#------------------------------------------------------------------------------ #$Date: 2021-11-04 01:58:51 +0200 (Thu, 04 Nov 2021) $ #$Revision: 270276 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708692.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_7708692 loop_ _publ_author_name 'Zhang, Yue' 'Chen, Dian' 'Jin, Kai-Hang' 'Zang, Shuang-Quan' 'Wang, Qing-Lun' _publ_section_title ; Room-temperature phosphorescence of manganese-based metal halides ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03206B _journal_year 2021 _chemical_formula_moiety 'Cl5 Mn, 2(C3 H8 N6), Cl' _chemical_formula_sum 'C6 H16 Cl6 Mn N12' _chemical_formula_weight 523.95 _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_Hall '-P 2yb' _space_group_name_H-M_alt 'P 1 21/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-02-26 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-09-17 deposited with the CCDC. 2021-11-01 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.166(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 5.40460(10) _cell_length_b 15.3969(4) _cell_length_c 10.8565(3) _cell_measurement_reflns_used 3206 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 73.5100 _cell_measurement_theta_min 2.8570 _cell_volume 902.03(4) _computing_cell_refinement 'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 32.00 58.00 0.50 0.50 -- 0.00 57.00 -60.00 52 2 \w -29.00 17.00 0.50 0.50 -- 0.00 38.00-150.00 92 3 \w 42.00 85.00 0.50 0.50 -- 0.00 57.00-120.00 86 4 \w -24.00 36.00 0.50 0.50 -- 0.00 57.00-120.00 120 5 \w 94.00 186.00 0.50 0.50 -- 98.80 45.00 -60.00 184 6 \w 41.00 133.00 0.50 0.50 -- 98.80 -77.00 -60.00 184 7 \w 69.00 175.00 0.50 0.50 -- 98.80 61.00 -90.00 212 8 \w 11.00 131.00 0.50 0.50 -- 98.80 -82.00 90.00 240 9 \w 88.00 128.00 0.50 0.50 -- 98.80 -82.00 150.00 80 10 \w 78.00 103.00 0.50 0.50 -- 98.80 -45.00 -30.00 50 11 \w 100.00 126.00 0.50 0.50 -- 98.80 45.00-150.00 52 12 \w 9.00 46.00 0.50 0.50 -- 98.80 -45.00 -30.00 74 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0562024000 _diffrn_orient_matrix_UB_12 0.0980793000 _diffrn_orient_matrix_UB_13 -0.0047106000 _diffrn_orient_matrix_UB_21 -0.2600164000 _diffrn_orient_matrix_UB_22 -0.0174343000 _diffrn_orient_matrix_UB_23 0.0457485000 _diffrn_orient_matrix_UB_31 0.1033511000 _diffrn_orient_matrix_UB_32 0.0094230000 _diffrn_orient_matrix_UB_33 0.1345184000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_unetI/netI 0.0415 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.968 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 4101 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.968 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.854 _diffrn_reflns_theta_min 4.078 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 14.338 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.40910 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.929 _exptl_crystal_description block _exptl_crystal_F_000 526 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.998 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.190 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 121 _refine_ls_number_reflns 1849 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.137 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0576 _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^)+(0.1083P)^2^+1.3796P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1676 _refine_ls_wR_factor_ref 0.1694 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1736 _reflns_number_total 1849 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 20190330c2_a.res in P2(1)/m 20190330c2.res created by SHELXL-2016/4 at 17:18:13 on 26-Feb-2020 REM Old TITL 20190330c2_a.res in P2(1)/m REM SHELXT solution in P2(1)/m REM R1 0.115, Rweak 0.009, Alpha 0.031, Orientation as input REM Formula found by SHELXT: C14 N1 Mn Cl6 CELL 1.54184 5.4046 15.3969 10.8565 90 93.166 90 ZERR 2 0.0001 0.0004 0.0003 0 0.002 0 LATT 1 SYMM -X,0.5+Y,-Z SFAC C H Cl Mn N UNIT 12 32 12 2 24 L.S. 10 PLAN 10 BOND $H list 4 MORE -1 CONF htab fmap 2 acta REM REM REM WGHT 0.108300 1.379600 FVAR 0.52990 MN1 4 0.489223 0.250000 0.390498 10.50000 0.02682 0.00856 = 0.01782 0.00000 0.00450 0.00000 CL1 3 0.506695 0.412263 0.398601 11.00000 0.02590 0.00965 = 0.02888 0.00054 0.01006 -0.00069 CL2 3 0.502951 0.250000 0.165615 10.50000 0.02163 0.02349 = 0.01914 0.00000 0.00278 0.00000 CL3 3 0.527476 0.250000 0.628402 10.50000 0.03225 0.01323 = 0.01881 0.00000 -0.00195 0.00000 CL4 3 0.006939 0.250000 0.407004 10.50000 0.02042 0.02195 = 0.02852 0.00000 0.00345 0.00000 N1 5 -0.078641 0.583274 0.402984 11.00000 0.03358 0.02059 = 0.02693 -0.00810 0.01246 -0.00009 AFIX 93 H1A 2 -0.025605 0.631488 0.434517 11.00000 -1.20000 H1B 2 -0.202013 0.557124 0.433341 