#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:48:43 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225907 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515791.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_4515791 loop_ _publ_author_name 'Wang, Huifei' 'Qiu, Shuxian' 'Wang, Sasa' 'Zhai, Hongbin' _publ_section_title ; Pd-Catalyzed Umpolung of \p--Allylpalladium Intermediates: Assembly of All-Carbon \a-Vinyl Quaternary Aldehydes through C(sp3)--C(sp3) Coupling ; _journal_issue 12 _journal_name_full 'ACS Catalysis' _journal_page_first 11960 _journal_paper_doi 10.1021/acscatal.8b03814 _journal_volume 8 _journal_year 2018 _chemical_formula_moiety 'C24 H24 N2 O2 S' _chemical_formula_sum 'C24 H24 N2 O2 S' _chemical_formula_weight 404.51 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2018-07-24 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 101.603(12) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.9646(15) _cell_length_b 31.521(5) _cell_length_c 6.9339(7) _cell_measurement_reflns_used 1731 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 72.4440 _cell_measurement_theta_min 2.7740 _cell_volume 2133.4(5) _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (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_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2684 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.955 _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 -45.00 -18.00 1.00 1.00 -- -41.11 -57.00 30.00 27 2 \w -62.00 27.00 1.00 1.00 -- -41.11 37.00 120.00 89 3 \w 1.00 70.00 1.00 1.00 -- 41.11 -99.00-120.00 69 4 \w 36.00 62.00 1.00 2.00 -- 106.95 -94.00 0.00 26 5 \w 83.00 109.00 1.00 2.00 -- 106.95 -94.00 0.00 26 6 \w 37.00 106.00 1.00 2.00 -- 106.95 -94.00 150.00 69 7 \w 34.00 105.00 1.00 2.00 -- 106.95-111.00 -30.00 71 8 \w 85.00 145.00 1.00 2.00 -- 106.95 -15.00-150.00 60 9 \w 106.00 175.00 1.00 2.00 -- 106.95 111.00-150.00 69 10 \w 87.00 174.00 1.00 2.00 -- 106.95 45.00 30.00 87 11 \w 28.00 54.00 1.00 2.00 -- 106.95 -15.00-150.00 26 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0260452000 _diffrn_orient_matrix_UB_12 -0.0483094000 _diffrn_orient_matrix_UB_13 -0.0200996000 _diffrn_orient_matrix_UB_21 0.0476179000 _diffrn_orient_matrix_UB_22 -0.0062174000 _diffrn_orient_matrix_UB_23 0.1565228000 _diffrn_orient_matrix_UB_31 -0.2201114000 _diffrn_orient_matrix_UB_32 0.0044110000 _diffrn_orient_matrix_UB_33 0.0033116000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_unetI/netI 0.0782 _diffrn_reflns_Laue_measured_fraction_full 0.982 _diffrn_reflns_Laue_measured_fraction_max 0.955 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 7943 _diffrn_reflns_point_group_measured_fraction_full 0.982 _diffrn_reflns_point_group_measured_fraction_max 0.955 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.601 _diffrn_reflns_theta_min 2.804 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.518 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.40413 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (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 1.259 _exptl_crystal_description block _exptl_crystal_F_000 856 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.567 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 263 _refine_ls_number_reflns 4121 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.1276 _refine_ls_R_factor_gt 0.0965 _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^)+(0.1423P)^2^+2.1181P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2589 _refine_ls_wR_factor_ref 0.2933 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2778 _reflns_number_total 4121 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 180720_a.res in P2(1)/c 180720.res created by SHELXL-2018/3 at 17:16:48 on 24-Jul-2018 REM Old TITL 180720 in P2(1)/m REM SHELXT solution in P2(1)/c: R1 0.241, Rweak 0.249, Alpha 0.050 REM 1.296 for 87 systematic absences, Orientation a'=c, b'=-b, c'=a REM Formula found by SHELXT: C19 N3 O6 S CELL 1.54184 9.9646 31.5215 6.9339 90 101.603 90 ZERR 4 0.0015 0.0047 0.0007 0 0.012 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O S UNIT 96 96 8 8 4 L.S. 20 PLAN 20 BOND list 4 fmap 2 53 acta REM REM REM WGHT 0.142300 2.118100 FVAR 0.49920 S1 5 0.234646 0.293047 0.134107 11.00000 0.03737 0.07142 = 0.02786 -0.00001 0.00689 -0.00117 O1 4 0.207074 0.322775 -0.023925 11.00000 0.04182 0.08532 = 0.02957 0.00661 0.00491 0.00197 O2 4 0.175506 0.251651 0.110447 11.00000 0.05542 0.07468 = 0.03423 -0.00911 0.01341 -0.01261 N1 3 0.224053 0.354020 0.369786 11.00000 0.02760 0.06027 = 0.03840 0.00593 0.00313 0.00447 N2 3 0.177683 0.312903 0.320551 11.00000 0.03235 0.06071 = 0.03298 0.00269 0.00801 -0.00186 AFIX 43 H2 2 0.124363 0.299309 0.382149 11.00000 -1.20000 AFIX 0 C12 1 0.231451 0.364480 0.548813 11.00000 0.02270 0.05837 = 0.04048 0.00905 0.00011 0.00477 AFIX 43 H12 2 0.212652 0.344550 0.638672 11.00000 -1.20000 AFIX 0 C18 1 0.413041 0.287774 0.209812 11.00000 0.04111 0.06036 = 0.02918 0.00160 0.01310 0.00267 C23 1 0.467448 0.248546 0.275818 11.00000 0.05693 0.06094 = 0.03016 -0.00007 0.01788 0.00751 AFIX 43 H23 2 0.410699 0.225156 0.276775 11.00000 -1.20000 AFIX 0 C19 1 0.495497 0.323193 0.206619 11.00000 0.03759 0.06450 = 0.03779 0.00571 0.01170 0.01060 AFIX 43 H19 2 0.457827 0.349169 0.160618 11.00000 -1.20000 AFIX 0 C22 1 0.607887 0.244999 0.340132 11.00000 0.05813 0.06811 = 0.03241 0.00805 0.01496 0.02064 AFIX 43 H22 2 0.645683 0.218813 0.382484 11.00000 -1.20000 AFIX 0 C20 1 0.635577 0.318744 0.273943 11.00000 0.03801 0.07011 = 0.04712 0.00489 0.01416 0.00518 AFIX 43 H20 2 0.692430 0.342128 0.273520 11.00000 -1.20000 AFIX 0 C11 1 0.270570 0.409048 0.615596 11.00000 0.03895 0.05382 = 0.05095 0.00651 -0.00067 0.00676 C21 1 0.692748 0.279759 0.342365 11.00000 0.04689 0.08669 = 0.03457 0.00858 0.01474 0.02123 C8 1 0.409993 0.408580 0.758884 11.00000 0.04408 0.04603 = 0.05051 0.00493 -0.00753 -0.00584 C7 1 0.513110 0.384600 0.723675 11.00000 0.03850 0.05201 = 0.05930 0.00679 -0.00455 -0.00430 AFIX 43 H7 2 0.498396 0.366634 0.615071 11.00000 -1.20000 AFIX 0 C6 1 0.646405 0.386053 0.850566 11.00000 0.04504 0.05149 = 0.09265 0.02323 -0.00064 -0.00821 C13 1 0.283293 0.436832 0.435367 11.00000 0.05522 0.07215 = 0.06193 0.02111 -0.00831 -0.00197 AFIX 23 H13A 2 0.342495 0.422052 0.362423 11.00000 -1.20000 H13B 2 0.193352 0.438556 0.350395 11.00000 -1.20000 AFIX 0 C5 1 0.752644 0.361095 0.813812 11.00000 0.04060 0.06523 = 0.09680 0.01127 0.00697 -0.00666 AFIX 43 H5 2 0.739429 0.342948 0.705890 11.00000 -1.20000 AFIX 0 C24 1 0.846203 0.276085 0.415238 11.00000 0.04603 0.10363 = 0.05343 0.00709 0.01163 0.01846 AFIX 137 H24A 2 0.871895 0.290194 0.539910 11.00000 -1.50000 H24B 2 0.892628 0.289047 0.321767 11.00000 -1.50000 H24C 2 0.871305 0.246687 0.430204 11.00000 -1.50000 AFIX 0 C16 1 0.156400 0.422903 0.722825 11.00000 0.06499 0.07287 = 0.07801 -0.00129 0.01792 0.01374 AFIX 43 H16 2 0.149733 0.408286 0.837024 11.00000 -1.20000 AFIX 0 C1 1 