#------------------------------------------------------------------------------ #$Date: 2022-09-23 12:26:15 +0300 (Fri, 23 Sep 2022) $ #$Revision: 278121 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/10/58/8105856.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_8105856 loop_ _publ_author_name 'Tan, Bo' 'Wu, Qi-Yun' 'Wu, Ji-Chun' 'Huo, Shao-Jie' 'He, Xi-Cheng' 'Du, Jiang' _publ_section_title ; Crystal structure of (E)-N-((3R,5S,10S, 13S,14S,17S)-17-((S)-1-(dimethylamino)ethyl)-10,13-dimethylhexadecahydro-1H-cyclopenta[a]phenanthren-3-yl)-2-methylbut-2-enamide -- water -- methanol (1/1/1), C29H54N2O3 ; _journal_issue 4 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 801 _journal_page_last 803 _journal_paper_doi 10.1515/ncrs-2019-0122 _journal_volume 234 _journal_year 2019 _chemical_absolute_configuration . _chemical_formula_moiety 'C28 H48 N2 O, H2 O, C H4 O' _chemical_formula_sum 'C29 H54 N2 O3' _chemical_formula_weight 478.74 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _cell_angle_alpha 90 _cell_angle_beta 93.171(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.8091(11) _cell_length_b 7.6661(8) _cell_length_c 19.095(2) _cell_measurement_reflns_used 2768 _cell_measurement_temperature 250 _cell_measurement_theta_max 23.899 _cell_measurement_theta_min 2.864 _cell_volume 1433.7(3) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _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 250 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_unetI/netI 0.1118 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 14394 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.905 _diffrn_reflns_theta_min 2.864 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6257 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1103 before and 0.0557 after correction. The Ratio of minimum to maximum transmission is 0.8392. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.109 _exptl_crystal_description block _exptl_crystal_F_000 532 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.169 _refine_diff_density_min -0.163 _refine_diff_density_rms 0.036 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0(3) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 320 _refine_ls_number_reflns 6775 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.1498 _refine_ls_R_factor_gt 0.0657 _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^)+(0.0443P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1082 _refine_ls_wR_factor_ref 0.1362 _reflns_Friedel_coverage 0.849 _reflns_Friedel_fraction_full 0.989 _reflns_Friedel_fraction_max 0.980 _reflns_number_gt 3520 _reflns_number_total 6775 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL A_a.res in P2(1) a.res created by SHELXL-2018/3 at 16:13:51 on 16-Jan-2019 CELL 0.71073 9.8091 7.6661 19.0947 90 93.171 90 ZERR 2 0.0011 0.0008 0.0021 0 0.004 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O UNIT 58 108 4 6 L.S. 10 PLAN -5 0 0 SIZE 0.19 0.08 0.05 TEMP -23.15 HTAB BOND $H CONF fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.044300 BASF 0.34838 FVAR 0.98642 O1 4 0.737755 0.531627 0.850831 11.00000 0.03944 0.10923 = 0.05604 -0.00538 0.00712 0.00100 N1 3 0.510097 0.542019 0.848320 11.00000 0.04134 0.07019 = 0.02987 -0.00367 0.00364 -0.00752 AFIX 43 H1 2 0.437562 0.543957 0.872548 11.00000 -1.20000 AFIX 0 N2 3 0.093841 0.513652 0.210278 11.00000 0.05588 0.06394 = 0.03682 0.00329 -0.00723 0.00564 C1 1 0.211639 0.218524 0.401544 11.00000 0.04411 0.03122 = 0.03902 -0.00122 0.00053 0.00250 AFIX 23 H1A 2 0.131620 0.165700 0.421626 11.00000 -1.20000 H1B 2 0.283751 0.130434 0.399698 11.00000 -1.20000 AFIX 0 C2 1 0.174409 0.293837 0.327415 11.00000 0.04157 0.04423 = 0.03497 -0.00166 0.00109 -0.00007 AFIX 23 H2A 2 0.235172 0.246006 0.293170 11.00000 -1.20000 H2B 2 0.080061 0.263994 0.312543 11.00000 -1.20000 AFIX 0 C19 1 0.097824 0.595173 0.280575 11.00000 0.04156 0.04640 = 0.03340 0.00431 0.00029 0.00463 AFIX 13 H19 2 0.004336 0.587170 0.297370 11.00000 -1.20000 AFIX 0 C3 1 0.191353 0.492540 0.332747 11.00000 0.02777 0.03220 = 0.03172 0.00466 0.00430 -0.00309 AFIX 13 H3 2 0.286723 0.520011 0.322282 11.00000 -1.20000 AFIX 0 C4 1 0.176578 0.529481 0.412167 11.00000 0.02615 0.02478 = 0.03270 0.00314 0.00306 -0.00129 C5 1 0.239156 0.696693 0.442149 11.00000 0.05600 0.02786 = 0.03757 0.00632 -0.00493 -0.00304 AFIX 23 H5A 2 0.184545 0.796424 0.424905 11.00000 -1.20000 H5B 2 0.331472 0.710182 0.425728 11.00000 -1.20000 AFIX 0 C6 1 0.246086 0.696717 0.522175 11.00000 0.07642 0.02597 = 0.04081 -0.00379 -0.01015 0.00732 AFIX 23 H6A 2 0.152863 0.702258 0.538039 11.00000 -1.20000 H6B 2 0.293884 0.802371 0.538821 11.00000 -1.20000 AFIX 0 C7 1 0.317875 0.538031 0.556079 11.00000 0.03289 0.02003 = 0.03260 0.00349 0.00272 -0.00051 AFIX 13 H7 2 0.414649 0.545785 0.544183 11.00000 -1.20000 AFIX 0 C8 1 0.262907 0.366065 0.524046 11.00000 0.02736 0.02138 = 0.03241 0.00417 0.00162 -0.00006 AFIX 13 H8 2 0.167861 0.350396 0.537834 11.00000 -1.20000 AFIX 0 C9 1 0.261090 0.376143 0.444216 11.00000 0.02492 0.02190 = 0.03366 -0.00244 0.00370 0.00010 AFIX 13 H9 2 0.356651 