3 23 2 2.68 0.44 4 -23 -1 13.58 0.93 -4 23 1 13.03 0.92 -4 23 1 13.03 0.66 5 -23 0 5.05 0.50 5 -23 0 4.89 0.65 -5 23 0 7.13 0.65 -5 23 0 6.07 0.49 6 -23 1 15.78 0.92 6 -23 1 14.97 0.78 -6 23 -1 15.36 0.72 2 -22 -4 6.34 0.48 -2 22 4 6.28 0.49 3 -22 -3 19.70 1.07 3 -22 -3 20.89 0.97 -3 22 3 22.49 1.11 4 -22 -2 0.85 0.41 4 -22 -2 1.03 0.28 -4 22 2 1.19 0.23 -4 22 2 1.05 0.42 5 -22 -1 1.76 0.38 5 -22 -1 1.06 0.25 5 -22 -1 0.86 0.41 -5 22 1 1.24 0.30 -5 22 1 1.48 0.42 6 -22 0 7.48 0.78 6 -22 0 7.41 0.70 -6 22 0 5.09 0.66 -6 22 0 7.68 0.59 7 -22 1 8.56 0.65 7 -22 1 8.53 0.69 -7 22 -1 9.40 0.59 3 -21 -4 4.08 0.48 -3 21 4 4.05 0.51 4 -21 -3 13.78 0.83 4 -21 -3 12.46 1.05 -4 21 3 14.14 0.96 5 -21 -2 57.52 2.14 5 -21 -2 61.22 2.45 -5 21 2 57.82 2.04 6 -21 -1 1.31 0.44 6 -21 -1 1.19 0.25 -6 21 1 1.83 0.34 -6 21 1 2.02 0.53 7 -21 0 0.06 0.35 7 -21 0 0.60 0.44 -7 21 0 0.59 0.38 -7 21 0 0.19 0.27 -7 21 0 -0.17 0.16 8 -21 1 9.05 0.77 8 -21 1 8.00 0.67 -8 21 -1 8.75 0.50 -8 21 -1 8.94 0.61 9 -21 2 9.69 0.64 -9 21 -2 9.57 0.50 -9 21 -2 9.36 0.47 3 -20 -5 3.04 0.40 -3 20 5 3.73 0.38 4 -20 -4 3.98 0.56 -4 20 4 4.30 0.60 5 -20 -3 1.30 0.37 5 -20 -3 1.35 0.48 -5 20 3 0.82 0.39 6 -20 -2 27.08 1.56 6 -20 -2 26.33 1.26 -6 20 2 27.12 1.17 -6 20 2 28.72 1.50 7 -20 -1 1.23 0.26 7 -20 -1 1.60 0.67 -7 20 1 1.47 0.48 -7 20 1 1.49 0.36 8 -20 0 22.52 1.30 -8 20 0 22.58 1.28 -8 20 0 23.47 1.09 -8 20 0 22.29 0.91 9 -20 1 7.70 0.67 9 -20 1 7.65 0.78 -9 20 -1 7.63 0.51 -9 20 -1 7.60 0.60 10 -20 2 0.79 0.29 -10 20 -2 0.79 0.19 -10 20 -2 1.00 0.21 4 -19 -5 7.20 0.47 4 -19 -5 7.09 0.56 -4 19 5 8.47 0.74 5 -19 -4 20.98 1.07 5 -19 -4 18.98 0.85 -5 19 4 19.60 1.16 -5 19 4 22.75 1.17 6 -19 -3 8.15 0.92 6 -19 -3 8.76 0.91 -6 19 3 6.68 0.91 -6 19 3 6.55 0.44 7 -19 -2 7.03 0.97 7 -19 -2 5.81 0.76 -7 19 2 5.94 0.61 -7 19 2 7.85 1.03 8 -19 -1 4.00 0.66 8 -19 -1 6.69 0.51 -8 19 1 5.74 0.62 -8 19 1 4.91 0.67 9 -19 0 5.44 0.86 -9 19 0 5.26 0.48 -9 19 0 6.44 0.74 10 -19 1 32.01 1.53 10 -19 1 30.44 1.35 -10 19 -1 31.37 1.27 -10 19 -1 31.35 