#------------------------------------------------------------------------------ #$Date: 2022-01-16 14:40:05 +0200 (Sun, 16 Jan 2022) $ #$Revision: 272063 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/59/1565986.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_1565986 loop_ _publ_author_name 'Haddaoui, Souhir' 'Ouerghi, Zeineb' 'Arfaoui, Youssef' 'Maris, Thierry' 'Kefi, Riadh' _publ_section_title ; Structural characterization, dielectric properties, optical and theoretical DFT study of (C8H14N2)(BF4)2·H2O compound ; _journal_issue 8 _journal_name_full 'Journal of the Iranian Chemical Society' _journal_page_first 2065 _journal_page_last 2077 _journal_paper_doi 10.1007/s13738-021-02165-4 _journal_volume 18 _journal_year 2021 _chemical_formula_moiety '2(B F4), H2 O, C8 H14 N2' _chemical_formula_sum 'C8 H16 B2 F8 N2 O' _chemical_formula_weight 329.85 _chemical_name_common ; Xylenediaminium bis(tetrafluoroborate) monohydrate ; _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 mixed _atom_sites_solution_primary dual _audit_creation_date 2018-11-27 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 95.105(1) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.4839(2) _cell_length_b 10.9453(3) _cell_length_c 23.0760(6) _cell_measurement_reflns_used 9116 _cell_measurement_temperature 150 _cell_measurement_theta_max 54.932 _cell_measurement_theta_min 3.347 _cell_volume 1379.59(7) _computing_cell_refinement ; SAINT (2013) V8.37A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.' ; _computing_data_collection ; APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_reduction ; SAINT (2013) V8.37A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.' ; _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 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 150 _diffrn_detector 'CMOS Area detector' _diffrn_detector_area_resol_mean 10.24 _diffrn_detector_type 'Bruker Photon 100 CMOS Detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker Venture Metaljet' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_collimation 'Focusing mirrors' _diffrn_radiation_monochromator 'Helios MX Mirror Optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_unetI/netI 0.0193 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 19157 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 54.907 _diffrn_reflns_theta_min 3.346 _diffrn_source 'Metal Jet' _diffrn_source_target Ga _diffrn_source_type 'Gallium Liquid Metal Jet Source' _exptl_absorpt_coefficient_mu 1.008 _exptl_absorpt_correction_T_max 0.5122 _exptl_absorpt_correction_T_min 0.4063 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1188 before and 0.0532 after correction. The Ratio of minimum to maximum transmission is 0.7932. The \l/2 correction factor is Not present.' ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.588 _exptl_crystal_description Block _exptl_crystal_F_000 672 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.446 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.093 _refine_ls_extinction_coef 0.070(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 196 _refine_ls_number_reflns 2619 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.096 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0469 _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^)+(0.0665P)^2^+0.7265P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1170 _refine_ls_wR_factor_ref 0.1177 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2549 _reflns_number_total 2619 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file haddou1.cif _cod_data_source_block haddou1 _cod_database_code 1565986 _shelx_res_file ; haddou1.res created by SHELXL-2014/7 TITL haddou1_a.res in P2(1)/c REM Old TITL haddou1 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.176, Rweak 0.006, Alpha 0.032, Orientation as input REM Formula found by SHELXT: C8 B2 N2 F9 CELL 1.34139 5.4839 10.9453 23.076 90 95.105 90 ZERR 4 0.0002 0.0003 0.0006 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B F N O DISP B 0.0073 0.003 27.2049 DISP C 0.0137 0.0067 57.1 DISP F 0.058 0.0411 317.6292 DISP H -0 0 0.6481 DISP N 0.0241 0.0137 109.9 UNIT 32 64 8 32 8 4 EQIV $1 1+X,+Y,+Z EQIV $2 2-X,0.5+Y,0.5-Z EQIV $3 1-X,0.5+Y,0.5-Z EQIV $4 +X,-1+Y,+Z EQIV $5 1+X,-1+Y,+Z L.S. 30 PLAN 10 SIZE 0.1 0.12 0.24 TEMP -123 HTAB O1 F5_$1 HTAB O1 F8 HTAB N1 O1 HTAB N1 F4_$1 HTAB N1 F8_$2 HTAB N1 F3 HTAB N1 F7_$3 HTAB N2 F5_$1 HTAB N2 F1_$4 HTAB N2 F6 HTAB N2 F4_$5 BOND $H list 4 HTAB CONF fmap 2 acta REM REM REM WGHT 0.066500 0.726500 EXTI 0.070314 FVAR 0.97882 F1 4 