0.396786 0.432204 11.00000 -1.20000 AFIX 0 C10 1 0.347518 0.212936 0.552871 11.00000 0.05336 0.02312 = 0.03684 0.00043 -0.00518 0.00865 AFIX 23 H10A 2 0.304575 0.103884 0.536417 11.00000 -1.20000 H10B 2 0.438613 0.218472 0.534343 11.00000 -1.20000 AFIX 0 C11 1 0.361928 0.210697 0.632621 11.00000 0.05345 0.02544 = 0.04249 0.00522 -0.00428 0.00404 AFIX 23 H11A 2 0.273393 0.181629 0.650978 11.00000 -1.20000 H11B 2 0.426767 0.119104 0.647723 11.00000 -1.20000 AFIX 0 C12 1 0.410452 0.382717 0.663472 11.00000 0.02890 0.02973 = 0.03202 0.00320 0.00034 0.00164 AFIX 13 H12 2 0.501525 0.404408 0.645320 11.00000 -1.20000 AFIX 0 C13 1 0.318413 0.536455 0.637464 11.00000 0.03438 0.02626 = 0.02786 0.00067 0.00456 -0.00173 C14 1 0.383092 0.705243 0.667793 11.00000 0.06614 0.03053 = 0.03982 -0.00202 -0.00087 -0.00286 AFIX 23 H14A 2 0.470448 0.724494 0.646471 11.00000 -1.20000 H14B 2 0.323207 0.803623 0.654666 11.00000 -1.20000 AFIX 0 C15 1 0.407733 0.703272 0.747629 11.00000 0.06809 0.04414 = 0.03713 -0.00574 -0.00392 -0.00665 AFIX 23 H15A 2 0.454270 0.811084 0.762765 11.00000 -1.20000 H15B 2 0.319747 0.699130 0.769513 11.00000 -1.20000 AFIX 0 C16 1 0.493345 0.548157 0.771901 11.00000 0.03719 0.05722 = 0.02876 0.00054 0.00178 -0.00935 AFIX 13 H16 2 0.584950 0.561315 0.753231 11.00000 -1.20000 AFIX 0 C17 1 0.431079 0.377571 0.743031 11.00000 0.04156 0.03748 = 0.03646 0.00302 0.00150 0.00059 AFIX 23 H17A 2 0.491491 0.280133 0.756730 11.00000 -1.20000 H17B 2 0.342987 0.357747 0.763530 11.00000 -1.20000 AFIX 0 C18 1 0.173623 0.518995 0.662594 11.00000 0.03688 0.06120 = 0.04219 -0.00757 0.00670 0.00613 AFIX 137 H18A 2 0.131507 0.414208 0.642848 11.00000 -1.50000 H18B 2 0.120116 0.619948 0.647484 11.00000 -1.50000 H18C 2 0.177446 0.511760 0.713381 11.00000 -1.50000 AFIX 0 C20 1 0.134680 0.789493 0.279177 11.00000 0.07561 0.04453 = 0.04549 0.01363 -0.00086 0.00225 AFIX 137 H20A 2 0.229513 0.802484 0.268184 11.00000 -1.50000 H20B 2 0.121101 0.840699 0.324720 11.00000 -1.50000 H20C 2 0.076738 0.848210 0.243743 11.00000 -1.50000 AFIX 0 C23 1 0.026082 0.517840 0.428912 11.00000 0.03491 0.04776 = 0.03946 0.00599 0.00620 0.00868 AFIX 137 H23A 2 -0.016645 0.421416 0.403169 11.00000 -1.50000 H23B 2 -0.019813 0.625728 0.415349 11.00000 -1.50000 H23C 2 0.019308 0.498998 0.478832 11.00000 -1.50000 AFIX 0 C22 1 -0.015634 0.590966 0.163363 11.00000 0.11768 0.10743 = 0.05954 0.00766 -0.04593 0.01654 AFIX 137 H22A 2 -0.102612 0.579310 0.184732 11.00000 -1.50000 H22B 2 -0.019566 0.530640 0.118642 11.00000 -1.50000 H22C 2 0.003690 0.713505 0.156036 11.00000 -1.50000 AFIX 0 C21 1 0.224198 0.522620 0.175951 11.00000 0.09529 0.08306 = 0.04169 0.00600 0.02278 -0.00124 AFIX 137 H21A 2 0.218052 0.453577 0.133323 11.00000 -1.50000 H21B 2 0.296733 0.477228 0.207410 11.00000 -1.50000 H21C 2 0.243802 0.642971 0.164475 11.00000 -1.50000 AFIX 0 C24 1 0.632196 0.533564 0.882379 11.00000 0.04271 0.04261 = 0.03865 -0.00636 -0.00280 -0.00150 C25 1 0.640020 0.517031 0.960668 11.00000 0.04881 0.05273 = 0.04550 -0.00776 -0.00287 -0.00583 C26 1 0.544457 0.576915 0.998280 11.00000 0.05394 0.07335 = 0.04474 -0.00766 -0.00380 -0.00047 AFIX 43 H26 2 0.468001 0.627580 0.974387 11.00000 -1.20000 AFIX 0 C27 1 0.545997 0.571850 1.078064 11.00000 0.11059 0.11337 = 0.03689 -0.01016 0.01272 -0.00515 AFIX 137 H27A 2 0.538767 0.451908 1.093607 11.00000 -1.50000 H27B 2 0.469506 0.638541 1.093902 11.00000 -1.50000 H27C 2 0.630699 0.621876 1.097493 11.00000 -1.50000 AFIX 0 C28 1 0.770680 0.435370 0.991680 11.00000 0.06639 0.11328 = 0.06637 0.00136 -0.01428 0.02922 AFIX 137 H28A 2 0.788454 0.327649 0.967142 11.00000 -1.50000 H28B 2 0.761027 0.410795 1.040991 11.00000 -1.50000 H28C 2 0.846106 0.515449 0.986735 11.00000 -1.50000 AFIX 6 O2 4 0.996527 0.666014 0.836028 11.00000 0.05049 0.09083 = 0.09051 0.02065 -0.01052 0.00167 H2C 2 0.977259 0.758986 0.812309 11.00000 -1.50000 H2D 2 0.919488 0.631922 0.850582 11.00000 -1.50000 AFIX 0 O3 4 1.227597 0.524702 0.898422 11.00000 0.04519 0.14628 = 0.06022 0.02343 0.00729 0.01267 AFIX 147 H3A 2 1.161022 0.556122 0.872776 11.00000 -1.50000 AFIX 0 C29 1 1.181834 0.445589 0.958539 11.00000 0.06994 0.09816 = 0.07257 0.01264 -0.00327 -0.00477 AFIX 137 H29A 2 1.109155 0.364139 0.945447 11.00000 -1.50000 H29B 2 1.147718 0.534076 0.989386 11.00000 -1.50000 H29C 2 1.256792 0.383512 0.982606 11.00000 -1.50000 AFIX 0 HKLF 4 REM A_a.res in P2(1) REM wR2 = 0.1362, GooF = S = 1.013, Restrained GooF = 1.013 for all data REM R1 = 0.0657 for 3520 Fo > 4sig(Fo) and 0.1498 for all 6775 data REM 320 parameters refined using 1 restraints END WGHT 0.0443 0.0000 REM Instructions for potential hydrogen bonds EQIV $1 x-1, y, z HTAB N1 O3_$1 HTAB O3 O2 REM Highest difference peak 0.169, deepest hole -0.163, 1-sigma level 0.036 Q1 1 0.1045 0.5112 0.3706 11.00000 0.05 0.17 Q2 1 0.6485 0.5335 1.1039 11.00000 0.05 0.16 Q3 1 0.0834 0.7104 0.5384 11.00000 0.05 0.16 Q4 1 0.8068 0.5244 0.8908 11.00000 0.05 0.15 Q5 1 0.2447 -0.0112 0.3464 11.00000 0.05 0.15 REM The information below was added by Olex2. REM REM R1 = 0.0657 for 3520 Fo > 4sig(Fo) and 0.1498 for all 14410 