1.21 11 -19 2 12.76 0.75 -11 19 -2 13.68 0.60 -11 19 -2 13.18 0.61 5 -18 -5 0.49 0.27 5 -18 -5 0.48 0.31 -5 18 5 0.24 0.37 -5 18 5 0.48 0.26 6 -18 -4 67.67 2.36 6 -18 -4 72.82 2.60 6 -18 -4 67.52 2.71 -6 18 4 67.66 2.79 -6 18 4 74.62 2.69 7 -18 -3 21.54 1.42 7 -18 -3 22.27 1.20 -7 18 3 22.22 1.39 -7 18 3 23.50 1.38 -7 18 3 22.40 0.95 8 -18 -2 14.00 0.91 8 -18 -2 14.99 1.27 -8 18 2 12.51 1.09 -8 18 2 14.88 1.18 -8 18 2 14.94 0.84 9 -18 -1 2.11 0.30 9 -18 -1 4.21 0.74 -9 18 1 3.65 0.64 -9 18 1 2.54 0.30 10 -18 0 1.12 0.57 -10 18 0 1.38 0.43 -10 18 0 0.87 0.27 11 -18 1 1.84 0.46 11 -18 1 1.45 0.35 -11 18 -1 1.63 0.32 -11 18 -1 1.46 0.29 12 -18 2 12.54 0.70 -12 18 -2 13.27 0.58 -12 18 -2 11.93 0.58 6 -17 -5 57.20 2.09 6 -17 -5 55.47 1.96 -6 17 5 57.06 2.07 -6 17 5 53.29 2.32 7 -17 -4 3.86 0.51 7 -17 -4 4.48 0.63 7 -17 -4 4.30 0.82 -7 17 4 2.25 0.51 -7 17 4 3.49 0.66 8 -17 -3 11.70 0.90 8 -17 -3 10.21 1.08 -8 17 3 10.10 0.64 -8 17 3 11.42 1.08 -8 17 3 11.19 1.13 9 -17 -2 1.00 0.35 9 -17 -2 0.84 0.56 -9 17 2 1.01 0.33 -9 17 2 1.17 0.54 10 -17 -1 3.07 0.62 -10 17 1 5.67 0.75 -10 17 1 4.18 0.37 -10 17 1 4.53 0.60 11 -17 0 18.55 1.22 -11 17 0 17.65 0.95 -11 17 0 17.91 0.84 12 -17 1 6.32 0.58 12 -17 1 6.95 0.69 -12 17 -1 7.21 0.51 -12 17 -1 6.63 0.54 6 -16 -6 25.08 0.98 6 -16 -6 26.04 1.04 -6 16 6 23.75 1.24 7 -16 -5 8.75 0.63 7 -16 -5 8.32 0.72 -7 16 5 7.43 0.91 -7 16 5 7.71 0.71 8 -16 -4 11.41 1.06 8 -16 -4 14.50 0.73 8 -16 -4 10.02 1.23 -8 16 4 10.51 1.13 -8 16 4 14.66 1.27 9 -16 -3 0.55 0.53 9 -16 -3 0.34 0.42 -9 16 3 0.34 0.27 -9 16 3 0.64 0.50 10 -16 -2 33.76 1.84 10 -16 -2 32.90 1.48 -10 16 2 32.58 1.72 -10 16 2 34.66 1.42 11 -16 -1 5.22 0.79 -11 16 1 5.40 0.63 -11 16 1 4.81 0.39 -11 16 1 4.83 0.69 12 -16 0 4.13 0.65 -12 16 0 3.99 0.55 -12 16 0 4.89 0.47 13 -16 1 0.34 0.29 13 -16 1 0.07 0.38 -13 16 -1 0.11 0.22 -13 16 -1 0.64 0.25 7 -15 -6 9.78 0.62 7 -15 -6 10.30 0.59 -7 15 6 9.53 0.83 8 -15 -5 17.95 1.02 8 -15 -5 17.82 0.88 -8 15 5 18.97 1.34 -8 15 5 19.11 1.01 9 -15 -4 9.83 1.03 9 -15 -4 9.39 1.21 9 -15 -4 8.89 0.59 -9 15 4 11.80 1.19 10 -15 -3 0.23 0.36 10 -15 -3 -0.07 0.48 -10 15 3 0.45 0.26 -10 15 3 0.53 0.51 11 -15 -2 23.11 1.26 11 -15 -2 22.60 1.49 -11 15 2 23.07 1.09 -11 15 2 21.82 1.68 12 -15 -1 30.46 2.27 -12 15 1 29.04 1.36 -12 15 1 24.22 0.97 -12 15 1 29.06 1.46 13 -15 0 5.89 0.78 -13 15 0 6.64 0.48 -13 15 0 6.63 0.58 14 -15 1 1.47 0.24 -14 15 -1 2.12 0.40 8 -14 -6 4.28 0.43 8 -14 -6 4.19 0.48 -8 14 6 4.72 0.71 9 -14 -5 10.39 0.65 9 -14 -5 9.93 0.80 -9 14 5 10.13 1.05 -9 14 5 10.18 0.78 10 -14 -4 2.54 0.58 10 -14 -4 3.67 0.52 10 -14 -4 2.76 0.38 -10 14 4 3.12 0.56 11 -14 -3 16.54 1.21 11 -14 -3 19.46 1.36 -11 14 3 19.50 0.87 12 -14 -2 31.44 1.92 12 -14 -2 23.72 1.13 -12 14 2 24.09 1.41 13 -14 -1 10.88 1.04 -13 14 1 11.61 0.94 -13 14 1 11.50 0.73 14 -14 0 30.30 1.39 -14 14 0 29.18 1.10 -14 14 0 30.75 1.22 -15 14 -1 25.11 0.97 9 -13 -6 8.50 0.59 9 -13 -6 8.51 0.48 -9 13 6 7.81 0.77 10 -13 -5 1.53 0.35 10 -13 -5 1.26 0.37 -10 13 5 1.48 0.59 -10 13 5 1.46 0.41 11 -13 -4 1.07 0.59 11 -13 -4 0.31 0.40 -11 13 4 0.57 0.44 12 -13 -3 9.70 1.03 12 -13 -3 9.94 0.81 -12 13 3 10.74 0.99 -12 13 3 10.52 0.61 13 -13 -2 4.84 0.73 13 -13 -2 6.07 0.53 -13 13 2 5.93 0.55 -13 13 2 4.90 0.66 14 -13 -1 10.12 0.96 -14 13 1 9.51 0.64 -14 13 1 9.66 0.80 15 -13 0 -0.10 0.27 15 -13 0 0.03 0.30 -15 13 0 0.57 0.23 11 -12 -5 26.40 1.17 -11 12 5 25.92 1.17 -11 12 5 24.43 1.47 12 -12 -4 98.06 3.35 12 -12 -4 94.24 3.52 -12 12 4 100.03 3.48 13 -12 -3 0.91 0.44 13 -12 -3 1.08 0.35 -13 12 3 1.14 0.25 -13 12 3 1.08 0.43 14 -12 -2 0.29 0.48 -14 12 2 0.28 0.41 -14 12 2 0.67 0.26 15 -12 -1 3.50 0.51 -15 12 1 4.63 0.47 16 -12 0 30.17 1.15 -16 12 0 30.16 1.12 12 -11 -5 5.39 0.54 -12 11 5 4.26 0.51 -12 11 5 4.94 0.79 13 -11 -4 20.88 1.15 13 -11 -4 19.85 0.98 -13 11 4 18.66 1.05 14 -11 -3 9.46 0.87 14 -11 -3 8.33 0.59 -14 11 3 8.73 0.50 -14 11 3 9.12 0.77 15 -11 -2 45.46 1.89 -15 11 2 44.55 1.57 -15 11 2 43.88 1.78 -16 11 1 34.88 1.36 13 -10 -5 14.28 0.73 -13 10 5 14.84 0.97 -13 10 5 14.95 0.73 14 -10 -4 7.17 0.73 14 -10 -4 9.46 0.66 -14 10 4 7.65 0.65 15 -10 -3 19.32 1.06 -15 10 3 19.37 1.01 16 -10 -2 10.04 0.75 -16 10 2 9.37 0.47 -16 10 2 10.22 0.65 -5 24 1 6.79 0.48 5 -23 -2 3.80 0.53 -5 23 2 4.49 0.51 6 -23 -1 15.66 0.87 -6 23 1 12.55 0.79 -6 23 1 14.24 0.66 7 -23 0 56.81 2.02 7 -23 0 58.13 2.06 -7 23 0 57.99 1.94 5 -22 -3 2.58 0.51 5 -22 -3 2.20 0.28 -5 22 3 1.72 0.32 6 -22 -2 50.95 1.92 6 -22 -2 56.28 2.08 6 -22 -2 50.75 1.75 -6 22 2 50.04 1.72 -6 22 2 54.98 2.04 7 -22 -1 8.91 0.79 7 -22 -1 9.10 0.76 -7 22 1 8.87 0.54 -7 22 1 9.13 0.67 8 -22 0 5.51 0.57 8 -22 0 6.31 0.63 -8 22 0 6.57 0.47 5 -21 -4 0.59 0.23 -5 21 4 0.70 0.25 6 -21 -3 3.71 0.45 6 -21 -3 2.53 0.44 -6 21 3 3.31 0.48 7 -21 -2 0.04 0.23 7 -21 -2 -0.01 0.36 -7 21 2 0.11 0.20 -7 21 2 0.05 0.33 8 -21 -1 8.64 0.81 -8 21 1 8.99 0.56 -8 21 1 6.66 0.68 9 -21 0 2.81 0.43 9 -21 0 4.28 0.56 -9 21 0 4.50 0.43 6 -20 -4 19.63 0.92 -6 20 4 19.85 0.96 7 -20 -3 19.05 0.92 7 -20 -3 18.23 1.30 -7 20 3 19.82 1.11 8 -20 -2 10.34 0.73 8 -20 -2 11.14 0.94 -8 20 2 11.18 0.88 -8 20 2 10.09 0.59 9 -20 -1 7.95 0.82 -9 20 1 7.81 0.74 -9 20 1 6.98 0.56 10 -20 0 0.12 0.31 10 -20 0 0.23 0.32 -10 20 0 0.30 0.24 7 -19 -4 14.32 0.80 -7 19 4 15.36 0.88 8 -19 -3 2.17 0.45 8 -19 -3 2.12 0.37 -8 19 3 2.21 0.51 9 -19 -2 1.40 0.30 9 -19 -2 1.67 0.55 -9 19 2 1.35 0.45 -9 19 2 1.06 0.27 10 -19 -1 31.16 1.50 -10 19 1 29.25 1.20 -10 19 1 29.34 1.37 11 -19 0 -0.06 0.28 11 -19 0 0.01 0.30 -11 19 0 -0.03 0.20 7 -18 -5 10.60 0.61 -7 18 5 10.79 0.57 8 -18 -4 7.53 0.84 8 -18 -4 9.22 0.66 -8 18 4 8.92 0.72 -8 18 4 8.44 0.75 9 -18 -3 0.62 0.41 9 -18 -3 0.91 0.31 -9 18 3 1.13 0.39 -9 18 3 0.93 0.39 10 -18 -2 11.19 0.98 10 -18 -2 10.87 0.79 -10 18 2 7.50 0.81 -10 18 2 9.78 0.60 -10 18 2 6.78 0.75 11 -18 -1 1.15 0.48 -11 18 1 1.54 0.30 -11 18 1 1.67 0.41 12 -18 0 56.59 2.07 12 -18 0 56.34 2.18 -12 18 0 56.09 1.94 8 -17 -5 19.58 0.92 -8 17 5 16.08 0.95 -8 17 5 16.44 0.79 9 -17 -4 27.63 1.51 9 -17 -4 31.47 1.28 -9 17 4 31.10 1.37 -9 17 4 30.11 1.66 10 -17 -3 7.33 0.61 