0.646640 0.974566 0.428407 11.00000 0.03798 0.02043 = 0.04058 -0.00381 0.00555 -0.00368 F2 4 0.603008 0.775102 0.452613 11.00000 0.04740 0.02926 = 0.05361 0.01462 -0.00199 -0.00191 F3 4 0.745132 0.827588 0.366481 11.00000 0.03926 0.04456 = 0.05617 -0.01500 0.01665 0.00717 F4 4 0.346021 0.859301 0.380513 11.00000 0.02311 0.02456 = 0.06594 0.00486 -0.00397 -0.00028 B1 3 0.585837 0.858857 0.407751 11.00000 0.02132 0.01652 = 0.03655 -0.00015 0.00436 0.00131 F5 4 0.269361 0.228389 0.271868 11.00000 0.03168 0.03654 = 0.03730 0.00099 0.00672 0.00939 F6 4 0.536417 0.091964 0.313659 11.00000 0.03434 0.08194 = 0.04796 0.03295 0.00513 0.01337 F7 4 0.473072 0.101432 0.215504 11.00000 0.03043 0.05660 = 0.04264 -0.01682 0.00680 0.00163 F8 4 0.683339 0.249815 0.264718 11.00000 0.04501 0.05358 = 0.06833 -0.01328 0.02214 -0.02420 B2 3 0.492060 0.168641 0.266391 11.00000 0.01968 0.03533 = 0.02666 0.00299 0.00308 -0.00118 AFIX 6 O1 6 0.996595 0.452891 0.249090 11.00000 0.03143 0.02413 = 0.03219 0.00037 0.00358 0.00020 H1D 2 1.119590 0.405424 0.252946 11.00000 -1.50000 H1E 2 0.875791 0.407653 0.255366 11.00000 -1.50000 AFIX 0 N1 5 1.049020 0.641135 0.332442 11.00000 0.02422 0.02017 = 0.02262 0.00202 0.00315 0.00097 AFIX 137 H1A 2 1.031173 0.581252 0.305036 11.00000 -1.20000 H1B 2 1.145025 0.701735 0.319893 11.00000 -1.20000 H1C 2 0.899447 0.672066 0.338574 11.00000 -1.20000 AFIX 0 N2 5 1.047517 0.072790 0.364296 11.00000 0.02262 0.02010 = 0.02843 -0.00287 0.00558 0.00085 AFIX 137 H2A 2 1.078127 0.119489 0.333132 11.00000 -1.20000 H2B 2 0.883261 0.061126 0.364411 11.00000 -1.20000 H2C 2 1.123295 -0.000790 0.361978 11.00000 -1.20000 AFIX 0 C1 1 1.130997 0.362313 0.400801 11.00000 0.01847 0.02766 = 0.01808 -0.00209 0.00122 0.00045 AFIX 43 H1 2 1.271365 0.352950 0.379870 11.00000 -1.20000 AFIX 0 C2 1 1.034204 0.478290 0.407765 11.00000 0.02298 0.02158 = 0.01781 0.00066 -0.00312 -0.00294 C3 1 0.823819 0.491008 0.437114 11.00000 0.02506 0.02108 = 0.02212 -0.00331 -0.00254 0.00498 AFIX 43 H3 2 0.755277 0.569676 0.441935 11.00000 -1.20000 AFIX 0 C4 1 0.714757 0.388744 0.459255 11.00000 0.01928 0.02965 = 0.02122 -0.00316 0.00235 0.00119 AFIX 43 H4 2 0.569838 0.397572 0.478565 11.00000 -1.20000 AFIX 0 C5 1 0.816076 0.273518 0.453373 11.00000 0.02293 0.02217 = 0.02100 0.00021 -0.00003 -0.00333 AFIX 43 H5 2 0.742539 0.204119 0.469376 11.00000 -1.20000 AFIX 0 C6 1 1.025603 0.259864 0.423985 11.00000 0.02184 0.02022 = 0.01996 -0.00300 -0.00310 0.00283 C7 1 1.166235 0.589193 0.387953 11.00000 0.03311 0.02808 = 0.02561 0.00577 -0.00680 -0.00900 AFIX 23 H7A 2 1.169714 0.652523 0.418647 11.00000 -1.20000 H7B 2 1.337613 0.566794 0.382515 11.00000 -1.20000 AFIX 0 C8 1 1.142429 0.136009 0.419025 11.00000 0.03052 0.02398 = 0.02935 -0.00368 -0.00370 0.00732 AFIX 23 H8A 2 1.322104 0.145696 0.419555 11.00000 -1.20000 H8B 2 1.108129 0.085334 0.452896 11.00000 -1.20000 AFIX 0 HKLF 4 REM haddou1_a.res in P2(1)/c REM R1 = 0.0469 for 2549 Fo > 4sig(Fo) and 0.0475 for all 2619 data REM 196 parameters refined using 0 restraints END WGHT 0.0665 0.7262 REM Instructions for potential hydrogen bonds HTAB O1 F5_$1 HTAB O1 F8 HTAB N1 O1 HTAB N1 F4_$1 HTAB N1 F8_$2 HTAB N1 F3 HTAB N1 F7_$3 HTAB N2 F5_$1 HTAB N2 F1_$4 HTAB N2 F6 HTAB N2 F4_$5 HTAB C7 F7_$2 HTAB C8 F1_$5 REM Highest difference peak 0.446, deepest hole -0.392, 1-sigma level 0.093 Q1 1 0.6135 0.2996 0.2358 11.00000 0.05 0.45 Q2 1 0.9532 0.4857 0.4204 11.00000 0.05 0.34 Q3 1 0.6117 0.1635 0.3185 11.00000 0.05 0.33 Q4 1 0.3342 0.8797 0.4122 11.00000 0.05 0.32 Q5 1 0.9682 0.6852 0.4211 11.00000 0.05 0.30 Q6 1 0.9877 0.7457 0.4471 11.00000 0.05 0.30 Q7 1 0.6486 0.7577 0.4172 11.00000 0.05 0.29 Q8 1 0.3075 0.3162 0.2676 11.00000 0.05 0.29 Q9 1 0.6078 0.3214 0.2792 11.00000 0.05 0.28 Q10 1 0.6618 0.7705 0.3658 11.00000 0.05 0.24 ; _shelx_res_checksum 68554 _shelx_hkl_file ; 1 0 0 3.30 0.40 -1 0 0 3.40 0.40 -1 0 0 2.50 0.40 -2 0 0 321.77 10.80 2 0 0 327.07 10.90 2 0 0 328.97 10.90 -3 0 0 1217.88 38.80 -3 0 0 1182.88 39.30 -3 0 0 1242.78 39.20 -3 0 0 1187.28 39.00 3 0 0 1235.68 39.50 3 0 0 1170.68 39.30 -3 0 0 1194.58 38.80 -3 0 0 1269.77 39.30 -4 0 0 332.47 12.00 -4 0 0 354.76 11.30 -4 0 0 338.07 11.60 4 0 0 347.67 12.20 5 0 0 6.30 1.30 5 0 0 6.10 0.80 -5 0 0 6.20 0.90 -5 0 0 6.20 0.70 -6 0 0 387.36 13.10 -6 0 0 390.16 13.40 6 0 0 408.06 13.90 6 0 0 400.86 13.30 0 -1 0 0.20 0.10 0 -1 0 0.10 0.10 1 -1 0 438.36 14.40 1 -1 0 399.96 13.50 1 -1 0 431.26 13.60 1 1 0 410.06 13.50 -1 1 0 414.96 13.60 -1 1 0 409.16 13.60 2 -1 0 27.00 1.40 2 -1 0 29.80 1.40 2 1 0 26.20 1.40 -2 1 0 25.70 1.40 2 