11.00000 -1.20000 AFIX 0 N2 5 -0.053547 0.474899 0.257275 11.00000 0.02320 0.01130 = 0.02401 -0.00052 0.01142 -0.00216 AFIX 43 H2 2 -0.176269 0.448128 0.287254 11.00000 -1.20000 AFIX 0 N3 5 0.220290 0.588910 0.259818 11.00000 0.02317 0.00961 = 0.01986 -0.00315 0.00292 -0.00307 AFIX 43 H3 2 0.279722 0.635927 0.292372 11.00000 -1.20000 AFIX 0 N4 5 -0.032633 0.367814 0.112753 11.00000 0.03327 0.01119 = 0.02878 -0.00598 0.01335 -0.00920 AFIX 93 H4A 2 0.028619 0.344784 0.049005 11.00000 -1.20000 H4B 2 -0.152988 0.342753 0.147299 11.00000 -1.20000 AFIX 0 N5 5 0.507833 0.597585 0.112094 11.00000 0.02510 0.01824 = 0.03181 -0.00432 0.00981 -0.01198 AFIX 93 H5A 2 0.576569 0.577882 0.048204 11.00000 -1.20000 H5B 2 0.559677 0.645208 0.145911 11.00000 -1.20000 AFIX 0 N6 5 0.243572 0.481271 0.105654 11.00000 0.02107 0.01192 = 0.01731 0.00001 0.00462 -0.00264 C1 1 0.028221 0.549753 0.308953 11.00000 0.02219 0.01279 = 0.01981 0.00047 0.00282 0.00427 C2 1 0.057099 0.440825 0.157089 11.00000 0.01878 0.01271 = 0.01441 0.00210 0.00139 -0.00019 C3 1 0.322933 0.554770 0.158207 11.00000 0.02034 0.00998 = 0.02011 0.00357 0.00334 -0.00014 CL5 3 -0.086134 0.750000 0.122358 10.50000 0.02898 0.01625 = 0.02356 0.00000 0.00190 0.00000 HKLF 4 REM 20190330c2_a.res in P2(1)/m REM R1 = 0.0576 for 1736 Fo > 4sig(Fo) and 0.0611 for all 1849 data REM 121 parameters refined using 0 restraints END WGHT 0.1083 1.3796 REM Instructions for potential hydrogen bonds EQIV $1 -x, -y+1, -z+ HTAB N1 CL4_$1 EQIV $2 x-1, y, HTAB N1 CL1_$2 HTAB N1 CL1_$1 HTAB N2 CL1_$2 EQIV $3 -x+1, -y+1, -z+ HTAB N3 CL3_$3 EQIV $4 -x, -y+1, - HTAB N4 CL5_$4 HTAB N4 CL2_$2 EQIV $5 -x+1, -y+1, - HTAB N5 N6_$5 EQIV $6 x+1, y, HTAB N5 CL5_$6 REM Highest difference peak 0.998, deepest hole -0.846, 1-sigma level 0.190 Q1 1 0.5122 0.3288 0.4385 11.00000 0.05 1.00 Q2 1 0.6331 0.3327 0.4035 11.00000 0.05 0.87 Q3 1 0.2440 0.2500 0.3944 10.50000 0.05 0.79 Q4 1 0.3440 0.3328 0.3901 11.00000 0.05 0.71 Q5 1 0.7247 0.2500 0.3992 10.50000 0.05 0.70 Q6 1 -0.2498 0.7500 0.0710 10.50000 0.05 0.63 Q7 1 0.6802 0.2500 0.2219 10.50000 0.05 0.57 Q8 1 0.4606 0.6628 0.3637 11.00000 0.05 0.57 Q9 1 0.4985 0.3415 0.1395 11.00000 0.05 0.56 Q10 1 0.4394 0.5029 0.3938 11.00000 0.05 0.56 REM The information below was added by Olex2. REM REM R1 = 0.0576 for 1736 Fo > 4sig(Fo) and 0.0611 for all 4114 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.00, deepest hole -0.85 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0611 REM R1_gt = 0.0576 REM wR_ref = 0.1694 REM GOOF = 1.137 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 4114 REM Reflections_gt = 1736 REM Parameters = n/a REM Hole = -0.85 REM Peak = 1.00 REM Flack = n/a ; _cod_data_source_file d1dt03206b2.cif _cod_data_source_block 4 _cod_database_code 7708692 _shelx_shelxl_version_number 2016/4 _chemical_oxdiff_formula 'C N H Cu S' _chemical_oxdiff_usercomment ' ' _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. ; _reflns_odcompleteness_completeness 99.23 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All N(H) groups, All N(H,H) groups 2.a Aromatic/amide H refined with riding coordinates: N2(H2), N3(H3) 2.b X=CH2 refined with riding coordinates: N1(H1A,H1B), N4(H4A,H4B), N5(H5A,H5B) ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.095 _oxdiff_exptl_absorpt_empirical_full_min 0.526 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' 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 Mn1 Mn 0.48922(17) 0.250000 0.39050(8) 0.0176(3) Uani 1 2 d S T P . . Cl1 Cl 0.50670(17) 0.41226(6) 0.39860(9) 0.0212(3) Uani 1 1 d . . . . . Cl2 Cl 0.5030(2) 0.250000 0.16562(12) 0.0214(3) Uani 1 2 d S T P . . Cl3 Cl 0.5275(3) 0.250000 0.62840(13) 0.0216(3) Uani 1 2 d S T P . . Cl4 Cl 0.0069(2) 0.250000 0.40700(13) 0.0236(4) Uani 1 2 d S T P . . N1 N -0.0786(7) 0.5833(2) 0.4030(3) 0.0266(8) Uani 1 1 d . . . . . H1A H -0.025605 0.631488 0.434517 0.032 Uiso 1 1 calc R . . . . H1B H -0.202013 0.557124 0.433341 0.032 Uiso 1 1 calc R . . . . N2 N -0.0535(6) 0.4749(2) 0.2573(3) 0.0191(7) Uani 1 1 d . . . . . H2 H -0.176269 0.448128 0.287254 0.023 Uiso 1 1 calc R . . . . N3 N 0.2203(6) 0.58891(19) 0.2598(3) 0.0175(7) Uani 1 1 d . . . . . H3 H 0.279722 0.635927 0.292372 0.021 Uiso 1 1 calc R . . . . N4 N -0.0326(7) 0.3678(2) 0.1128(3) 0.0240(8) Uani 1 1 d . . . . . H4A H 0.028619 0.344784 0.049005 0.029 Uiso 1 1 calc R . . . . H4B H -0.152988 0.342753 0.147299 0.029 Uiso 1 1 calc R . . . . N5 N 0.5078(6) 0.5976(3) 0.1121(3) 0.0247(8) Uani 1 1 d . . . . . H5A H 0.576569 0.577882 0.048204 0.030 Uiso 1 1 calc R . . . . H5B H 0.559677 0.645208 0.145911 0.030 Uiso 1 1 calc R . . . . N6 N 0.2436(6) 0.4813(2) 0.1057(3) 0.0166(7) Uani 1 1 d . . . . . C1 C 0.0282(7) 0.5498(2) 0.3090(4) 0.0182(8) Uani 1 1 d . . . . . C2 C 0.0571(7) 0.4408(2) 0.1571(3) 0.0153(7) Uani 1 1 d . . . . . C3 C 0.3229(7) 0.5548(2) 0.1582(4) 0.0167(8) Uani 1 1 d . . . . . Cl5 Cl -0.0861(3) 0.750000 0.12236(13) 0.0229(4) Uani 1 2 d S T P . . 