10 -17 -3 8.17 0.87 -10 17 3 6.08 0.41 -10 17 3 7.21 0.77 -10 17 3 6.41 0.80 11 -17 -2 34.71 1.36 11 -17 -2 41.81 1.83 -11 17 2 39.87 1.69 -11 17 2 40.03 1.45 12 -17 -1 7.94 0.81 -12 17 1 6.92 0.53 -12 17 1 5.32 0.68 13 -17 0 20.88 1.08 -13 17 0 19.56 0.88 9 -16 -5 4.29 0.52 -9 16 5 4.77 0.46 -9 16 5 3.75 0.61 10 -16 -4 0.73 0.44 10 -16 -4 1.92 0.37 -10 16 4 2.14 0.51 -10 16 4 3.65 0.51 11 -16 -3 7.96 0.86 11 -16 -3 8.83 0.60 -11 16 3 6.48 0.41 -11 16 3 9.34 0.83 12 -16 -2 9.37 0.90 -12 16 2 8.13 0.53 -12 16 2 7.75 0.77 13 -16 -1 0.25 0.36 -13 16 1 1.45 0.61 -13 16 1 0.32 0.24 14 -16 0 60.72 2.13 14 -16 0 60.10 2.07 -14 16 0 59.83 2.01 10 -15 -5 14.92 0.76 -10 15 5 15.94 0.76 -10 15 5 15.16 0.97 11 -15 -4 5.65 0.56 11 -15 -4 6.77 0.89 -11 15 4 5.49 0.79 -11 15 4 6.33 0.67 12 -15 -3 6.92 0.79 12 -15 -3 5.97 0.50 -12 15 3 6.20 0.71 -12 15 3 4.38 0.34 13 -15 -2 2.44 0.51 -13 15 2 1.91 0.43 -13 15 2 2.89 0.37 14 -15 -1 1.58 0.38 -14 15 1 2.93 0.36 12 -14 -4 16.57 1.04 12 -14 -4 16.84 1.04 -12 14 4 16.52 0.91 13 -14 -3 6.32 0.76 13 -14 -3 6.10 0.45 -13 14 3 7.17 0.68 14 -14 -2 1.73 0.41 -14 14 2 1.41 0.25 -14 14 2 2.16 0.37 15 -14 -1 21.95 1.09 -15 14 1 23.67 0.89 13 -13 -4 58.79 2.00 -13 13 4 59.41 2.12 14 -13 -3 16.21 0.93 -14 13 3 15.25 0.84 15 -13 -2 21.32 0.98 -15 13 2 16.58 0.69 9 -21 -2 9.83 0.69 -9 21 2 9.58 0.61 9 -20 -3 1.24 0.38 -9 20 3 2.45 0.36 10 -20 -2 2.02 0.39 -10 20 2 0.47 0.27 10 -19 -3 20.35 1.01 -10 19 3 20.35 0.96 11 -19 -2 13.24 0.77 -11 19 2 10.55 0.74 -11 19 2 10.24 0.54 11 -18 -3 -0.24 0.26 -11 18 3 0.42 0.27 12 -18 -2 12.41 0.77 -12 18 2 12.62 0.69 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 56921 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1, -y+1, z+1/2' '-x+1, y+1, 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 _atom_site_refinement_flags_adp N1 N 0.38476(9) 0.51326(7) 0.4096(2) 0.0163(3) Uani 1 1 d D . H1X H 0.4248(12) 0.4773(9) 0.390(3) 0.020 Uiso 1 1 d D U N2 N 0.23745(9) 0.55023(6) 0.4869(2) 0.0140(3) Uani 1 1 d . . N3 N 0.15235(9) 