0.662919 0.414339 1.015120 11.00000 0.07308 0.04895 = 0.07265 0.00499 -0.02739 -0.01237 C9 1 0.432144 0.436488 0.927428 11.00000 0.07488 0.06556 = 0.05703 -0.00117 -0.00955 -0.00220 AFIX 43 H9 2 0.360366 0.452955 0.953328 11.00000 -1.20000 AFIX 0 C14 1 0.332802 0.477881 0.469999 11.00000 0.06039 0.07606 = 0.09369 0.02618 -0.00258 -0.00639 AFIX 43 H14 2 0.404896 0.481852 0.576648 11.00000 -1.20000 AFIX 0 C10 1 0.557888 0.438796 1.048771 11.00000 0.08959 0.06048 = 0.07274 -0.00913 -0.01628 -0.00548 AFIX 43 H10 2 0.571805 0.457280 1.155480 11.00000 -1.20000 AFIX 0 C4 1 0.877951 0.363560 0.939330 11.00000 0.04058 0.07428 = 0.14681 0.02810 -0.01255 -0.00597 AFIX 43 H4 2 0.949965 0.346798 0.916491 11.00000 -1.20000 AFIX 0 C3 1 0.898992 0.391643 1.104972 11.00000 0.05552 0.07464 = 0.14716 0.03341 -0.04039 -0.01581 AFIX 43 H3 2 0.984357 0.392612 1.189050 11.00000 -1.20000 AFIX 0 C2 1 0.799863 0.416068 1.140311 11.00000 0.07466 0.06289 = 0.13275 0.01373 -0.04358 -0.01569 AFIX 43 H2A 2 0.816944 0.434718 1.246358 11.00000 -1.20000 AFIX 0 C15 1 0.286835 0.511926 0.365152 11.00000 0.08054 0.08213 = 0.14421 0.03281 0.01848 0.00826 AFIX 93 H15A 2 0.214867 0.509478 0.257163 11.00000 -1.20000 H15B 2 0.326542 0.538267 0.399558 11.00000 -1.20000 AFIX 0 C17 1 0.070727 0.452509 0.668880 11.00000 0.11734 0.16256 = 0.20751 0.07573 0.09288 0.08382 AFIX 93 H17A 2 0.073696 0.467951 0.555528 11.00000 -1.20000 H17B 2 0.004987 0.458760 0.742709 11.00000 -1.20000 AFIX 0 HKLF 4 REM 180720_a.res in P2(1)/c REM wR2 = 0.2933, GooF = S = 1.046, Restrained GooF = 1.046 for all data REM R1 = 0.0965 for 2778 Fo > 4sig(Fo) and 0.1276 for all 4121 data REM 263 parameters refined using 0 restraints END WGHT 0.1418 2.0985 REM Highest difference peak 0.567, deepest hole -0.377, 1-sigma level 0.088 Q1 1 0.6544 0.4380 1.2132 11.00000 0.05 0.57 Q2 1 0.1969 0.2911 0.4342 11.00000 0.05 0.56 Q3 1 0.2166 0.2959 0.2685 11.00000 0.05 0.50 Q4 1 0.7901 0.4257 1.3175 11.00000 0.05 0.48 Q5 1 0.2224 0.2389 0.3181 11.00000 0.05 0.40 Q6 1 0.2146 0.2991 -0.1884 11.00000 0.05 0.38 Q7 1 0.6659 0.3757 0.7126 11.00000 0.05 0.38 Q8 1 0.0485 0.4798 0.9115 11.00000 0.05 0.37 Q9 1 0.8878 0.4018 1.2713 11.00000 0.05 0.36 Q10 1 0.2184 0.3389 0.3133 11.00000 0.05 0.35 Q11 1 0.2331 0.3058 -0.0032 11.00000 0.05 0.35 Q12 1 0.2147 0.2549 0.1430 11.00000 0.05 0.33 Q13 1 0.5275 0.3782 0.6110 11.00000 0.05 0.33 Q14 1 0.2204 0.3153 0.6517 11.00000 0.05 0.33 Q15 1 0.2140 0.2149 0.1323 11.00000 0.05 0.33 Q16 1 0.2400 0.3380 -0.0263 11.00000 0.05 0.31 Q17 1 0.1985 0.3369 0.0883 11.00000 0.05 0.30 Q18 1 0.0136 0.4187 0.6533 11.00000 0.05 0.29 Q19 1 0.7172 0.3963 0.9597 11.00000 0.05 0.29 Q20 1 0.2070 0.3731 0.8319 11.00000 0.05 0.27 REM The information below was added by Olex2. REM REM R1 = 0.0965 for 2778 Fo > 4sig(Fo) and 0.1276 for all 8068 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.57, deepest hole -0.38 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1276 REM R1_gt = 0.0965 REM wR_ref = 0.2933 REM GOOF = 1.046 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 8068 REM Reflections_gt = 2778 REM Parameters = n/a REM Hole = -0.38 REM Peak = 0.57 REM Flack = n/a ; _cod_data_source_file cs8b03814_si_001.cif _cod_data_source_block 180720 _cod_database_code 4515791 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 98.00 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. 