#------------------------------------------------------------------------------ #$Date: 2025-03-04 21:28:44 +0200 (Tue, 04 Mar 2025) $ #$Revision: 298154 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573834.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_1573834 loop_ _publ_author_name 'Zhu, Ming' 'Huang, Pei-Zhi' 'Li, Lin-Mei' 'Yang, Yi-Xuan' 'Pan, Lei' 'Wang, Zhi-Jie' 'Ni, Hao-Fei' 'Zhang, Feng-Wen' 'Teri, Gele' 'Zhang, Zhi-Xu' 'Liu, Zunqi' 'Fu, Da-Wei' 'Zhang, Yi' _publ_section_title ; Thermal-responsive luminescence/dielectric responses with reversibly shifted light emissions. ; _journal_issue 9 _journal_name_full 'Chemical science' _journal_page_first 4101 _journal_page_last 4108 _journal_paper_doi 10.1039/d4sc06631f _journal_volume 16 _journal_year 2025 _chemical_formula_moiety 'F6 P, 2(C6 H9 N2)' _chemical_formula_sum 'C12 H18 F6 N4 P' _chemical_formula_weight 363.27 _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 iterative _audit_creation_date 2024-09-24 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-09-24 deposited with the CCDC. 2025-01-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.439(11) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.8459(16) _cell_length_b 9.828(2) _cell_length_c 10.5087(15) _cell_measurement_reflns_used 2496 _cell_measurement_temperature 303.00 _cell_measurement_theta_max 70.998 _cell_measurement_theta_min 5.651 _cell_volume 809.6(3) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_temperature 303.00 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_unetI/netI 0.0463 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 9067 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.309 _diffrn_reflns_theta_min 5.644 _diffrn_source_current 1.1 _diffrn_source_power 0.05500000000000001 _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 2.137 _exptl_absorpt_correction_T_max 0.7536 _exptl_absorpt_correction_T_min 0.5850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1163 before and 0.0669 after correction. The Ratio of minimum to maximum transmission is 0.7763. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.490 _exptl_crystal_description block _exptl_crystal_F_000 374 _refine_diff_density_max 0.740 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.084 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 107 _refine_ls_number_reflns 1592 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.125 _refine_ls_R_factor_all 0.1085 _refine_ls_R_factor_gt 0.0805 _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^)+(0.1397P)^2^+0.4675P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2289 _refine_ls_wR_factor_ref 0.2562 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1088 _reflns_number_total 1592 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc06631f2.cif _cod_data_source_block cu_zm_pp_1_0m_a _cod_depositor_comments 'Adding full bibliography for 1573833--1573838.cif.' _cod_database_code 1573834 _shelx_shelxl_version_number 2018/3 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B) 2.b Aromatic/amide H refined with riding coordinates: C6(H6), C3(H3), C4(H4), C5(H5) 2.c Idealised Me refined as rotating group: N2(H2A,H2B,H2C) ; _shelx_res_file ; TITL cu_ZM_PP_1_0m_a.res in P2(1)/c cu_zm_pp_1_0m_a.res created by SHELXL-2018/3 at 18:11:02 on 24-Sep-2024 REM Old TITL Integration of ZM_PP_1 REM SHELXT solution in P2(1)/c: R1 0.237, Rweak 0.020, Alpha 0.045 REM 0.451 for 102 systematic absences, Orientation as input REM Formula found by SHELXT: C12 F8 N2 P CELL 1.54184 7.8459 9.8277 10.5087 90 92.439 90 ZERR 2 0.0016 0.0021 0.0015 0 0.011 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H F N P UNIT 24 36 12 8 2 EQIV $1 -X,1-Y,1-Z EQIV $2 -X,-0.5+Y,0.5-Z EQIV $3 -1+X,+Y,+Z EQIV $4 +X,0.5-Y,-0.5+Z EQIV $5 1-X,1-Y,1-Z L.S. 20 PLAN 1 TEMP 15.85 CONF HTAB N2 F2_$2 HTAB N2 F1_$2 HTAB N2 F2_$1 HTAB N2 F1 HTAB N2 N1_$3 HTAB C1 F1_$2 HTAB C1 F2_$1 HTAB C3 F3_$4 HTAB C5 F2_$5 HTAB C5 F3_$5 LIST 4 MORE -1 BOND $H htab fmap 2 acta REM REM REM WGHT 0.139700 0.467500 FVAR 1.22572 P1 5 0.000000 0.500000 0.500000 10.50000 0.04674 0.05461 = 0.04483 -0.00146 0.00132 -0.00106 F2 3 0.011342 0.662985 0.451432 11.00000 0.12051 0.05497 = 0.05019 0.00305 0.00464 -0.00656 N2 4 0.043904 