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.17, deepest hole -0.16 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1498 REM R1_gt = 0.0657 REM wR_ref = 0.1362 REM GOOF = 1.013 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 14410 REM Reflections_gt = 3520 REM Parameters = n/a REM Hole = -0.16 REM Peak = 0.17 REM Flack = n/a ; _cod_data_source_file suppl_ncrs-2019-0122_suppl.cif _cod_data_source_block a _cod_database_code 8105856 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.996 _shelx_estimated_absorpt_t_min 0.987 _olex2_refinement_description ; 1. Twinned data refinement Scales: 1(3) 0(3) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups, All O(H,H) groups 3.a Free rotating group: O2(H2C,H2D) 3.b Ternary CH refined with riding coordinates: C19(H19), C3(H3), C7(H7), C8(H8), C9(H9), C12(H12), C16(H16) 3.c Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C5(H5A,H5B), C6(H6A,H6B), C10(H10A,H10B), C11(H11A, H11B), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B) 3.d Aromatic/amide H refined with riding coordinates: N1(H1), C26(H26) 3.e Idealised Me refined as rotating group: C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C22(H22A,H22B, H22C), C21(H21A,H21B,H21C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A, H29B,H29C) 3.f Idealised tetrahedral OH refined as rotating group: O3(H3A) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz '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 O1 O 0.7378(3) 0.5316(5) 0.85083(14) 0.0681(9) Uani 1 1 d . . . . . N1 N 0.5101(3) 0.5420(5) 0.84832(14) 0.0471(9) Uani 1 1 d . . . . . H1 H 0.437562 0.543957 0.872548 0.056 Uiso 1 1 calc R . . . . N2 N 0.0938(4) 0.5137(5) 0.21028(17) 0.0526(9) Uani 1 1 d . . . . . C1 C 0.2116(4) 0.2185(5) 0.40154(19) 0.0382(10) Uani 1 1 d . . . . . H1A H 0.131620 0.165700 0.421626 0.046 Uiso 1 1 calc R . . . . H1B H 0.283751 0.130434 0.399698 0.046 Uiso 1 1 calc R . . . . C2 C 0.1744(4) 0.2938(5) 0.3274(2) 0.0403(11) Uani 1 1 d . . . . . H2A H 0.235172 0.246006 0.293170 0.048 Uiso 1 1 calc R . . . . H2B H 0.080061 0.263994 0.312543 0.048 Uiso 1 1 calc R . . . . C19 C 0.0978(4) 0.5952(5) 0.28057(19) 0.0405(11) Uani 1 1 d . . . . . H19 H 0.004336 0.587170 0.297370 0.049 Uiso 1 1 calc R . . . . C3 C 0.1914(4) 0.4925(5) 0.33275(18) 0.0305(9) Uani 1 1 d . . . . . H3 H 0.286723 0.520011 0.322282 0.037 Uiso 1 1 calc R . . . . C4 C 0.1766(3) 0.5295(6) 0.41217(17) 0.0278(8) Uani 1 1 d . . . . . C5 C 0.2392(4) 0.6967(5) 0.44215(19) 0.0408(11) Uani 1 1 d . . . . . H5A H 0.184545 0.796424 0.424905 0.049 Uiso 1 1 calc R . . . . H5B H 0.331472 0.710182 0.425728 0.049 Uiso 1 1 calc R . . . . C6 C 0.2461(5) 0.6967(5) 0.5222(2) 0.0482(13) Uani 1 1 d . . . . . H6A H 0.152863 0.702258 0.538039 0.058 Uiso 1 1 calc R . . . . H6B H 0.293884 0.802371 0.538821 0.058 Uiso 1 1 calc R . . . . C7 C 0.3179(3) 0.5380(5) 0.55608(16) 0.0285(8) Uani 1 1 d . . . . . H7 H 0.414649 0.545785 0.544183 0.034 Uiso 1 1 calc R . . . . C8 C 0.2629(4) 0.3661(5) 0.52405(19) 0.0271(9) Uani 1 1 d . . . . . H8 H 0.167861 0.350396 0.537834 0.032 Uiso 1 1 calc R . . . . C9 C 0.2611(4) 0.3761(5) 0.44422(18) 0.0268(8) Uani 1 1 d . . . . . H9 H 0.356651 0.396786 0.432204 0.032 Uiso 1 1 calc R . . . . C10 C 0.3475(4) 0.2129(5) 0.55287(18) 0.0381(10) Uani 1 1 d . . . . . H10A H 0.304575 0.103884 0.536417 0.046 Uiso 1 1 calc R . . . . H10B H 0.438613 0.218472 0.534343 0.046 Uiso 1 1 calc R . . . . C11 C 0.3619(4) 0.2107(5) 0.63262(19) 0.0407(11) Uani 1 1 d . . . . . H11A H 0.273393 0.181629 0.650978 0.049 Uiso 1 1 calc R . . . . H11B H 0.426767 0.119104 0.647723 0.049 Uiso 1 1 calc R . . . . C12 C 0.4105(4) 0.3827(5) 0.66347(18) 0.0303(9) Uani 1 1 d . . . . . H12 H 0.501525 0.404408 0.645320 0.036 Uiso 1 1 calc R . . . . C13 C 0.3184(3) 0.5365(5) 0.63746(16) 0.0294(8) Uani 1 1 d . . . . . C14 C 0.3831(5) 0.7052(6) 0.6678(2) 0.0456(11) Uani 1 1 d . . . . . H14A H 0.470448 0.724494 0.646471 0.055 Uiso 1 1 calc R . . . . H14B H 0.323207 0.803623 0.654666 0.055 Uiso 1 1 calc R . . . . C15 C 0.4077(5) 0.7033(6) 0.7476(2) 0.0500(12) Uani 1 1 d . . . . . H15A H 0.454270 0.811084 0.762765 0.060 Uiso 1 1 calc R . . . . H15B H 0.319747 0.699130 0.769513 0.060 Uiso 1 1 calc R . . . . C16 C 0.4933(4) 0.5482(6) 0.77190(18) 0.0411(10) Uani 1 1 d . . . . . H16 H 0.584950 0.561315 0.753231 0.049 Uiso 1 1 calc R . . . . C17 C 0.4311(4) 0.3776(6) 0.74303(19) 0.0385(10) Uani 1 1 d . . . . . H17A H 0.491491 0.280133 0.756730 0.046 Uiso 1 1 calc R . . . . H17B H 0.342987 0.357747 0.763530 0.046 Uiso 1 1 calc R . . . . C18 C 0.1736(4) 0.5190(6) 0.66259(19) 0.0466(11) Uani 1 1 d . . . . . H18A H 0.131507 0.414208 0.642848 0.070 Uiso 1 1 calc GR . . . . H18B H 0.120116 0.619948 0.647484 0.070 Uiso 1 1 calc GR . . . . H18C H 0.177446 0.511760 0.713381 0.070 Uiso 1 1 calc GR . . . . C20 C 0.1347(5) 0.7895(6) 0.2792(2) 0.0554(13) Uani 1 1 d . . . . . H20A H 0.229513 0.802484 0.268184 0.083 Uiso 1 1 calc GR . . . . H20B H 0.121101 0.840699 0.324720 0.083 Uiso 1 1 calc GR . . . . H20C H 0.076738 0.848210 0.243743 0.083 Uiso 1 1 calc GR . . . . C23 C 0.0261(3) 0.5178(6) 0.42891(19) 