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 2.a Secondary CH2 refined with riding coordinates: C13(H13A,H13B) 2.b Aromatic/amide H refined with riding coordinates: N2(H2), C12(H12), C23(H23), C19(H19), C22(H22), C20(H20), C7(H7), C5(H5), C16(H16), C9(H9), C14(H14), C10(H10), C4(H4), C3(H3), C2(H2A) 2.c X=CH2 refined with riding coordinates: C15(H15A,H15B), C17(H17A,H17B) 2.d Idealised Me refined as rotating group: C24(H24A,H24B,H24C) ; _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 - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.981 _oxdiff_exptl_absorpt_empirical_full_min 0.683 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn S1 S 0.23465(11) 0.29305(4) 0.13411(14) 0.0455(4) Uani 1 1 d . O1 O 0.2071(3) 0.32277(13) -0.0239(4) 0.0526(9) Uani 1 1 d . O2 O 0.1755(4) 0.25165(13) 0.1104(5) 0.0542(9) Uani 1 1 d . N1 N 0.2241(4) 0.35402(13) 0.3698(5) 0.0426(9) Uani 1 1 d . N2 N 0.1777(4) 0.31290(13) 0.3206(5) 0.0418(9) Uani 1 1 d . H2 H 0.124363 0.299309 0.382149 0.050 Uiso 1 1 calc R C12 C 0.2315(4) 0.36448(16) 0.5488(6) 0.0414(10) Uani 1 1 d . H12 H 0.212652 0.344550 0.638672 0.050 Uiso 1 1 calc R C18 C 0.4130(5) 0.28777(16) 0.2098(6) 0.0427(10) Uani 1 1 d . C23 C 0.4674(5) 0.24855(17) 0.2758(6) 0.0481(11) Uani 1 1 d . H23 H 0.410699 0.225156 0.276775 0.058 Uiso 1 1 calc R C19 C 0.4955(5) 0.32319(17) 0.2066(6) 0.0460(11) Uani 1 1 d . H19 H 0.457827 0.349169 0.160618 0.055 Uiso 1 1 calc R C22 C 0.6079(5) 0.24500(18) 0.3401(6) 0.0521(13) Uani 1 1 d . H22 H 0.645683 0.218813 0.382484 0.062 Uiso 1 1 calc R C20 C 0.6356(5) 0.31874(18) 0.2739(7) 0.0510(12) Uani 1 1 d . H20 H 0.692430 0.342128 0.273520 0.061 Uiso 1 1 calc R C11 C 0.2706(5) 0.40905(17) 0.6156(7) 0.0493(11) Uani 1 1 d . C21 C 0.6927(5) 0.2798(2) 0.3424(7) 0.0551(14) Uani 1 1 d . C8 C 0.4100(5) 0.40858(16) 0.7589(7) 0.0493(11) Uani 1 1 d . C7 C 0.5131(5) 0.38460(17) 0.7237(8) 0.0519(12) Uani 1 1 d . H7 H 0.498396 0.366634 0.615071 0.062 Uiso 1 1 calc R C6 C 0.6464(6) 0.38605(18) 0.8506(10) 0.0651(16) Uani 1 1 d . C13 C 0.2833(6) 0.4368(2) 0.4354(9) 0.0659(15) Uani 1 1 d . H13A H 0.342495 0.422052 0.362423 0.079 Uiso 1 1 calc R H13B H 0.193352 0.438556 0.350395 0.079 Uiso 1 1 calc R C5 C 0.7526(6) 0.3611(2) 0.8138(11) 0.0685(16) Uani 1 1 d . H5 H 0.739429 0.342948 0.705890 0.082 Uiso 1 1 calc R C24 C 0.8462(6) 0.2761(2) 0.4152(8) 0.0675(17) Uani 1 1 d . H24A H 0.871895 0.290194 0.539910 0.101 Uiso 1 1 calc GR H24B H 0.892628 0.289047 0.321767 0.101 Uiso 1 1 calc GR H24C H 0.871305 0.246687 0.430204 0.101 Uiso 1 1 calc GR C16 C 0.1564(7) 0.4229(2) 0.7228(10) 0.0715(16) Uani 1 1 d . H16 H 0.149733 0.408286 0.837024 0.086 Uiso 1 1 calc R C1 C 0.6629(7) 0.41434(19) 1.0151(9) 0.0708(18) Uani 1 1 d . C9 C 0.4321(7) 0.4365(2) 0.9274(9) 0.0690(16) Uani 1 1 d . H9 H 0.360366 0.452955 0.953328 0.083 Uiso 1 1 calc R C14 C 0.3328(7) 0.4779(2) 0.4700(11) 0.0792(19) Uani 1 1 d . H14 H 0.404896 0.481852 0.576648 0.095 Uiso 1 1 calc R C10 C 0.5579(8) 0.4388(2) 1.0488(10) 0.0788(19) Uani 1 1 d . H10 H 0.571805 0.457280 1.155480 0.095 Uiso 1 1 calc R C4 C 0.8780(6) 0.3636(2) 0.9393(14) 0.092(3) Uani 1 1 d . H4 H 0.949965 0.346798 0.916491 0.110 Uiso 1 1 calc R C3 C 0.8990(7) 0.3916(3) 1.1050(14) 0.101(3) Uani 1 1 d . H3 H 0.984357 0.392612 1.189050 0.121 Uiso 1 1 calc R C2 C 0.7999(8) 0.4161(2) 1.1403(14) 0.099(3) Uani 1 1 d . H2A H 0.816944 0.434718 1.246358 0.119 Uiso 1 1 calc R C15 C 0.2868(8) 0.5119(3) 0.3652(15) 0.103(3) Uani 1 1 d . H15A H 0.214867 0.509478 0.257163 0.123 Uiso 1 1 calc R H15B H 0.326542 0.538267 0.399558 0.123 Uiso 1 1 calc R C17 C 0.0707(11) 