0.177427 0.315520 11.00000 0.03184 0.06425 = 0.05198 -0.00159 0.00468 0.00026 AFIX 137 H2A 2 0.061043 0.158569 0.234222 11.00000 -1.20000 H2B 2 0.070951 0.263919 0.331314 11.00000 -1.20000 H2C 2 -0.065327 0.163752 0.331291 11.00000 -1.20000 AFIX 0 F1 3 0.004795 0.449929 0.349002 11.00000 0.27959 0.05649 = 0.04525 -0.00253 0.00946 -0.00396 N1 4 0.689279 0.140834 0.350962 11.00000 0.03267 0.08659 = 0.07828 0.00842 0.00542 -0.00007 C2 1 0.340540 0.109431 0.379559 11.00000 0.03095 0.06154 = 0.05019 0.00398 -0.00088 0.00172 F3 3 0.205083 0.492756 0.509763 11.00000 0.05013 0.14895 = 0.23663 0.04719 0.00120 0.00496 C1 1 0.152126 0.087654 0.398265 11.00000 0.03417 0.06590 = 0.05976 0.00649 0.00487 -0.00072 AFIX 23 H1A 2 0.123428 -0.006497 0.379768 11.00000 -1.20000 H1B 2 0.128300 0.105009 0.486619 11.00000 -1.20000 AFIX 0 C6 1 0.433419 0.198865 0.453991 11.00000 0.04371 0.07232 = 0.07858 -0.01190 0.01044 -0.00025 AFIX 43 H6 2 0.380788 0.251419 0.514569 11.00000 -1.20000 AFIX 0 C3 1 0.423021 0.040515 0.287476 11.00000 0.03913 0.09980 = 0.07246 -0.02607 0.00190 -0.00500 AFIX 43 H3 2 0.362942 -0.017767 0.232155 11.00000 -1.20000 AFIX 0 C4 1 0.597585 0.058423 0.277358 11.00000 0.04217 0.10588 = 0.07720 -0.01623 0.01418 0.00451 AFIX 43 H4 2 0.652307 0.009529 0.215262 11.00000 -1.20000 AFIX 0 C5 1 0.607904 0.210119 0.437786 11.00000 0.04146 0.08586 = 0.08897 -0.01059 -0.00125 -0.01289 AFIX 43 H5 2 0.670571 0.269299 0.490607 11.00000 -1.20000 AFIX 0 HKLF 4 REM cu_ZM_PP_1_0m_a.res in P2(1)/c REM wR2 = 0.2562, GooF = S = 1.125, Restrained GooF = 1.125 for all data REM R1 = 0.0805 for 1088 Fo > 4sig(Fo) and 0.1085 for all 1592 data REM 107 parameters refined using 0 restraints END WGHT 0.1397 0.4675 REM Instructions for potential hydrogen bonds HTAB N2 F2_$2 HTAB N2 F1_$2 HTAB N2 F2_$1 HTAB N2 F1 HTAB N2 N1_$3 HTAB C1 F1_$2 HTAB C1 F2_$1 HTAB C3 F3_$4 HTAB C5 F2_$5 HTAB C5 F3_$5 REM Highest difference peak 0.740, deepest hole -0.599, 1-sigma level 0.084 Q1 1 0.1600 0.4298 0.4307 11.00000 0.05 0.74 ; _shelx_res_checksum 14561 _shelx_hkl_file ; -1 0 0 3464.42 196.51 -1 0 0 3447.89 204.74 1 0 0 3376.46 196.49 1 0 0 3492.83 204.10 -2 0 0 6427.97 382.47 -2 0 0 6608.08 401.01 2 0 0 6846.95 382.55 2 0 0 6941.43 398.29 -3 0 0 6178.25 359.53 3 0 0 6410.40 359.63 3 0 0 6557.48 386.40 -3 0 0 5974.81 392.59 -4 0 0 3.41 4.61 -4 0 0 1.62 6.55 -4 0 0 -117.80 91.97 4 0 0 -1.08 5.50 4 0 0 1.52 6.36 -4 0 0 6.97 2.07 4 0 0 10.94 8.70 4 0 0 -19.15 70.56 5 0 0 2624.05 172.27 -5 0 0 2827.14 163.41 -5 0 0 2817.81 159.93 5 0 0 2824.35 340.78 5 0 0 2821.19 166.65 -5 0 0 2772.65 164.27 5 0 0 2722.59 165.64 6 0 0 243.37 23.93 6 0 0 249.53 22.61 -6 0 0 226.04 28.69 -6 0 0 225.89 20.53 -6 0 0 260.48 17.21 6 0 0 194.64 28.03 -7 0 0 228.18 33.78 -7 0 0 187.22 19.48 7 0 0 209.91 19.10 7 0 0 241.73 22.09 7 0 0 216.33 22.79 8 0 0 51.87 11.37 -8 0 0 52.22 17.17 8 0 0 65.05 12.62 9 0 0 13.44 5.01 9 0 0 11.25 5.24 -9 0 0 8.03 7.89 0 -1 0 -0.38 0.54 0 -1 0 0.18 0.37 0 -1 0 0.47 1.11 0 -1 0 1.81 6.96 0 1 0 -1.12 6.70 0 1 0 -0.08 1.08 0 1 0 1.30 0.90 -1 -1 0 11.10 1.67 -1 -1 0 16.22 2.77 -1 -1 0 10.97 1.27 1 -1 0 24.27 4.25 1 -1 0 21.24 5.06 -1 -1 0 7.09 13.52 1 -1 0 13.51 1.87 -1 1 0 23.63 10.40 1 1 0 11.33 4.17 1 1 0 8.24 13.14 1 1 0 16.35 2.78 -1 1 0 14.27 2.65 1 1 0 12.53 1.74 -2 -1 0 1143.47 88.34 2 -1 0 1073.15 79.22 -2 -1 0 1079.29 61.11 2 -1 0 1027.66 65.72 2 -1 0 1100.54 63.36 -2 -1 0 1033.00 62.42 2 -1 0 1069.52 61.76 -2 -1 0 1070.97 61.71 -2 1 0 1033.69 61.17 -2 1 0 1084.95 62.35 2 1 0 962.92 65.23 2 1 0 1032.12 62.56 -2 1 0 1092.59 61.88 2 1 0 1083.15 84.96 2 1 0 1107.51 61.84 -2 1 0 1024.97 81.07 3 -1 0 517.93 71.13 3 -1 0 559.74 33.87 3 -1 0 552.11 39.63 -3 -1 0 540.35 32.50 -3 -1 0 564.82 34.79 3 -1 0 545.65 35.79 -3 -1 0 651.43 83.60 -3 -1 0 532.63 33.76 3 1 0 544.88 35.02 -3 1 0 591.11 34.55 -3 1 0 550.18 32.66 3 1 0 563.08 33.89 -3 1 0 598.29 84.33 -3 1 0 574.09 34.13 3 1 0 547.32 81.33 3 1 0 493.24 38.72 4 -1 0 72.45 74.81 -4 -1 0 69.37 8.99 4 -1 0 81.71 16.25 -4 -1 0 93.96 11.07 -4 -1 0 146.57 103.55 4 -1 0 79.89 11.82 -4 -1 0 69.37 5.81 4 -1 0 74.94 9.66 4 1 0 77.43 16.03 4 1 0 78.17 10.72 -4 1 0 68.98 10.35 -4 1 0 72.56 8.70 -4 1 0 66.59 5.97 4 1 0 36.82 78.26 -4 1 0 -135.30 94.74 -5 -1 0 103.64 