#------------------------------------------------------------------------------ #$Date: 2024-08-05 21:11:07 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293772 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/19/1571943.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_1571943 loop_ _publ_author_name 'Arnold, Robert E.' 'Saska, Jan' 'Mesquita-Ribeiro, Raquel' 'Dajas-Bailador, Federico' 'Taylor, Laurence' 'Lewis, William' 'Argent, Stephen' 'Shao, Huiling' 'Houk, Kendall N.' 'Denton, Ross M.' _publ_section_title ; Total synthesis, biological evaluation and biosynthetic re-evaluation of Illicium-derived neolignans. ; _journal_issue 30 _journal_name_full 'Chemical science' _journal_page_first 11783 _journal_page_last 11793 _journal_paper_doi 10.1039/d4sc03232b _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C27 H26 O3' _chemical_formula_sum 'C27 H26 O3' _chemical_formula_weight 398.48 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2022-08-09 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _audit_update_record ; 2024-01-23 deposited with the CCDC. 2024-06-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.545(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 11.5253(3) _cell_length_b 11.2640(3) _cell_length_c 33.0222(10) _cell_measurement_reflns_used 11417 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 73.4190 _cell_measurement_theta_min 2.6550 _cell_volume 4282.7(2) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_environment 'N2 gas' _diffrn_ambient_temperature 120(2) _diffrn_crystal_treatment 'flash frozen in gaseous N2' _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 4.2207 _diffrn_detector_type 'Agilent Diffraction Titan S2 detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.976 _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 -119.00 -14.00 1.00 30.00 -- -42.81 -19.00 30.00 105 2 \w -50.00 28.00 1.00 30.00 -- -42.81 38.00-150.00 78 3 \w 23.00 96.00 1.00 30.00 -- 42.81-125.00-120.00 73 4 \w 34.00 98.00 1.00 120.00 -- 103.00 -45.00 0.00 64 5 \w 94.00 175.00 1.00 120.00 -- 103.00 125.00-120.00 81 6 \w 22.00 110.00 1.00 120.00 -- 103.00 -94.00 -30.00 88 7 \w 94.00 175.00 1.00 120.00 -- 103.00 125.00-180.00 81 8 \w 67.00 178.00 1.00 120.00 -- 103.00 15.00 -30.00 111 9 \w 34.00 98.00 1.00 120.00 -- 103.00 -45.00 90.00 64 10 \w 73.00 175.00 1.00 120.00 -- 103.00 77.00 150.00 102 11 \w 34.00 98.00 1.00 120.00 -- 103.00 -45.00 -90.00 64 12 \w -50.00 28.00 1.00 30.00 -- -42.81 38.00 0.00 78 13 \w 19.00 112.00 1.00 30.00 -- 42.81 57.00 -30.00 93 14 \w 12.00 115.00 1.00 30.00 -- 42.81 77.00-150.00 103 15 \w 30.00 64.00 1.00 120.00 -- 103.00 -30.00-180.00 34 ; _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'SuperNova, Titan S2' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0103967000 _diffrn_orient_matrix_UB_12 0.0361423000 _diffrn_orient_matrix_UB_13 0.0446910000 _diffrn_orient_matrix_UB_21 0.0691336000 _diffrn_orient_matrix_UB_22 -0.1113632000 _diffrn_orient_matrix_UB_23 0.0134511000 _diffrn_orient_matrix_UB_31 0.1140700000 _diffrn_orient_matrix_UB_32 0.0706979000 _diffrn_orient_matrix_UB_33 -0.0016557000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_unetI/netI 0.0498 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.976 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_number 32607 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.976 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.971 _diffrn_reflns_theta_min 2.679 _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'Agilent Diffraction microfocus tube' _exptl_absorpt_coefficient_mu 0.627 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.657 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Numerical absorption correction based on gaussian integration over a multifaceted crystal model 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 1.236 _exptl_crystal_description plate _exptl_crystal_F_000 1696 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: ethylacetate, pentane' _exptl_crystal_size_max 0.418 _exptl_crystal_size_mid 0.108 _exptl_crystal_size_min 0.039 _refine_diff_density_max 0.351 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.057 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 556 _refine_ls_number_reflns 8478 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.091 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0707 _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^)+(0.0437P)^2^+6.0770P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1523 _refine_ls_wR_factor_ref 0.1651 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6588 _reflns_number_total 8478 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03232b2.cif _cod_data_source_block 2-simonsol-C _cod_depositor_comments 'Adding full bibliography for 1571943--1571950.cif.' _cod_database_code 1571943 _nottingham_internal_coll_name REARDK _nottingham_internal_coll_number 17991 _nottingham_internal_coll_client REA/RD _nottingham_internal_coll_type custom _nottingham_internal_coll_frame_method '\w scans' _nottingham_internal_coll_frame_time '30.00, 120.00' _nottingham_internal_coll_frame_width 1.00 _nottingham_internal_coll_user pczlt _nottingham_internal_coll_date 30/11/2018 _nottingham_internal_coll_location NOTTS _nottingham_internal_coll_instrument 'GVA, PL13110002' _nottingham_internal_process_date 03/12/2018 _nottingham_internal_process_user pczlt _nottingham_internal_solution_date 03/12/2018 _nottingham_internal_solution_user pczlt _nottingham_internal_refinement_date 09/08/2022 _nottingham_internal_refinement_user pczlt/pczspa _nottingham_internal_validation_date 09/08/2022 _nottingham_internal_validation_user pczspa _nottingham_internal_archive_date 09/08/2022 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C27 H26 O3' _chemical_oxdiff_usercomment 'REARDK3 #17991 GVA-1541 IN FOMBLIN FILM ON A MICROMOUNT FOR RA/RD' _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 0.976 _shelx_estimated_absorpt_t_min 0.780 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All O(H) groups 2. Restrained distances C20B-C19B \\sim C20A-C19A with sigma of 0.02 C18B-C19B \\sim C19A-C18A with sigma of 0.02 C18B-C15A \\sim C18A-C15A with sigma of 0.02 3. Restrained planarity C16A, C15A, C18B, C14A