1 0 27.10 1.40 -2 1 0 26.80 1.40 -3 -1 0 52.39 2.40 3 -1 0 50.49 2.50 -3 -1 0 55.89 2.50 -3 -1 0 51.29 2.00 -3 -1 0 52.39 2.10 -3 -1 0 52.39 1.90 3 -1 0 51.09 2.40 -3 1 0 54.59 2.30 3 1 0 53.19 2.60 -3 1 0 50.59 2.10 -3 1 0 51.19 2.50 -3 1 0 53.39 2.00 3 1 0 52.09 2.40 -3 1 0 52.79 2.40 -4 -1 0 84.39 3.10 4 -1 0 70.69 3.60 -4 -1 0 80.09 3.70 -4 -1 0 86.49 3.80 -4 -1 0 86.89 3.30 -4 1 0 81.99 3.60 -4 1 0 83.19 3.30 -4 1 0 86.19 3.10 -4 1 0 94.89 3.90 5 -1 0 413.26 14.00 -5 -1 0 419.46 13.80 -5 -1 0 429.16 14.90 -5 -1 0 439.56 14.20 5 -1 0 399.56 14.60 5 1 0 411.46 14.00 5 1 0 411.16 14.80 -5 1 0 423.26 14.20 -5 1 0 425.86 13.90 6 -1 0 13.80 1.50 6 -1 0 14.70 1.00 -6 -1 0 16.40 1.20 -6 -1 0 13.80 0.90 6 1 0 14.40 1.50 6 1 0 13.40 1.10 -6 1 0 15.80 1.00 -6 1 0 15.20 1.20 0 -2 0 642.24 21.00 0 -2 0 610.24 20.80 0 -2 0 721.13 20.90 0 2 0 634.84 20.80 1 -2 0 1737.83 53.59 1 -2 0 1563.64 52.79 2 -2 0 3755.72 106.59 2 -2 0 3588.14 104.69 2 -2 0 2975.10 104.49 2 2 0 2966.30 104.49 -2 2 0 3106.39 104.79 -2 2 0 3240.28 104.69 -3 -2 0 104.89 4.20 -3 -2 0 103.99 3.70 -3 -2 0 100.09 4.00 3 -2 0 103.79 4.10 -3 -2 0 103.39 3.50 3 -2 0 100.89 3.60 -3 -2 0 100.19 3.50 3 2 0 101.29 4.10 -3 2 0 104.09 3.60 -3 2 0 104.39 3.70 -3 2 0 99.79 3.80 -3 2 0 105.99 4.20 3 2 0 96.29 4.30 -3 2 0 102.09 4.20 -4 -2 0 5.20 0.60 4 -2 0 5.80 0.70 4 -2 0 6.50 1.10 -4 -2 0 4.60 0.70 -4 -2 0 7.50 1.20 -4 2 0 6.10 1.20 4 2 0 7.40 1.40 -4 2 0 6.90 1.40 -4 2 0 4.60 0.60 -4 2 0 7.40 0.80 5 -2 0 55.59 2.40 -5 -2 0 57.19 2.60 -5 -2 0 56.49 2.30 -5 -2 0 55.69 3.20 5 -2 0 59.19 3.00 5 2 0 59.29 3.30 -5 2 0 56.49 2.60 -5 2 0 56.19 2.40 6 -2 0 94.99 3.60 6 -2 0 93.49 4.20 -6 -2 0 101.29 4.70 -6 -2 0 99.49 3.80 6 2 0 94.39 3.80 -6 2 0 97.69 3.90 6 2 0 94.49 4.30 -6 2 0 98.99 3.60 1 -3 0 255.47 8.60 1 -3 0 258.77 9.30 -1 3 0 257.17 8.80 1 3 0 250.77 9.60 -1 3 0 263.27 8.70 -1 3 0 270.57 9.60 -2 -3 0 612.54 20.50 -2 -3 0 599.34 20.20 2 -3 0 623.74 20.60 2 -3 0 653.93 20.60 -2 -3 0 586.24 20.80 2 -3 0 686.13 22.20 2 3 0 622.44 20.50 -2 3 0 629.44 21.00 -2 3 0 612.14 20.30 -2 3 0 664.53 20.80 -3 -3 0 73.89 2.70 -3 -3 0 71.69 3.00 -3 -3 0 77.19 3.40 3 -3 0 70.79 2.60 -3 -3 0 67.99 2.50 3 -3 0 70.59 3.10 -3 -3 0 71.69 2.60 -3 3 0 67.09 2.80 -3 3 0 70.19 3.30 -3 3 0 75.19 2.80 3 3 0 68.09 4.30 -3 3 0 72.29 3.40 -4 -3 0 3.10 0.60 -4 -3 0 3.40 0.40 -4 -3 0 3.90 0.90 -4 3 0 3.50 0.70 -4 3 0 3.80 0.60 -5 -3 0 99.89 4.70 5 -3 0 102.69 4.40 -5 -3 0 100.69 3.90 5 -3 0 102.19 3.70 -5 -3 0 99.09 3.60 -5 3 0 101.59 3.80 -5 3 0 89.39 3.90 5 3 0 91.29 4.60 -5 3 0 103.09 4.00 -6 -3 0 0.70 0.90 6 -3 0 1.10 0.40 -6 -3 0 0.60 0.30 6 -3 0 0.70 0.60 6 3 0 0.90 0.50 -6 3 0 0.70 0.40 -6 3 0 1.20 0.40 0 -4 0 282.07 9.80 0 4 0 254.17 8.80 0 4 0 282.17 9.70 0 4 0 250.17 8.90 1 -4 0 461.95 16.10 -1 -4 0 471.45 15.20 1 -4 0 470.35 15.20 -1 -4 0 445.86 15.30 1 4 0 486.15 16.70 -1 4 0 462.75 15.40 1 4 0 477.65 15.20 -1 4 0 464.45 15.60 -1 4 0 471.45 16.50 -2 -4 0 837.62 27.40 2 -4 0 827.62 26.50 2 -4 0 838.92 28.50 -2 -4 0 842.92 26.90 -2 -4 0 826.52 26.50 2 4 0 815.72 27.00 -2 4 0 825.02 27.20 -2 4 0 828.12 26.60 2 4 0 812.32 29.10 -2 4 0 828.72 27.50 3 -4 0 1564.94 52.29 -3 -4 0 1639.64 51.39 -3 -4 0 1633.64 52.19 -3 -4 0 1614.44 51.59 3 -4 0 1636.64 51.49 -3 4 0 1604.34 52.39 -3 4 0 1616.34 51.59 -3 4 0 1613.54 52.69 3 4 0 1629.84 55.49 -3 4 0 1530.15 51.79 4 -4 0 14.30 0.90 4 -4 0 14.40 1.30 -4 -4 0 16.80 1.60 -4 -4 0 13.50 1.70 -4 -4 0 12.10 1.00 -4 4 0 12.20 1.00 -4 4 0 12.40 1.10 -4 4 0 14.00 2.30 4 4 0 15.50 1.80 5 -4 0 413.86 13.50 -5 -4 0 415.06 13.80 5 -4 0 425.16 14.30 -5 -4 0 396.36 14.70 -5 -4 0 406.06 14.50 5 4 0 412.76 14.70 -5 4 0 410.26 13.80 -5 4 0 394.36 13.90 -5 4 0 413.46 13.70 6 -4 0 26.00 1.80 6 -4 0 25.00 1.30 -6 -4 0 25.20 2.10 -6 4 0 27.30 1.40 6 4 0 26.40 1.50 -6 4 0 24.50 1.50 0 -5 0 0.10 0.50 0 5 0 0.00 0.20 0 5 0 0.70 0.60 0 5 0 0.20 0.30 1 -5 0 0.50 0.30 1 -5 0 0.40 0.60 -1 -5 0 -0.70 0.60 1 -5 0 0.70 0.40 -1 -5 0 1.00 0.30 1 5 0 0.40 0.30 -1 5 0 0.40 0.40 -1 5 0 0.40 0.60 -1 5 0 0.50 0.40 2 -5 0 1151.58 35.10 -2 -5 0 1056.79 34.60 -2 -5 0 1138.09 34.80 -2 -5 0 1016.60 34.80 -2 -5 0 1086.39 35.00 -2 -5 0 936.01 34.80 2 -5 0 1144.39 36.80 -2 -5 0 1025.50 35.50 2 -5 0 1074.49 34.60 2 5 0 1069.59 35.20 -2 5 0 1054.79 34.70 -2 5 0 1134.39 35.50 2 5 0 1189.18 37.90 -2 5 0 1068.19 35.80 3 -5 0 390.56 12.40 3 -5 0 397.96 13.00 -3 -5 0 369.66 13.40 -3 -5 0 371.16 12.50 -3 -5 0 381.96 13.00 -3 5 0 379.46 12.50 -3 5 0 373.86 13.80 -3 5 0 374.76 13.50 -3 5 0 369.06 12.50 3 5 0 387.16 16.30 4 -5 0 995.40 33.70 -4 -5 0 985.60 33.10 4 -5 0 1018.20 