19.10 -5 -1 0 111.19 12.61 5 -1 0 117.73 16.91 5 -1 0 113.07 20.96 -5 -1 0 106.41 8.96 5 -1 0 123.31 20.56 5 -1 0 114.10 15.22 -5 -1 0 -86.03 255.64 5 -1 0 -70.19 176.15 5 1 0 140.10 16.98 -5 1 0 116.88 9.07 5 1 0 56.66 190.81 -5 1 0 137.64 22.42 -5 1 0 143.18 240.61 5 1 0 121.46 16.76 5 1 0 143.26 24.13 -5 1 0 116.98 12.19 5 1 0 73.19 11.92 -5 1 0 114.64 21.39 6 -1 0 10.04 8.13 -6 -1 0 6.00 6.02 -6 -1 0 0.02 3.85 6 -1 0 -4.74 9.21 6 -1 0 -8.24 5.76 6 -1 0 3.41 7.59 -6 1 0 4.64 5.77 6 1 0 -3.17 6.55 6 1 0 1.56 7.19 6 1 0 0.72 6.33 6 1 0 1.28 5.74 -6 1 0 4.10 10.94 7 -1 0 74.94 14.74 7 -1 0 78.30 13.67 7 -1 0 44.52 18.39 -7 -1 0 69.53 18.71 7 -1 0 94.00 15.27 -7 -1 0 64.66 12.20 -7 1 0 104.50 13.94 7 1 0 102.50 16.80 -7 1 0 86.87 21.40 7 1 0 112.00 16.55 8 -1 0 10.94 6.69 -8 -1 0 1.68 10.08 8 -1 0 -4.99 5.99 8 1 0 -1.79 6.29 -8 1 0 3.29 9.92 8 1 0 -0.56 4.98 9 -1 0 22.76 6.26 9 -1 0 17.23 5.62 -9 -1 0 18.99 8.73 -9 1 0 21.98 8.10 9 1 0 29.62 6.92 0 -2 0 4320.66 238.06 0 -2 0 4274.57 251.00 0 2 0 3676.52 238.28 0 2 0 4131.66 238.60 0 2 0 4515.05 252.50 -1 -2 0 1304.09 76.41 1 -2 0 1312.96 75.09 1 -2 0 1295.63 78.84 -1 -2 0 1326.03 93.66 -1 -2 0 1321.78 75.58 1 -2 0 1313.50 75.54 -1 -2 0 1316.56 75.15 1 -2 0 1279.11 76.93 1 2 0 1386.95 77.93 1 2 0 1448.52 96.64 1 2 0 1303.15 75.55 -1 2 0 1171.67 75.78 1 2 0 1325.16 75.76 -1 2 0 1330.12 92.84 -2 -2 0 126.81 9.99 2 -2 0 121.45 7.70 2 -2 0 123.57 11.15 -2 -2 0 120.61 39.61 2 -2 0 125.62 8.93 2 -2 0 137.50 13.64 2 -2 0 112.81 8.97 -2 -2 0 118.58 7.75 -2 -2 0 125.42 8.99 2 2 0 202.33 41.73 2 2 0 92.50 11.66 -2 2 0 86.49 28.13 -2 2 0 109.64 34.36 -2 2 0 132.03 9.50 2 2 0 119.28 8.92 2 2 0 122.92 9.32 3 -2 0 262.85 18.39 -3 -2 0 257.89 18.11 -3 -2 0 251.44 75.26 3 -2 0 317.67 21.07 -3 -2 0 271.37 19.01 -3 -2 0 243.06 16.17 3 -2 0 273.98 23.77 -3 2 0 288.11 62.29 3 2 0 214.96 21.96 -3 2 0 272.83 18.20 3 2 0 290.52 18.52 3 2 0 185.36 61.02 3 2 0 263.36 18.13 4 -2 0 88.04 11.45 -4 -2 0 81.65 11.38 -4 -2 0 79.42 6.75 4 -2 0 114.47 12.87 4 -2 0 108.31 18.83 -4 -2 0 196.15 128.02 -4 -2 0 86.29 10.15 4 2 0 79.11 15.41 4 2 0 96.27 10.08 4 2 0 188.76 102.64 -4 2 0 183.50 107.32 -4 2 0 101.88 9.90 -5 -2 0 590.03 37.06 5 -2 0 607.90 42.88 5 -2 0 536.94 43.23 5 -2 0 601.71 50.16 5 -2 0 617.66 42.99 -5 -2 0 619.85 41.65 5 -2 0 596.14 36.81 -5 2 0 610.85 39.98 5 2 0 621.62 43.05 5 2 0 644.69 43.68 -5 2 0 415.35 399.58 5 2 0 690.44 40.35 -5 2 0 589.08 49.00 6 -2 0 180.91 18.88 -6 -2 0 167.97 17.95 6 -2 0 169.51 19.30 6 -2 0 109.98 24.88 6 -2 0 195.91 21.27 6 -2 0 195.20 15.45 -6 2 0 155.59 15.81 -6 2 0 179.38 28.50 6 2 0 188.54 15.66 6 2 0 178.65 18.93 6 2 0 174.89 19.70 7 -2 0 46.27 12.03 7 -2 0 25.59 14.68 7 -2 0 56.95 12.45 7 -2 0 58.01 12.02 -7 -2 0 36.02 14.36 -7 -2 0 46.15 11.56 -7 2 0 49.70 16.04 7 2 0 43.44 11.34 7 2 0 54.28 11.90 -7 2 0 42.67 8.89 8 -2 0 40.42 10.59 8 -2 0 19.86 7.89 -8 -2 0 42.64 16.93 -8 2 0 25.80 12.60 8 2 0 40.32 9.71 8 2 0 35.32 9.38 -9 -2 0 74.88 14.59 9 -2 0 33.81 6.92 9 2 0 30.27 6.48 0 -3 0 1.43 4.58 0 -3 0 50.09 26.97 0 3 0 43.57 30.23 -1 -3 0 494.82 28.10 -1 -3 0 488.12 30.14 1 -3 0 468.43 30.54 -1 -3 0 472.70 28.75 1 -3 0 467.80 60.20 -1 -3 0 475.99 64.20 1 -3 0 482.48 28.06 1 -3 0 498.19 28.89 1 -3 0 475.25 33.08 -1 3 0 520.81 64.16 1 3 0 475.35 28.76 1 3 0 429.16 29.34 1 3 0 511.21 28.69 -1 3 0 466.47 28.70 1 3 0 525.17 66.51 1 3 0 501.30 31.53 -1 3 0 450.08 28.80 2 -3 0 112.73 13.76 -2 -3 0 93.83 9.20 2 -3 0 107.98 9.25 2 -3 0 96.83 8.68 2 -3 0 97.41 6.80 2 -3 0 96.13 10.91 -2 -3 0 111.49 49.44 -2 -3 0 99.83 6.90 -2 -3 0 114.26 8.92 -2 3 0 105.20 8.48 -2 3 0 115.48 36.57 -2 3 0 95.89 48.04 2 3 0 108.66 8.26 2 3 0 111.48 11.31 2 3 0 96.02 8.67 2 3 0 111.28 51.53 3 -3 0 -6.32 4.91 -3 -3 0 0.19 4.23 -3 -3 0 4.98 1.64 3 -3 0 0.60 5.61 3 -3 0 -2.58 5.50 -3 -3 0 6.17 5.18 3 -3 0 -3.39 6.34 -3 -3 0 -12.95 87.78 3 -3 0 1.12 1.30 3 3 0 0.96 3.24 -3 3 0 -86.98 66.99 3 3 0 3.69 5.58 -3 3 0 -18.63 59.00 -3 3 0 1.00 3.04 3 3 0 -5.05 5.13 3 3 0 -41.07 72.00 -4 -3 0 66.00 12.31 4 -3 0 60.28 11.80 4 -3 0 64.80 5.54 -4 -3 0 82.77 11.25 4 -3 0 84.15 18.25 4 -3 0 62.18 12.23 -4 -3 0 60.11 5.85 4 -3 0 71.55 12.23 -4 -3 0 -107.35 173.62 -4 3 0 79.49 9.35 4 3 0 2.97 132.95 -4 3 0 107.38 132.50 -4 3 0 -136.17 129.18 4 3 