with sigma of 0.1 4. Uiso/Uaniso restraints and constraints C18B \\sim C18A \\sim C19B \\sim C19A \\sim C20B \\sim C20A \\sim C15A: within 0.01A with sigma of 3.5 and sigma for terminal atoms of 0.005 within 0.01A 5. Rigid body (RIGU) restrains C20A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C30A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C10A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C10B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C2 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C30B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(H20C)=Sof(H20D)=Sof(C18B)=Sof(H18C)= Sof(H18D)=1-FVAR(1) Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)= Sof(H20B)=FVAR(1) 7.a Ternary CH refined with riding coordinates: C6A(H6A), C6B(H6B) 7.b Secondary CH2 refined with riding coordinates: C7A(H7AA,H7AB), C8A(H8AA,H8AB), C18A(H18A,H18B), C28A(H28A,H28B), C7B(H7BA, H7BB), C8B(H8BA,H8BB), C3(H3C,H3D), C28B(H28C,H28D), C18B(H18C,H18D) 7.c Aromatic/amide H refined with riding coordinates: C3A(H3A), C4A(H4A), C9A(H9A), C14A(H14A), C16A(H16A), C19A(H19A), C23A(H23A), C24A(H24A), C26A(H26A), C29A(H29A), C3B(H3B), C4B(H4B), C9B(H9B), C14B(H14B), C16B(H16B), C1(H1), C23B(H23B), C24B(H24B), C26B(H26B), C29B(H29B), C19B(H19B) 7.d X=CH2 refined with riding coordinates: C10A(H10A,H10B), C20A(H20A,H20B), C30A(H30A,H30B), C10B(H10C,H10D), C2(H2A, H2B), C30B(H30C,H30D), C20B(H20C,H20D) 7.e Idealised tetrahedral OH refined as rotating group: O27A(H27A), O27B(H27B) ; _shelx_res_file ; TITL reardk3_a.res in P2(1)/n reardk3.res created by SHELXL-2018/3 at 12:05:49 on 09-Aug-2022 REM Old TITL REARDK3 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.185, Rweak 0.177, Alpha 0.037, Orientation as input REM Formula found by SHELXT: C48 O12 CELL 1.54184 11.5253 11.264 33.0222 90 92.545 90 ZERR 8 0.0003 0.0003 0.001 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O UNIT 216 208 24 EQIV $1 -1+X,+Y,+Z SADI C20B C19B C20A C19A SADI C18B C19B C19A C18A SADI C18B C15A C18A C15A SIMU 3.5 0.005 0.01 C18B C18A C19B C19A C20B C20A C15A FLAT C16A C15A C18B C14A RIGU C20A RIGU C30A RIGU C10A RIGU C10B RIGU C2 RIGU C30B L.S. 10 PLAN 5 SIZE 0.039 0.108 0.418 TEMP -153(2) CONF HTAB O27A O1B HTAB O27B O1A_$1 BOND $H list 4 MORE -1 fmap 2 53 acta REM REM REM WGHT 0.043700 6.077000 FVAR 0.35529 0.84896 O1A 3 0.600168 0.170966 0.306129 11.00000 0.01788 0.03495 = 0.06829 0.00766 -0.00485 0.00039 C2A 1 0.495377 0.166143 0.311959 11.00000 0.02314 0.01717 = 0.04798 -0.00455 -0.00835 0.00183 C3A 1 0.451029 0.116062 0.348846 11.00000 0.02747 0.02024 = 0.04346 0.00110 -0.01121 0.00278 AFIX 43 H3A 2 0.503176 0.076590 0.367424 11.00000 -1.20000 AFIX 0 C4A 1 0.338884 0.124083 0.357308 11.00000 0.02967 0.01670 = 0.04085 0.00070 -0.00563 -0.00031 AFIX 43 H4A 2 0.314090 0.082819 0.380478 11.00000 -1.20000 AFIX 0 C5A 1 0.248639 0.194020 0.332701 11.00000 0.02058 0.01747 = 0.04407 0.00001 -0.00673 -0.00004 C6A 1 0.304100 0.264280 0.298471 11.00000 0.02505 0.01900 = 0.03412 -0.00545 -0.00883 0.00360 AFIX 13 H6A 2 0.243684 0.282096 0.276646 11.00000 -1.20000 AFIX 0 C7A 1 0.408274 