0.52783(6) 0.5341(2) 0.0162(3) Uani 1 1 d . . O1 O 0.49538(8) 0.58658(6) 0.3362(2) 0.0205(3) Uani 1 1 d . . C1 C 0.19786(11) 0.72277(8) 0.3690(3) 0.0178(4) Uani 1 1 d . . H1 H 0.2408 0.7244 0.2686 0.021 Uiso 1 1 calc R U C2 C 0.13804(11) 0.77486(8) 0.3961(3) 0.0207(4) Uani 1 1 d . . H2 H 0.1397 0.8116 0.3129 0.025 Uiso 1 1 calc R U C3 C 0.07612(11) 0.77328(8) 0.5441(3) 0.0219(4) Uani 1 1 d . . H3 H 0.0362 0.8092 0.5643 0.026 Uiso 1 1 calc R U C4 C 0.07281(12) 0.71885(9) 0.6625(3) 0.0215(4) Uani 1 1 d . . H4 H 0.0299 0.7175 0.7631 0.026 Uiso 1 1 calc R U C5 C 0.13136(12) 0.66634(8) 0.6358(3) 0.0180(4) Uani 1 1 d . . H5 H 0.1282 0.6292 0.7172 0.022 Uiso 1 1 calc R U C6 C 0.19484(11) 0.66822(8) 0.4892(3) 0.0158(4) Uani 1 1 d . . C7 C 0.26260(11) 0.61534(8) 0.4627(2) 0.0150(3) Uani 1 1 d . . C8 C 0.34982(11) 0.62747(8) 0.4157(3) 0.0164(3) Uani 1 1 d . . H8 H 0.3687 0.6718 0.4028 0.020 Uiso 1 1 calc R U C9 C 0.41562(11) 0.57598(8) 0.3841(3) 0.0164(3) Uani 1 1 d . . C10 C 0.29714(10) 0.49924(8) 0.4609(3) 0.0148(3) Uani 1 1 d . . C11 C 0.25071(11) 0.44218(8) 0.4937(2) 0.0163(3) Uani 1 1 d . . H11 H 0.2732 0.3986 0.4877 0.020 Uiso 1 1 calc R U C12 C 0.16163(11) 0.46280(8) 0.5384(3) 0.0156(3) Uani 1 1 d . . C13 C 0.08257(11) 0.42071(8) 0.5909(3) 0.0200(4) Uani 1 1 d . . H13A H 0.0706 0.4248 0.7274 0.030 Uiso 1 1 calc R U H13B H 0.0962 0.3748 0.5604 0.030 Uiso 1 1 calc R U H13C H 0.0291 0.4349 0.5193 0.030 Uiso 1 1 calc R U 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 N1 0.0134(6) 0.0154(6) 0.0202(7) -0.0002(6) 0.0006(5) 0.0022(5) N2 0.0130(6) 0.0137(6) 0.0153(7) 0.0003(5) 0.0008(5) 0.0001(5) N3 0.0134(6) 0.0180(7) 0.0170(7) 0.0007(6) 0.0019(6) -0.0015(5) O1 0.0135(5) 0.0208(6) 0.0273(7) 0.0029(5) 0.0022(5) 0.0006(5) C1 0.0166(8) 0.0169(8) 0.0200(9) -0.0002(7) -0.0001(7) -0.0014(6) C2 0.0219(8) 0.0147(7) 0.0255(10) -0.0003(7) -0.0083(8) -0.0005(6) C3 0.0177(8) 0.0180(8) 0.0300(10) -0.0079(7) -0.0074(7) 0.0051(6) C4 0.0171(8) 0.0229(9) 0.0246(10) -0.0064(7) 0.0013(7) 0.0004(7) C5 0.0186(8) 