0 51.59 7.47 5 -3 0 289.13 18.86 5 -3 0 278.65 24.56 5 -3 0 322.80 33.06 5 -3 0 295.48 26.51 -5 -3 0 249.51 23.01 5 -3 0 254.12 24.93 5 3 0 298.41 24.85 -5 3 0 261.13 20.76 -5 3 0 260.44 30.60 5 3 0 322.84 25.44 5 3 0 293.92 20.34 6 -3 0 -4.05 8.62 6 -3 0 -2.65 6.99 -6 -3 0 -5.05 5.86 6 -3 0 -0.26 11.71 6 -3 0 -0.69 6.84 6 3 0 3.91 6.60 6 3 0 4.12 4.89 -6 3 0 14.10 11.91 -6 3 0 9.03 5.63 6 3 0 -0.15 7.33 6 3 0 -4.67 8.69 7 -3 0 4.97 6.59 7 -3 0 11.97 8.66 7 -3 0 4.16 12.49 7 -3 0 5.67 7.98 -7 -3 0 -4.68 6.60 7 3 0 -1.94 5.78 -7 3 0 -0.63 10.19 7 3 0 7.00 7.78 8 -3 0 1.32 6.01 8 -3 0 -3.58 4.86 -8 -3 0 2.67 10.74 8 3 0 0.17 4.70 -8 3 0 5.67 8.57 9 -3 0 16.45 4.89 9 -3 0 7.71 3.86 -9 -3 0 18.05 7.57 9 3 0 16.89 5.04 0 -4 0 187.41 51.68 0 -4 0 259.69 20.30 0 -4 0 228.73 13.88 0 -4 0 232.53 15.40 0 4 0 216.42 14.08 0 4 0 236.50 14.45 0 4 0 182.63 15.74 0 4 0 308.70 56.80 -1 -4 0 13.90 47.01 -1 -4 0 -0.74 3.45 1 -4 0 43.14 43.61 1 -4 0 -1.83 4.14 1 -4 0 1.37 3.53 1 -4 0 -0.12 1.35 1 -4 0 3.17 5.82 -1 -4 0 0.68 1.37 -1 -4 0 -5.73 3.31 -1 4 0 -4.21 3.19 1 4 0 1.53 2.14 -1 4 0 3.37 2.43 -1 4 0 -38.71 53.80 1 4 0 0.76 3.40 1 4 0 -1.64 1.69 1 4 0 20.80 56.29 -2 -4 0 302.08 18.92 2 -4 0 313.92 18.93 2 -4 0 294.38 21.25 2 -4 0 303.88 20.97 -2 -4 0 300.29 78.54 -2 -4 0 296.44 20.89 2 -4 0 266.72 23.07 -2 -4 0 292.55 22.03 2 -4 0 341.75 27.38 -2 4 0 321.64 82.33 2 4 0 313.76 23.78 2 4 0 324.65 19.37 -2 4 0 335.35 20.04 2 4 0 492.03 85.61 -3 -4 0 151.76 14.42 -3 -4 0 174.71 16.60 3 -4 0 157.21 10.45 3 -4 0 154.95 18.03 3 -4 0 131.74 15.82 3 -4 0 125.55 16.56 -3 -4 0 216.19 124.75 -3 -4 0 146.69 10.55 3 -4 0 153.02 19.63 -3 4 0 38.34 89.37 3 4 0 142.65 118.51 3 4 0 164.37 11.23 -3 4 0 187.85 113.68 -3 4 0 168.85 12.09 4 -4 0 168.38 19.18 4 -4 0 216.15 24.93 -4 -4 0 177.31 17.44 4 -4 0 202.91 19.90 -4 4 0 225.31 32.49 4 4 0 189.15 18.10 -4 4 0 183.38 14.41 5 -4 0 859.53 69.39 5 -4 0 961.69 62.20 -5 -4 0 843.19 59.60 5 -4 0 956.92 63.19 5 -4 0 867.64 60.52 5 4 0 1018.72 61.34 5 4 0 857.57 60.08 -5 4 0 865.38 66.03 6 -4 0 93.42 17.46 -6 -4 0 72.70 14.31 6 -4 0 58.27 12.61 6 -4 0 35.34 11.78 6 -4 0 47.33 18.85 6 4 0 71.75 13.47 6 4 0 74.46 13.85 -6 4 0 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3.63 -6 0 9 -0.56 6.60 6 0 -9 0.03 4.68 5 0 -9 -2.43 6.26 -5 0 9 16.66 10.24 -4 0 9 -5.97 7.73 4 0 -9 2.53 8.06 -3 0 9 -4.71 7.16 -2 0 9 -2.52 6.85 -1 0 9 -0.94 6.41 -1 0 9 -19.25 7.36 0 0 9 4.87 7.12 0 0 9 1.29 9.80 1 0 9 1.97 9.50 1 0 9 -2.74 6.04 2 0 9 -8.70 5.45 2 0 9 3.44 9.95 3 0 9 13.42 10.95 3 0 9 1.94 7.63 4 0 9 5.95 7.36 4 0 9 14.04 10.56 -4 0 -9 -9.35 13.61 5 0 9 -4.54 5.21 5 0 9 5.66 8.52 -5 0 -9 8.84 12.34 6 0 9 -4.08 4.40 -6 0 -9 10.17 8.01 6 0 9 -0.93 5.28 7 -1 -9 5.30 3.76 7 1 -9 -0.04 3.18 -6 -1 9 10.01 7.75 6 -1 -9 5.99 5.04 6 1 -9 6.59 5.32 -6 1 9 18.94 9.82 -5 -1 9 19.01 10.11 5 -1 -9 2.58 7.06 -5 1 9 20.66 10.99 5 1 -9 -0.25 6.83 -4 -1 9 94.73 17.59 4 1 -9 62.65 13.44 -4 1 9 81.96 16.38 -3 -1 9 10.25 8.97 -3 1 9 -3.75 8.35 3 1 -9 16.41 9.51 -2 -1 9 -0.50 6.74 -2 1 9 4.43 7.65 2 1 -9 3.97 10.43 -1 -1 9 -13.29 7.14 -1 -1 9 18.83 9.29 -1 1 9 13.90 8.74 0 -1 9 27.22 9.78 0 -1 9 13.67 11.25 0 1 9 21.99 9.54 0 1 9 22.23 11.87 1 -1 9 58.14 13.50 1 -1 9 68.89 16.45 1 1 9 56.49 15.18 1 1 9 74.49 14.74 2 -1 9 19.13 9.07 2 -1 9 24.88 12.83 2 1 9 31.02 12.66 2 1 9 15.13 8.96 -2 1 -9 28.23 14.79 3 -1 9 37.85 13.90 3 -1 9 26.60 10.57 3 1 9 37.65 13.41 -3 1 -9 23.89 15.20 3 1 9 32.98 11.02 4 -1 9 92.86 16.31 4 -1 9 75.06 16.52 -4 1 -9 96.21 21.38 4 1 9 62.19 15.74 4 1 9 79.39 15.20 5 -1 9 12.40 7.32 5 -1 9 14.45 9.27 -5 -1 -9 50.14 25.40 5 1 9 8.10 7.75 5 1 9 15.95 9.59 -5 1 -9 13.63 11.07 6 -1 9 -0.21 4.46 6 -1 9 -1.70 5.29 6 1 9 7.65 6.03 -6 1 -9 -10.24 6.64 6 1 9 2.19 4.33 7 2 -9 11.58 4.70 6 -2 -9 2.87 5.19 -6 -2 9 0.41 6.15 6 2 -9 1.21 4.66 -6 2 9 4.23 7.48 -5 -2 9 78.43 13.89 -5 2 9 78.96 15.87 5 2 -9 79.23 13.74 -4 -2 9 4.75 9.03 -4 2 9 21.04 10.77 4 2 -9 -3.86 6.95 -3 -2 9 -4.01 7.36 -3 -2 9 0.21 1.27 3 2 -9 4.34 8.60 -3 2 9 -4.59 7.32 -2 -2 9 35.07 11.25 -2 -2 9 34.29 3.38 -2 2 9 41.44 12.71 2 2 -9 31.12 12.22 -1 -2 9 1.48 2.09 -1 -2 9 4.80 7.11 -1 -2 9 0.35 6.19 -1 -2 9 1.99 1.26 -1 2 9 -3.92 6.14 1 2 -9 -0.97 9.53 0 -2 9 1.11 1.19 0 -2 9 2.57 1.66 0 -2 9 5.98 9.62 0 -2 9 -3.50 5.68 0 2 -9 7.11 10.70 0 2 9 -3.30 5.99 0 2 9 -6.79 8.36 1 -2 9 188.23 12.27 1 -2 9 217.05 21.70 1 -2 9 218.64 25.45 1 2 9 218.07 24.69 -1 2 -9 187.82 29.21 1 2 9 213.40 22.43 2 -2 9 12.26 11.62 2 -2 9 5.51 7.06 2 2 9 9.39 10.54 -2 2 -9 -7.05 11.84 2 2 9 0.97 7.37 3 -2 9 33.99 13.44 3 -2 9 19.48 9.13 3 2 9 33.65 12.35 3 2 9 27.58 10.48 -3 2 -9 1.79 12.27 4 -2 9 5.61 9.89 4 -2 9 -4.38 5.75 4 2 9 6.03 9.77 -4 2 -9 0.29 11.22 4 2 9 -0.28 6.56 5 -2 9 24.92 9.74 5 -2 9 18.36 7.15 5 2 9 26.01 10.27 -5 2 -9 16.70 11.36 5 2 9 28.04 9.76 6 -2 9 13.39 5.32 6 2 9 16.60 6.52 -6 2 -9 10.12 7.03 6 2 9 5.08 5.48 6 3 -9 139.19 14.96 -5 3 9 26.63 11.21 5 3 -9 36.92 10.68 -4 -3 9 207.68 23.07 4 3 -9 232.30 25.02 -4 3 9 238.74 25.53 -3 -3 9 59.94 5.06 -3 -3 9 51.12 12.87 3 3 -9 56.43 14.26 -3 3 9 50.91 13.99 -2 -3 9 91.72 6.85 -2 -3 9 78.71 14.19 2 3 -9 82.31 18.52 -2 3 9 112.20 19.17 2 3 -9 94.44 16.93 -1 -3 9 256.63 16.22 -1 -3 9 256.02 23.88 -1 3 9 273.83 26.06 1 3 -9 254.82 26.24 1 3 -9 255.05 29.39 0 -3 9 36.41 10.09 0 -3 9 33.09 12.78 0 -3 9 34.29 3.72 0 3 9 22.27 10.01 0 3 9 25.35 11.23 0 3 -9 36.67 14.94 0 3 -9 35.06 12.76 1 -3 9 151.01 17.26 1 -3 9 147.02 9.87 1 -3 9 127.70 21.58 1 3 9 180.05 22.22 -1 3 -9 116.80 18.46 1 3 9 185.25 19.84 -1 3 -9 98.75 21.15 2 -3 9 5.96 7.20 2 -3 9 9.32 2.14 2 -3 9 3.75 10.52 -2 3 -9 21.55 13.58 2 3 9 5.57 9.20 -2 3 -9 10.86 12.53 2 3 9 8.23 7.92 3 -3 9 96.88 20.24 3 -3 9 91.57 15.55 3 3 9 103.76 17.34 -3 3 -9 74.97 18.65 3 3 9 75.52 17.06 4 -3 9 -1.78 6.09 4 -3 9 22.64 10.49 4 3 9 19.70 9.07 4 3 9 24.66 10.62 -4 3 -9 14.79 10.99 5 -3 9 11.72 6.84 5 3 9 19.58 8.72 -5 3 -9 -0.75 7.78 5 3 9 11.85 6.65 6 -3 9 43.26 7.52 6 3 9 14.63 5.58 -6 3 -9 24.42 7.74 6 3 9 26.22 5.12 -6 4 9 2.42 5.53 6 4 -9 3.01 3.97 -5 4 9 5.95 8.22 5 4 -9 4.22 7.01 4 4 -9 1.00 7.31 -4 4 9 6.61 8.95 3 4 -9 -1.70 7.87 -3 4 9 17.46 9.80 -2 -4 9 -2.52 1.55 -2 -4 9 14.00 9.35 -2 4 9 3.23 7.84 2 4 -9 2.97 9.19 -1 -4 9 1.03 6.69 -1 -4 9 1.57 1.80 -1 4 9 4.72 7.76 1 4 -9 14.85 10.29 1 4 -9 1.85 10.53 -1 4 9 -16.73 6.14 0 -4 9 38.69 4.50 0 -4 9 43.06 10.85 0 4 -9 42.21 12.30 0 4 -9 43.63 16.57 0 4 9 50.63 12.60 0 4 9 57.70 13.97 1 -4 9 38.29 4.30 1 -4 9 35.39 9.60 -1 4 -9 36.32 14.69 -1 4 -9 19.00 13.66 1 4 9 34.19 10.96 1 4 9 35.24 12.23 2 -4 9 28.53 3.82 2 -4 9 38.98 13.67 2 -4 9 25.32 8.44 2 4 9 37.93 12.61 2 4 9 29.36 10.08 -2 4 -9 31.82 15.53 3 -4 9 -6.90 4.85 3 4 9 3.86 8.35 3 4 9 -1.13 5.81 -3 4 -9 1.16 10.41 4 -4 9 -1.00 4.58 4 4 9 4.14 6.10 4 4 9 6.02 7.96 -4 4 -9 2.71 9.40 5 -4 9 4.02 4.56 5 4 9 3.83 6.34 5 4 9 8.70 4.77 -5 4 -9 4.98 6.90 -5 5 9 24.98 9.05 5 5 -9 18.37 7.23 4 5 -9 8.56 7.68 -4 5 9 17.93 9.18 3 5 -9 9.42 9.48 -3 5 9 28.90 11.28 2 5 -9 26.51 12.34 -2 5 9 31.67 10.71 -1 -5 9 13.04 3.33 1 5 -9 17.58 11.00 -1 5 9 9.84 8.65 0 -5 9 216.37 14.85 0 5 9 200.79 22.41 0 5 -9 202.73 30.64 0 5 9 248.66 22.87 1 5 9 12.82 8.67 1 5 9 11.42 7.47 -1 5 -9 -7.25 8.35 2 -5 9 36.45 8.60 -2 5 -9 19.17 12.23 2 5 9 20.19 9.82 2 5 9 8.36 6.94 3 -5 9 44.84 8.31 3 5 9 52.95 13.07 -3 5 -9 38.87 14.43 4 -5 9 34.57 6.93 -4 5 -9 8.94 7.87 4 5 9 34.01 10.47 -5 5 -9 19.19 6.57 5 6 -9 0.17 3.75 -4 6 9 0.35 5.82 4 6 -9 -1.67 4.83 -3 6 9 14.92 8.23 3 6 -9 30.95 10.68 -2 6 9 -0.12 7.90 2 6 -9 7.38 9.34 1 6 -9 13.15 10.29 -1 6 9 18.13 8.66 -1 6 9 -1.48 5.79 0 6 -9 29.22 11.82 0 6 9 37.82 10.01 -1 6 -9 3.95 8.65 1 6 9 -2.03 5.96 1 6 9 4.79 5.39 -2 6 -9 2.24 8.56 2 6 9 8.93 7.83 3 6 9 29.45 9.85 -3 6 -9 7.51 7.14 -4 6 -9 -1.01 5.67 4 6 9 8.54 6.04 4 7 -9 5.31 4.24 3 7 -9 5.05 4.94 2 7 -9 12.38 6.83 1 7 -9 27.30 10.15 0 7 -9 23.02 9.05 0 7 9 40.59 9.45 -1 7 -9 17.42 9.09 1 7 9 21.81 7.30 -2 7 -9 1.23 5.82 2 7 9 3.36 5.14 -3 7 -9 13.90 6.91 3 7 9 22.53 7.64 3 8 -9 2.29 3.62 2 8 -9 -1.50 3.72 1 8 -9 -2.67 5.06 0 8 9 -0.96 4.56 0 8 -9 -4.36 4.26 -1 8 -9 6.12 5.25 1 8 9 2.48 4.51 2 8 9 3.70 4.17 -2 8 -9 -3.36 3.83 -6 0 10 51.99 9.76 6 0 -10 40.00 7.26 5 0 -10 55.70 10.00 -5 0 10 75.22 14.53 -4 0 10 22.15 10.01 4 0 -10 14.22 8.99 -3 0 10 3.80 8.25 -2 0 10 10.43 8.39 -1 0 10 0.14 6.57 0 0 10 6.14 9.52 0 0 10 0.53 6.40 1 0 10 26.46 10.26 1 0 10 9.44 10.02 2 0 10 33.46 10.89 2 0 10 65.51 16.31 3 0 10 -4.83 5.78 3 0 10 14.62 10.14 4 0 10 -8.44 5.28 4 0 10 9.53 8.65 5 0 10 -3.23 4.08 5 0 10 