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 Mn1 0.0268(5) 0.0086(5) 0.0178(5) 0.000 0.0045(4) 0.000 Cl1 0.0259(6) 0.0097(5) 0.0289(6) 0.0005(3) 0.0101(4) -0.0007(3) Cl2 0.0216(7) 0.0235(7) 0.0191(7) 0.000 0.0028(5) 0.000 Cl3 0.0322(8) 0.0132(6) 0.0188(6) 0.000 -0.0020(5) 0.000 Cl4 0.0204(7) 0.0220(7) 0.0285(8) 0.000 0.0034(6) 0.000 N1 0.034(2) 0.0206(18) 0.0269(19) -0.0081(15) 0.0125(16) -0.0001(14) N2 0.0232(16) 0.0113(15) 0.0240(17) -0.0005(13) 0.0114(14) -0.0022(12) N3 0.0232(17) 0.0096(15) 0.0199(17) -0.0032(12) 0.0029(13) -0.0031(12) N4 0.0333(19) 0.0112(16) 0.0288(19) -0.0060(13) 0.0134(15) -0.0092(13) N5 0.0251(19) 0.0182(17) 0.032(2) -0.0043(14) 0.0098(16) -0.0120(13) N6 0.0211(17) 0.0119(15) 0.0173(16) 0.0000(12) 0.0046(13) -0.0026(12) C1 0.0222(19) 0.0128(17) 0.0198(19) 0.0005(15) 0.0028(15) 0.0043(14) C2 0.0188(18) 0.0127(17) 0.0144(18) 0.0021(14) 0.0014(14) -0.0002(13) C3 0.0203(18) 0.0100(16) 0.0201(18) 0.0036(14) 0.0033(15) -0.0001(14) Cl5 0.0290(7) 0.0162(6) 0.0236(7) 0.000 0.0019(6) 0.000 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 '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' 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 Cl1 Mn1 Cl1 174.25(6) . 4_565 ? Cl1 Mn1 Cl3 87.94(3) . . ? Cl1 Mn1 Cl3 87.94(3) 4_565 . ? Cl1 Mn1 Cl4 87.82(3) 4_565 1_655 ? Cl1 Mn1 Cl4 91.91(3) . . ? Cl1 Mn1 Cl4 91.91(3) 4_565 . ? Cl1 Mn1 Cl4 87.82(3) . 1_655 ? Cl2 Mn1 Cl1 91.83(3) . 4_565 ? Cl2 Mn1 Cl1 91.83(3) . . ? Cl2 Mn1 Cl3 173.68(6) . . ? Cl2 Mn1 Cl4 88.77(5) . 1_655 ? Cl2 Mn1 Cl4 98.81(6) . . ? Cl3 Mn1 Cl4 84.90(5) . 1_655 ? Cl3 Mn1 Cl4 87.51(5) . . ? Cl4 Mn1 Cl4 172.42(7) . 1_655 ? Mn1 Cl4 Mn1 172.42(7) . 1_455 ? H1A N1 H1B 120.0 . . ? C1 N1 H1A 120.0 . . ? C1 N1 H1B 120.0 . . ? C1 N2 H2 119.7 . . ? C1 N2 C2 120.7(3) . . ? C2 N2 H2 119.7 . . ? C1 N3 H3 119.8 . . ? C1 N3 C3 120.5(3) . . ? C3 N3 H3 119.8 . . ? H4A N4 H4B 120.0 . . ? C2 N4 H4A 120.0 . . ? C2 N4 H4B 120.0 . . ? H5A N5 H5B 120.0 . . ? C3 N5 H5A 120.0 . . ? C3 N5 H5B 120.0 . . ? C3 N6 C2 116.9(3) . . ? N1 C1 N2 121.0(4) . . ? N1 C1 N3 121.3(4) . . ? N3 C1 N2 117.7(3) . . ? N4 C2 N2 116.8(3) . . ? N4 C2 N6 121.4(4) . . ? N6 C2 N2 121.7(4) . . ? N5 C3 N3 117.6(4) . . ? N5 C3 N6 119.8(4) . . ? N6 C3 N3 122.6(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 Mn1 Cl1 2.5015(9) . ? Mn1 Cl1 2.5015(9) 4_565 ? Mn1 Cl2 2.4467(16) . ? Mn1 Cl3 2.5797(16) . ? Mn1 Cl4 2.6226(16) . ? Mn1 Cl4 2.7939(16) 1_655 ? Cl4 Mn1 2.7939(16) 1_455 ? N1 H1A 0.8600 . ? N1 H1B 0.8600 . ? N1 C1 1.307(5) . ? N2 H2 0.8600 . ? N2 C1 1.346(5) . ? N2 C2 1.374(5) . ? N3 H3 0.8600 . ? N3 C1 1.337(5) . ? N3 C3 1.367(5) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? N4 C2 1.306(5) . ? N5 H5A 0.8600 . ? N5 H5B 0.8600 . ? N5 C3 1.319(5) . ? N6 C2 1.333(5) . ? N6 C3 1.328(5) . ? 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 C1 N2 C2 N4 179.7(4) . . . . ? C1 N2 C2 N6 -1.8(6) . . . . ? C1 N3 C3 N5 178.3(4) . . . . ? C1 N3 C3 N6 -1.7(6) . . . . ? C2 N2 C1 N1 178.9(4) . . . . ? C2 N2 C1 N3 -0.4(6) . . . . ? C2 N6 C3 N3 -0.4(6) . . . . ? C2 N6 C3 N5 179.6(4) . . . . ? C3 N3 C1 N1 -177.2(4) . . . . ? C3 N3 C1 N2 2.0(6) . . . . ? C3 N6 C2 N2 2.1(6) . . . . ? C3 N6 C2 N4 -179.5(4) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 0 -1 551.28 14.7 0 0 -2 329.57 9.18 0 0 -3 143.52 4.58 0 0 -4 9697.96 261.48 0 0 -4 9932.99 259.76 0 0 -5 882.26 24.83 0 0 -5 877.79 26.42 0 0 -6 1572.72 42.53 0 0 -6 1472.51 43.59 0 0 7 998.67 31.23 0 0 7 867.35 25.55 0 0 8 1310.63 38.26 0 0 8 1589.2 45.58 0 0 9 1099.95 38.85 0 0 10 485.47 22.14 0 0 11 111.53 9.37 0 0 12 7.16 2.8 0 1 0 0.87 0.15 0 -1 0 2.35 0.26 0 -1 1 232.45 7.4 0 -1 -1 277.41 7.12 0 1 -2 640.54 17.5 0 -1 2 639.64 17.5 0 1 -3 888.89 24.71 0 -1 -3 912.98 24.41 0 -1 -4 1336.81 37.62 0 -1 -4 1379.64 36.34 0 1 -4 1292.71 38.24 0 1 -4 1321.08 36.61 0 1 -5 3.43 0.72 0 1 -5 3 0.98 0 -1 -5 3.14 0.59 0 -1 -5 3.46 0.85 0 -1 6 478.02 17.48 0 -1 -6 475.46 15.06 0 1 -6 436.22 15.8 0 1 -6 485.81 14.74 0 1 7 59.11 5.38 0 1 7 60.73 3.37 0 -1 7 71.17 5.91 0 -1 8 856.36 28.61 0 1 8 788.14 27.54 0 -1 9 368.01 17.29 0 1 9 332.34 16.58 0 1 10 69.53 7.17 0 -1 10 65.42 7.44 0 1 10 50.9 3.47 0 1 11 4.11 3.09 0 -1 11 3.39 3.32 0 1 12 203.47 10.53 0 -1 12 214.12 11.55 0 -1 13 229.46 9.48 0 2 0 46.85 1.71 0 2 -1 446.59 14.6 0 2 1 543.14 13.99 0 -2 2 501.59 14.3 0 2 -2 500.87 14.31 0 -2 -2 511.56 13.6 0 2 -3 7.02 0.8 0 2 -3 7.13 1.25 0 -2 -3 8.74 0.48 0 -2 3 9.18 0.87 0 -2 -4 1850.95 48.46 0 2 -4 1730.76 49.8 0 -2 -4 1856.49 49.15 0 2 -4 1737.88 51.5 0 -2 -4 1888.39 