32.90 -4 -5 0 1007.80 34.10 -4 -5 0 1025.20 33.80 -4 5 0 1018.60 33.10 -4 5 0 1050.39 33.50 4 5 0 1118.39 34.40 -4 5 0 986.10 33.10 5 -5 0 106.99 4.60 -5 -5 0 108.29 5.00 5 -5 0 109.89 3.90 -5 -5 0 109.09 4.80 -5 -5 0 115.09 4.10 5 5 0 90.49 6.00 -5 5 0 107.29 4.10 -5 5 0 103.99 4.30 -5 5 0 110.69 4.10 -6 -5 0 316.37 11.70 6 -5 0 317.47 10.60 6 -5 0 317.87 11.30 -6 5 0 315.07 10.70 6 5 0 335.37 10.90 -6 5 0 316.67 10.70 0 -6 0 777.22 25.30 0 -6 0 738.13 24.10 0 -6 0 728.93 24.30 0 -6 0 723.23 24.70 0 6 0 767.92 24.80 0 6 0 724.23 25.70 0 6 0 794.62 24.50 1 -6 0 60.89 2.30 1 -6 0 72.89 3.70 1 -6 0 53.29 2.70 -1 -6 0 66.99 2.60 1 -6 0 65.69 2.60 -1 6 0 64.59 2.40 1 6 0 71.49 2.80 -1 6 0 68.89 3.20 -1 6 0 58.99 2.80 1 6 0 68.29 2.50 1 6 0 52.99 3.80 -2 -6 0 253.77 10.00 2 -6 0 266.17 8.70 -2 -6 0 259.27 9.20 -2 6 0 267.37 8.80 2 6 0 272.67 9.00 2 6 0 261.07 11.60 -2 6 0 281.37 10.20 -2 6 0 263.87 9.60 3 -6 0 7.60 0.60 -3 -6 0 6.70 1.40 3 -6 0 9.00 1.10 -3 6 0 8.30 2.00 -3 6 0 7.00 1.40 -3 6 0 8.20 0.80 3 6 0 8.50 3.20 -4 -6 0 198.58 7.70 -4 -6 0 190.58 7.30 4 -6 0 183.98 7.20 4 -6 0 191.38 6.40 -4 6 0 194.08 6.60 4 6 0 170.58 7.70 -4 6 0 183.68 7.00 -4 6 0 191.48 6.60 5 -6 0 13.10 0.80 -5 -6 0 14.10 1.70 5 -6 0 14.70 1.50 -5 -6 0 12.00 1.60 -5 6 0 12.80 1.00 -5 6 0 12.40 1.20 -5 6 0 15.00 1.30 0 -7 0 0.30 0.80 0 -7 0 0.30 0.50 0 -7 0 0.10 0.30 0 -7 0 0.30 0.30 0 7 0 0.60 0.50 0 7 0 0.90 0.60 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2.30 -4 -2 22 33.90 1.80 4 -2 -22 34.40 1.90 4 -2 -22 35.70 1.50 4 2 -22 35.10 1.60 -4 2 22 35.20 1.90 4 2 -22 34.20 1.80 3 -2 -22 0.50 0.30 3 -2 -22 1.30 0.60 -3 -2 22 -0.10 0.50 3 2 -22 0.60 0.30 -3 2 22 0.30 0.40 -3 2 22 1.20 0.60 -2 -2 22 496.85 16.60 2 -2 -22 486.55 16.80 2 -2 -22 486.85 16.20 2 2 -22 466.95 16.40 -2 2 22 506.15 16.40 2 2 -22 494.85 16.20 -2 2 22 507.25 16.70 -1 -2 22 31.50 1.90 1 -2 -22 29.60 1.90 -1 -2 22 30.20 1.60 1 -2 -22 30.60 1.50 1 2 -22 31.30 1.50 -1 2 22 30.40 1.80 -1 2 22 31.10 1.70 0 -2 22 477.35 15.80 0 -2 22 468.15 16.50 0 -2 22 493.05 17.20 0 -2 -22 476.15 15.70 0 -2 -22 476.35 16.10 0 -2 -22 453.05 15.80 0 2 22 469.85 15.80 0 2 -22 482.55 16.00 0 2 -22 485.85 15.70 0 2 22 482.95 15.90 1 -2 22 120.69 4.50 -1 -2 -22 120.59 5.00 1 -2 22 114.29 5.20 -1 -2 -22 104.29 4.90 -1 -2 -22 123.99 4.40 1 -2 22 121.89 5.70 1 2 22 122.49 5.20 -1 2 -22 119.59 4.80 -2 -2 -22 130.29 5.10 -2 -2 -22 130.49 5.00 -2 -2 -22 133.09 4.80 2 -2 22 132.79 4.90 2 2 22 124.49 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224.48 7.80 4 -2 -23 212.28 7.30 4 2 -23 218.78 7.40 -4 2 23 213.78 7.70 4 2 -23 219.98 7.60 3 -2 -23 56.39 2.30 3 -2 -23 56.69 2.70 -3 -2 23 55.79 2.70 3 2 -23 59.19 2.60 -3 2 23 59.89 2.70 -3 2 23 57.79 2.40 3 2 -23 58.09 2.30 -2 -2 23 22.90 1.60 2 -2 -23 24.20 1.30 2 -2 -23 24.40 1.60 -2 -2 23 22.90 1.30 -2 2 23 23.60 1.40 2 2 -23 23.40 1.30 -2 2 23 22.00 1.50 1 -2 -23 0.60 0.50 -1 -2 23 0.70 0.50 1 -2 -23 0.70 0.30 -1 -2 23 0.50 0.40 1 -2 -23 1.00 0.50 1 2 -23 0.30 0.30 -1 2 23 0.40 0.50 -1 2 23 0.90 0.40 0 -2 23 -0.10 0.40 0 -2 23 0.10 0.70 0 -2 23 0.10 0.80 0 -2 -23 0.50 0.30 0 -2 -23 0.40 0.50 0 -2 -23 0.10 0.40 0 2 -23 0.10 0.40 0 2 -23 0.90 0.40 0 2 23 0.10 0.40 0 2 23 -0.60 0.90 1 -2 23 298.57 10.30 -1 -2 -23 297.57 10.40 -1 -2 -23 299.47 10.60 -1 -2 -23 302.87 10.20 1 2 23 309.47 10.30 -1 2 -23 305.07 10.20 -1 2 -23 310.17 10.60 2 -2 23 1.80 0.50 -2 -2 -23 2.30 0.50 -2 -2 -23 1.30 0.40 -2 -2 -23 2.90 0.80 -2 2 -23 2.00 0.50 -2 2 -23 2.60 0.50 -2 2 -23 3.40 0.80 2 2 23 2.50 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2.40 3 -5 -23 0.70 0.40 3 -5 -23 -0.90 1.40 3 5 -23 0.10 0.30 -3 5 23 0.50 0.50 -3 5 23 0.40 0.40 2 -5 -23 0.20 0.40 2 -5 -23 1.00 0.50 -2 -5 23 0.00 0.70 -2 -5 23 1.30 0.50 2 -5 -23 0.50 1.50 -2 -5 23 0.00 0.70 -2 5 23 0.40 0.40 -2 5 23 0.20 0.50 2 5 -23 0.10 0.30 -1 -5 23 303.07 11.80 1 -5 -23 290.47 11.80 1 -5 -23 294.47 10.50 1 -5 -23 292.27 9.90 -1 -5 23 300.07 10.10 -1 -5 23 290.27 11.00 1 5 -23 304.17 9.90 -1 5 23 294.27 10.20 -1 5 23 301.57 10.20 0 -5 23 3.80 1.10 0 -5 -23 3.10 0.50 0 -5 -23 3.90 0.90 0 -5 23 4.50 0.70 0 -5 23 2.30 0.90 0 5 -23 3.70 0.80 0 5 -23 2.70 0.50 0 5 23 2.70 0.60 -1 -5 -23 1.30 0.40 -1 -5 -23 1.10 0.60 1 -5 23 0.80 0.50 -1 5 -23 0.60 0.40 1 5 23 0.70 0.40 1 5 23 0.90 1.00 -2 -5 -23 40.30 2.10 -2 -5 -23 38.70 1.70 -2 5 -23 40.00 1.80 -2 5 -23 39.90 2.10 2 5 23 41.50 1.90 2 5 23 34.40 2.70 2 -6 -23 15.80 1.30 -2 -6 23 13.90 1.80 -2 -6 23 15.50 2.20 2 -6 -23 17.70 2.80 -2 6 23 16.30 1.30 -2 6 23 17.70 1.20 2 6 -23 15.50 1.00 1 -6 -23 24.00 1.30 -1 -6 