0.0406(10) Uani 1 1 d . . . . . H23A H -0.016645 0.421416 0.403169 0.061 Uiso 1 1 calc GR . . . . H23B H -0.019813 0.625728 0.415349 0.061 Uiso 1 1 calc GR . . . . H23C H 0.019308 0.498998 0.478832 0.061 Uiso 1 1 calc GR . . . . C22 C -0.0156(6) 0.5910(8) 0.1634(3) 0.097(2) Uani 1 1 d . . . . . H22A H -0.102612 0.579310 0.184732 0.145 Uiso 1 1 calc GR . . . . H22B H -0.019566 0.530640 0.118642 0.145 Uiso 1 1 calc GR . . . . H22C H 0.003690 0.713505 0.156036 0.145 Uiso 1 1 calc GR . . . . C21 C 0.2242(5) 0.5226(8) 0.1760(2) 0.0726(15) Uani 1 1 d . . . . . H21A H 0.218052 0.453577 0.133323 0.109 Uiso 1 1 calc GR . . . . H21B H 0.296733 0.477228 0.207410 0.109 Uiso 1 1 calc GR . . . . H21C H 0.243802 0.642971 0.164475 0.109 Uiso 1 1 calc GR . . . . C24 C 0.6322(4) 0.5336(6) 0.88238(19) 0.0415(10) Uani 1 1 d . . . . . C25 C 0.6400(4) 0.5170(6) 0.9607(2) 0.0492(11) Uani 1 1 d . . . . . C26 C 0.5445(5) 0.5769(7) 0.9983(2) 0.0576(13) Uani 1 1 d . . . . . H26 H 0.468001 0.627580 0.974387 0.069 Uiso 1 1 calc R . . . . C27 C 0.5460(6) 0.5719(8) 1.0781(2) 0.0866(18) Uani 1 1 d . . . . . H27A H 0.538767 0.451908 1.093607 0.130 Uiso 1 1 calc GR . . . . H27B H 0.469506 0.638541 1.093902 0.130 Uiso 1 1 calc GR . . . . H27C H 0.630699 0.621876 1.097493 0.130 Uiso 1 1 calc GR . . . . C28 C 0.7707(5) 0.4354(8) 0.9917(3) 0.0827(19) Uani 1 1 d . . . . . H28A H 0.788454 0.327649 0.967142 0.124 Uiso 1 1 calc GR . . . . H28B H 0.761027 0.410795 1.040991 0.124 Uiso 1 1 calc GR . . . . H28C H 0.846106 0.515449 0.986735 0.124 Uiso 1 1 calc GR . . . . O2 O 0.9965(3) 0.6660(5) 0.8360(2) 0.0778(12) Uani 1 1 d . . . . . H2C H 0.977259 0.758986 0.812309 0.117 Uiso 1 1 d G . . . . H2D H 0.919488 0.631922 0.850582 0.117 Uiso 1 1 d G . . . . O3 O 1.2276(3) 0.5247(7) 0.89842(17) 0.0837(11) Uani 1 1 d . . . . . H3A H 1.161022 0.556122 0.872776 0.126 Uiso 1 1 calc GR . . . . C29 C 1.1818(6) 0.4456(8) 0.9585(3) 0.0805(18) Uani 1 1 d . . . . . H29A H 1.109155 0.364139 0.945447 0.121 Uiso 1 1 calc GR . . . . H29B H 1.147718 0.534076 0.989386 0.121 Uiso 1 1 calc GR . . . . H29C H 1.256792 0.383512 0.982606 0.121 Uiso 1 1 calc GR . . . . 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 O1 0.0394(17) 0.109(3) 0.0560(19) -0.005(2) 0.0071(14) 0.001(2) N1 0.041(2) 0.070(2) 0.0299(17) -0.004(2) 0.0036(14) -0.008(2) N2 0.056(2) 0.064(3) 0.037(2) 0.003(2) -0.0072(16) 0.006(2) C1 0.044(3) 0.031(2) 0.039(2) -0.001(2) 0.0005(19) 0.002(2) C2 0.042(3) 0.044(3) 0.035(2) -0.002(2) 0.001(2) 0.000(2) C19 0.042(3) 0.046(3) 0.033(2) 0.004(2) 0.0003(19) 0.005(2) C3 0.028(2) 0.032(2) 0.032(2) 0.0047(18) 0.0043(16) -0.0031(18) C4 0.0262(18) 0.0248(19) 0.0327(19) 0.0031(19) 0.0031(14) -0.001(2) C5 0.056(3) 0.028(2) 0.038(3) 0.006(2) -0.005(2) -0.003(2) C6 0.076(4) 0.026(2) 0.041(3) -0.004(2) -0.010(2) 0.007(3) C7 0.0329(19) 0.0200(19) 0.0326(19) 0.0035(19) 0.0027(15) -0.001(2) C8 0.027(2) 0.021(2) 0.032(2) 0.0042(17) 0.0016(17) -0.0001(18) C9 0.0249(19) 0.0219(19) 0.034(2) -0.0024(19) 0.0037(16) 0.0001(18) C10 0.053(3) 0.023(2) 0.037(2) 0.0004(19) -0.0052(19) 0.009(2) C11 0.053(3) 0.025(2) 0.042(3) 0.005(2) -0.004(2) 0.004(2) C12 0.029(2) 0.030(2) 0.032(2) 0.003(2) 0.0003(17) 0.002(2) C13 0.034(2) 0.026(2) 0.0279(19) 0.0007(19) 0.0046(15) -0.002(2) C14 0.066(3) 0.031(2) 0.040(3) -0.002(2) -0.001(2) -0.003(2) C15 0.068(3) 0.044(3) 0.037(3) -0.006(2) -0.004(2) -0.007(3) C16 0.037(2) 0.057(3) 0.029(2) 0.001(2) 0.0018(16) -0.009(2) C17 0.042(2) 0.037(2) 0.036(2) 0.003(2) 0.0015(19) 0.001(2) C18 0.037(2) 0.061(3) 0.042(2) -0.008(2) 0.0067(17) 0.006(3) C20 0.076(3) 0.045(3) 0.045(3) 0.014(2) -0.001(2) 0.002(3) C23 0.035(2) 0.048(3) 0.039(2) 0.006(2) 0.0062(16) 0.009(2) C22 0.118(5) 0.107(5) 0.060(3) 0.008(3) -0.046(3) 0.017(4) C21 0.095(4) 0.083(4) 0.042(3) 0.006(3) 0.023(2) -0.001(4) C24 0.043(2) 0.043(2) 0.039(2) -0.006(2) -0.0028(19) -0.002(3) C25 0.049(3) 0.053(3) 0.045(2) -0.008(3) -0.003(2) -0.006(3) C26 0.054(3) 0.073(4) 0.045(3) -0.008(3) -0.004(2) 0.000(3) C27 0.111(4) 0.113(5) 0.037(3) -0.010(3) 0.013(3) -0.005(4) C28 0.066(4) 0.113(5) 0.066(4) 0.001(3) -0.014(3) 0.029(3) O2 0.050(2) 0.091(3) 0.091(3) 0.021(2) -0.011(2) 0.002(2) O3 0.0452(19) 0.146(4) 0.060(2) 0.023(3) 0.0073(15) 0.013(3) C29 0.070(4) 0.098(4) 0.073(4) 0.013(3) -0.003(3) -0.005(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 C16 N1 H1 118.7 . . C24 N1 H1 118.7 . . C24 N1 C16 122.5(3) . . C19 N2 C22 111.2(4) . . C21 N2 C19 113.9(3) . . C21 N2 C22 109.3(4) . . H1A C1 H1B 108.9 . . C2 C1 H1A 110.9 . . C2 C1 H1B 110.9 . . C9 C1 H1A 110.9 . . C9 C1 H1B 110.9 . . C9 C1 C2 104.2(3) . . C1 C2 H2A 110.4 . . C1 C2 H2B 110.4 . . H2A C2 H2B 108.6 . . C3 C2 C1 106.8(3) . . C3 C2 H2A 110.4 . . C3 C2 H2B 110.4 . . N2 C19 H19 106.8 . . N2 C19 C3 110.9(3) . . N2 C19 C20 112.9(3) . . C3 C19 H19 106.8 . . C20 C19 H19 106.8 . . C20 C19 C3 112.1(3) . . C2 C3 H3 107.3 . . C2 C3 C4 103.3(3) . . C19 C3 C2 114.0(3) . . C19 C3 H3 107.3 . . C19 C3 C4 117.0(3) . . C4 C3 H3 107.3 . . C5 C4 C3 117.6(3) . . C5 C4 C9 107.2(3) . . C5 C4 C23 110.2(3) . . C9 C4 C3 99.8(3) . . C23 C4 C3 109.6(3) . . C23 C4 C9 112.1(3) . . C4 C5 H5A 