49.99 0 2 -5 1065.68 32.77 0 2 -5 1067.52 31.11 0 -2 -5 1076.16 30.91 0 2 -6 50.14 3.07 0 2 -6 43.94 3.55 0 2 6 46.33 2.77 0 -2 6 48.31 4.36 0 2 7 48.73 4.76 0 -2 7 54.67 5.45 0 2 7 56.65 3.39 0 2 8 135.14 6.3 0 2 8 146.4 9.34 0 -2 9 161.42 11.19 0 2 9 148.86 10.23 0 2 9 126.53 6.26 0 2 10 28.37 4.74 0 -2 10 23.58 5.12 0 2 10 18.47 2.26 0 2 11 0.61 2.37 0 2 11 0.64 1.02 0 -2 11 0.13 3.35 0 -2 12 92.82 7.47 0 -2 13 14.3 2.28 0 3 0 0.67 0.32 0 -3 -1 356.74 9.23 0 3 -1 270.94 9.9 0 3 -2 108.46 4.74 0 -3 2 117.7 4.18 0 3 -3 112.18 4.21 0 -3 3 114.45 4.26 0 3 -4 225.56 7.45 0 -3 4 202.91 7.2 0 -3 -4 212.36 6.5 0 -3 -4 215.74 6.2 0 3 -4 235.8 8.97 0 -3 -5 73.12 2.88 0 3 -5 75.1 4.51 0 -3 -5 69.91 2.63 0 -3 6 8.2 1.54 0 3 6 17.44 1.69 0 3 7 104.19 7.05 0 -3 7 110.05 6.3 0 -3 7 122.92 8.17 0 3 7 121.68 5.6 0 -3 8 305.82 12.76 0 3 8 287.66 11.14 0 3 8 315.83 14.66 0 3 9 133.15 6.7 0 3 9 152.65 9.95 0 3 10 28.8 2.9 0 -3 10 43.19 6.42 0 3 11 75.46 4.5 0 -3 11 100.41 8.92 0 -3 12 50.27 5.51 0 -3 13 106.96 5.89 0 4 0 1817.59 48.61 0 4 -1 89.43 3.55 0 4 1 83.37 2.71 0 -4 1 87.22 3.37 0 4 -2 106.47 4.66 0 4 2 112.29 3.77 0 -4 3 1.73 0.6 0 4 -3 1.82 0.78 0 -4 4 806.63 23.56 0 4 -4 835.06 24.96 0 4 -5 309.21 11.73 0 4 6 32.24 2.3 0 -4 6 29.44 3.01 0 4 6 39.8 2.72 0 -4 6 37.51 4.11 0 4 7 3.51 1.17 0 -4 7 1.35 1.38 0 4 8 148.72 7 0 -4 8 137.04 8.17 0 -4 9 214.2 12.92 0 4 9 188.11 8.55 0 4 10 2.08 1.5 0 -4 10 3.02 3.75 0 -4 11 10.41 4.05 0 4 11 9.73 1.81 0 -4 12 10.03 3.1 0 4 12 8.43 1.39 0 -4 13 29.51 2.88 0 5 0 1.43 0.43 0 -5 0 0.98 0.42 0 -5 1 98.85 3.78 0 5 -1 98.4 3.78 0 5 -2 593.51 17.48 0 5 2 569.2 16.59 0 -5 3 103.54 4.52 0 5 -3 109.02 5.05 0 -5 4 886.08 25.87 0 -5 5 48.29 3.68 0 -5 5 62.75 4.64 0 5 6 386.62 13.24 0 5 6 408.07 12.93 0 -5 6 341.55 14.29 0 -5 6 450.7 16.61 0 -5 7 68.72 5.41 0 -5 7 77.75 6.81 0 5 7 79.14 4.68 0 5 7 81.17 4.34 0 5 8 614.82 20.43 0 -5 8 585.19 22.28 0 5 9 146.18 7.46 0 5 10 108.98 6.18 0 -5 11 30.5 5.17 0 5 11 22.2 2.59 0 5 12 95.56 4.7 0 -5 12 122.57 7.63 0 -5 13 189.63 7.59 0 6 0 8861.32 235.77 0 -6 0 9022.66 235.93 0 -6 1 1938.93 50.14 0 6 -1 1937.88 50.16 0 -6 2 13.58 1.37 0 6 2 13.19 1.29 0 6 -2 16.06 1.58 0 6 -3 48.77 3.18 0 -6 4 3969.01 110.28 0 6 -4 4234.78 111.02 0 6 5 2457.92 65.55 0 -6 5 2533.64 68.58 0 -6 5 2354.26 67.11 0 6 5 2412 65.65 0 -6 6 352.6 14.84 0 -6 6 337.67 12.85 0 -6 6 329.48 13.56 0 6 6 347.56 11.88 0 6 7 238.78 9.33 0 -6 7 259.82 12.78 0 6 7 254.7 9.97 0 -6 8 564.43 21.79 0 6 8 521.29 17.74 0 6 9 1074.24 33.94 0 -6 9 1204.78 39.3 0 -6 10 291.99 15.07 0 6 10 258.75 10.93 0 6 11 118.34 6.03 0 6 12 0.65 0.88 0 -7 0 1.38 0.54 0 7 0 1.14 0.45 0 7 -1 9.15 1.12 0 -7 -1 8.46 0.97 0 7 1 6.92 0.73 0 -7 1 7.71 1.06 0 7 -2 1414.59 38.22 0 -7 2 1379.12 38.04 0 7 -3 437.7 14.47 0 -7 4 929.06 27.62 0 -7 4 884.87 27.04 0 7 4 919.27 26.23 0 7 4 853.47 26.38 0 -7 5 51.75 4.19 0 -7 5 49.01 3.88 0 7 5 52.8 3.45 0 7 5 46.47 3.25 0 -7 5 49.83 4.44 0 -7 6 502.3 18 0 7 6 505.05 16.27 0 -7 6 439.01 16.82 0 -7 6 500.98 18.72 0 7 6 461.22 15.84 0 -7 7 43.43 5.14 0 -7 7 39.64 4.6 0 7 7 37.57 3.17 0 -7 7 40.29 3.89 0 -7 8 852.37 30.29 0 -7 8 779.58 28.9 0 7 8 851.95 26.75 0 7 9 509.38 18.19 0 -7 9 531.36 21.86 0 7 10 30.96 3.39 0 -7 10 35.23 4.94 0 -7 11 3.99 2.49 0 7 11 3.23 1.44 0 7 12 329.66 11.07 0 -7 12 341.74 12.77 0 -8 0 1912.54 51.42 0 8 0 1841.08 50.98 0 8 -1 10.16 1.27 0 -8 -1 9.86 1.15 0 8 1 9.85 1.45 0 -8 1 10.12 1.28 0 8 2 64.39 3.73 0 -8 2 68.16 3.85 0 8 -2 74.15 3.95 0 -8 -2 67.9 3.22 0 -8 3 4.95 1.41 0 -8 3 4.7 1.31 0 8 3 4.93 1.05 0 -8 4 1471.5 46.35 0 -8 4 1634.22 45.9 0 8 4 1667.04 44.69 0 -8 4 1670.87 46.31 0 8 4 1475.68 44.93 0 8 5 86.94 4.73 0 8 5 76.15 4.62 0 -8 5 85.2 5.41 0 -8 5 84.14 5.9 0 -8 6 189.5 9.33 0 8 6 199.25 8.42 0 -8 6 208 10.18 0 -8 6 172.13 9.85 0 8 6 177.3 8.06 0 -8 7 10.81 3.09 0 8 7 14.57 2.58 0 -8 7 10.45 2.37 0 8 7 12.2 2.04 0 -8 7 11.6 3.12 0 -8 8 536.32 21.29 0 -8 8 533.65 21.36 0 8 9 16.72 2.99 0 -8 9 19.41 3.89 0 8 10 92.8 5.54 0 -8 10 75.65 6.44 0 -8 11 11.38 2.73 0 8 11 16.53 2.15 0 8 12 58.62 3.05 0 -8 12 48.18 3.37 0 -9 0 0.17 0.77 0 -9 0 0.31 0.49 0 -9 -1 477.78 15.6 0 9 1 495.57 16.96 0 -9 2 177.5 7.55 0 -9 2 177.57 7.69 0 9 3 4.68 1.11 0 -9 3 3.53 1.42 0 -9 4 43.25 3.89 0 -9 4 46.25 3.96 0 9 4 36.89 3.25 0 9 4 43.37 3.12 0 -9 5 132.47 7.25 0 9 5 111.06 6.09 0 9 5 130.38 6.17 0 -9 5 107.57 6.85 0 -9 5 136.59 7.58 0 -9 6 22.12 3.33 0 -9 6 29.56 3.7 0 9 6 20.44 2.61 0 9 7 76.42 5.19 0 -9 7 66.79 6.14 0 9 7 50.52 4.12 0 -9 7 63.23 5.36 0 -9 7 55.17 5.41 0 -9 8 73.37 6.53 0 9 8 73.26 5.23 0 -9 8 54.07 4.86 0 -9 8 57.82 5.61 0 -9 9 16.97 3.51 0 9 10 22.89 2.77 0 -9 10 15.79 3.03 0 -9 11 30.6 3.13 0 9 11 40.67 3.01 0 -10 0 1771.49 49.98 0 -10 -1 7.74 1.47 0 -10 1 8.7 1.73 0 -10 2 47.55 3.74 0 -10 