0.207826 0.279971 11.00000 0.02242 0.02492 = 0.03674 -0.00530 -0.00495 0.00484 AFIX 23 H7AA 2 0.382395 0.139543 0.262990 11.00000 -1.20000 H7AB 2 0.445375 0.266223 0.262252 11.00000 -1.20000 AFIX 0 C8A 1 0.145090 0.114144 0.318929 11.00000 0.02460 0.02323 = 0.07126 -0.00603 -0.01213 -0.00182 AFIX 23 H8AA 2 0.100467 0.094102 0.342935 11.00000 -1.20000 H8AB 2 0.093143 0.159997 0.300066 11.00000 -1.20000 AFIX 0 C9A 1 0.177712 0.002706 0.298771 11.00000 0.03308 0.03601 = 0.03947 -0.00750 0.00156 -0.00767 AFIX 43 H9A 2 0.210808 0.008824 0.273014 11.00000 -1.20000 AFIX 0 C10A 1 0.164552 -0.103156 0.313617 11.00000 0.04403 0.02197 = 0.05021 -0.00288 -0.00234 -0.00210 AFIX 93 H10A 2 0.131764 -0.112897 0.339298 11.00000 -1.20000 H10B 2 0.187730 -0.170734 0.298779 11.00000 -1.20000 AFIX 0 O11A 3 0.345323 0.375963 0.317235 11.00000 0.02826 0.01786 = 0.03063 -0.00254 -0.00062 -0.00155 C12A 1 0.278687 0.394370 0.349855 11.00000 0.02004 0.02013 = 0.02883 0.00108 -0.00160 -0.00016 C13A 1 0.213967 0.295580 0.359724 11.00000 0.02242 0.01679 = 0.03863 0.00030 -0.00458 -0.00035 C14A 1 0.141936 0.299611 0.392163 11.00000 0.02116 0.02099 = 0.04970 0.00420 0.00307 -0.00308 AFIX 43 H14A 2 0.096540 0.232517 0.398761 11.00000 -1.20000 AFIX 0 C15A 1 0.136905 0.403487 0.415026 11.00000 0.02377 0.02734 = 0.04158 0.00188 0.00607 0.00035 C16A 1 0.206021 0.499519 0.405014 11.00000 0.02653 0.02045 = 0.03460 -0.00191 0.00191 0.00022 AFIX 43 H16A 2 0.203551 0.569177 0.421173 11.00000 -1.20000 AFIX 0 C17A 1 0.279189 0.498236 0.372161 11.00000 0.02240 0.01701 = 0.03000 0.00155 -0.00212 0.00098 PART 1 C18A 1 0.065323 0.407747 0.452775 21.00000 0.02655 0.03573 = 0.04547 0.00510 0.00658 0.00116 AFIX 23 H18A 2 0.068088 0.489297 0.463957 21.00000 -1.20000 H18B 2 -0.016650 0.389492 0.444939 21.00000 -1.20000 AFIX 0 C19A 1 0.106787 0.322717 0.485063 21.00000 0.03571 0.03274 = 0.04823 0.00469 0.01145 -0.00097 AFIX 43 H19A 2 0.106914 0.240768 0.478265 21.00000 -1.20000 AFIX 0 C20A 1 0.142640 0.351412 0.521610 21.00000 0.03487 0.05344 = 0.05286 0.00531 0.00775 0.00412 AFIX 93 H20A 2 0.143942 0.432368 0.529685 21.00000 -1.20000 H20B 2 0.167556 0.291441 0.540264 21.00000 -1.20000 AFIX 0 PART 0 C21A 1 0.356425 0.599347 0.363256 11.00000 0.02213 0.01681 = 0.03067 -0.00086 -0.00011 0.00050 C22A 1 0.355756 0.654210 0.325468 11.00000 0.02343 0.02024 = 0.02987 -0.00335 -0.00087 0.00213 C23A 1 0.430527 0.748209 0.318468 11.00000 0.02953 0.01977 = 0.03362 0.00195 0.00311 -0.00016 AFIX 43 H23A 2 0.428882 0.785541 0.292652 11.00000 -1.20000 AFIX 0 C24A 1 0.507477 0.787624 0.349045 11.00000 0.02383 0.01731 = 0.04234 -0.00113 0.00340 -0.00230 AFIX 43 H24A 2 0.558936 0.851273 0.343984 11.00000 -1.20000 AFIX 0 C25A 1 0.509689 0.734234 0.387222 11.00000 0.02301 0.02154 = 0.03826 -0.00352 -0.00116 -0.00045 C26A 1 0.434291 0.641474 0.393804 11.00000 0.02532 0.01972 = 0.03117 -0.00106 0.00098 -0.00051 AFIX 43 H26A 2 0.435236 0.605180 0.419785 11.00000 -1.20000 AFIX 0 O27A 3 0.279948 0.624173 0.293854 11.00000 0.03372 0.02265 = 0.03140 0.00293 -0.00538 -0.00546 AFIX 147 H27A 2 0.246999 0.559829 0.299119 11.00000 -1.50000 AFIX 0 C28A 1 