11.06 7.88 -6 -1 10 4.82 4.86 6 1 -10 5.58 4.13 -6 1 10 0.91 5.15 -5 -1 10 7.36 7.04 -5 1 10 2.62 7.58 5 1 -10 5.54 5.49 -4 -1 10 9.57 8.80 -4 1 10 8.90 8.74 4 1 -10 4.81 7.67 -3 -1 10 0.13 7.02 -3 1 10 -2.02 7.89 3 1 -10 2.27 9.28 -2 -1 10 14.22 8.73 2 1 -10 9.59 10.98 -2 1 10 9.54 8.70 -1 -1 10 -2.47 6.21 -1 1 10 1.10 6.48 0 -1 10 3.90 9.27 0 -1 10 -3.46 5.86 0 1 10 1.41 7.56 0 1 10 -5.83 8.09 1 -1 10 112.85 19.28 1 -1 10 106.68 17.19 1 1 10 72.64 14.63 1 1 10 72.01 15.84 2 -1 10 18.68 8.77 2 -1 10 42.91 13.91 2 1 10 17.54 8.84 -2 1 -10 0.47 22.00 2 1 10 21.14 10.87 3 -1 10 9.87 7.66 3 -1 10 11.21 9.61 3 1 10 18.93 10.22 3 1 10 2.74 6.85 -3 1 -10 10.85 13.54 4 -1 10 15.64 7.67 4 -1 10 33.86 10.68 4 1 10 42.87 11.98 -4 1 -10 41.34 13.60 4 1 10 37.97 10.79 5 -1 10 -4.49 5.48 5 -1 10 -4.48 4.02 5 1 10 -2.45 4.29 -5 1 -10 21.60 9.51 5 1 10 -1.09 5.93 -6 2 10 5.69 4.86 6 2 -10 9.71 4.11 -5 -2 10 18.76 8.02 -5 2 10 42.78 11.22 5 2 -10 37.66 8.67 -4 -2 10 0.24 7.80 4 2 -10 -4.71 5.80 -4 2 10 11.57 8.87 -3 -2 10 17.30 9.06 3 2 -10 19.33 9.82 -3 2 10 16.25 9.90 -2 -2 10 12.28 7.87 -2 2 10 13.71 8.97 2 2 -10 1.57 10.76 -1 -2 10 1.46 6.50 -1 2 10 -3.71 6.95 1 2 -10 2.16 9.54 0 -2 10 122.94 15.95 0 -2 10 118.26 18.85 0 2 10 132.38 19.56 0 2 10 72.65 15.73 0 2 -10 104.79 20.38 1 -2 10 1.33 6.16 1 -2 10 7.90 9.77 -1 2 -10 17.54 12.19 1 2 10 4.61 6.96 1 2 10 10.43 10.19 2 -2 10 55.68 14.34 2 -2 10 52.58 12.37 2 2 10 51.39 14.43 2 2 10 45.48 11.84 -2 2 -10 37.57 14.63 3 -2 10 28.44 11.29 3 -2 10 31.27 9.73 3 2 10 16.14 10.18 3 2 10 23.83 9.18 -3 2 -10 32.62 15.67 4 -2 10 30.59 8.74 4 -2 10 18.18 8.60 4 2 10 36.32 9.94 4 2 10 34.61 10.52 -4 2 -10 29.08 12.29 5 -2 10 69.52 10.82 5 2 10 81.97 13.15 -5 2 -10 55.96 12.54 5 2 10 57.29 10.32 5 3 -10 -4.58 4.27 -5 3 10 6.69 6.78 -4 -3 10 28.56 10.48 4 3 -10 34.00 9.37 -4 3 10 55.12 13.34 -3 -3 10 0.79 8.42 3 3 -10 12.66 8.05 -3 3 10 2.34 7.75 -2 -3 10 3.96 6.98 2 3 -10 -1.57 8.78 -2 3 10 0.42 7.25 -1 -3 10 0.26 6.51 1 3 -10 -1.68 8.72 -1 3 10 -4.37 6.20 0 -3 10 66.99 12.79 0 3 -10 74.21 18.14 0 3 10 62.56 14.56 0 3 10 69.80 14.16 1 -3 10 31.23 11.38 1 -3 10 39.33 10.03 1 3 10 55.67 12.79 1 3 10 46.24 13.32 -1 3 -10 48.05 15.63 2 -3 10 -6.77 4.94 2 -3 10 -4.94 7.29 2 3 10 14.19 10.48 -2 3 -10 5.38 10.79 2 3 10 -2.08 5.88 3 -3 10 -4.20 6.45 3 -3 10 -1.63 5.02 3 3 10 4.35 6.17 3 3 10 11.52 8.54 -3 3 -10 -1.61 8.83 4 -3 10 4.88 5.28 4 3 10 2.35 6.82 -4 3 -10 4.74 9.40 4 3 10 6.53 5.68 5 -3 10 7.38 4.39 5 3 10 9.17 6.15 5 3 10 6.94 4.08 -5 3 -10 0.38 5.59 -5 4 10 -0.70 6.37 5 4 -10 3.80 4.50 4 4 -10 106.95 15.83 -4 4 10 67.35 13.08 -3 4 10 40.48 10.57 3 4 -10 48.43 11.11 2 4 -10 32.72 12.28 -2 4 10 26.70 10.40 -1 -4 10 74.83 12.06 1 4 -10 39.79 12.77 -1 4 10 54.28 12.46 0 -4 10 77.71 12.85 0 4 10 99.62 16.68 0 4 -10 58.10 17.27 1 -4 10 24.28 7.97 -1 4 -10 12.14 11.15 1 4 10 19.82 8.56 1 4 10 21.81 9.96 2 -4 10 53.65 9.39 -2 4 -10 32.82 11.91 2 4 10 47.39 10.40 2 4 10 43.21 12.13 3 -4 10 50.88 8.60 3 4 10 43.06 9.11 -3 4 -10 50.65 13.72 3 4 10 84.70 14.52 4 -4 10 19.75 5.42 -4 4 -10 7.80 7.27 4 4 10 42.18 10.15 4 4 10 16.42 5.62 -5 5 10 -7.22 3.85 5 5 -10 -0.58 3.41 -4 5 10 22.33 8.56 4 5 -10 25.80 8.33 -3 5 10 10.54 8.35 3 5 -10 5.32 7.00 2 5 -10 -1.29 7.58 -2 5 10 7.91 7.23 1 5 -10 7.00 8.52 -1 5 10 -2.84 6.54 0 5 -10 1.93 7.98 0 5 10 17.17 8.53 0 5 10 -12.90 4.85 1 5 10 4.37 6.78 -1 5 -10 10.14 9.48 1 5 10 0.74 5.74 -2 5 -10 -5.21 7.77 2 5 10 -1.00 6.65 2 5 10 9.33 6.04 3 5 10 14.85 5.54 -3 5 -10 -0.26 6.00 3 5 10 4.50 6.67 4 5 10 14.62 6.79 -4 5 -10 5.02 5.04 4 6 -10 38.25 6.84 -3 6 10 20.31 6.79 3 6 -10 20.36 7.59 2 6 -10 31.15 10.22 -2 6 10 20.28 8.73 -1 6 10 1.93 7.78 1 6 -10 8.21 7.06 0 6 10 -8.23 4.43 0 6 10 -8.89 5.22 0 6 -10 2.54 7.40 1 6 10 5.85 6.87 -1 6 -10 -6.50 6.02 2 6 10 12.76 6.66 -2 6 -10 20.34 9.18 3 6 10 5.53 5.39 -3 6 -10 7.71 6.34 2 7 -10 3.11 4.69 1 7 -10 9.88 5.66 0 7 -10 -0.56 5.01 1 7 10 -2.60 4.42 -1 7 -10 -1.63 4.03 -2 7 -10 -1.74 4.40 2 7 10 -0.65 4.21 -5 0 11 -1.67 4.46 -4 0 11 5.57 6.89 -3 0 11 0.98 6.54 -2 0 11 -6.22 5.54 -1 0 11 1.65 6.04 0 0 11 1.53 6.55 0 0 11 -2.55 5.48 1 0 11 0.48 6.10 1 0 11 -1.28 8.31 2 0 11 5.16 8.20 2 0 11 -4.86 5.04 3 0 11 2.48 7.05 3 0 11 -0.34 5.40 4 0 11 -2.94 5.49 4 0 11 -2.30 