2 50.75 3.72 0 -10 3 54.39 4.2 0 10 3 53.03 3.3 0 -10 4 1063.44 32.38 0 -10 4 1100.64 32.56 0 10 4 1009.93 30.32 0 10 4 979.48 31.24 0 -10 5 124.16 7.33 0 10 5 130.23 6.21 0 -10 5 130.73 7.63 0 10 5 108.7 6.16 0 10 6 339.05 12.09 0 10 6 268.36 11.6 0 -10 6 250.55 12.14 0 -10 6 343.26 13.85 0 -10 6 306.26 13.69 0 10 7 49.55 4.1 0 -10 7 44.65 4.64 0 -10 7 50.79 5.72 0 -10 7 57.25 5.25 0 -10 8 23.02 3.33 0 10 8 27.99 3.39 0 -10 8 26.38 4.32 0 -10 8 20.04 3.38 0 10 9 159.93 7.52 0 -10 9 121.14 7.43 0 -10 10 9.32 2.09 0 10 11 1.03 0.96 0 -10 11 0.92 1.01 0 -11 0 1.28 1.33 0 -11 -1 6.81 1.57 0 -11 1 4.48 1.57 0 -11 2 306.9 12.15 0 -11 2 321.05 12.08 0 -11 3 135.8 7.48 0 -11 3 145.08 7.4 0 11 3 137.13 6.05 0 -11 4 545.62 19.02 0 11 4 504.48 16.8 0 11 4 505.62 17.95 0 -11 4 537.48 18.93 0 11 5 6.58 1.89 0 11 5 6.39 1.98 0 -11 5 6.22 2.71 0 -11 5 10.47 2.67 0 11 6 226.16 10.04 0 -11 6 257.66 11.8 0 11 6 256.55 9.98 0 -11 6 258.06 11.96 0 -11 7 21.9 3.65 0 11 7 26.49 3.19 0 11 7 17.6 2.62 0 -11 7 13.32 2.59 0 -11 8 409.93 15.09 0 11 8 448.56 14.35 0 11 9 162.43 6.93 0 -11 9 101.38 5.85 0 -11 10 19.56 2.15 0 11 10 33.31 2.64 0 -12 0 3933.1 107.63 0 -12 1 1000.63 31.04 0 -12 -1 1006.84 30.32 0 -12 2 80.29 5.45 0 -12 2 75.65 5.05 0 -12 3 80.7 5.61 0 -12 3 72.49 5.33 0 12 4 1856.99 55.02 0 -12 4 2006.21 56.18 0 12 4 1891 53.52 0 -12 5 1578.78 45.56 0 12 5 1470.66 42.44 0 -12 5 1493.42 45.09 0 12 6 497.18 17.34 0 -12 6 551.03 20.08 0 -12 6 561.64 19.96 0 12 6 482.57 17.77 0 12 7 23.87 2.87 0 -12 7 28.41 3.81 0 12 7 28.58 3.05 0 -12 8 482.18 17.51 0 12 8 481.04 16.09 0 12 9 543.44 17.25 0 12 10 202.39 7.27 0 -13 0 3.13 1.74 0 -13 1 192.31 9.09 0 -13 -1 201.62 8.8 0 -13 2 808.06 26.32 0 -13 2 816.55 25.91 0 -13 3 170.59 8.52 0 -13 3 169.09 8.85 0 -13 4 344.47 14.13 0 13 4 334.82 13.29 0 13 4 341.74 11.93 0 -13 5 13.16 3.24 0 13 5 14.48 2.67 0 -13 5 14.93 3.39 0 13 5 13.42 2.01 0 13 6 228.24 8.98 0 13 6 210.61 9.68 0 13 7 15.29 2.37 0 13 7 16.44 2.23 0 -13 7 18.15 3.09 0 13 8 504.33 15.81 0 -13 8 477.83 16.88 0 13 9 253.52 8.7 0 -14 0 1344.29 40.13 0 -14 1 86.82 5.87 0 -14 -1 97.92 5.73 0 -14 2 6.01 2.42 0 14 2 3.74 1.89 0 14 3 8.4 2.29 0 -14 3 12.99 2.99 0 -14 3 10.81 2.42 0 14 4 410.6 15.25 0 14 5 118.65 6.52 0 -14 5 127.5 7.59 0 14 5 107.76 5.14 0 14 6 19.93 2.11 0 14 6 22.19 2.67 0 -14 6 25.23 3.46 0 -14 7 2.06 1.84 0 14 7 0.63 1.14 0 14 7 0.61 1.01 0 -14 8 157.17 6.77 0 14 8 159 5.92 0 -15 0 1.28 1.89 0 15 1 25.73 3.02 0 -15 1 26.86 3.38 0 15 2 3.16 1.82 0 -15 2 4.1 2.36 0 15 3 39.45 3.63 0 -15 3 44.41 4.4 0 -15 4 110.53 6.9 0 15 5 28.19 2.96 0 -15 5 24.55 3.54 0 15 6 26.11 2.64 0 -15 6 30.38 3.34 0 -15 7 37.88 3.2 0 16 0 323.77 12.07 0 -16 0 359.49 12.71 0 -16 1 7.04 2.16 0 16 1 7.3 1.77 0 16 -1 7.71 1.68 0 16 -2 0.81 1.09 0 -16 2 1.36 1.97 0 16 2 -0.54 1.41 0 16 3 44.66 3.55 0 -16 3 49.38 4.19 0 -16 4 501.88 17.3 0 16 5 34.39 2.84 0 -16 6 179.43 7.52 0 16 6 163.28 6.65 0 -16 7 3.39 1.04 0 17 0 0.46 1.02 0 -17 1 151.27 6.69 0 17 1 139.95 6.1 0 17 -1 136.23 5.8 0 17 2 5.4 1.47 0 -17 2 5.15 1.73 0 17 -2 5.34 1.09 0 -17 3 63.51 4.16 0 17 3 57.48 3.59 0 -17 4 36.04 3.04 0 17 5 0.59 0.85 0 -17 6 3.98 1 0 18 0 1330 36.82 0 18 -1 229.31 7.77 0 18 1 254.02 8.31 0 -18 2 13.19 1.64 0 18 2 15.14 1.58 0 -18 3 44.22 2.8 0 18 3 39.01 2.39 0 -18 4 512.06 15.21 0 18 4 492.11 14.76 -1 0 13 123.69 6.52 -1 0 12 25.19 4.46 -1 0 11 141.04 10.38 -1 0 10 225.3 13.11 -1 0 10 172.14 7.42 -1 0 9 844.77 26.35 -1 0 9 868.38 26.29 -1 0 8 75.31 4.15 -1 0 8 74.43 4.01 -1 0 7 281.73 9.84 -1 0 7 304.94 13.05 1 0 -6 57.9 3.3 -1 0 6 58.36 4.46 1 0 -6 61.78 3.64 -1 0 6 55.32 3.04 1 0 -5 2444.82 66.22 1 0 -4 1778.28 48.11 1 0 -3 514.78 15.12 1 0 -2 32.56 1.72 -1 0 1 2322.48 61.49 1 0 0 192.36 6 -1 0 0 209.18 6.04 -1 0 -1 156.84 4.76 1 0 1 149.16 4.83 1 0 2 552.3 16.78 1 0 2 583.34 16.34 1 0 3 27.53 1.23 -1 0 -3 29.24 1.61 -1 0 -4 1106.6 30.72 -1 0 -5 1712.95 47.15 1 0 6 5.69 1.76 1 0 7 193.95 10.72 1 0 8 107.26 8.4 1 0 9 531.37 23.12 1 0 10 4.43 2.86 1 0 11 15.64 3.49 -1 -1 13 41.56 3.78 -1 1 12 213.99 11.6 -1 -1 12 223.96 12.21 -1 1 11 5.21 3.4 -1 -1 11 3.21 3.42 -1 1 11 3.22 1.19 -1 1 10 0.21 1.11 -1 1 10 1.21 2.88 -1 -1 10 -0.37 3.21 -1 -1 9 1.45 1.01 -1 -1 9 1.89 3.06 -1 1 9 1.34 2.89 -1 1 9 1.16 1.05 -1 1 9 1.56 1.19 -1 -1 8 343.27 11.93 -1 1 8 421.73 17.42 -1 1 8 339.7 12.24 -1 -1 8 443.35 17.34 -1 -1 8 354.23 11.98 -1 -1 7 11.03 1.39 -1 1 7 12.21 1.59 -1 1 7 12.35 2.6 -1 -1 7 14.07 2.73 -1 -1 7 11.67 1.39 1 1 -6 34.05 2.5 -1 1 6 32.75 2.33 1 -1 -6 34.64 2.38 1 -1 -6 35.29 2.43 -1 1 6 31.9 3.28 -1 -1 6 30.22 3.21 1 -1 -5 71.1 3.43 1 1 -5 70.94 3.46 1 1 -5 76.59 2.92 1 -1 -5 69.54 3.32 1 -1 -4 917.31 27.54 1 1 -4 949.6 27.6 1 -1 -3 18.38 1.31 1 1 -3 20.54 1.22 1 1 -3 20.43 1.3 1 1 -2 3.3 0.49 1 -1 -2 2.23 