23 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-3 3 24 95.79 3.60 -2 -3 24 47.80 2.10 2 -3 -24 46.50 2.00 2 -3 -24 44.40 4.50 2 -3 -24 48.20 2.40 -2 3 24 50.69 2.20 -2 3 24 45.30 2.30 2 3 -24 46.60 2.00 -1 -3 24 115.89 5.80 1 -3 -24 120.79 4.80 -1 -3 24 115.49 5.20 1 -3 -24 123.39 4.40 -1 -3 24 126.79 4.50 1 3 -24 118.89 4.30 -1 3 24 120.99 4.60 -1 3 24 119.79 4.50 0 -3 24 174.48 7.50 0 -3 -24 164.88 5.90 0 -3 24 151.28 6.70 0 -3 -24 172.08 6.40 0 -3 24 173.88 6.10 0 3 -24 175.08 6.30 0 3 24 171.08 6.10 0 3 -24 168.38 5.90 0 3 24 168.38 6.20 -1 -3 -24 68.89 2.70 -1 -3 -24 67.09 3.10 1 -3 24 70.99 2.90 -1 3 -24 66.79 3.10 -1 3 -24 67.79 2.70 1 3 24 69.39 2.80 -2 -3 -24 0.30 0.30 2 -3 24 -0.40 0.40 -2 -3 -24 -0.60 0.60 2 3 24 0.50 0.50 -2 3 -24 -0.10 0.40 -2 3 -24 1.00 0.50 -2 3 -24 0.20 0.40 3 -4 -24 33.20 3.60 3 -4 -24 32.00 1.40 3 -4 -24 33.50 1.80 3 4 -24 31.40 1.40 -3 4 24 28.00 1.70 -3 4 24 29.70 1.50 -2 -4 24 378.16 14.20 -2 -4 24 369.46 12.50 2 -4 -24 379.26 14.40 2 -4 -24 388.36 12.40 -2 -4 24 350.36 13.30 2 -4 -24 381.46 12.90 -2 4 24 378.36 12.60 2 4 -24 373.56 12.40 -2 4 24 368.36 12.70 -1 -4 24 28.10 2.60 -1 -4 24 22.40 1.30 1 -4 -24 24.10 1.20 1 -4 -24 27.00 1.70 -1 -4 24 21.50 2.10 -1 4 24 23.90 1.60 -1 4 24 20.10 1.40 1 4 -24 23.70 1.30 0 -4 24 66.49 2.80 0 -4 24 59.89 3.50 0 -4 24 67.39 4.10 0 -4 -24 69.69 3.10 0 -4 -24 65.29 2.60 0 4 -24 65.79 2.60 0 4 24 64.99 2.80 0 4 -24 70.89 3.00 -1 -4 -24 44.00 2.30 -1 -4 -24 43.20 1.90 1 -4 24 40.10 2.00 1 4 24 41.80 2.00 -1 4 -24 46.20 2.30 -1 4 -24 41.70 1.80 -2 -4 -24 2.30 0.70 -2 -4 -24 3.30 0.60 -2 4 -24 4.30 0.80 -2 4 -24 4.30 0.70 2 4 24 3.00 0.60 -2 -5 24 -0.30 0.50 -2 -5 24 0.30 0.80 2 -5 -24 -0.30 1.60 2 -5 -24 0.60 0.50 -2 -5 24 0.50 0.90 2 -5 -24 0.40 0.40 -2 5 24 -0.10 0.50 2 5 -24 0.80 0.40 -2 5 24 0.90 0.40 -1 -5 24 8.70 2.00 1 -5 -24 10.80 1.20 -1 -5 24 8.30 1.60 1 -5 -24 7.90 2.20 -1 -5 24 8.90 0.90 1 -5 -24 8.80 0.80 -1 5 24 8.60 0.90 1 5 -24 8.60 0.90 -1 5 24 8.70 1.20 1 5 -24 9.00 0.90 0 -5 -24 53.99 2.70 0 -5 24 51.09 3.20 0 -5 -24 50.59 2.20 0 -5 24 51.69 3.60 0 -5 24 55.89 2.40 0 5 -24 53.09 2.20 0 5 -24 56.19 2.60 0 5 24 53.19 2.40 -1 -5 -24 1.70 0.40 1 -5 24 1.80 0.50 1 5 24 1.90 0.50 -1 5 -24 2.00 0.50 2 -6 -24 16.50 2.90 2 -6 -24 17.30 1.30 2 6 -24 16.50 1.10 -2 6 24 16.30 1.30 -2 6 24 16.60 1.10 1 -6 -24 7.60 1.10 1 -6 -24 8.80 0.80 1 -6 -24 6.30 2.00 -1 -6 24 6.50 2.00 -1 6 24 10.00 0.90 1 6 -24 8.10 0.90 0 -6 -24 0.00 0.40 0 -6 -24 0.20 0.50 0 6 24 0.20 0.40 0 6 -24 0.30 0.40 -1 -6 -24 2.30 0.70 -1 -6 -24 1.70 0.40 1 6 24 1.70 0.50 -1 6 -24 1.50 0.50 3 0 -25 -0.20 0.50 3 0 -25 0.20 0.30 -3 0 25 0.70 0.50 -3 0 25 0.10 0.50 -2 0 25 0.10 0.40 -2 0 25 0.60 0.50 2 0 -25 0.00 0.50 1 0 -25 -0.20 0.30 -1 0 25 -0.30 0.50 1 0 -25 0.30 0.60 1 0 -25 0.60 0.40 -1 0 25 0.00 0.40 0 0 -25 1.00 0.40 0 0 -25 0.50 0.40 0 0 25 0.30 0.40 1 0 25 0.20 0.40 -1 0 -25 -0.20 0.30 2 0 25 -0.10 0.40 -2 0 -25 0.30 0.40 -2 0 -25 0.10 0.30 3 -1 -25 71.29 2.70 3 -1 -25 67.09 3.00 -3 -1 25 69.59 3.00 -3 1 25 69.69 2.70 3 1 -25 69.39 2.70 3 1 -25 64.09 2.90 -3 1 25 69.79 3.00 2 -1 -25 23.50 1.60 -2 -1 25 23.80 1.60 2 -1 -25 23.60 1.30 -2 -1 25 25.30 1.40 2 1 -25 24.00 1.70 -2 1 25 23.80 1.60 -2 1 25 23.70 1.30 2 1 -25 27.50 1.40 1 -1 -25 8.20 0.80 -1 -1 25 9.00 0.90 1 -1 -25 8.80 0.90 -1 -1 25 8.10 1.10 -1 -1 25 8.40 1.60 -1 -1 25 7.30 2.10 1 -1 -25 7.20 1.10 -1 1 25 8.00 1.10 -1 1 25 7.50 0.80 1 1 -25 8.20 0.90 1 1 -25 8.00 0.80 0 -1 -25 22.30 1.70 0 -1 -25 23.10 1.30 0 -1 -25 22.90 1.50 0 -1 25 25.60 1.40 0 1 -25 23.20 1.50 0 1 25 23.60 1.40 0 1 -25 23.60 1.30 -1 -1 -25 6.20 0.70 -1 -1 -25 4.30 0.90 1 -1 25 5.90 0.80 1 1 25 5.70 0.80 -1 1 -25 4.80 0.70 -1 1 -25 4.60 0.80 -2 -1 -25 3.20 0.60 2 -1 25 4.60 0.80 -2 -1 -25 2.70 0.50 2 1 25 2.80 0.50 -2 1 -25 3.90 0.80 3 -2 -25 66.39 2.50 -3 -2 25 66.59 2.90 3 -2 -25 67.39 2.90 -3 2 25 62.49 2.60 -3 2 25 63.99 2.90 3 2 -25 65.79 2.60 -2 -2 25 75.09 3.00 2 -2 -25 78.79 3.30 -2 -2 25 77.19 3.30 2 -2 -25 69.59 3.00 2 -2 -25 76.99 2.90 -2 2 25 74.29 3.00 -2 2 25 75.59 3.20 2 2 -25 77.29 2.90 1 -2 -25 140.79 5.40 -1 -2 25 145.49 5.20 -1 -2 25 137.19 5.90 1 -2 -25 138.39 5.20 -1 -2 25 138.79 6.50 1 -2 -25 142.89 5.10 -1 2 25 142.79 5.20 1 2 -25 141.39 5.00 -1 2 25 146.29 5.30 0 -2 -25 74.39 3.30 0 -2 -25 69.29 3.00 0 -2 -25 71.39 2.90 0 -2 25 73.49 3.00 0 2 -25 73.49 2.90 0 2 -25 72.89 3.20 0 2 25 74.49 3.00 1 -2 25 10.60 0.90 -1 -2 -25 8.30 1.20 -1 -2 -25 7.60 1.00 -1 -2 -25 10.10 0.80 1 2 25 9.70 0.90 -1 2 -25 9.00 0.80 -1 2 -25 10.00 1.10 -2 -2 -25 10.40 0.80 2 -2 25 9.30 0.90 -2 -2 -25 9.80 1.10 -2 2 -25 10.20 1.10 2 2 25 10.30 1.00 -2 2 -25 9.80 0.90 3 -3 -25 6.10 2.60 3 -3 -25 9.40 0.80 3 -3 -25 9.00 1.00 -3 3 25 8.30 0.80 -3 3 25 10.40 1.00 3 3 -25 8.60 0.80 -2 -3 25 13.60 2.20 2 -3 -25 14.00 1.30 2 -3 -25 12.90 0.90 -2 -3 25 11.80 1.00 -2 -3 25 10.70 1.70 -2 3 25 12.90 1.20 -2 3 25 12.50 1.00 2 3 -25 12.40 0.90 1 -3 -25 11.70 1.20 1 -3 -25 12.20 0.90 -1 -3 25 10.50 0.90 -1 -3 25 10.80 2.10 -1 3 25 9.00 1.10 1 3 -25 9.10 0.90 -1 3 25 8.50 0.90 0 -3 -25 4.90 0.70 0 -3 25 3.10 1.20 0 -3 25 5.10 0.80 0 -3 -25 3.50 0.80 0 -3 25 4.50 1.30 0 3 -25 5.30 0.70 0 3 -25 4.00 0.80 0 3 25 4.80 0.70 -1 -3 -25 35.70 2.00 -1 -3 -25 35.10 1.60 1 -3 25 35.60 1.80 -1 3 -25 36.60 2.00 1 3 25 35.90 1.80 -1 3 -25 34.40 1.60 2 -3 25 70.09 2.80 -2 -3 -25 68.99 2.70 -2 3 -25 64.49 2.70 -2 3 -25 72.19 3.00 2 3 25 72.19 2.80 -2 3 -25 64.29 2.60 -2 -4 25 152.58 7.00 -2 -4 25 163.68 7.80 -2 -4 25 166.48 5.80 2 -4 -25 166.28 5.80 2 -4 -25 178.78 8.50 2 -4 -25 169.38 6.30 -2 4 25 166.18 6.10 2 4 -25 169.98 5.80 -2 4 25 171.18 6.00 -1 -4 25 70.39 4.20 1 -4 -25 72.49 3.20 -1 -4 25 63.69 3.60 1 -4 -25 74.09 2.80 -1 -4 25 73.89 2.90 1 4 -25 72.79 3.10 -1 4 25 72.89 3.00 1 4 -25 70.89 2.80 -1 4 25 70.19 2.90 0 -4 25 12.30 1.00 0 -4 -25 13.80 1.30 0 -4 25 13.90 2.30 0 -4 -25 12.70 0.90 0 -4 25 12.30 2.00 0 4 -25 13.80 1.00 0 4 25 11.80 1.00 0 4 -25 13.00 1.20 -1 -4 -25 88.99 3.40 1 -4 25 88.49 3.60 -1 -4 -25 95.09 3.90 1 4 25 91.99 3.50 -1 4 -25 92.49 3.40 -1 4 -25 96.59 3.80 2 -5 -25 3.10 2.00 2 -5 -25 2.70 0.40 2 -5 -25 3.40 0.80 2 5 -25 2.70 0.50 -2 5 25 2.70 0.70 -2 5 25 2.60 0.50 -1 -5 25 23.30 1.40 1 -5 -25 23.40 1.60 1 -5 -25 23.40 1.20 1 5 -25 23.00 1.30 -1 5 25 22.50 1.60 -1 5 25 23.90 1.40 1 5 -25 25.80 1.50 0 -5 -25 37.60 2.10 0 -5 25 39.00 1.90 0 -5 -25 35.00 1.60 0 5 -25 35.90 1.70 0 5 -25 37.80 2.00 0 5 25 35.40 1.80 -1 -5 -25 39.10 2.10 1 -5 25 35.80 1.80 -1 -5 -25 36.90 1.60 1 5 25 37.20 1.80 -1 5 -25 40.30 2.00 1 -6 -25 114.89 4.70 1 6 -25 118.09 4.50 -1 6 25 121.29 4.40 0 -6 -25 123.09 4.80 0 -6 -25 119.49 4.30 0 6 -25 125.69 4.70 0 6 25 124.99 4.50 3 0 -26 39.40 2.00 -3 0 26 38.10 2.00 3 0 -26 37.90 1.70 -3 0 26 35.40 1.80 2 0 -26 183.28 6.40 -2 0 26 188.48 6.70 -2 0 26 186.98 6.40 2 0 -26 176.88 6.60 1 0 -26 95.89 4.50 -1 0 26 96.69 3.70 1 0 -26 99.09 3.70 -1 0 26 96.39 4.00 1 0 -26 96.79 3.80 0 0 -26 0.90 0.40 0 0 26 0.20 0.40 0 0 -26 0.50 0.40 -1 0 -26 220.48 7.70 -1 0 -26 226.08 8.00 1 0 26 232.08 7.80 -2 0 -26 160.58 5.90 2 0 26 165.18 5.70 -2 0 -26 158.88 5.60 3 -1 -26 23.30 1.20 -3 -1 26 23.90 1.50 3 -1 -26 25.00 1.60 -3 1 26 25.60 1.50 3 1 -26 25.10 1.30 3 1 -26 20.90 1.70 -2 -1 26 8.20 1.00 2 -1 -26 8.60 0.90 2 -1 -26 9.70 1.20 -2 -1 26 10.10 0.90 2 -1 -26 10.50 0.80 -2 1 26 10.20 0.90 2 1 -26 11.30 0.90 -2 1 26 11.30 1.10 1 -1 -26 18.70 1.30 1 -1 -26 17.50 1.40 -1 -1 26 19.10 1.20 1 -1 -26 20.10 1.20 -1 1 26 17.90 1.20 -1 1 26 19.20 1.40 1 1 -26 18.70 1.30 1 1 -26 19.40 1.10 0 -1 -26 11.00 1.10 0 -1 -26 8.60 1.30 0 -1 26 10.60 0.90 0 -1 -26 9.40 0.90 0 1 26 8.70 0.90 0 1 -26 8.10 0.80 0 1 -26 9.50 1.00 -1 -1 -26 36.50 1.80 -1 -1 -26 32.80 1.60 1 -1 26 36.00 1.70 -1 1 -26 37.10 1.90 -1 1 -26 33.20 1.60 1 1 26 35.00 1.70 -2 -2 26 30.50 1.50 2 -2 -26 27.10 1.40 2 -2 -26 29.40 1.80 2 2 -26 27.40 1.40 -2 2 26 29.20 1.70 -2 2 26 29.50 1.50 1 -2 -26 504.25 16.90 -1 -2 26 494.95 18.20 -1 -2 26 466.75 17.40 -1 -2 26 511.75 16.60 1 -2 -26 495.65 16.50 1 2 -26 510.15 16.90 -1 2 26 517.55 16.80 1 2 -26 516.25 16.50 -1 2 26 512.25 16.70 0 -2 26 227.38 7.70 0 -2 -26 207.18 7.70 0 -2 -26 216.48 7.90 0 -2 -26 221.18 7.60 0 2 26 228.58 7.70 0 2 -26 224.28 7.60 0 2 -26 229.08 8.00 1 -2 26 0.10 0.40 -1 -2 -26 0.30 0.30 -1 -2 -26 1.20 0.80 -1 -2 -26 -0.20 0.50 1 2 26 0.40 0.40 -1 2 -26 -0.20 0.40 -1 2 -26 -0.20 0.40 -2 -3 26 4.10 0.80 2 -3 -26 5.90 1.00 2 -3 -26 5.10 0.60 -2 3 26 5.80 0.90 2 3 -26 5.90 0.70 -2 3 26 5.00 0.70 -1 -3 26 101.89 5.20 1 -3 -26 112.79 4.60 -1 -3 26 118.19 4.30 -1 -3 26 114.19 6.30 1 -3 -26 118.29 4.20 1 3 -26 120.39 4.50 1 3 -26 115.89 4.20 -1 3 26 116.69 4.30 -1 3 26 118.09 4.40 0 -3 26 0.70 0.40 0 -3 -26 -0.10 0.30 0 -3 -26 0.10 0.50 0 3 26 1.00 0.40 0 3 -26 0.60 0.40 0 3 -26 0.10 0.40 1 -3 26 31.90 1.60 -1 -3 -26 31.50 1.90 -1 -3 -26 29.70 1.50 -1 3 -26 30.80 1.50 -1 3 -26 32.70 1.80 1 3 26 31.00 1.60 -2 -4 26 1.10 0.70 2 -4 -26 1.40 0.40 -2 4 26 1.00 0.40 -2 4 26 1.30 0.60 2 4 -26 2.30 0.40 1 -4 -26 0.20 0.50 1 -4 -26 0.50 0.30 -1 -4 26 0.40 0.40 -1 4 26 0.40 0.40 1 4 -26 0.10 0.40 -1 4 26 1.10 0.70 1 4 -26 0.10 0.40 0 -4 -26 28.80 1.40 0 -4 26 30.10 