109.2 . . C4 C5 H5B 109.2 . . C4 C5 C6 111.8(3) . . H5A C5 H5B 107.9 . . C6 C5 H5A 109.2 . . C6 C5 H5B 109.2 . . C5 C6 H6A 108.6 . . C5 C6 H6B 108.6 . . C5 C6 C7 114.7(3) . . H6A C6 H6B 107.6 . . C7 C6 H6A 108.6 . . C7 C6 H6B 108.6 . . C6 C7 H7 106.2 . . C6 C7 C8 111.7(3) . . C6 C7 C13 113.9(3) . . C8 C7 H7 106.2 . . C8 C7 C13 111.9(3) . . C13 C7 H7 106.2 . . C7 C8 H8 108.2 . . C9 C8 C7 109.8(3) . . C9 C8 H8 108.2 . . C10 C8 C7 110.2(3) . . C10 C8 H8 108.2 . . C10 C8 C9 112.1(3) . . C1 C9 C4 104.1(3) . . C1 C9 C8 118.7(3) . . C1 C9 H9 106.3 . . C4 C9 H9 106.3 . . C8 C9 C4 114.2(3) . . C8 C9 H9 106.3 . . C8 C10 H10A 109.0 . . C8 C10 H10B 109.0 . . H10A C10 H10B 107.8 . . C11 C10 C8 112.9(3) . . C11 C10 H10A 109.0 . . C11 C10 H10B 109.0 . . C10 C11 H11A 109.0 . . C10 C11 H11B 109.0 . . H11A C11 H11B 107.8 . . C12 C11 C10 113.0(3) . . C12 C11 H11A 109.0 . . C12 C11 H11B 109.0 . . C11 C12 H12 106.3 . . C11 C12 C13 111.9(3) . . C11 C12 C17 112.8(3) . . C13 C12 H12 106.3 . . C17 C12 H12 106.3 . . C17 C12 C13 112.5(3) . . C12 C13 C7 107.2(3) . . C14 C13 C7 110.4(3) . . C14 C13 C12 107.3(3) . . C18 C13 C7 111.3(3) . . C18 C13 C12 111.6(3) . . C18 C13 C14 109.0(3) . . C13 C14 H14A 108.8 . . C13 C14 H14B 108.8 . . H14A C14 H14B 107.7 . . C15 C14 C13 113.9(3) . . C15 C14 H14A 108.8 . . C15 C14 H14B 108.8 . . C14 C15 H15A 109.3 . . C14 C15 H15B 109.3 . . H15A C15 H15B 108.0 . . C16 C15 C14 111.5(4) . . C16 C15 H15A 109.3 . . C16 C15 H15B 109.3 . . N1 C16 C15 111.2(3) . . N1 C16 H16 108.0 . . N1 C16 C17 110.6(3) . . C15 C16 H16 108.0 . . C15 C16 C17 110.9(3) . . C17 C16 H16 108.0 . . C12 C17 C16 111.4(3) . . C12 C17 H17A 109.3 . . C12 C17 H17B 109.3 . . C16 C17 H17A 109.3 . . C16 C17 H17B 109.3 . . H17A C17 H17B 108.0 . . C13 C18 H18A 109.5 . . C13 C18 H18B 109.5 . . C13 C18 H18C 109.5 . . H18A C18 H18B 109.5 . . H18A C18 H18C 109.5 . . H18B C18 H18C 109.5 . . C19 C20 H20A 109.5 . . C19 C20 H20B 109.5 . . C19 C20 H20C 109.5 . . H20A C20 H20B 109.5 . . H20A C20 H20C 109.5 . . H20B C20 H20C 109.5 . . C4 C23 H23A 109.5 . . C4 C23 H23B 109.5 . . C4 C23 H23C 109.5 . . H23A C23 H23B 109.5 . . H23A C23 H23C 109.5 . . H23B C23 H23C 109.5 . . N2 C22 H22A 109.5 . . N2 C22 H22B 109.5 . . N2 C22 H22C 109.5 . . H22A C22 H22B 109.5 . . H22A C22 H22C 109.5 . . H22B C22 H22C 109.5 . . N2 C21 H21A 109.5 . . N2 C21 H21B 109.5 . . N2 C21 H21C 109.5 . . H21A C21 H21B 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . O1 C24 N1 121.4(3) . . O1 C24 C25 119.4(4) . . N1 C24 C25 119.1(4) . . C24 C25 C28 114.8(4) . . C26 C25 C24 121.6(4) . . C26 C25 C28 123.5(4) . . C25 C26 H26 117.4 . . C25 C26 C27 125.3(5) . . C27 C26 H26 117.4 . . C26 C27 H27A 109.5 . . C26 C27 H27B 109.5 . . C26 C27 H27C 109.5 . . H27A C27 H27B 109.5 . . H27A C27 H27C 109.5 . . H27B C27 H27C 109.5 . . C25 C28 H28A 109.5 . . C25 C28 H28B 109.5 . . C25 C28 H28C 109.5 . . H28A C28 H28B 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . H2C O2 H2D 104.5 . . C29 O3 H3A 109.5 . . O3 C29 H29A 109.5 . . O3 C29 H29B 109.5 . . O3 C29 H29C 109.5 . . H29A C29 H29B 109.5 . . H29A C29 H29C 109.5 . . H29B C29 H29C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O1 C24 1.226(4) . N1 H1 0.8700 . N1 C16 1.460(4) . N1 C24 1.332(4) . N2 C19 1.479(5) . N2 C22 1.483(5) . N2 C21 1.470(5) . C1 H1A 0.9800 . C1 H1B 0.9800 . C1 C2 1.553(5) . C1 C9 1.522(5) . C2 H2A 0.9800 . C2 H2B 0.9800 . C2 C3 1.535(5) . C19 H19 0.9900 . C19 C3 1.534(5) . C19 C20 1.533(5) . C3 H3 0.9900 . C3 C4 1.557(5) . C4 C5 1.519(5) . C4 C9 1.545(5) . C4 C23 1.530(4) . C5 H5A 0.9800 . C5 H5B 0.9800 . C5 C6 1.526(5) . C6 H6A 0.9800 . C6 H6B 0.9800 . C6 C7 1.531(5) . C7 H7 0.9900 . C7 C8 1.538(5) . C7 C13 1.554(4) . C8 H8 0.9900 . C8 C9 1.525(5) . C8 C10 1.523(5) . C9 H9 0.9900 . C10 H10A 0.9800 . C10 H10B 0.9800 . C10 C11 1.522(5) . C11 H11A 0.9800 . C11 H11B 0.9800 . C11 C12 1.510(5) . C12 H12 0.9900 . C12 C13 1.550(5) . C12 C17 1.522(5) . C13 C14 1.540(6) . C13 C18 1.530(5) . C14 H14A 0.9800 . C14 H14B 0.9800 . C14 C15 1.530(5) . C15 H15A 0.9800 . C15 H15B 0.9800 . C15 C16 1.514(6) . C16 H16 0.9900 . C16 C17 1.533(6) . C17 H17A 0.9800 . C17 H17B 0.9800 . C18 H18A 0.9700 . C18 H18B 0.9700 . C18 H18C 0.9700 . C20 H20A 0.9700 . C20 H20B 0.9700 . C20 H20C 0.9700 . C23 H23A 0.9700 . C23 H23B 0.9700 . C23 H23C 0.9700 . C22 H22A 0.9700 . C22 H22B 0.9700 . C22 H22C 0.9700 . C21 H21A 0.9700 . C21 H21B 0.9700 . C21 H21C 0.9700 . C24 C25 1.498(5) . C25 C26 1.296(6) . C25 C28 1.517(6) . C26 H26 0.9400 . C26 C27 1.523(6) . C27 H27A 0.9700 . C27 H27B 0.9700 . C27 H27C 0.9700 . C28 H28A 0.9700 . C28 H28B 0.9700 . C28 H28C 0.9700 . O2 H2C 0.8599 . O2 H2D 0.8601 . O3 H3A 0.8300 . O3 C29 1.394(5) . C29 H29A 0.9700 . C29 H29B 0.9700 . C29 H29C 0.9700 . 