0.4525(4) 0.669(2) 0.154(6) Uani 1 1 d . H17A H 0.073696 0.467951 0.555528 0.185 Uiso 1 1 calc R H17B H 0.004987 0.458760 0.742709 0.185 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 S1 0.0374(6) 0.0714(8) 0.0279(5) 0.0000(5) 0.0069(4) -0.0012(5) O1 0.0418(17) 0.085(3) 0.0296(14) 0.0066(15) 0.0049(13) 0.0020(16) O2 0.055(2) 0.075(2) 0.0342(15) -0.0091(15) 0.0134(14) -0.0126(18) N1 0.0276(17) 0.060(2) 0.0384(18) 0.0059(16) 0.0031(14) 0.0045(16) N2 0.0324(18) 0.061(2) 0.0330(17) 0.0027(16) 0.0080(14) -0.0019(16) C12 0.0227(18) 0.058(3) 0.040(2) 0.0090(19) 0.0001(15) 0.0048(17) C18 0.041(2) 0.060(3) 0.0292(19) 0.0016(18) 0.0131(16) 0.003(2) C23 0.057(3) 0.061(3) 0.030(2) -0.0001(18) 0.0179(19) 0.008(2) C19 0.038(2) 0.064(3) 0.038(2) 0.006(2) 0.0117(17) 0.011(2) C22 0.058(3) 0.068(3) 0.032(2) 0.008(2) 0.015(2) 0.021(3) C20 0.038(2) 0.070(3) 0.047(2) 0.005(2) 0.0142(19) 0.005(2) C11 0.039(2) 0.054(3) 0.051(3) 0.007(2) -0.0007(19) 0.007(2) C21 0.047(3) 0.087(4) 0.035(2) 0.009(2) 0.015(2) 0.021(3) C8 0.044(2) 0.046(3) 0.051(3) 0.005(2) -0.008(2) -0.006(2) C7 0.038(2) 0.052(3) 0.059(3) 0.007(2) -0.005(2) -0.004(2) C6 0.045(3) 0.051(3) 0.093(4) 0.023(3) -0.001(3) -0.008(2) C13 0.055(3) 0.072(4) 0.062(3) 0.021(3) -0.008(2) -0.002(3) C5 0.041(3) 0.065(4) 0.097(4) 0.011(3) 0.007(3) -0.007(2) C24 0.046(3) 0.104(5) 0.053(3) 0.007(3) 0.012(2) 0.018(3) C16 0.065(4) 0.073(4) 0.078(4) -0.001(3) 0.018(3) 0.014(3) C1 0.073(4) 0.049(3) 0.073(4) 0.005(3) -0.027(3) -0.012(3) C9 0.075(4) 0.066(4) 0.057(3) -0.001(3) -0.010(3) -0.002(3) C14 0.060(4) 0.076(4) 0.094(5) 0.026(4) -0.003(3) -0.006(3) C10 0.090(5) 0.060(4) 0.073(4) -0.009(3) -0.016(3) -0.005(3) C4 0.041(3) 0.074(4) 0.147(7) 0.028(5) -0.013(4) -0.006(3) C3 0.056(4) 0.075(5) 0.147(7) 0.033(5) -0.040(4) -0.016(3) C2 0.075(5) 0.063(4) 0.133(7) 0.014(4) -0.044(4) -0.016(4) C15 0.081(5) 0.082(5) 0.144(8) 0.033(5) 0.018(5) 0.008(4) C17 0.117(8) 0.163(11) 0.208(12) 0.076(10) 0.093(8) 0.084(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 O1 S1 O2 120.1(2) O1 S1 N2 108.2(2) O1 S1 C18 108.6(2) O2 S1 N2 103.86(19) O2 S1 C18 108.5(2) N2 S1 C18 106.91(19) C12 N1 N2 115.5(4) N1 N2 S1 113.5(3) N1 C12 C11 120.2(4) C23 C18 S1 119.1(4) C19 C18 S1 119.0(4) C19 C18 C23 121.8(4) C22 C23 C18 118.7(5) C20 C19 C18 118.2(5) C21 C22 C23 121.1(5) C19 C20 C21 121.2(5) C12 C11 C8 109.5(4) C12 C11 C13 109.7(4) C12 C11 C16 104.0(4) C8 C11 C13 108.4(4) C8 C11 C16 110.5(5) C16 C11 C13 114.6(5) C22 C21 C20 119.1(5) C22 C21 C24 121.1(5) C20 C21 C24 119.7(6) C7 C8 C11 121.0(5) C7 C8 C9 119.6(5) C9 C8 C11 119.2(5) C8 C7 C6 121.3(5) C5 C6 C7 121.1(6) C5 C6 C1 122.1(6) C1 C6 C7 116.8(6) C14 C13 C11 118.1(6) C4 C5 C6 118.9(7) C17 C16 C11 125.7(8) C6 C1 C2 116.1(7) C10 C1 C6 121.5(5) C10 C1 C2 122.4(7) C10 C9 C8 120.3(6) C15 C14 C13 126.0(7) C1 C10 C9 120.5(6) C5 C4 C3 120.7(7) C2 C3 C4 121.2(6) C3 C2 C1 120.9(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 O1 1.426(4) S1 O2 1.428(4) S1 N2 1.637(4) S1 C18 1.757(5) N1 N2 1.395(6) N1 C12 1.272(6) C12 C11 1.506(7) C18 C23 1.390(7) C18 C19 1.389(7) C23 C22 1.385(7) C19 C20 1.387(7) C22 C21 1.382(9) C20 C21 1.397(8) C11 C8 1.537(6) C11 C13 1.552(7) C11 C16 1.542(8) C21 C24 1.515(7) C8 C7 1.337(8) C8 C9 1.444(8) C7 C6 1.439(7) C6 C5 1.383(9) C6 C1 1.431(10) C13 C14 1.388(10) C5 C4 1.373(9) C16 C17 1.269(11) C1 C10 1.357(10) C1 C2 1.464(8) C9 C10 1.363(9) C14 C15 1.325(10) C4 C3 1.432(13) C3 C2 1.314(13) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma -1 0 0 2934.3 