0.48 -1 1 1 453.08 12.72 1 1 -1 457.84 12.81 -1 -1 1 457.58 12.59 1 -1 -1 423.23 12.52 -1 -1 0 3.04 0.43 -1 -1 0 2.26 0.39 1 -1 1 147.73 4.8 -1 -1 -1 138.32 4.4 1 1 1 157.09 4.66 -1 1 -1 148.64 4.78 1 1 2 415.28 10.65 -1 1 -2 412.48 11.69 -1 1 -3 166.64 5.8 1 -1 3 155.92 6.4 -1 -1 -3 173.51 5.27 1 -1 3 161.41 5.26 1 1 3 161.94 6 -1 -1 -4 57.14 2.48 -1 1 -4 50.94 2.84 1 -1 4 59.32 2.49 -1 -1 -5 54.27 2.62 -1 1 -5 51.06 3.07 1 1 6 19.52 2.81 -1 1 -6 27.75 2.35 1 -1 6 22.43 3.22 1 -1 7 30.17 4.18 1 1 7 31.89 2.28 1 1 7 23.04 3.5 1 1 8 212.26 12.01 1 -1 8 232.85 13.03 1 1 8 209.75 8.09 1 1 9 58.18 6.36 1 -1 9 64.42 7.04 1 1 10 30.63 4.63 1 -1 10 34.72 5.48 1 -1 11 58.07 6.15 1 -1 12 50.57 4.52 -1 -2 13 201.01 9.18 -1 2 12 7.6 1.3 -1 -2 12 12.79 3.69 -1 2 12 12.47 2.9 -1 2 11 236.68 12.96 -1 -2 11 253.04 13.67 -1 2 10 32.62 5.22 -1 -2 10 31.72 5.66 -1 2 10 23.1 2.65 -1 -2 9 413.1 18 -1 2 9 393.57 17.7 -1 -2 8 5.92 2.73 -1 -2 8 5.87 1.19 -1 2 8 4.39 1.42 -1 2 8 3.81 2.4 -1 -2 7 112.45 4.89 -1 2 7 117.44 7.34 -1 2 7 117.37 5.43 -1 -2 7 108.89 4.72 -1 -2 6 1.37 0.64 1 -2 -6 2.31 0.71 -1 2 6 1.1 0.71 -1 2 6 1.32 1.2 1 -2 -5 25.68 1.76 1 2 -5 26.11 1.99 1 2 -5 28.88 1.85 1 2 -4 16.52 1.36 1 -2 -4 16.06 1.25 1 2 -4 16.81 1.38 1 2 -3 539.36 15.62 1 -2 -3 530.41 15.15 1 2 -2 9.92 0.94 1 -2 -2 9.18 0.76 1 2 -2 9.37 0.82 1 2 -1 5.57 0.55 1 2 -1 6.66 0.72 -1 2 0 1022.6 28.67 1 2 0 1019.98 28.16 1 -2 0 1055.87 28.61 -1 -2 -1 1095.47 29.69 1 2 1 1107.19 29.41 -1 -2 -1 1147.88 30.03 1 2 2 3395.11 93.84 1 -2 2 3497.64 94.7 -1 2 -2 3535.83 94.55 -1 -2 -2 3658.57 93.5 -1 2 -3 36.17 2.25 1 -2 3 40.94 2.08 1 -2 4 12.01 1.12 -1 -2 -4 13.47 0.9 -1 2 -4 10.69 1.32 1 -2 5 471.47 14.35 -1 2 -5 467.12 15.53 -1 -2 -5 501 13.9 1 -2 6 726.33 25.34 1 2 6 708.26 21.02 1 2 7 35.99 2.64 1 -2 7 36.63 4.78 1 2 8 27.02 4.01 1 -2 8 30.03 4.89 1 2 8 34.42 2.79 1 2 9 460.71 15.54 1 -2 9 519.44 22.75 1 -2 10 157.87 11.25 1 -2 11 156.3 10.42 1 -2 12 3.62 2.1 -1 -3 13 9.34 2.09 -1 3 12 57.69 3.45 -1 -3 12 81.1 6.72 -1 3 11 37.87 3.29 -1 3 11 49.12 5.52 -1 -3 11 46.02 6.04 -1 3 10 19.56 2.3 -1 3 10 22.21 2.69 -1 -3 10 24.99 5.24 -1 3 10 26.04 4.59 -1 3 9 267.49 13.6 -1 3 9 215.43 9.39 -1 -3 8 2.45 0.97 -1 3 8 3.13 2.26 -1 3 8 2.72 1.36 -1 -3 7 305.97 10.46 -1 -3 7 311.48 12.2 -1 -3 7 342.53 14.13 -1 3 7 316.95 13.55 -1 3 7 307.47 11.18 -1 -3 6 934.5 26.92 -1 -3 6 920.1 28.89 -1 3 6 970.78 30.04 -1 3 6 944.06 27.7 -1 -3 6 999.87 29.94 1 3 -5 830.91 24.33 1 -3 -5 836.12 23.55 1 3 -5 861.11 24.53 1 3 -4 123.39 5.07 1 3 -4 118.96 4.72 1 -3 -4 125.02 4.27 1 -3 -3 312.7 8.98 1 3 -3 284.78 9.77 -1 3 2 6052.82 153.66 1 3 -2 5719.91 153.55 1 3 -2 5605.6 154.23 1 3 -1 330.68 10.28 1 -3 -1 333.79 9.62 -1 3 1 312.91 9.72 1 3 -1 352.47 9.72 1 3 0 332.63 9.81 1 3 0 324.79 9.45 1 -3 0 343.34 9.85 1 3 0 350.99 10.22 1 -3 1 12.38 1.07 1 3 1 13.74 0.83 -1 3 -1 11.69 1.07 1 3 2 9954.77 261.95 -1 -3 -2 9999 262.5 -1 -3 -3 71.73 2.73 1 -3 3 58.03 2.96 -1 -3 -3 68.88 2.09 -1 3 -3 52.41 3.12 1 -3 4 13.12 1.33 -1 -3 -4 11.74 0.62 -1 -3 -4 13.71 1.04 1 -3 5 140 7.8 -1 3 -5 132.65 6.26 1 -3 5 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1.12 -2 -1 5 3.82 0.89 2 -1 -4 216.63 7.84 2 1 -4 209.29 8.19 2 1 -3 580.64 19.54 2 -1 -3 634.58 19.19 2 1 -2 535.97 16.51 -2 -1 2 573.72 16.17 -2 1 2 535.31 15.58 2 -1 -2 543.51 16.24 -2 -1 1 900.48 24.51 2 1 -1 845.56 24.95 2 -1 0 276.68 8.91 -2 -1 0 279.02 8.51 -2 -1 0 273.59 8.62 -2 1 0 267.61 8.81 2 1 0 259.85 8.78 -2 -1 -1 921.35 25.63 2 -1 1 958.15 26.14 -2 1 -1 873.44 25.77 2 1 1 933.08 26.02 -2 -1 -2 224.07 7.2 -2 1 -2 218.8 7.46 2 -1 2 229.08 7.85 2 1 2 205.3 7.49 2 -1 3 130.61 5.74 2 1 3 120.13 5.4 2 -1 3 129.51 4.97 2 1 3 140.41 4.05 -2 1 -3 152.76 5.59 -2 -1 -3 155.33 5.15 2 -1 4 1593.77 48.83 2 1 4 1680.34 48.24 -2 -1 -4 1750.38 46.36 2 -1 5 4.72 1.67 2 -1 6 88.77 6.52 2 1 7 31.85 3.79 2 -1 7 28.03 4.06 2 -1 8 683.87 26.08 2 -1 9 70.66 6.64 2 -1 10 29.6 4.03 2 1 10 35.68 3.31 2 -1 11 17.59 2.92 2 -1 11 15.29 2.3 -2 -2 13 41.1 3.31 -2 -2 12 10.67 3 -2 2 12 9.42 2.64 -2 -2 11 8.28 3.73 -2 2 11 8.16 3.4 -2 2 11 6.38 1.64 -2 2 11 7.38 1.62 -2 2 10 4.58 1.69 -2 2 10 1.21 2.95 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3 23.72 1.81 2 -2 3 24.9 2.21 -2 -2 -3 28.37 1.62 2 -2 4 1038.85 31.95 2 -2 5 34.72 3.88 2 -2 6 26.64 3.92 2 2 6 51.5 3.43 2 -2 7 19.26 3.75 2 2 7 29.88 2.5 2 -2 8 82.41 7.39 2 2 9 60.09 4.3 2 -2 9 46.57 5.71 2 -2 10 29.07 4.19 2 -2 11 93.96 6.62 -2 3 12 11.49 1.66 -2 3 12 12.5 2.44 -2 3 11 4.2 2.8 -2 3 11 1.91 1.24 -2 3 11 2.8 1.27 -2 3 10 7.92 1.9 -2 3 10 10.29 3.56 -2 3 10 6.73 1.89 -2 -3 9 586.52 22.87 -2 3 9 614.55 23.5 -2 3 9 552.55 19.37 -2 3 8 28.69 3.06 -2 -3 8 29.6 2.63 -2 3 8 31.21 4.46 -2 -3 8 30.07 4.4 -2 -3 8 27.16 2.65 -2 -3 7 123.18 5.8 -2 