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 O1 C24 C25 C26 155.5(5) . . . . O1 C24 C25 C28 -21.1(7) . . . . N1 C16 C17 C12 179.0(3) . . . . N1 C24 C25 C26 -27.5(7) . . . . N1 C24 C25 C28 155.8(5) . . . . N2 C19 C3 C2 -43.1(4) . . . . N2 C19 C3 C4 -163.8(3) . . . . C1 C2 C3 C19 -151.3(3) . . . . C1 C2 C3 C4 -23.2(4) . . . . C2 C1 C9 C4 32.0(4) . . . . C2 C1 C9 C8 160.4(3) . . . . C2 C3 C4 C5 157.3(3) . . . . C2 C3 C4 C9 41.9(3) . . . . C2 C3 C4 C23 -75.9(4) . . . . C19 C3 C4 C5 -76.5(4) . . . . C19 C3 C4 C9 168.1(3) . . . . C19 C3 C4 C23 50.3(4) . . . . C3 C4 C5 C6 -167.0(3) . . . . C3 C4 C9 C1 -46.0(3) . . . . C3 C4 C9 C8 -177.1(3) . . . . C4 C5 C6 C7 53.7(5) . . . . C5 C4 C9 C1 -169.1(3) . . . . C5 C4 C9 C8 59.9(4) . . . . C5 C6 C7 C8 -49.5(4) . . . . C5 C6 C7 C13 -177.5(3) . . . . C6 C7 C8 C9 49.5(4) . . . . C6 C7 C8 C10 173.4(3) . . . . C6 C7 C13 C12 -172.6(3) . . . . C6 C7 C13 C14 -56.0(4) . . . . C6 C7 C13 C18 65.2(5) . . . . C7 C8 C9 C1 179.3(3) . . . . C7 C8 C9 C4 -57.2(4) . . . . C7 C8 C10 C11 51.9(4) . . . . C7 C13 C14 C15 -171.2(3) . . . . C8 C7 C13 C12 59.5(4) . . . . C8 C7 C13 C14 176.1(3) . . . . C8 C7 C13 C18 -62.7(4) . . . . C8 C10 C11 C12 -51.3(5) . . . . C9 C1 C2 C3 -5.2(4) . . . . C9 C4 C5 C6 -55.7(4) . . . . C9 C8 C10 C11 174.5(3) . . . . C10 C8 C9 C1 56.5(4) . . . . C10 C8 C9 C4 -180.0(3) . . . . C10 C11 C12 C13 54.6(4) . . . . C10 C11 C12 C17 -177.3(3) . . . . C11 C12 C13 C7 -57.4(4) . . . . C11 C12 C13 C14 -176.0(3) . . . . C11 C12 C13 C18 64.7(4) . . . . C11 C12 C17 C16 174.5(3) . . . . C12 C13 C14 C15 -54.7(4) . . . . C13 C7 C8 C9 178.6(3) . . . . C13 C7 C8 C10 -57.5(4) . . . . C13 C12 C17 C16 -57.7(4) . . . . C13 C14 C15 C16 55.3(5) . . . . C14 C15 C16 N1 -176.9(3) . . . . C14 C15 C16 C17 -53.4(4) . . . . C15 C16 C17 C12 55.1(4) . . . . C16 N1 C24 O1 0.5(7) . . . . C16 N1 C24 C25 -176.4(4) . . . . C17 C12 C13 C7 174.3(3) . . . . C17 C12 C13 C14 55.7(4) . . . . C17 C12 C13 C18 -63.6(4) . . . . C18 C13 C14 C15 66.3(4) . . . . C20 C19 C3 C2 -170.4(4) . . . . C20 C19 C3 C4 69.0(4) . . . . C23 C4 C5 C6 66.5(4) . . . . C23 C4 C9 C1 69.9(4) . . . . C23 C4 C9 C8 -61.1(4) . . . . C22 N2 C19 C3 169.1(4) . . . . C22 N2 C19 C20 -64.1(5) . . . . C21 N2 C19 C3 -66.9(5) . . . . C21 N2 C19 C20 59.9(5) . . . . C24 N1 C16 C15 -126.0(5) . . . . C24 N1 C16 C17 110.3(5) . . . . C24 C25 C26 C27 -177.7(4) . . . . C28 C25 C26 C27 -1.4(8) . . . . loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma -2 0 0 2499.05 61.99 2 0 0 2496.35 62.19 2 0 0 2581.14 61.79 -2 0 0 2479.25 62.09 3 0 0 297.27 13.4 3 0 0 282.67 12.6 -3 0 0 292.67 13.7 -3 0 0 271.67 13 4 0 0 1170.98 37 4 0 0 1158.98 35.2 -4 0 0 1143.39 36.2 -4 0 0 1145.89 36.3 5 0 0 732.23 27.1 -5 0 0 754.02 28.9 -5 0 0 732.63 28.7 -6 0 0 48.7 9.4 -6 0 0 38.9 8.5 -7 0 0 27.4 9 -7 0 0 39.4 9.3 -8 0 0 103.79 13.7 -8 0 0 87.59 14.9 -9 0 0 14.7 9.6 -9 0 0 8.9 7.7 -10 0 0 7.1 8.5 -10 0 0 0.7 8.1 -11 0 0 34.1 14.3 -11 0 0 41.2 12.5 -12 0 0 35 13.5 -12 0 0 87.79 17.9 0 1 0 7 2.8 0 1 0 3.5 2.3 -1 -1 0 5721.93 133.19 -1 1 0 5699.53 134.99 -2 -1 0 2878.21 67.89 2 -1 0 2914.21 73.49 -2 -1 0 2901.91 71.39 2 -1 0 2899.61 70.99 -2 1 0 2847.32 71.09 2 1 0 2832.72 67.79 2 1 0 2759.32 71.19 -2 1 0 2876.31 73.59 -3 -1 0 258.97 10.9 -3 -1 0 250.27 12.7 3 -1 0 266.37 14.4 3 -1 0 260.77 13.2 3 1 0 258.77 13.5 3 1 0 253.27 10.5 -3 1 0 255.27 13.3 -3 1 0 261.27 14.9 -4 -1 0 212.68 12.9 -4 -1 0 210.58 11.3 4 -1 0 230.68 14.4 4 -1 0 240.08 14.1 -4 1 0 198.78 13.8 4 1 0 222.28 11 -4 1 0 221.78 13.1 4 1 0 206.98 13.4 -5 -1 0 2.5 4 -5 -1 0 3.8 5.5 -5 1 0 -3.9 5.7 -5 1 0 5.7 5.5 -6 -1 0 36.2 7.8 -6 -1 0 37.5 9.2 -6 1 0 32.4 9 6 1 0 27.4 6.9 -6 1 0 31.7 8.2 -7 -1 0 104.89 14.1 -7 -1 0 85.19 10.8 -7 1 0 123.19 14.4 -7 1 0 94.99 13.6 -8 -1 0 41 11.6 -8 -1 0 29.5 8.8 -8 1 0 30.7 9.6 -8 1 0 32.5 10.8 -9 -1 0 215.48 19.4 -9 -1 0 171.78 18.2 -9 1 0 194.78 20.3 -9 1 0 234.38 21.4 -10 -1 0 26.3 12.8 -10 1 0 29 11.8 -10 1 0 56.29 14 -11 -1 0 -0.8 10.6 -11 -1 0 28.8 9.8 -11 1 0 7.9 11.2 -11 1 0 1.8 9.4 -12 -1 0 47.2 14.3 -12 -1 0 48.6 17 -12 1 0 22.3 12 -12 1 0 45.3 13.4 0 -2 0 8944.91 208.98 0 -2 0 9047.69 210.08 0 2 0 8924.81 209.08 0 2 0 8942.71 209.98 -1 -2 0 13.8 3.5 -1 -2 0 17.8 4.6 1 -2 0 12.8 4.3 1 -2 0 15.3 4.4 -1 -2 0 14.6 3.8 -1 -2 0 18.8 4.7 1 2 0 17.6 4.1 -1 2 0 9.3 5.2 -1 2 0 26.6 5.2 1 2 0 18.7 4.4 -2 -2 0 959.2 26.4 2 -2 0 950.3 29.6 2 -2 0 940.81 36.4 -2 -2 0 954 30.2 -2 -2 0 957.6 27 -2 2 0 957.7 30.3 -2 2 0 955.6 33 2 2 0 908.51 29.8 2 2 0 887.01 26.5 3 -2 0 709.53 28.5 -3 -2 0 745.53 21.7 3 -2 0 720.03 25.7 -3 -2 0 766.32 26.8 -3 2 0 711.83 29.4 -3 2 0 738.73 26.8 3 2 0 654.53 25.5 3 2 0 706.73 21.9 -4 -2 0 406.16 15.2 -4 -2 0 385.06 19.4 -4 2 0 411.16 20 -4 2 0 366.96 21.7 4 2 0 392.16 15.1 -5 -2 0 83.59 8 -5 -2 0 90.39 11.4 -5 2 0 77.69 13.3 -5 2 0 73.29 9.4 5 2 0 72.49 7.5 -6 -2 0 288.17 15.3 -6 -2 0 323.27 20.7 -6 2 0 278.27 20.5 6 2 0 271.97 14.6 -6 2 0 273.97 18.3 -7 -2 0 174.98 20.7 -7 -2 0 116.29 11.3 -7 2 0 115.39 16 7 2 0 105.49 11.9 -8 -2 0 43.2 12.3 -8 -2 0 66.59 11.2 -8 2 0 43.2 11.8 -8 2 0 53.59 13.1 -9 -2 0 33.6 13.5 -9 -2 0 56.49 11.3 -9 2 0 40.9 13.9 -9 2 0 47.1 13 -10 -2 0 28.9 10.4 -10 -2 0 41.5 13.9 -10 2 0 19.1 11.9 -10 2 0 34 13.5 -11 -2 0 7.8 11.7 -11 -2 0 -9.9 8 -11 2 0 6.2 10.1 -11 2 0 11.9 10.9 -12 -2 0 55.79 13.1 -12 2 0 25.7 13.6 -12 2 0 40.3 13.8 0 -3 0 -3.3 3.5 0 -3 0 0.5 3.5 0 3 0 3.6 4.6 0 3 0 -3.6 4.1 1 -3 0 152.98 10.5 -1 -3 0 129.49 9.8 -1 -3 0 141.09 10.1 1 -3 0 146.09 12.1 -1 -3 0 139.19 11.3 -1 -3 0 140.29 10.6 1 3 0 126.09 