0.0160(9) 0.0194(9) -0.0013(7) 0.0007(7) -0.0006(6) C6 0.0131(7) 0.0148(7) 0.0196(9) -0.0029(7) -0.0025(6) -0.0005(6) C7 0.0180(8) 0.0142(7) 0.0129(8) 0.0000(6) -0.0009(6) 0.0008(6) C8 0.0165(8) 0.0138(7) 0.0190(9) 0.0009(7) 0.0001(7) -0.0004(6) C9 0.0156(8) 0.0191(8) 0.0145(8) 0.0017(6) -0.0008(6) 0.0004(6) C10 0.0140(7) 0.0174(7) 0.0132(7) -0.0007(6) -0.0009(6) 0.0030(6) C11 0.0174(8) 0.0144(7) 0.0172(9) -0.0012(6) -0.0016(6) 0.0007(6) C12 0.0175(8) 0.0164(7) 0.0128(8) -0.0001(6) -0.0018(7) -0.0009(6) C13 0.0183(8) 0.0200(8) 0.0217(10) 0.0004(7) 0.0003(7) -0.0028(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 C9 N1 C10 122.84(14) C9 N1 H1X 119.6(12) C10 N1 H1X 117.6(12) C10 N2 N3 111.50(13) C10 N2 C7 122.31(13) N3 N2 C7 126.18(13) C12 N3 N2 103.96(12) C2 C1 C6 120.17(16) C2 C1 H1 119.9 C6 C1 H1 119.9 C3 C2 C1 120.19(16) C3 C2 H2 119.9 C1 C2 H2 119.9 C2 C3 C4 119.53(15) C2 C3 H3 120.2 C4 C3 H3 120.2 C3 C4 C5 120.83(17) C3 C4 H4 119.6 C5 C4 H4 119.6 C4 C5 C6 119.85(16) C4 C5 H5 120.1 C6 C5 H5 120.1 C5 C6 C1 119.41(15) C5 C6 C7 121.81(15) C1 C6 C7 118.71(15) C8 C7 N2 117.35(14) C8 C7 C6 122.73(14) N2 C7 C6 119.92(14) C7 C8 C9 122.99(14) C7 C8 H8 118.5 C9 C8 H8 118.5 O1 C9 N1 120.85(14) O1 C9 C8 123.47(15) N1 C9 C8 115.68(14) C11 C10 N1 133.84(15) C11 C10 N2 107.36(14) N1 C10 N2 118.81(15) C10 C11 C12 104.51(14) C10 C11 H11 127.7 C12 C11 H11 127.7 N3 C12 C11 112.67(14) N3 C12 C13 119.73(14) C11 C12 C13 127.59(14) C12 C13 H13A 109.5 C12 C13 H13B 109.5 H13A C13 H13B 109.5 C12 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C9 1.369(2) N1 C10 1.373(2) N1 H1X 0.951(17) N2 C10 1.375(2) N2 N3 1.3776(19) N2 C7 1.388(2) N3 C12 1.332(2) O1 C9 1.244(2) C1 C2 1.394(2) C1 C6 1.397(2) C1 H1 0.9500 C2 C3 1.386(3) C2 H2 0.9500 C3 C4 1.388(3) C3 H3 0.9500 C4 C5 1.388(2) C4 H4 0.9500 C5 C6 1.394(2) C5 H5 0.9500 C6 C7 1.482(2) C7 C8 1.353(2) C8 C9 1.447(2) C8 H8 0.9500 C10 C11 1.369(2) C11 C12 1.416(2) C11 H11 0.9500 C12 C13 1.495(2) C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800