3 7 123.87 6.35 -2 -3 7 130.26 5.8 -2 -3 7 125.23 7.61 -2 3 7 134.33 8.37 -2 -3 7 133.68 7.2 -2 -3 6 6.32 1.73 -2 -3 6 5.77 1.25 -2 -3 6 8.36 1.99 -2 -3 6 6.05 1.18 -2 3 5 175.41 7.16 2 -3 -5 165.99 6.49 -2 -3 5 166.9 6.58 -2 -3 5 191.22 6.89 -2 -3 5 171.22 7.69 -2 -3 5 177.39 8.42 -2 -3 4 51.32 2.82 2 -3 -4 48.88 2.73 2 3 -4 47.21 2.75 -2 3 3 88.46 3.19 2 3 -3 77.81 4.35 2 3 -3 81.73 3.64 -2 3 2 87.98 4.15 2 3 -2 81.16 3.47 2 3 -2 84.76 4.28 2 -3 -2 92.33 3.87 2 3 -1 240.87 7.73 -2 3 1 259.75 8.76 2 3 -1 253.56 8.79 2 -3 -1 257.71 8.31 -2 -3 0 45.8 2.54 2 -3 0 48.29 2.66 -2 3 0 46.55 2.65 2 3 0 47.26 2.05 2 3 0 49.53 2.68 -2 -3 -1 51.89 2.62 2 3 1 46.09 1.84 2 3 2 11.13 1.13 2 -3 2 10.97 1.36 -2 -3 -2 12.78 1.22 2 -3 3 126.09 5.44 2 -3 3 134.51 6.23 -2 -3 -3 141.24 4.6 2 3 3 123.7 5.02 2 3 4 16.5 1.78 2 -3 4 13.65 2.37 2 -3 4 11.97 1.39 -2 -3 -4 13.56 1.35 2 -3 5 299.19 13.35 2 -3 6 14.6 3.18 2 3 6 23.7 2.73 2 3 7 63.11 4.21 2 -3 7 56.59 6.06 2 3 7 61 3.94 2 3 8 143.34 6.93 2 -3 8 146.86 10.24 2 3 8 145.76 6.77 2 -3 9 29.26 4.95 2 3 9 31.64 2.87 2 -3 10 6.43 2.73 2 -3 11 3.41 2.15 2 -3 12 86.33 5.06 -2 -4 12 1.61 2.14 -2 4 12 0.8 0.97 -2 4 11 2.16 1.26 -2 4 11 3.29 2.26 -2 -4 11 2.88 2.57 -2 4 11 1.2 1.32 -2 4 10 48.19 3.82 -2 4 10 49.92 4.18 -2 -4 10 58.5 6.12 -2 4 9 907.7 29.59 -2 -4 9 959.11 32.96 -2 4 8 41.95 3.76 -2 -4 8 32.65 4.39 -2 -4 8 33 3.67 -2 -4 7 87.59 6.29 -2 4 7 93.75 7.03 -2 -4 7 101.98 6.36 -2 -4 6 53.97 3.38 -2 4 6 51.51 3.7 -2 -4 6 51.09 4.18 -2 -4 6 59.6 4.61 -2 -4 5 757.73 22.77 -2 4 5 782.77 23.49 -2 -4 5 734.19 23.88 -2 -4 4 19.7 1.79 -2 4 4 21.13 2.01 -2 4 4 21.16 2.07 -2 -4 4 23.93 2.8 2 4 -3 125.52 4.87 2 -4 -3 125.7 4.82 -2 4 2 503.48 15.14 2 4 -2 472.16 14.08 2 -4 -2 485.38 14.28 2 -4 -1 1422.77 38.65 2 4 -1 1346.79 39.25 2 4 -1 1404.9 38.11 -2 4 1 1408.47 39.24 2 4 0 651.43 19.14 2 4 0 701.58 20.28 -2 4 0 705.22 20.59 2 -4 1 171.23 6.4 -2 4 -1 144.22 6.11 2 4 1 147.86 4.85 -2 -4 -1 188.04 6.19 -2 -4 -2 237.88 7.47 2 4 2 182.19 6.7 2 -4 3 112.97 5.79 -2 -4 -3 113.41 4.6 2 -4 3 100.39 4.81 -2 4 -3 102.36 5.22 2 -4 4 22.07 2.05 2 4 4 21.55 2.01 2 -4 4 20.71 3.03 2 -4 4 25.58 2.55 -2 -4 -4 29.07 2.05 2 4 5 403.83 13.68 2 -4 5 419.13 17.16 2 -4 5 440.93 15.1 2 4 6 3.38 1.2 2 -4 6 2.53 2.32 2 4 6 4.22 1.73 2 4 7 32.37 3.03 2 -4 7 29.6 4.66 2 4 7 26.64 2.61 2 -4 8 59.38 6.64 2 4 8 58.71 4.16 2 -4 9 154.9 10.47 2 4 9 146.28 7.03 2 -4 10 23.86 4.14 2 4 10 25.04 2.44 2 -4 11 21.44 3.58 2 -4 12 3.91 1.44 -2 -5 12 126.96 6.91 -2 5 12 116.6 5.27 -2 5 11 36.23 2.96 -2 5 11 35.01 3.1 -2 -5 11 37.28 4.5 -2 5 10 87.9 5.25 -2 5 10 92.76 5.76 -2 -5 10 108.12 7.83 -2 5 10 115.11 7.74 -2 5 9 45.45 4.15 -2 -5 9 46.45 5.38 -2 5 9 51.99 5.52 -2 -5 9 44.95 4.32 -2 -5 8 600.2 23.03 -2 5 8 673.63 24.23 -2 -5 8 659.52 22.62 -2 -5 7 156.64 8.86 -2 5 7 177.82 9.85 -2 5 7 164.34 7.95 -2 5 6 153.3 7.16 -2 -5 6 139.38 7.54 -2 -5 5 1.51 1.52 -2 -5 5 1.01 1.03 -2 5 5 1.3 0.96 -2 -5 5 1.19 1.12 -2 5 4 193.59 7.65 -2 -5 4 202.6 8.56 -2 -5 4 166.15 7.29 -2 5 4 192.4 7.84 -2 -5 4 193.21 8.84 -2 5 4 197.88 7.53 -2 5 3 600.83 17.06 -2 -5 3 630.42 18.57 -2 5 3 595.35 16.57 2 -5 -3 574.94 15.99 2 5 -2 376.34 11.46 -2 5 2 409.1 12.66 2 -5 -2 403.85 11.78 2 -5 -1 94.01 4.03 2 5 -1 90.85 3.61 -2 5 1 97.15 4.54 2 5 0 342.86 10.16 2 5 0 318.71 10.91 -2 5 0 327.94 11.34 -2 5 -1 629.74 20.33 2 -5 1 726.33 20.44 2 -5 2 149.14 6.55 2 -5 3 53.19 3.37 2 -5 3 54.91 4.43 2 -5 3 64.97 4.22 2 5 4 2553.93 70.64 2 -5 4 2661.2 72.76 2 5 5 6.99 1.47 2 -5 5 4.03 1.46 2 -5 6 378.07 18.21 2 5 6 533.97 17.64 2 -5 7 8.89 3.37 2 5 7 4.58 1.59 2 -5 8 1274.62 41.37 2 5 8 1168.37 35.79 2 -5 9 24.56 4.55 2 5 9 27.22 2.92 2 -5 10 106.69 7.77 2 5 10 96.36 5.19 2 -5 11 124.67 7.88 -2 -6 12 0.52 1.27 -2 6 12 0.65 0.83 -2 6 11 274.36 10.38 -2 -6 11 280.34 12.27 -2 6 11 274.06 10.06 -2 6 10 441.61 15.94 -2 -6 10 448.62 17.84 -2 -6 9 559.49 22.06 -2 -6 9 597.68 21.35 -2 6 8 253.09 11.1 -2 -6 8 237.56 12.02 -2 6 8 270.99 12.84 -2 6 7 167.25 8.14 -2 -6 7 152.38 8.74 -2 6 7 180.14 9.72 -2 6 6 235.02 9.89 -2 -6 6 286.06 10.67 -2 -6 6 203.85 10.07 -2 -6 6 270.4 11.35 -2 -6 5 2561.01 64.66 -2 -6 5 2491.72 65.55 -2 6 4 3860.58 108.02 -2 6 4 3921.32 107.66 -2 -6 4 4084.22 108.9 -2 -6 4 4063.67 109.33 -2 6 4 3998.46 107.49 2 -6 -3 127.65 5.25 -2 6 3 148.76 6.11 -2 -6 3 153.94 7.11 -2 6 3 146.15 5.98 -2 6 3 134.56 6.21 2 6 -2 292.59 9.35 2 -6 -2 322.72 9.57 -2 6 2 302.57 10.34 2 -6 -1 1002.27 26.12 2 6 -1 942.91 25.5 -2 6 1 947.37 26.81 -2 6 0 4053.21 110.54 2 6 0 3865.75 109.86 2 -6 1 491.48 15.46 -2 6 -1 437.49 15.48 2 6 2 300.44 10.98 2 -6 2 282.8 11.68 2 6 3 393.66 13.09 2 -6 3 369.49 14.52 2 6 4 3225.43 90.42 2 -6 4 3162.72 92.89 2 -6 5 627.22 22.03 2 -6 5 528.78 19.7 2 6 6 223.81 9.41 2 -6 6 133.03 8.13 2 6 7 