1.60 0 -4 -26 30.50 1.80 0 4 -26 28.10 1.40 0 4 26 29.90 1.50 0 4 -26 29.80 1.70 -1 -4 -26 10.40 1.20 -1 -4 -26 11.00 0.80 1 -4 26 11.40 1.00 -1 4 -26 10.10 1.10 -1 4 -26 11.10 1.00 1 4 26 11.60 1.00 -1 -5 26 46.30 2.10 1 -5 -26 46.70 2.30 1 -5 -26 45.80 1.90 1 5 -26 45.80 2.20 -1 5 26 48.10 2.10 0 -5 26 42.70 2.00 0 -5 -26 43.10 1.80 2 0 -27 -0.20 0.80 2 0 -27 0.30 0.40 2 0 -27 0.10 0.30 -2 0 27 -0.40 0.40 -2 0 27 1.00 0.50 -1 0 27 -0.10 0.40 1 0 -27 -0.40 0.40 1 0 -27 -0.10 0.30 0 0 27 0.10 0.40 0 0 -27 -0.20 0.30 0 0 -27 0.50 0.40 -1 0 -27 -0.10 0.40 -1 0 -27 0.60 0.40 1 0 27 0.40 0.40 2 -1 -27 41.30 2.00 2 -1 -27 38.80 1.80 2 -1 -27 37.60 1.70 -2 -1 27 38.00 1.70 2 1 -27 36.90 1.70 -2 1 27 39.40 2.00 -2 1 27 37.30 1.70 1 -1 -27 0.30 0.40 1 -1 -27 -0.20 0.70 1 -1 -27 -0.10 0.30 -1 -1 27 0.00 0.40 1 1 -27 -0.40 0.30 -1 1 27 0.10 0.40 1 1 -27 -0.10 0.40 0 -1 27 14.80 1.10 0 -1 -27 14.90 1.20 0 -1 -27 16.70 1.00 0 1 27 16.50 1.10 0 1 -27 15.80 1.00 0 1 -27 16.20 1.20 -1 -1 -27 27.80 1.40 -1 -1 -27 30.00 1.60 1 -1 27 30.30 1.50 -1 1 -27 29.00 1.40 -1 1 -27 30.70 1.70 1 1 27 30.00 1.50 2 -2 -27 0.90 0.30 2 -2 -27 1.00 0.60 -2 -2 27 1.10 0.50 -2 2 27 0.70 0.40 2 2 -27 0.80 0.40 -2 2 27 1.30 0.50 1 -2 -27 60.79 2.40 1 -2 -27 57.69 2.70 -1 -2 27 60.59 2.50 -1 2 27 58.59 2.70 -1 2 27 62.29 2.50 1 2 -27 58.89 2.40 1 2 -27 58.79 2.60 0 -2 -27 2.70 0.80 0 -2 27 4.30 0.70 0 -2 -27 2.30 0.50 0 2 -27 4.30 0.80 0 2 -27 3.70 0.50 0 2 27 5.20 0.80 -1 -2 -27 1.60 0.40 -1 2 -27 1.70 0.50 -1 2 -27 1.10 0.40 1 2 27 2.20 0.50 1 -3 -27 39.50 1.70 -1 -3 27 40.10 1.80 1 -3 -27 40.10 2.10 -1 3 27 39.40 2.10 1 3 -27 41.40 2.00 -1 3 27 40.60 1.80 1 3 -27 38.50 1.80 0 -3 -27 29.10 1.80 0 -3 -27 27.60 1.40 0 -3 27 29.80 1.50 0 3 27 27.40 1.50 0 3 -27 28.10 1.60 0 3 -27 26.60 1.40 -1 0 28 2.50 0.50 1 0 -28 1.60 0.40 1 0 -28 1.10 0.40 0 0 -28 3.90 0.80 0 0 28 4.40 0.70 0 0 -28 5.60 0.70 -1 -1 28 3.60 0.70 1 -1 -28 2.60 0.50 1 -1 -28 3.60 0.90 1 1 -28 4.10 0.60 1 1 -28 4.00 0.80 -1 1 28 3.90 0.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 95196 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 '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 F1 F 0.64664(18) 0.97457(9) 0.42841(4) 0.0329(3) Uani 1 1 d . . . . . F2 F 0.6030(2) 0.77510(10) 0.45261(5) 0.0438(3) Uani 1 1 d . . . . . F3 F 0.7451(2) 0.82759(11) 0.36648(5) 0.0459(3) Uani 1 1 d . . . . . F4 F 0.34602(18) 0.85930(9) 0.38051(5) 0.0383(3) Uani 1 1 d . . . . . B1 B 0.5858(3) 0.85886(15) 0.40775(8) 0.0247(4) Uani 1 1 d . . . . . F5 F 0.26936(18) 0.22839(10) 0.27187(4) 0.0350(3) Uani 1 1 d . . . . . F6 F 0.5364(2) 0.09196(14) 0.31366(5) 0.0547(4) Uani 1 1 d . . . . . F7 F 0.47307(19) 0.10143(12) 0.21550(5) 0.0430(3) Uani 1 1 d . . . . . F8 F 0.6833(2) 0.24981(12) 0.26472(6) 0.0546(4) Uani 1 1 d . . . . . B2 B 0.4921(3) 0.16864(19) 0.26639(8) 0.0272(4) Uani 1 1 d . . . . . O1 O 0.9966(2) 0.45289(11) 0.24909(5) 0.0292(3) Uani 1 1 d . . . . . H1D H 1.1196 0.4054 0.2529 0.044 Uiso 1 1 d G . . . . H1E H 0.8758 0.4077 0.2554 0.044 Uiso 1 1 d G . . . . N1 N 1.0490(2) 0.64114(11) 0.33244(5) 0.0223(3) Uani 1 1 d . . . . . H1A H 1.0312 0.5813 0.3050 0.027 Uiso 1 1 calc GR . . . . H1B H 1.1450 0.7017 0.3199 0.027 Uiso 1 1 calc GR . . . . H1C H 0.8994 0.6721 0.3386 0.027 Uiso 1 1 calc GR . . . . N2 N 1.0475(2) 0.07279(12) 0.36430(6) 0.0235(3) Uani 1 1 d . . . . . H2A H 1.0781 0.1195 0.3331 0.028 Uiso 1 1 calc GR . . . . H2B H 0.8833 0.0611 0.3644 0.028 Uiso 1 1 calc GR . . . . H2C H 1.1233 -0.0008 0.3620 0.028 Uiso 1 1 calc GR . . . . C1 C 1.1310(3) 0.36231(14) 0.40080(6) 0.0214(3) Uani 1 1 d . . . . . H1 H 1.2714 0.3529 0.3799 0.026 Uiso 1 1 calc R . . . . C2 C 1.0342(3) 0.47829(14) 0.40776(6) 0.0211(3) Uani 1 1 d . . . . . C3 C 0.8238(3) 0.49101(14) 0.43711(6) 0.0230(3) Uani 1 1 d . . . . . H3 H 0.7553 0.5697 0.4419 0.028 Uiso 1 1 calc R . . . . C4 C 0.7148(3) 0.38874(15) 0.45925(6) 0.0233(3) Uani 1 1 d . . . . . H4 H 0.5698 0.3976 0.4786 0.028 Uiso 1 1 calc R . . . . C5 C 0.8161(3) 0.27352(14) 0.45337(6) 0.0222(3) Uani 1 1 d . . . . . H5 H 0.7425 0.2041 0.4694 0.027 Uiso 1 1 calc R . . . . C6 C 1.0256(3) 0.25986(13) 0.42398(6) 0.0210(3) Uani 1 1 d . . . . . C7 C 1.1662(3) 0.58919(16) 0.38795(7) 0.0295(4) Uani 1 1 d . . . . . H7A H 1.1697 0.6525 0.4186 0.035 Uiso 1 1 calc R . . . . H7B H 1.3376 0.5668 0.3825 0.035 Uiso 1 1 calc R . . . . C8 C 1.1424(3) 0.13601(15) 0.41903(7) 0.0283(4) Uani 1 1 d . . . . . H8A H 1.3221 0.1457 0.4196 0.034 Uiso 1 1 calc R . . . . H8B H 1.1081 0.0853 0.4529 0.034 Uiso 1 1 calc R . . . . 