4.44 -5 -1 11 22.79 5.76 -5 1 11 14.05 6.15 -4 -1 11 13.71 8.12 -4 1 11 9.59 7.14 4 1 -11 2.79 7.02 -3 -1 11 45.76 10.62 -3 1 11 37.85 10.40 -2 -1 11 -1.78 6.12 -2 1 11 -2.44 6.51 -1 -1 11 1.27 6.20 -1 1 11 -2.26 5.73 0 -1 11 19.66 8.43 0 -1 11 1.54 5.00 0 1 11 -9.55 5.13 0 1 11 20.88 8.97 1 -1 11 52.41 13.38 1 -1 11 66.21 12.89 1 1 11 58.78 13.53 1 1 11 64.99 13.02 2 -1 11 11.08 6.78 2 -1 11 9.70 8.56 2 1 11 14.18 8.75 2 1 11 16.08 7.77 3 -1 11 4.84 6.52 3 -1 11 13.34 7.07 3 1 11 13.41 7.56 3 1 11 16.83 7.36 4 -1 11 0.10 5.03 4 -1 11 8.31 5.50 4 1 11 3.56 5.78 4 1 11 4.77 5.51 -5 2 11 2.31 4.37 -4 -2 11 -8.02 5.52 4 2 -11 -3.62 5.01 -4 2 11 6.53 6.57 -3 -2 11 13.28 7.49 -3 2 11 4.05 7.58 3 2 -11 -6.91 5.91 -2 -2 11 10.06 7.92 -2 2 11 15.00 8.20 2 2 -11 34.27 10.80 -1 -2 11 11.21 8.00 1 2 -11 32.53 11.66 -1 2 11 3.13 6.71 0 -2 11 18.98 8.02 0 2 11 16.92 8.40 0 2 -11 57.00 14.14 1 -2 11 7.35 6.39 1 2 11 -4.19 4.98 1 2 11 3.54 8.36 -1 2 -11 24.53 12.70 2 -2 11 -8.04 5.17 2 -2 11 2.34 5.00 2 2 11 -1.96 6.81 -2 2 -11 17.95 11.44 2 2 11 -1.81 5.37 3 -2 11 2.33 6.26 3 -2 11 3.22 5.67 -3 2 -11 14.99 10.47 3 2 11 9.51 6.98 3 2 11 -4.83 4.44 4 -2 11 2.43 4.17 4 2 11 8.61 6.53 4 2 11 2.59 4.75 4 3 -11 34.52 7.72 -4 3 11 34.32 9.01 3 3 -11 60.72 11.19 -3 3 11 49.07 11.38 -2 -3 11 118.45 15.10 2 3 -11 186.83 19.19 -2 3 11 131.02 16.86 -1 -3 11 126.80 14.43 1 3 -11 118.51 18.84 -1 3 11 130.38 16.15 0 -3 11 110.76 13.04 0 3 -11 91.13 15.95 0 3 11 79.14 13.70 1 -3 11 199.81 18.15 1 3 11 211.27 20.43 -1 3 -11 190.99 23.75 1 3 11 184.05 19.97 2 -3 11 45.61 8.69 -2 3 -11 87.71 15.74 2 3 11 88.98 14.60 2 3 11 69.61 12.38 3 -3 11 54.49 8.65 -3 3 -11 43.66 10.31 3 3 11 31.97 9.38 4 -3 11 78.84 8.07 4 3 11 94.38 9.49 4 3 11 90.62 11.07 4 4 -11 11.48 5.26 -4 4 11 10.88 5.21 3 4 -11 1.95 5.03 -3 4 11 10.75 7.02 2 4 -11 8.53 7.19 -2 4 11 11.99 7.68 1 4 -11 4.44 8.23 -1 4 11 1.93 5.97 0 4 11 21.30 7.25 0 4 -11 42.21 11.51 1 -4 11 20.90 6.31 -1 4 -11 1.23 7.67 1 4 11 11.42 7.30 1 4 11 1.36 5.93 2 -4 11 7.68 4.93 -2 4 -11 -1.18 7.34 2 4 11 3.57 5.61 2 4 11 0.23 5.94 -3 4 -11 2.47 5.79 3 4 11 6.24 4.60 3 4 11 5.29 5.15 -3 5 11 3.00 4.70 3 5 -11 1.02 3.93 -2 5 11 6.27 6.84 2 5 -11 10.73 5.81 -1 5 11 4.61 5.59 1 5 -11 5.72 7.33 0 5 11 7.91 6.53 0 5 -11 7.91 7.20 1 5 11 10.74 6.03 1 5 11 8.75 5.47 -1 5 -11 11.48 7.57 2 5 11 6.59 5.14 -2 5 -11 1.51 5.55 2 6 -11 14.67 5.23 1 6 -11 2.05 4.48 0 6 -11 13.88 6.20 -1 6 -11 2.85 4.84 -4 0 12 4.17 4.47 -3 0 12 3.70 6.02 -2 0 12 3.77 5.70 -1 0 12 16.63 7.44 0 0 12 0.61 5.30 1 0 12 170.72 16.97 2 0 12 11.96 6.17 2 0 12 6.18 5.13 3 0 12 4.09 3.95 3 0 12 15.01 5.31 -3 -1 12 3.11 5.90 -3 1 12 7.23 6.23 -2 -1 12 16.11 6.87 -2 1 12 14.91 6.81 -1 -1 12 10.00 6.26 -1 1 12 3.51 5.38 0 -1 12 0.94 5.34 0 1 12 2.01 6.18 1 -1 12 23.82 6.54 1 1 12 15.54 6.46 1 1 12 18.09 5.98 2 -1 12 -3.31 3.93 2 1 12 -4.03 4.01 2 1 12 -2.70 4.76 3 -1 12 -5.36 3.09 3 1 12 -0.57 3.16 3 1 12 0.11 2.97 -3 2 12 44.56 9.37 -2 -2 12 35.44 8.10 -2 2 12 32.55 8.26 -1 -2 12 59.84 9.51 -1 2 12 23.01 7.38 0 -2 12 50.00 9.15 0 2 12 19.53 7.05 1 -2 12 68.14 10.86 1 2 12 78.35 13.29 2 -2 12 46.97 8.48 2 2 12 24.25 6.34 2 2 12 37.34 7.91 -3 3 12 11.60 5.89 -2 3 12 3.69 5.26 -1 3 12 1.59 4.89 1 3 -12 10.88 10.87 0 -3 12 9.23 4.85 0 3 12 -3.05 4.24 1 -3 12 -0.96 4.10 1 3 12 4.59 4.55 2 3 12 4.54 5.19 2 3 12 11.72 4.76 -2 4 12 12.56 5.37 1 4 -12 68.47 12.78 -1 4 12 54.40 9.22 0 4 12 28.70 7.82 0 4 -12 55.67 12.31 1 4 12 6.29 4.14 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7536 _exptl_absorpt_correction_T_min 0.5850 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 1.54185 7.841 9.838 10.496 90.003 92.475 89.975 ) _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 85234 _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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.000000 0.500000 0.500000 0.0487(5) Uani 1 2 d S . P . . F2 F 0.0113(5) 0.6630(3) 0.4514(3) 0.0752(9) Uani 1 1 d . . . . . N2 N 0.0439(4) 0.1774(4) 0.3155(3) 0.0493(9) Uani 1 1 d . . . . . H2A H 0.061043 0.158569 0.234222 0.059 Uiso 1 1 calc R U . . . H2B H 0.070951 0.263919 0.331314 0.059 Uiso 1 1 calc R U . . . H2C H -0.065327 0.163752 0.331291 0.059 Uiso 1 1 calc R U . . . F1 F 0.0048(7) 0.4499(4) 0.3490(3) 