1.1 1.64 2 -6 8 172.5 10.94 2 6 8 178.16 8.37 2 -6 9 335.85 15.34 2 6 9 313.9 12.37 2 -6 10 507.36 19.36 2 6 10 453.98 15.62 2 -6 11 4.65 2.45 -2 7 12 76.07 3.66 -2 7 11 60.18 3.62 -2 7 11 63.06 3.95 -2 -7 11 61.18 4.7 -2 -7 10 28.59 3.86 -2 -7 10 29.6 3.29 -2 7 9 430.46 15.67 -2 -7 9 442.34 16.47 -2 7 8 273.92 11.49 -2 -7 8 299.57 12.56 -2 7 7 197 10.08 -2 -7 7 218.41 10.22 -2 7 7 188.24 8.88 -2 -7 6 307.15 11.44 -2 -7 6 298.63 12.15 -2 7 5 6.34 1.57 -2 -7 5 4.75 1.83 -2 -7 5 5.62 1.52 -2 7 5 7.8 1.66 -2 -7 5 6.63 1.82 -2 7 4 132.83 6.05 -2 -7 4 124.13 6.48 -2 7 4 118.1 5.79 -2 7 4 109.17 5.93 -2 -7 3 307.45 12.17 -2 7 3 295.64 11.52 -2 -7 3 303.38 12.27 -2 7 3 326.98 11.29 -2 -7 2 579.84 19.23 -2 -7 2 581.51 19.13 -2 7 2 583.33 17.92 2 -7 -1 451.66 14.62 -2 7 1 455.25 15.44 2 -7 0 137.05 6.72 -2 -7 0 131.04 6.18 2 -7 1 416.47 14.61 2 -7 1 284.24 12.12 2 7 2 583.45 18.86 2 -7 2 480.87 19.21 2 7 3 497.42 17.21 2 -7 3 602.81 20.21 2 -7 4 472.64 16.83 2 -7 4 335.19 14.78 2 -7 5 3.94 2.27 2 -7 5 3.18 1.67 2 -7 6 37.16 4.73 2 7 6 46.53 4.21 2 -7 7 57.41 6.13 2 7 7 76.98 5.16 2 7 8 744.62 24.19 2 7 9 187.92 8.55 2 -7 10 1.82 2.52 2 7 10 1.66 1.35 2 -7 11 7.37 2.3 2 7 11 5.09 1.02 -2 8 11 6.72 1.28 -2 -8 11 4.34 1.5 -2 -8 10 1.91 1.68 -2 -8 10 1.38 1.69 -2 8 10 2.85 1.77 -2 8 9 361.5 13.35 -2 -8 9 365.77 14.2 -2 8 8 324.15 12.46 -2 -8 8 350.24 13.62 -2 8 7 84.9 5.51 -2 -8 7 86.4 5.36 -2 -8 7 94.27 6.4 -2 -8 6 0.77 1.39 -2 8 6 0.97 1.43 -2 -8 6 1.49 1.59 -2 -8 6 3.09 2.38 -2 -8 5 651.12 20.76 -2 8 5 630.47 19.96 -2 8 4 828.98 28.87 -2 8 4 1111 29.23 -2 -8 4 1004.51 29.63 -2 8 4 924.91 28.83 -2 -8 4 941.22 29.81 -2 8 3 66.76 4.41 -2 -8 3 75.5 4.87 -2 -8 3 75.3 4.88 -2 8 3 74.47 4.26 -2 -8 2 30.15 2.96 -2 8 2 33.92 2.67 -2 -8 1 367.17 13.46 2 -8 -1 395.32 13.47 -2 -8 1 357.64 13.24 -2 8 1 378.83 12.46 -2 -8 0 1368.8 40.99 2 -8 0 1342.42 41.46 -2 -8 0 1317.93 40.4 2 -8 1 7.16 2.15 2 -8 1 6.01 1.64 -2 -8 -1 4.44 1.33 -2 -8 -2 31.97 2.82 2 -8 2 22.29 2.92 2 -8 3 21.33 3.46 2 -8 4 503 16.92 2 -8 4 271.73 13.91 2 -8 5 144.23 8.43 2 -8 5 80.74 6.37 2 -8 6 81.92 6.73 2 -8 6 52.62 5.28 2 -8 7 34.42 4.85 2 8 7 41.49 3.89 2 -8 8 137.71 9.22 2 8 8 157.27 7.82 2 8 9 66.43 4.66 2 8 10 12.82 2.01 -2 9 11 31.75 2.2 -2 9 11 39.08 2.56 -2 -9 10 4.54 1.81 -2 -9 10 2.24 1.28 -2 9 10 2.41 1.46 -2 9 9 84.74 5.3 -2 -9 9 88.36 5.88 -2 9 8 13.51 2.59 -2 -9 8 10.5 2.36 -2 -9 8 17.16 3.1 -2 -9 7 29.48 3.25 -2 9 7 32.09 3.4 -2 -9 7 30.97 4.09 -2 -9 6 36.27 3.67 -2 9 6 33.58 3.35 -2 -9 6 34.35 4.09 -2 -9 5 50.14 4.21 -2 9 5 48.13 3.73 -2 9 5 39.98 3.69 -2 9 4 29.38 2.95 -2 -9 4 33.51 3.39 -2 9 4 37.46 3.04 -2 -9 4 32.62 3.37 -2 9 4 26.7 2.96 -2 9 3 26.24 2.82 -2 -9 3 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22.75 1.98 5 10 5 10.49 1.1 -5 -11 5 0.37 0.6 -5 -11 4 4.4 0.98 -5 -11 4 6.44 1.12 -5 -11 3 22.74 1.96 -5 -11 3 20.56 1.84 -5 -11 2 2.09 0.96 -5 -11 1 6.96 1.31 -5 -11 1 7.22 1.19 -5 -11 0 16.97 1.78 -5 -11 -1 2.23 0.92 5 11 2 9.36 1.44 -5 -11 -2 4.68 0.95 5 11 4 5.18 0.85 -5 -12 3 1.64 0.71 -5 -12 1 51.59 2.75 -5 -12 0 323.65 10.18 -5 -12 -1 5 0.81 5 12 1 7.45 1.06 5 12 2 3.18 0.75 -6 0 5 372.12 12.44 -6 0 4 254.79 9.43 -6 0 4 241.46 9.45 -6 0 3 8.04 1.92 -6 0 2 29.2 3.38 -6 0 1 212.02 9.87 -6 0 0 418.95 15.79 -6 0 -1 237 10.48 -6 0 -3 34.15 3.56 -6 0 -4 190.42 8.1 -6 0 -5 210.98 8.01 -6 1 6 4.28 1.1 -6 1 5 71.13 4.15 -6 1 4 69.13 4.21 -6 -1 4 64.56 4.14 -6 -1 3 189.34 8.59 -6 1 3 171.93 8.01 -6 -1 2 64.25 4.84 -6 1 2 62.53 4.74 -6 -1 1 288.03 11.91 -6 1 1 276.28 11.82 -6 -1 0 0.64 2.16 -6 1 0 3.78 2.38 -6 1 -1 104.53 6.5 -6 -1 -2 19.33 3.07 -6 1 -2 22.88 3.25 -6 -1 -3 213.05 9.13 -6 -1 -4 188.58 8.03 -6 1 -4 193.72 8.25 -6 1 -5 3.37 1.25 -6 2 6 25.99 2.24 -6 2 5 224.89 8.79 -6 -2 4 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28.64 2.42 -6 -5 5 23.67 1.87 -6 -5 4 7.73 1.05 -6 -5 4 11.46 1.65 -6 -5 3 216.42 8.26 -6 -5 3 222.89 8.78 -6 -5 2 92.56 5.11 -6 -5 2 90.16 5.19 -6 -5 1 47.82 3.69 -6 -5 0 8.54 1.91 -6 5 0 9.69 2.11 -6 -5 -1 70.5 4.37 -6 5 -1 71.81 4.61 -6 -5 -2 16.06 2.04 -6 5 -2 18.45 2.6 -6 -5 -3 59.72 3.31 -6 5 -3 60.25 3.98 -6 5 -4 160.31 6.73 -6 -6 4 245.83 8.6 -6 -6 3 -0.19 1.06 -6 -6 3 0.93 0.83 -6 -6 2 31.1 2.62 -6 -6 1 61.49 3.97 -6 -6 1 65.07 4.07 -6 -6 0 379.13 13.08 -6 -6 -1 189.8 7.78 -6 -6 -1 191.45 7.56 -6 6 -1 173.53 7.44 -6 -6 -2 1.68 0.94 -6 6 -2 4.11 1.58 -6 -6 -2 0.71 1.03 -6 6 -3 32.39 2.63 -6 -7 4 102.4 4.26 -6 -7 3 60.23 3.02 -6 -7 2 9.98 1.43 -6 -7 2 10.58 1.56 -6 -7 1 397.75 13.06 -6 -7 1 404.75 13.06 -6 -7 0 6.04 1.28 -6 -7 0 5.69 1.37 -6 -7 -1 98.53 4.7 -6 -7 -1 100.61 4.44 -6 -7 -2 12.82 1.45 -6 -8 3 0.44 0.63 -6 -8 2 12.69 1.3 -6 -8 2 15.85 1.5 -6 -8 1 119.54 4.89 -6 -8 1 126.7 4.94 -6 -8 0 37.77 2.38 -6 -8 0 37.92 2.25 -6 -8 -1 1.89 0.69