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 F1 0.0380(6) 0.0204(5) 0.0406(6) -0.0038(4) 0.0056(4) -0.0037(4) F2 0.0474(7) 0.0293(6) 0.0536(7) 0.0146(5) -0.0020(5) -0.0019(5) F3 0.0393(6) 0.0446(7) 0.0562(7) -0.0150(5) 0.0167(5) 0.0072(5) F4 0.0231(5) 0.0246(5) 0.0659(7) 0.0049(5) -0.0040(5) -0.0003(4) B1 0.0213(8) 0.0165(8) 0.0365(9) -0.0002(7) 0.0044(7) 0.0013(6) F5 0.0317(6) 0.0365(6) 0.0373(6) 0.0010(4) 0.0067(4) 0.0094(4) F6 0.0343(6) 0.0819(10) 0.0480(7) 0.0329(7) 0.0051(5) 0.0134(6) F7 0.0304(6) 0.0566(7) 0.0426(6) -0.0168(5) 0.0068(4) 0.0016(5) F8 0.0450(7) 0.0536(8) 0.0683(9) -0.0133(6) 0.0221(6) -0.0242(6) B2 0.0197(8) 0.0353(10) 0.0267(9) 0.0030(7) 0.0031(6) -0.0012(7) O1 0.0314(6) 0.0241(6) 0.0322(6) 0.0004(5) 0.0036(5) 0.0002(5) N1 0.0242(6) 0.0202(6) 0.0226(6) 0.0020(5) 0.0031(5) 0.0010(5) N2 0.0226(6) 0.0201(6) 0.0284(7) -0.0029(5) 0.0056(5) 0.0008(5) C1 0.0185(7) 0.0277(8) 0.0181(7) -0.0021(6) 0.0012(5) 0.0004(6) C2 0.0230(7) 0.0216(7) 0.0178(7) 0.0007(5) -0.0031(5) -0.0029(6) C3 0.0251(7) 0.0211(7) 0.0221(7) -0.0033(6) -0.0025(6) 0.0050(6) C4 0.0193(7) 0.0296(8) 0.0212(7) -0.0032(6) 0.0023(5) 0.0012(6) C5 0.0229(7) 0.0222(8) 0.0210(7) 0.0002(6) 0.0000(5) -0.0033(6) C6 0.0218(7) 0.0202(7) 0.0200(7) -0.0030(5) -0.0031(5) 0.0028(5) C7 0.0331(9) 0.0281(8) 0.0256(8) 0.0058(6) -0.0068(6) -0.0090(7) C8 0.0305(8) 0.0240(8) 0.0294(8) -0.0037(6) -0.0037(6) 0.0073(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0137 0.0067 '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' B B 0.0073 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0580 0.0411 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0241 0.0137 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0389 0.0241 '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 F1 B1 F3 108.32(14) . . F1 B1 F4 109.75(13) . . F2 B1 F1 110.58(14) . . F2 B1 F3 110.19(14) . . F2 B1 F4 109.65(14) . . F3 B1 F4 108.31(14) . . F6 B2 F5 107.83(13) . . F6 B2 F7 110.03(16) . . F7 B2 F5 108.95(13) . . F8 B2 F5 111.93(16) . . F8 B2 F6 109.46(15) . . F8 B2 F7 108.63(14) . . H1D O1 H1E 104.4 . . H1A N1 H1B 109.5 . . H1A N1 H1C 109.5 . . H1B N1 H1C 109.5 . . C7 N1 H1A 109.5 . . C7 N1 H1B 109.5 . . C7 N1 H1C 109.5 . . H2A N2 H2B 109.5 . . H2A N2 H2C 109.5 . . H2B N2 H2C 109.5 . . C8 N2 H2A 109.5 . . C8 N2 H2B 109.5 . . C8 N2 H2C 109.5 . . C2 C1 H1 119.5 . . C6 C1 H1 119.5 . . C6 C1 C2 121.05(13) . . C1 C2 C3 119.18(13) . . C1 C2 C7 120.14(14) . . C3 C2 C7 120.51(14) . . C2 C3 H3 120.0 . . C4 C3 C2 120.01(14) . . C4 C3 H3 120.0 . . C3 C4 H4 119.8 . . C3 C4 C5 120.46(13) . . C5 C4 H4 119.8 . . C4 C5 H5 120.0 . . C4 C5 C6 119.94(14) . . C6 C5 H5 120.0 . . C1 C6 C5 119.33(13) . . C1 C6 C8 120.12(14) . . C5 C6 C8 120.51(14) . . N1 C7 C2 112.68(12) . . N1 C7 H7A 109.1 . . N1 C7 H7B 109.1 . . C2 C7 H7A 109.1 . . C2 C7 H7B 109.1 . . H7A C7 H7B 107.8 . . N2 C8 C6 111.25(12) . . N2 C8 H8A 109.4 . . N2 C8 H8B 109.4 . . C6 C8 H8A 109.4 . . C6 C8 H8B 109.4 . . H8A C8 H8B 108.0 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 F1 B1 1.383(2) . F2 B1 1.380(2) . F3 B1 1.391(2) . F4 B1 1.406(2) . F5 B2 1.401(2) . F6 B2 1.381(2) . F7 B2 1.382(2) . F8 B2 1.378(2) . O1 H1D 0.8498 . O1 H1E 0.8498 . N1 H1A 0.9100 . N1 H1B 0.9100 . N1 H1C 0.9100 . N1 C7 1.4936(19) . N2 H2A 0.9100 . N2 H2B 0.9100 . N2 H2C 0.9100 . N2 C8 1.493(2) . C1 H1 0.9500 . C1 C2 1.391(2) . C1 C6 1.390(2) . C2 C3 1.396(2) . C2 C7 1.505(2) . C3 H3 0.9500 . C3 C4 1.388(2) . C4 H4 0.9500 . C4 C5 1.390(2) . C5 H5 0.9500 . C5 C6 1.393(2) . C6 C8 1.508(2) . C7 H7A 0.9900 . C7 H7B 0.9900 . C8 H8A 0.9900 . C8 H8B 0.9900 . 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 O1 H1D F5 0.85 2.13 2.9003(15) 149.7 1_655 O1 H1E F8 0.85 2.05 2.8516(17) 158.0 . N1 H1A O1 0.91 1.91 2.8159(18) 178.6 . N1 H1B F4 0.91 2.42 3.0436(16) 125.5 1_655 N1 H1B F8 0.91 2.30 3.0301(18) 136.7 2_755 N1 H1C F3 0.91 2.03 2.7914(16) 140.2 . N1 H1C F7 0.91 2.42 3.0078(17) 122.1 2_655 N2 H2A F5 0.91 2.19 3.0646(17) 161.8 1_655 N2 H2B F1 0.91 2.26 2.9591(16) 133.4 1_545 N2 H2B F6 0.91 2.17 2.9466(18) 142.9 . N2 H2C F4 0.91 1.98 2.8585(16) 161.3 1_645 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 C1 C2 C3 C4 0.4(2) . . . . C1 C2 C7 N1 104.09(16) . . . . C1 C6 C8 N2 -89.43(17) . . . . C2 C1 C6 C5 1.6(2) . . . . C2 C1 C6 C8 -176.32(13) . . . . C2 C3 C4 C5 1.2(2) . . . . C3 C2 C7 N1 -80.68(18) . . . . C3 C4 C5 C6 -1.4(2) . . . . C4 C5 C6 C1 0.0(2) . . . . C4 C5 C6 C8 177.93(13) . . . . C5 C6 C8 N2 92.64(17) . . . . C6 C1 C2 C3 -1.8(2) . . . . C6 C1 C2 C7 173.46(13) . . . . C7 C2 C3 C4 -174.86(13) . . . . _cod_database_fobs_code 1565986