18.75 -2 0 0 9999 48.69 -3 0 0 3246.39 35.29 -4 0 0 304.8 12.31 5 0 0 535.03 31.29 6 0 0 23.51 8.4 -6 0 0 13.13 4.84 7 0 0 256.25 28.67 8 0 0 77.19 17.3 -8 0 0 58.45 9.17 -9 0 0 34.65 7.78 -10 0 0 8.4 4.27 10 0 0 5.26 2.95 -11 0 0 73.14 9.21 1 1 0 2532.78 28.22 -2 1 0 1138.24 15.23 -3 1 0 2957.27 31.97 -3 -1 0 2965.36 36.33 -4 -1 0 4106.05 48.89 -4 1 0 4132.97 42.43 5 -1 0 1898.85 60.64 5 1 0 1925.99 57.65 -5 -1 0 1917.18 51.26 6 -1 0 480.97 34.94 -6 1 0 452.05 28.37 -6 -1 0 453.79 26.64 6 1 0 465.15 32.97 7 -1 0 7.91 4.33 7 1 0 1.38 3.17 -8 -1 0 25.06 5.74 -8 1 0 16.26 4.86 8 -1 0 14.8 8.38 8 1 0 28 11.1 -8 1 0 28.53 7.35 -9 1 0 5.84 3.48 -9 -1 0 5.44 1.89 -9 -1 0 10.86 4.44 -10 -1 0 40.68 7.81 10 1 0 35.41 7.06 -10 1 0 41.05 7.64 -11 -1 0 26.61 6.24 -11 1 0 18.58 5.2 0 2 0 2122.56 20.15 1 2 0 23.31 3.02 -1 -2 0 19.66 2.33 -2 -2 0 965.94 22.2 2 2 0 979.58 25.23 3 2 0 2932.5 53.01 -3 -2 0 2981.63 42.56 -4 -2 0 84.16 9.67 4 2 0 81.89 10.76 -4 -2 0 72.17 6.86 -5 -2 0 827.14 32.67 5 2 0 796.29 37.07 6 2 0 1.96 2.64 -6 -2 0 -1.58 2.39 6 -2 0 3.05 3.04 7 2 0 149.08 21.51 7 -2 0 316.07 34.53 -8 -2 0 63.78 9.4 8 2 0 77.76 17.39 -8 2 0 59.19 10.3 8 -2 0 80.31 18.83 -9 2 0 4.09 3.21 -9 -2 0 5.02 3.32 -9 -2 0 5.96 3.46 -10 -2 0 4.65 3.63 10 2 0 0.38 1.99 -10 2 0 1.63 1.36 11 2 0 27.45 5.01 -11 -2 0 35.44 6.49 0 3 0 -0.17 0.43 1 3 0 129.04 7.76 -2 -3 0 339.88 13.35 2 3 0 423.98 17.25 3 3 0 62.42 8 -3 -3 0 57.19 6.56 -4 -3 0 580.82 21.53 4 3 0 588 27.84 -4 -3 0 593.12 24.66 -5 -3 0 20.01 5.23 5 3 0 21.38 6.42 -6 -3 0 61.91 9.86 6 -3 0 58.51 13.14 6 3 0 70.13 12.74 -7 3 0 28.39 7.12 7 3 0 32.84 9.43 7 -3 0 27.36 11.1 8 3 0 344.32 36.3 8 -3 0 349.98 38.91 -8 3 0 322.12 23.79 -8 -3 0 349.77 21.82 -9 -3 0 19.6 5.25 -9 3 0 16.6 5.05 10 3 0 5.05 2.82 -10 3 0 2.88 2.12 -10 -3 0 3.2 1.77 -11 -3 0 5.64 3.64 11 3 0 2.45 1.5 0 4 0 225.21 9.33 1 4 0 39.56 4.55 2 4 0 26.13 4.7 -2 -4 0 21.69 3.52 3 4 0 63.34 8.31 -3 -4 0 52.35 6.41 -4 -4 0 243.02 15.87 4 4 0 259.17 18.96 -4 -4 0 275.3 16.01 -5 -4 0 51.59 8.15 5 4 0 52.81 10.13 6 4 0 34.75 9.14 -6 -4 0 38.77 7.98 7 4 0 127.61 19.79 -7 4 0 106.29 12.91 7 -4 0 141.7 23.18 -7 -4 0 108.3 11.69 -8 -4 0 117.65 12.97 8 4 0 100.78 19.35 -8 4 0 111.97 14.03 8 -4 0 110.62 22.3 -9 -4 0 28.57 6.36 -9 4 0 29.39 6.88 10 4 0 6.13 3.35 -10 4 0 2.26 1.84 11 4 0 -1.06 1.12 -11 -4 0 1.33 1.88 0 5 0 1.49 1.24 1 5 0 163.65 9.59 2 5 0 0.57 1.26 3 5 0 724.1 29.29 -3 -5 0 618.69 22.32 -4 -5 0 182.62 13.88 4 5 0 187.57 16.72 -5 -5 0 -0.53 0.94 5 5 0 0.62 1.94 -5 -5 0 -2.03 1.76 6 5 0 168.89 20.05 7 5 0 5.54 4.43 -7 5 0 2.31 2.44 7 -5 0 1.35 3.29 -7 -5 0 4.82 3.44 -8 5 0 21.7 6.38 -8 -5 0 22.66 6.07 8 5 0 26.72 9.74 8 -5 0 28.11 11.18 -9 5 0 23.22 6.63 -9 -5 0 33.76 6.94 -10 -5 0 21.32 5.62 -10 5 0 13.64 4.59 -11 -5 0 9.74 3.21 11 5 0 11.46 3.27 1 6 0 400.56 15.86 2 6 0 354.54 18.14 3 6 0 6.29 2.68 -4 -6 0 603.46 25.66 4 6 0 659.03 32.53 -5 -6 0 -1.2 0.91 5 6 0 2.51 2.5 6 6 0 8.23 3.94 -7 6 0 298.18 22.16 7 6 0 285.45 28.71 -7 -6 0 241.94 17.81 7 -6 0 333.18 35.51 8 -6 0 33.47 12.19 -8 6 0 34.08 7.87 -8 -6 0 30.03 6.83 8 6 0 22.38 9.17 -9 -6 0 43.86 7.96 -9 6 0 53.3 9.77 -10 -6 0 2.68 2.49 -10 -6 0 0.86 2.31 -11 -6 0 9.57 3.48 11 6 0 11.1 3.36 1 7 0 1674.51 34.78 2 7 0 286.7 16.9 3 7 0 3.65 2.19 4 7 0 10.68 4.23 -5 -7 0 23.41 6.14 5 7 0 28.46 8.17 6 7 0 95.37 15.03 7 -7 0 9.16 7.75 -7 -7 0 1.23 1.55 7 7 0 6.43 5.61 -7 7 0 2.24 1.99 8 7 0 75.3 16.4 8 -7 0 112.34 22.42 -8 -7 0 92.06 11.44 -8 7 0 112.05 14.35 -9 7 0 3.32 2.44 -9 -7 0 6.32 2.86 -10 -7 0 11.03 3.92 -10 -7 0 14.73 4.35 11 7 0 0.13 1.5 -11 -7 0 1.47 0.83 1 8 0 9.22 2.85 2 8 0 98.69 10.28 3 8 0 9.43 3.87 4 8 0 44.39 8.76 -5 -8 0 265.86 20.94 5 8 0 228.49 22.05 6 8 0 10.78 4.82 -7 -8 0 1.29 2.05 -7 8 0 2.7 2.36 7 8 0 1.82 4.2 -8 -8 0 32.34 7.09 -8 8 0 36.71 8.34 8 8 0 19.36 8.21 -9 8 0 1.52 2.47 -9 -8 0 1.34 2.34 -10 -8 0 0.31 1.81 -11 -8 0 -0.29 1.67 11 8 0 -0.06 1.42 1 9 0 424.23 19.02 2 9 0 3.46 2.17 3 9 0 33.18 7.31 4 9 0 91.91 13.23 5 9 0 155.59 18.73 -5 -9 0 155.26 16.92 6 9 0 26.35 8.29 -7 9 0 178.94 17.84 -7 -9 0 132.79 13.76 7 9 0 129.47 19.32 -8 9 0 127.09 15.72 -8 -9 0 105.96 12.58 -9 -9 0 2.49 1.88 -10 -9 0 0.21 0.91 11 9 0 2.04 2.07 -11 -9 0 1.43 1.34 1 10 0 0.73 1.47 2 10 0 322.27 19.75 3 10 0 177.23 17.25 4 10 0 3.34 2.67 5 10 0 3.86 4.22 6 10 0 2.63 3.14 7 10 0 8.9 5.45 -7 10 0 3.18 3.41 -7 -10 0 8.5 3.91 -8 -10 0 24.59 6.44 -8 10 0 28.78 8.14 -9 -10 0 -0.51 1.84 -10 -10 0 3.15 2.93 -11 -10 0 2.25 1.74 11 10 0 0.4 0.8 1 11 0 18.19 4.31 2 11 0 243.3 17.79 3 11 0 91.38 12.68 4 11 0 5.47 4.14 5 11 0 82.44 14.17 6 11 0 177.56 22.08 -6 -11 0 161.7 15.15 -7 11 0 176.82 18.24 -7 -11 0 152.6 15.29 7 11 0 126.06 19.51 -8 -11 0 16.53 5.46 -9 -11 0 3.64 2.66 -10 -11 0 63.69 8.69 11 11 0 23.23 4.76 -11 -11 0 23.19 4.61 1 12 0 117.49 11.58 2 12 0 10.75 3.83 3 12 0 59.74 10.67 4 12 0 117.02 16.89 5 12 0 33.26 9.56 6 12 0 287.76 29 -6 -12 0 284.47 20.66 -7 -12 0 35.44 7.57 7 12 0 21.76 8.29 -8 -12 0 64.42 10.21 -9 -12 0 99.54 12.18 -10 -12 0 27.33 5.88 -11 -12 0 46.48 6.24 11 12 0 40.85 5.91 1 13 0 43.17 7.44 2 13 0 202.39 17.01 3 13 0 105.94 14.3 4 13 0 41.3 10.09 5 13 0 213.16 24.78 -6 -13 0 219.56 18.51 6 13 0 211.57 25.56 -7 -13 0 232.73 19.5 7 13 0 148.71 21.82 -8 -13 0 26.15 6.48 -9 -13 0 7.71 4.49 -10 -13 0 33.67 6.22 -11 -13 0 7.85 2.78 11 13 0 4.79 2.3 2 14 0 1094.26 40.88 3 14 0 26.65 7.33 4 14 0 338.43 30.02 5 14 0 23.4 8.26 6 14 0 410.77 36.91 -6 -14 0 444.04 26.63 -7 -14 0 57.19 10.09 -8 -14 0 15.93 5.24 -9 -14 0 120.13 13.26 -10 -14 0 23.63 5.05 -11 -14 0 81.56 7.72 11 14 0 78.71 7.85 2 15 0 602.95 31.62 3 15 0 124.21 16.11 4 15 0 1.5 2.94 5 15 0 64.11 14.35 -6 -15 0 45.16 8.61 6 15 0 27.36 9.9 -7 -15 0 283.02 22.07 -8 -15 0 18.96 5.64 -9 -15 0 50.63 8.61 -10 -15 0 16.78 4.32 11 15 0 3.95 2.11 -11 -15 0 7.11 2.26 2 16 0 130.51 15.17 3 16 0 348.22 27.57 4 16 0 -0.18 1.87 -5 -16 0 4.77 2.96 5 16 0 9.18 6.57 -6 -16 0 93.67 12.66 6 16 0 62.73 14.89 -7 -16 0 11.16 4.63 -8 -16 0 1.8 1.94 -9 -16 0 20.88 5.47 10 16 0 2.28 1.88 -10 -16 0 0.96 1.55 -11 -16 0 27.38 3.92 11 16 0 21.01 3.72 2 17 0 157.77 17.62 3 17 0 18.71 7.08 4 17 0 43.38 11.27 -5 -17 0 44.68 8.64 5 17 0 36 10.97 -6 -17 0 17.62 5.64 -7 -17 0 159.9 16.61 -8 -17 0 2.37 3.86 -9 -17 0 0.1 1.64 -10 -17 0 8.12 2.98 10 17 0 6.1 2.88 3 18 0 101.45 15.97 -4 -18 0 -0.74 2.71 4 18 0 1.07 1.85 5 18 0 113.16 19.9 -5 -18 0 122.55 14.31 -6 -18 0 2.35 2.73 -7 -18 0 4.08 3.14 -8 -18 0 9.5 3.91 -9 -18 0 6.59 3.1 10 18 0 4.2 2.44 -10 18 0 1.98 1.62 -10 -18 0 5.75 2.46 3 19 0 29.1 9.46 -4 -19 0 54.07 9.44 4 19 0 34.79 10.59 -5 -19 0 24.16 6.4 -6 -19 0 0.12 1.55 -7 -19 0 6.78 3.49 -8 -19 0 10.34 4.18 -9 -19 0 7.1 3.3 -10 19 0 3.87 1.74 10 19 0 10.32 3.3 -10 -19 0 5.65 2.06 -3 -20 0 13.93 4.75 3 20 0 8.67 3.74 4 20 0 44.62 12.74 -4 -20 0 48.1 8.93 -5 -20 0 30.33 7.55 -6 -20 0 192.79 18.65 -7 -20 0 0.51 1.9 -8 -20 0 4.8 2.8 -9 -20 0 4.94 2.57 10 20 0 2.84 1.67 -10 -20 0 3.01 1.46 -10 20 0 1.63 1.37 -3 -21 0 62.4 10.3 3 21 0 59.88 9.95 -3 21 0 52.77 8.43 -4 -21 0 6.97 3.81 -5 -21 0 3.76 2.57 -6 -21 0 8.59 4.47 -7 -21 0 3.7 2.54 -8 -21 0 7.21 3.19 -9 -21 0 7.14 3.11 -9 21 0 4.8 2.23 -10 -21 0 10.96 2.79 10 21 0 10.79 2.83 1 22 0 36.58 6.89 -1 22 0 33.89 6.54 -2 22 0 11.09 3.41 -2 -22 0 7.02 3.73 2 22 0 11.64 4.54 3 22 0 -2.28 2.29 -3 -22 0 3.05 2.93 -3 22 0 -0.35 2.09 -4 -22 0 11.88 4.63 -4 22 0 6.29 3.57 -5 -22 0 -2.32 2.3 -6 -22 0 4.85 3.17 -7 -22 0 2.02 2.43 -8 22 0 -1.46 1.87 -8 -22 0 0.44 2.17 9 22 0 4.5 2.18 -9 22 0 7.53 2.58 -9 -22 0 5.48 2.19 0 23 0 1.01 2.58 -1 23 0 42.31 7.58 1 23 0 43.53 7.99 -1 -23 0 43.86 8.07 -2 -23 0 13.31 4.73 2 23 0 21.49 6 -2 23 0 16.9 4.79 -3 23 0 5.44 2.71 -3 -23 0 9.67 3.93 3 23 0 9.15 4.2 -4 -23 0 2.25 1.16 -4 23 0 1.22 1.79 -5 23 0 0.74 1.74 -5 -23 0 3.13 2.89 -6 -23 0 15.16 5.17 -6 23 0 17.88 5.93 -7 -23 0 8.35 3.38 -7 23 0 7.51 4.23 -8 23 0 1.62 2.38 -8 -23 0 2.07 1.83 -9 -23 0 9.29 2.94 9 23 0 10.44 3.12 -9 23 0 4.45 2.23 0 24 0 24.74 5.97 1 24 0 3.61 2.91 -1 24 0 0.53 1.13 -1 -24 0 2.6 1.85 -2 -24 0 9.48 3.95 -2 24 0 7.01 3.18 2 24 0 12.02 4.03 3 24 0 3.84 2.74 -3 -24 0 6.72 3.54 -3 24 0 7.26 3.03 -4 24 0 17.3 5.33 -4 -24 0 14.42 4.64 -5 24 0 14.92 5 -5 -24 0 10.95 4.51 -6 -24 0 6.28 2.94 -6 24 0 10.25 4.1 -7 -24 0 17.49 5.12 -7 24 0 8.54 4.28 -8 24 0 11.41 3.64 -8 -24 0 10.1 3.69 -9 24 0 -0.7 0.92 -9 -24 0 2.12 1.27 9 24 0 0.86 1.07 0 -25 0 4.99 3.48 0 25 0 4.33 3.04 -1 -25 0 63.75 10.5 1 25 0 55.93 9.36 -1 25 0 62.66 9.53 -2 25 0 -0.25 1.66 -2 -25 0 0.75 1.46 2 25 0 -0.29 2 3 25 0 3.32 2.8 -3 25 0 2.54 2.58 -3 -25 0 1.14 1.49 -4 25 0 15.24 4.95 -4 -25 0 17.45 6.06 -5 -25 0 48.12 9.2 -5 25 0 53.79 9.62 -6 -25 0 9.24 4.61 -6 25 0 10.58 4.25 -7 25 0 19.88 5.53 -7 -25 0 15.3 4.83 -8 25 0 6.16 2.84 8 25 0 3.02 2.01 -8 -25 0 3.91 2.01 -9 -25 0 4.7 2.1 0 -26 0 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4 -8 6.79 2.34 0 -4 -8 3.85 1.68 0 4 -8 4.27 1.65 -1 4 -8 2.79 1.5 -2 4 -8 1.91 1.19 6 5 -8 7.4 2.22 5 5 -8 2.36 1.3 4 5 -8 35.03 4.93 3 5 -8 9.94 2.69 2 5 -8 -0.37 0.74 2 5 -8 6.3 2.88 1 5 -8 3.92 1.39 1 5 -8 6.41 2.47 0 -5 -8 -0.38 0.65 0 5 -8 5.21 2.2 -1 5 -8 0.37 1.28 6 6 -8 14.08 2.73 5 6 -8 0.09 0.62 4 6 -8 -0.63 1.38 3 6 -8 -2.04 1.8 2 6 -8 3.67 1.65 2 6 -8 16.12 3.69 1 6 -8 1.77 0.93 1 6 -8 4.72 1.85 0 6 -8 8.17 4.11 -1 6 -8 3.79 1.84 6 7 -8 10.32 2.33 5 7 -8 2.11 1.12 4 7 -8 16.04 3.34 3 -7 -8 33.84 4.5 3 7 -8 35.19 5.04 2 7 -8 -2.35 1.6 2 7 -8 3.68 2.1 1 7 -8 -3.22 1.63 1 7 -8 0.69 1.6 0 7 -8 0.8 1.39 -1 7 -8 3.58 1.71 6 8 -8 29.31 3.58 5 8 -8 0.64 0.77 4 8 -8 18.86 3.54 3 -8 -8 5.83 2.04 3 8 -8 -0.8 1.65 2 8 -8 -1.63 1.72 2 8 -8 2.11 1.61 1 8 -8 -3.34 1.87 1 8 -8 -0.25 0.76 0 8 -8 0.25 0.84 -1 8 -8 9.57 2.5 5 9 -8 5.86 1.8 4 -9 -8 4.97 1.62 4 9 -8 7.35 2.1 3 -9 -8 33.12 4.45 3 9 -8 36.1 5.02 2 -9 -8 29.4 4.57 2 9 -8 -1.38 1.26 1 9 -8 -0.01 0.77 1 9 -8 4.72 1.87 0 9 -8 -0.57 0.72 -1 9 -8 -0.67 0.7 5 10 -8 -0.31 0.72 4 -10 -8 13.32 2.55 4 10 -8 24.27 3.84 3 -10 -8 6.71 2.06 3 10 -8 2.65 1.3 2 -10 -8 26.71 4.27 2 10 -8 -0.59 1.25 1 10 -8 0.65 0.77 1 10 -8 0.39 1 0 10 -8 16.16 3.08 5 11 -8 -0.28 0.54 4 -11 -8 -0.82 0.99 4 11 -8 1.77 0.78 3 -11 -8 4.63 1.77 3 11 -8 7.38 2.24 2 -11 -8 39.51 4.89 2 11 -8 14.03 2.94 1 11 -8 0.32 0.57 1 11 -8 -0.2 0.73 0 11 -8 -1.28 1.12 4 12 -8 24.18 3.61 3 -12 -8 41.68 4.68 3 12 -8 36 4.65 2 -12 -8 24.13 3.91 2 12 -8 0.04 1.01 1 12 -8 13.28 2.69 4 13 -8 4.21 1.54 3 -13 -8 4.8 1.72 3 13 -8 2.05 0.91 2 -13 -8 55.61 5.39 2 13 -8 29.17 4.01 3 14 -8 34.53 4.19 2 14 -8 0.53 0.72