0.1270(18) Uani 1 1 d . . . . . N1 N 0.6893(4) 0.1408(5) 0.3510(4) 0.0658(12) Uani 1 1 d . . . . . C2 C 0.3405(4) 0.1094(4) 0.3796(4) 0.0476(10) Uani 1 1 d . . . . . F3 F 0.2051(5) 0.4928(5) 0.5098(7) 0.145(2) Uani 1 1 d . . . . . C1 C 0.1521(4) 0.0877(5) 0.3983(4) 0.0532(11) Uani 1 1 d . . . . . H1A H 0.123428 -0.006497 0.379768 0.064 Uiso 1 1 calc R U . . . H1B H 0.128300 0.105009 0.486619 0.064 Uiso 1 1 calc R U . . . C6 C 0.4334(5) 0.1989(5) 0.4540(5) 0.0646(13) Uani 1 1 d . . . . . H6 H 0.380788 0.251419 0.514569 0.078 Uiso 1 1 calc R U . . . C3 C 0.4230(5) 0.0405(6) 0.2875(5) 0.0705(14) Uani 1 1 d . . . . . H3 H 0.362942 -0.017767 0.232155 0.085 Uiso 1 1 calc R U . . . C4 C 0.5976(6) 0.0584(6) 0.2774(6) 0.0748(15) Uani 1 1 d . . . . . H4 H 0.652307 0.009529 0.215262 0.090 Uiso 1 1 calc R U . . . C5 C 0.6079(6) 0.2101(6) 0.4378(6) 0.0722(15) Uani 1 1 d . . . . . H5 H 0.670571 0.269299 0.490607 0.087 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 P1 0.0467(8) 0.0546(9) 0.0448(9) -0.0015(6) 0.0013(6) -0.0011(6) F2 0.121(3) 0.0550(16) 0.0502(16) 0.0030(12) 0.0046(14) -0.0066(14) N2 0.0318(15) 0.064(2) 0.052(2) -0.0016(16) 0.0047(13) 0.0003(13) F1 0.280(6) 0.0565(19) 0.0452(19) -0.0025(13) 0.009(2) -0.004(3) N1 0.0327(17) 0.087(3) 0.078(3) 0.008(2) 0.0054(17) -0.0001(18) C2 0.0310(17) 0.062(2) 0.050(2) 0.0040(19) -0.0009(15) 0.0017(16) F3 0.050(2) 0.149(4) 0.237(7) 0.047(4) 0.001(3) 0.005(2) C1 0.0342(18) 0.066(3) 0.060(3) 0.006(2) 0.0049(16) -0.0007(17) C6 0.044(2) 0.072(3) 0.079(3) -0.012(3) 0.010(2) 0.000(2) C3 0.039(2) 0.100(4) 0.072(3) -0.026(3) 0.002(2) -0.005(2) C4 0.042(2) 0.106(4) 0.077(4) -0.016(3) 0.014(2) 0.005(2) C5 0.041(2) 0.086(4) 0.089(4) -0.011(3) -0.001(2) -0.013(2) 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' F F 0.0727 0.0534 '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' P P 0.2955 0.4335 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 P1 F2 180.00(6) . 3_566 ? F1 P1 F2 89.35(16) 3_566 3_566 ? F1 P1 F2 89.35(16) . . ? F1 P1 F2 90.65(16) . 3_566 ? F1 P1 F2 90.65(16) 3_566 . ? F1 P1 F1 180.0(4) . 3_566 ? F3 P1 F2 90.2(2) . 3_566 ? F3 P1 F2 90.2(2) 3_566 . ? F3 P1 F2 89.8(2) . . ? F3 P1 F2 89.8(2) 3_566 3_566 ? F3 P1 F1 90.9(3) 3_566 . ? F3 P1 F1 90.9(3) . 3_566 ? F3 P1 F1 89.1(3) 3_566 3_566 ? F3 P1 F1 89.1(3) . . ? F3 P1 F3 180.0 3_566 . ? H2A N2 H2B 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C1 N2 H2A 109.5 . . ? C1 N2 H2B 109.5 . . ? C1 N2 H2C 109.5 . . ? C4 N1 C5 117.1(4) . . ? C6 C2 C1 121.1(4) . . ? C6 C2 C3 117.8(4) . . ? C3 C2 C1 121.1(4) . . ? N2 C1 C2 112.2(3) . . ? N2 C1 H1A 109.2 . . ? N2 C1 H1B 109.2 . . ? C2 C1 H1A 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C2 C6 H6 120.5 . . ? C2 C6 C5 119.0(4) . . ? C5 C6 H6 120.5 . . ? C2 C3 H3 120.3 . . ? C2 C3 C4 119.3(5) . . ? C4 C3 H3 120.3 . . ? N1 C4 C3 123.4(5) . . ? N1 C4 H4 118.3 . . ? C3 C4 H4 118.3 . . ? N1 C5 C6 123.3(5) . . ? N1 C5 H5 118.3 . . ? C6 C5 H5 118.3 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 F2 1.685(3) . ? P1 F2 1.685(3) 3_566 ? P1 F1 1.663(3) . ? P1 F1 1.663(3) 3_566 ? P1 F3 1.610(4) 3_566 ? P1 F3 1.610(4) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? N2 C1 1.481(5) . ? N1 C4 1.313(7) . ? N1 C5 1.324(7) . ? C2 C1 1.515(5) . ? C2 C6 1.366(6) . ? C2 C3 1.366(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C6 H6 0.9300 . ? C6 C5 1.391(6) . ? C3 H3 0.9300 . ? C3 C4 1.389(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N2 H2A F2 0.89 2.01 2.824(5) 151.6 2_545 yes N2 H2A F1 0.89 2.28 2.842(5) 121.0 2_545 yes N2 H2B F2 0.89 2.50 2.956(5) 112.0 3_566 yes N2 H2B F1 0.89 1.91 2.720(5) 150.2 . yes N2 H2C N1 0.89 1.96 2.846(4) 174.9 1_455 yes C1 H1A F1 0.97 2.60 3.135(6) 114.8 2_545 yes C1 H1B F2 0.97 2.62 3.212(6) 119.3 3_566 yes C3 H3 F3 0.93 2.61 3.335(9) 135.3 4_565 yes C5 H5 F2 0.93 2.63 3.397(6) 140.3 3_666 yes C5 H5 F3 0.93 2.53 3.304(7) 140.4 3_666 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C6 C5 N1 1.9(9) . . . . ? C2 C3 C4 N1 -1.2(10) . . . . ? C1 C2 C6 C5 176.6(5) . . . . ? C1 C2 C3 C4 -176.9(5) . . . . ? C6 C2 C1 N2 92.6(5) . . . . ? C6 C2 C3 C4 3.2(8) . . . . ? C3 C2 C1 N2 -87.2(6) . . . . ? C3 C2 C6 C5 -3.5(8) . . . . ? C4 N1 C5 C6 0.3(9) . . . . ? C5 N1 C4 C3 -0.6(9) . . . . ?