10.2 -1 3 0 142.59 11.6 -1 3 0 145.09 11.4 1 3 0 142.79 11 2 -3 0 2069.59 56.69 -2 -3 0 2046.2 57.59 -2 -3 0 1968.6 57.69 -2 -3 0 2009.4 53.59 2 -3 0 1957.1 60.39 -2 -3 0 1975.7 54.29 2 3 0 1844.82 56.49 -2 3 0 2020.1 62.59 -2 3 0 2051.19 61.89 -3 -3 0 126.79 11.6 -3 -3 0 108.09 8.1 3 -3 0 111.39 10.5 -3 -3 0 109.19 8.2 -3 3 0 109.89 12.1 3 3 0 107.79 8.3 -3 3 0 103.79 10.8 3 3 0 97.69 10.3 -4 -3 0 159.08 9.7 -4 -3 0 152.98 13.6 -4 3 0 153.08 12.5 -4 3 0 173.38 16.2 4 3 0 157.88 10 -5 -3 0 467.55 24.2 -5 -3 0 455.85 17.8 -5 3 0 409.96 26.7 -5 3 0 440.26 23.8 5 3 0 445.96 18.3 -6 -3 0 102.39 14.7 -6 3 0 89.89 13.8 6 3 0 94.59 15.1 -6 3 0 64.29 14.4 -7 -3 0 501.25 22 -7 -3 0 583.14 30.7 -7 3 0 502.25 29.2 -7 3 0 459.65 31.5 7 3 0 493.65 22.2 -8 -3 0 122.99 11.7 -8 -3 0 140.29 18.4 -8 3 0 89.39 17 -8 3 0 80.99 14.7 -9 -3 0 102.99 11.7 -9 -3 0 82.29 15.6 -9 3 0 83.09 15.5 -9 3 0 81.69 18 -10 -3 0 42.8 9.8 -10 -3 0 46.1 15.8 -10 3 0 43.2 13.2 -10 3 0 30.6 14.5 -11 -3 0 26.9 8.2 -11 -3 0 6 13 -11 3 0 18.4 13.5 -11 3 0 27.9 12.7 -12 -3 0 -3.3 12.6 -12 3 0 10.4 12.2 -12 3 0 11 12.3 0 -4 0 1722.63 54.79 0 -4 0 1729.03 53.29 0 4 0 1782.22 54.09 0 4 0 1758.52 55.29 -1 -4 0 7.1 5.4 -1 -4 0 8.6 5.4 1 -4 0 19.6 5.7 -1 -4 0 20.8 6.1 -1 -4 0 6.1 4.9 1 4 0 10 6 -1 4 0 14.7 7 1 4 0 16 6.7 -1 4 0 2.2 4.8 2 -4 0 479.15 25.8 -2 -4 0 542.75 24.9 -2 4 0 519.25 24.6 -2 4 0 503.65 27.4 -3 -4 0 269.97 18 -3 -4 0 276.37 14.3 -3 -4 0 242.68 14.5 -3 4 0 265.97 20 -3 4 0 237.08 17.1 -4 -4 0 75.99 8.5 -4 -4 0 74.19 7.9 -4 -4 0 63.69 11 -4 4 0 65.99 11.1 -4 4 0 62.29 13.9 -5 -4 0 389.76 17 -5 -4 0 377.56 23.7 -5 4 0 376.06 27.5 -5 4 0 359.36 23.2 5 4 0 348.77 19.2 -6 -4 0 415.26 20.4 -6 -4 0 430.76 20 -6 -4 0 427.16 29.9 -6 4 0 395.76 26.2 6 4 0 406.06 22.1 -6 4 0 386.86 29.3 -7 -4 0 281.37 23.1 -7 -4 0 277.77 15 -7 4 0 229.08 21.4 7 4 0 245.68 15.8 -7 4 0 273.57 25.9 -8 -4 0 45 13.7 -8 -4 0 25.7 6.9 8 4 0 5.9 12.5 -8 4 0 31.6 12 -8 4 0 27.8 13.5 -9 -4 0 20.6 7.2 -9 -4 0 12.1 12.6 -9 4 0 25.4 14.2 -9 4 0 24.4 11.8 -10 -4 0 3.3 6.5 -10 -4 0 18.2 12.8 -10 4 0 13 9.6 -10 4 0 18.1 13.3 -11 -4 0 -13.2 12.5 -11 4 0 -6.3 12.4 -11 4 0 4.2 10.7 0 -5 0 -11.3 4.2 0 5 0 -7.4 4.5 0 5 0 2.3 6.6 -1 -5 0 166.18 15.7 -1 -5 0 143.19 14.8 1 5 0 176.78 15.4 -1 5 0 145.69 14.5 -1 5 0 151.58 16.1 1 5 0 161.18 14.5 -2 -5 0 162.58 15.8 -2 -5 0 175.38 15.6 -2 -5 0 171.38 13.8 -2 5 0 143.09 14.4 -2 5 0 141.49 16.9 -3 -5 0 58.99 9.4 -3 -5 0 73.89 9.6 -3 -5 0 76.09 12.3 -3 5 0 65.09 12 -3 5 0 61.49 14.3 -4 -5 0 89.79 10 -4 -5 0 82.79 13.8 -4 -5 0 85.19 10.7 -4 5 0 86.89 14.2 -4 5 0 96.89 17.5 -5 -5 0 46.3 13.1 -5 -5 0 43 8.1 -5 -5 0 39.6 7.7 -5 5 0 33.5 10.6 -5 5 0 32.1 12.4 -6 -5 0 37.7 7 -6 -5 0 31.4 10.2 -6 -5 0 64.89 9 -6 5 0 45.3 11.1 -6 5 0 24 13 -7 -5 0 70.39 8.8 -7 -5 0 54.39 14.3 -7 5 0 55.39 13.7 -7 5 0 66.99 17.4 -8 -5 0 41.3 7.6 -8 -5 0 27.5 8.7 -8 -5 0 6.3 11.4 8 5 0 13.6 8.5 -8 5 0 56.99 17 -8 5 0 29.1 11.9 -9 -5 0 33.7 6.9 -9 -5 0 24.1 14.7 -9 5 0 29.3 12.1 -9 5 0 28.4 13.6 -10 5 0 26.8 13.3 -10 5 0 18.2 15.3 -11 -5 0 -13.5 12.3 -11 5 0 9.6 11.1 -11 5 0 30 13 0 -6 0 2149.48 70.59 0 -6 0 2105.89 72.49 0 6 0 2197.58 72.99 0 6 0 2182.68 70.59 -1 -6 0 508.35 28.5 -1 -6 0 496.15 28 -1 6 0 492.75 30.4 1 6 0 486.05 28.1 -1 6 0 463.25 27.4 1 6 0 498.45 28.3 -2 -6 0 205.88 19.9 -2 -6 0 184.98 16.2 -2 6 0 170.78 18.2 -3 -6 0 99.89 15.9 -3 -6 0 109.39 12.9 -3 6 0 142.89 17.2 -3 6 0 127.49 20 -4 -6 0 16.9 7.1 -4 6 0 27.3 10 -4 6 0 25.3 11.9 -5 -6 0 33 7.5 -5 -6 0 30.6 11.4 -5 6 0 37.8 13.1 -5 6 0 27.9 10.6 -6 -6 0 41.7 13.2 -6 -6 0 32.5 7.6 -6 6 0 42.3 16.3 -6 6 0 34.8 11.2 -7 -6 0 4.8 6 -7 -6 0 0.8 10.6 -7 6 0 13 12.9 -7 6 0 18.4 12.2 -8 -6 0 11.3 12.9 -8 -6 0 15.7 5.7 -8 6 0 14.2 12.2 -8 6 0 14.3 11.8 -9 -6 0 18.6 13.3 -9 6 0 -5.4 12.2 -9 6 0 6.5 10.3 -10 -6 0 -32.3 13 -10 6 0 1 10.5 -10 6 0 16.4 13.5 0 -7 0 6.6 9.1 0 -7 0 -5.5 6.7 0 7 0 0.3 8.2 0 7 0 -1 8 1 -7 0 244.98 20.6 -1 -7 0 238.18 22.3 -1 -7 0 234.08 20.8 1 7 0 243.28 21.1 -1 7 0 219.38 22.7 -1 7 0 260.37 22.4 -2 -7 0 3.1 7.9 -2 -7 0 26.4 11.1 -2 7 0 19 16.4 -2 7 0 8.2 10 -3 -7 0 2.5 7.9 -3 -7 0 12 9.6 -3 7 0 35.1 13.8 -3 7 0 3.6 8.4 -4 -7 0 6.1 7.8 -4 -7 0 0.4 6.8 -4 7 0 17.1 8.3 -4 7 0 6 10.3 -5 -7 0 15.4 8.2 -5 -7 0 20.9 11.7 -5 7 0 35.9 15.3 -5 7 0 34.1 11.9 -6 -7 0 -17.8 9.9 -6 7 0 -6.1 9.5 -7 -7 0 -23.2 9.7 -7 7 0 9.7 11.5 -7 7 0 11.1 10.2 -8 -7 0 16.2 15 -8 7 0 10.5 15.6 -9 -7 0 -2.9 14.1 -9 7 0 41 14.9 -9 7 0 39 16.1 0 -8 0 15.8 12.6 0 -8 0 9.4 9.7 0 8 0 41.3 13.4 0 8 0 15.8 10 1 -8 0 11.1 8.9 -1 -8 0 11 11.5 -1 -8 0 -7.9 7.4 1 -8 0 17.1 10.7 -1 8 0 26.9 12.2 1 8 0 13 10.4 -1 8 0 10.2 9.8 -2 -8 0 -13.1 8.1 -2 -8 0 -7.4 10 -2 8 0 4.5 9.9 -2 8 0 -9.3 10 -3 -8 0 13.5 9.8 -3 -8 0 6.1 11.6 -3 8 0 6.3 12.4 -3 8 0 7.1 7.6 -4 -8 0 -9.9 6.8 -4 -8 0 -5.6 11.3 -4 8 0 9.3 10.8 -4 8 0 26.3 16 -5 -8 0 18.2 12.9 -5 8 0 29.6 16.1 -5 8 0 16.9 12.1 -6 -8 0 54.39 17.5 -6 -8 0 36.7 10.3 -6 8 0 46.4 15.5 -6 8 0 87.19 21.7 -7 -8 0 21.4 16 -7 8 0 53.39 18.3 -7 8 0 54.29 21.5 0 -9 0 -18.7 8.9 0 -9 0 -8.8 9.5 0 9 0 1.7 12.6 -1 -9 0 -0.1 12.2 -1 -9 0 -10 9.7 1 -9 0 -8.1 8.9 1 -9 0 14.6 12.7 -1 9 0 16.6 14 -1 9 0 10.1 10.7 -2 -9 0 17.1 12.2 2 -9 0 14.1 16.5 2 -9 0 12.6 10.5 -2 -9 0 -5.4 10 -2 9 0 13.6 11.4 -2 9 0 12.3 13.9 -3 -9 0 -8.7 9.7 -3 -9 0 -11.1 11.1 -3 9 0 15.1 13.1 -3 9 0 19.2 11.8 -4 -9 0 19.6 15.7 -4 9 0 14.8 14.2 -4 9 0 44.2 15.1 -5 -9 0 64.19 20.8 -5 9 0 58.89 18 -5 9 0 97.99 20 0 -10 0 70.59 18.3 0 -10 0 54.19 18.5 0 10 0 78.89 19.9 1 -10 0 21.3 13.1 -1 -10 0 -0.9 13.6 1 -10 0 7.5 13.1 -1 -10 0 -19.3 9.9 -1 10 0 6.3 11.8 -1 10 0 16.7 14.6 -12 0 1 24.6 13.8 -12 0 1 -0.8 9.4 -11 0 1 8.2 9.9 -11 0 1 11.9 12.1 -10 0 1 50.59 12.8 -10 0 1 38 11.3 -9 0 1 63.09 13.6 -8 0 1 0.1 7.8 -8 0 1 2.5 6.5 -7 0 1 151.58 14.5 -7 0 1 147.29 15.8 -6 0 1 20.6 6.8 -6 0 1 8.4 6 -5 0 1 40.3 8.1 -5 0 1 39.7 7.4 5 0 -1 47.1 7.8 -4 0 1 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8.6 -2 -9 3 -6.8 11.8 -2 9 3 12.3 11.7 -2 9 3 -6.1 10 1 -9 -3 4.6 10.5 1 -9 -3 0.2 10.7 -1 -9 3 30.3 14.4 -1 -9 3 -20.6 13 -1 9 3 7.5 11.2 0 -9 -3 21.6 11.8 0 -9 3 25.2 15.6 0 -9 3 4.3 14 0 -9 -3 27.8 13.8 0 9 3 55.59 15.3 0 9 -3 57.89 16.3 0 9 -3 30.6 15.5 1 -9 3 112.19 27.4 -1 -9 -3 68.59 16 -1 -9 -3 72.59 15.9 1 -9 3 78.89 19.1 -1 9 -3 126.19 21.9 1 9 3 67.69 16.2 -2 -9 -3 3.4 10.8 2 -9 3 8.3 13 2 -9 3 22.1 14.1 -2 -9 -3 -9.6 9.5 -2 9 -3 39.3 14.1 -2 9 -3 17.6 14.2 3 -9 3 189.28 30.8 -3 -9 -3 159.88 21.7 -3 -9 -3 133.89 18.9 -3 9 -3 204.08 27.9 -3 9 -3 97.29 23.2 -4 -9 -3 25.3 14.7 4 -9 3 32.5 19.4 -4 9 -3 26.9 15.6 -4 9 -3 -4.2 13.5 5 -9 3 44.9 17.4 -5 -9 -3 14.2 13.2 -5 9 -3 32.2 18 -5 9 -3 20.4 14.4 0 -10 3 3.3 15.1 0 -10 -3 -3.7 11.9 0 -10 3 14.9 14.1 0 -10 -3 24.8 15.6 0 10 3 22.7 16.5 -12 0 4 3.1 11.6 -11 0 4 0.1 11 -11 0 4 10.3 11 -10 0 4 6.5 8.1 -10 0 4 8.4 10.6 -9 0 4 0.1 8.2 -9 0 4 -7.9 5.9 -8 0 4 20.9 9.6 -8 0 4 35.7 11.1 -7 0 4 173.58 16.6 -7 0 4 155.98 14.8 -6 0 4 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24 -2 1 4 705.73 24.7 -2 1 4 730.43 21.1 2 1 -4 678.43 25.1 -1 -1 4 982.5 30.5 -1 -1 4 935.01 29 -1 -1 4 953.6 30.2 1 -1 -4 950.2 27.8 1 -1 -4 913.11 24.1 1 1 -4 996.5 30.8 -1 1 4 918.91 27.7 1 1 -4 882.71 28.6 -1 1 4 953.5 23.7 0 -1 4 1371.06 39.5 0 -1 -4 1389.06 32.3 0 -1 -4 1388.96 35.4 0 -1 4 1423.16 39.8 0 -1 4 1390.66 39.3 0 1 -4 1354.36 39.1 0 1 4 1447.66 35.8 0 1 -4 1346.87 39.5 0 1 4 1191.88 32 1 -1 4 2261.07 62.09 -1 -1 -4 2397.66 56.49 -1 -1 -4 2370.66 55.99 1 -1 4 2342.27 61.79 1 -1 4 2307.37 62.19 1 1 4 2342.07 55.59 -1 1 -4 2327.37 62.49 1 1 4 2357.36 56.19 -1 1 -4 2333.67 62.39 2 -1 4 467.45 20 -2 -1 -4 490.05 17 2 -1 4 463.75 19 -2 1 -4 494.25 20.3 -2 1 -4 445.46 19.5 2 1 4 464.85 13.2 2 1 4 469.55 13.8 2 1 4 482.05 16.4 -3 -1 -4 104.39 6.4 -3 -1 -4 130.39 9.4 3 -1 4 119.69 10.4 -3 1 -4 124.79 10.9 -3 1 -4 103.29 12 3 1 4 126.69 10.3 3 1 4 112.89 6.2 -4 -1 -4 927.11 31.5 4 -1 4 898.41 33.6 -4 -1 -4 927.61 27.7 4 1 4 927.31 26.4 4 1 4 880.81 31.2 -4 1 -4 888.51 33.4 -4 1 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-6 -2 4 33.3 9.5 -6 -2 4 39.4 8.9 -6 2 4 37.5 8.7 -6 2 4 36.7 10.9 -5 -2 4 125.29 11.4 -5 -2 4 125.79 13.9 -5 2 4 117.09 11 -5 2 4 101.49 12.1 4 -2 -4 9.8 4.9 -4 -2 4 17.7 5.8 -4 -2 4 10.5 6.3 -4 2 4 9.8 4.4 -4 2 4 13.6 5.8 4 2 -4 1.8 4.6 -3 -2 4 46.2 8.2 3 -2 -4 49.5 6 3 -2 -4 38.4 8.1 -3 -2 4 49.2 7.9 3 2 -4 43.7 8.7 -3 2 4 43 6.2 -3 2 4 38.6 7.6 3 2 -4 42 7.2 -2 -2 4 96.29 10.5 -2 -2 4 79.69 8.5 2 -2 -4 82.19 8.8 2 -2 -4 91.79 6.2 -2 2 4 98.29 6.6 2 2 -4 71.39 8.7 -2 2 4 83.39 9.2 1 -2 -4 472.15 18 -1 -2 4 426.16 19.6 1 -2 -4 470.65 12.7 -1 -2 4 400.86 21.8 -1 -2 4 439.36 19.3 -1 2 4 427.66 18.1 -1 2 4 431.96 13.2 1 2 -4 445.16 19.5 0 -2 4 1939.31 56.69 0 -2 -4 1933.41 45.5 0 -2 -4 2048.9 50.59 0 -2 4 1994.8 60.99 0 -2 -4 1978.8 45.9 0 2 4 1994.8 51.29 0 2 -4 1906.61 56.79 0 2 -4 1747.73 57.79 0 2 -4 2010.4 57.39 1 -2 4 730.93 32.8 -1 -2 -4 790.32 21.3 -1 -2 -4 831.82 21.7 1 -2 4 748.73 29 1 -2 4 782.22 28.6 1 2 4 793.82 22.1 1 2 4 801.22 22.3 -1 2 -4 759.62 33.3 -1 2 -4 785.32 33.2 2 -2 4 2966.5 83.79 -2 -2 -4 3165.28 75.49 2 -2 4 3112.09 82.29 -2 2 -4 3003.2 84.09 -2 2 -4 3043.3 83.09 2 2 4 3012.9 75.69 3 -2 4 323.67 19.6 -3 -2 -4 339.47 17.2 -3 2 -4 312.57 19.5 -3 2 -4 307.37 18.4 -4 -2 -4 775.42 18.6 -4 -2 -4 795.42 28.5 4 2 4 746.13 28.6 -4 2 -4 770.82 33.8 -4 2 -4 731.83 31.4 -5 -2 -4 26.2 4 -5 -2 -4 33.6 7.4 5 2 4 26.2 3.5 -5 2 -4 23.4 7.9 -5 2 -4 24.1 8.6 -6 -2 -4 3.5 3.5 -6 -2 -4 19.7 8.1 -6 2 -4 8.9 8.2 6 2 4 -0.5 3.2 -6 2 -4 4.6 7.1 -7 -2 -4 2.5 4.1 -7 -2 -4 9.3 7.5 7 2 4 -7.5 4.1 -7 2 -4 -10.5 6.7 -7 2 -4 7.8 7.5 -8 -2 -4 25.9 11.2 -8 -2 -4 26.5 6.5 -8 2 -4 28.4 11.1 -8 2 -4 23.7 9.2 8 2 4 11.2 6.3 -9 -2 -4 24.1 7.5 -9 -2 -4 44.5 12.2 -9 2 -4 22.3 9.7 -9 2 -4 43.3 12.4 -10 -2 -4 -7.6 8.8 -10 -2 -4 22.5 6.9 -10 2 -4 1.5 10.4 -10 2 -4 -6.5 14.8 -11 -2 -4 5.4 6.9 -11 -2 -4 -11.9 7.3 -11 2 -4 8.7 11.6 -11 2 -4 6.9 11.7 -12 -2 -4 -0.7 12.3 -12 2 -4 -5.4 11.7 -12 2 -4 33.1 15.4 -12 -3 4 15.2 11.3 -12 -3 4 8.6 15.7 -12 3 4 25.7 14.3 -12 3 4 19.4 12.4 -11 -3 4 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-4.2 13.2 -1 0 25 -29 12.5 -1 0 25 -13.9 14 0 0 25 3.1 13.5 0 0 25 69.19 20.1 -1 -1 25 -24.3 12.5 -1 -1 25 -17.3 12.6 loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 1(3) 2 0(3)