0.589796 0.780462 0.421239 11.00000 0.02796 0.03246 = 0.04561 -0.00065 -0.00535 -0.01047 AFIX 23 H28A 2 0.611063 0.714597 0.439982 11.00000 -1.20000 H28B 2 0.661984 0.810962 0.409827 11.00000 -1.20000 AFIX 0 C29A 1 0.532859 0.878118 0.444351 11.00000 0.03811 0.03941 = 0.03797 -0.00233 -0.00229 -0.01015 AFIX 43 H29A 2 0.466809 0.858290 0.459187 11.00000 -1.20000 AFIX 0 C30A 1 0.568363 0.988600 0.445356 11.00000 0.05487 0.04168 = 0.05028 -0.00584 -0.00572 -0.01102 AFIX 93 H30A 2 0.634147 1.011450 0.430859 11.00000 -1.20000 H30B 2 0.528327 1.045872 0.460583 11.00000 -1.20000 AFIX 0 O1B 3 0.095975 0.451435 0.278271 11.00000 0.01961 0.03051 = 0.05004 0.00884 0.00428 0.00062 C2B 1 -0.000973 0.454783 0.292307 11.00000 0.02074 0.01997 = 0.03771 0.00857 -0.00138 -0.00057 C3B 1 -0.027289 0.537184 0.324884 11.00000 0.02783 0.02225 = 0.04098 0.00019 -0.00385 -0.00466 AFIX 43 H3B 2 0.029867 0.593414 0.333681 11.00000 -1.20000 AFIX 0 C4B 1 -0.128719 0.535851 0.342573 11.00000 0.03343 0.01878 = 0.03403 0.00027 -0.00087 0.00129 AFIX 43 H4B 2 -0.140931 0.594606 0.362579 11.00000 -1.20000 AFIX 0 C5B 1 -0.225617 0.449264 0.333587 11.00000 0.02346 0.01714 = 0.03422 0.00079 0.00122 0.00306 C6B 1 -0.190561 0.349428 0.304587 11.00000 0.01936 0.01643 = 0.03176 0.00109 -0.00121 0.00061 AFIX 13 H6B 2 -0.261744 0.321085 0.289077 11.00000 -1.20000 AFIX 0 C7B 1 -0.099209 0.380785 0.274743 11.00000 0.02135 0.02260 = 0.03124 0.00098 0.00203 -0.00082 AFIX 23 H7BA 2 -0.066929 0.306379 0.263932 11.00000 -1.20000 H7BB 2 -0.137035 0.424370 0.251710 11.00000 -1.20000 AFIX 0 C8B 1 -0.338105 0.513725 0.319083 11.00000 0.02412 0.02692 = 0.04097 0.00453 0.00374 0.00940 AFIX 23 H8BA 2 -0.403312 0.456455 0.318567 11.00000 -1.20000 H8BB 2 -0.355378 0.576939 0.338755 11.00000 -1.20000 AFIX 0 C9B 1 -0.330400 0.567692 0.277987 11.00000 0.02705 0.02756 = 0.04544 0.01006 0.00266 0.00663 AFIX 43 H9B 2 -0.273807 0.627789 0.274616 11.00000 -1.20000 AFIX 0 C10B 1 -0.396011 0.538021 0.246393 11.00000 0.04023 0.04266 = 0.04464 0.00901 -0.00451 0.00669 AFIX 93 H10C 2 -0.453515 0.478255 0.248665 11.00000 -1.20000 H10D 2 -0.386283 0.576180 0.221113 11.00000 -1.20000 AFIX 0 O11B 3 -0.145334 0.251888 0.330318 11.00000 0.02390 0.01696 = 0.03058 0.00227 0.00291 0.00274 C12B 1 -0.191222 0.267157 0.367633 11.00000 0.01819 0.01964 = 0.02953 -0.00021 0.00058 -0.00147 C13B 1 -0.240525 0.378775 0.372337 11.00000 0.02016 0.01659 = 0.03425 0.00200 0.00017 -0.00006 C14B 1 -0.288296 0.410391 0.408360 11.00000 0.02465 0.02172 = 0.03709 -0.00192 -0.00002 0.00264 AFIX 43 H14B 2 -0.323027 0.486241 0.411225 11.00000 -1.20000 AFIX 0 C15B 1 -0.285175 0.329869 0.440623 11.00000 0.02127 0.02827 = 0.03209 -0.00177 -0.00103 -0.00216 C16B 1 -0.234453 0.219189 0.435175 11.00000 0.02228 0.02477 = 0.03280 0.00271 -0.00117 -0.00256 AFIX 43 H16B 2 -0.231169 0.165283 0.457321 11.00000 -1.20000 AFIX 0 C17B 1 -0.187708 0.183172 0.398392 11.00000 0.01753 0.01994 = 0.03526 0.00167 -0.00103 -0.00138 C3 1 -0.341637 0.360129 0.479725 11.00000 0.03509 0.03184 = 0.03233 -0.00053 0.00138 0.00128 AFIX 23 H3C 2 -0.312296 0.304779 0.501101 11.00000 -1.20000 H3D 2 -0.317883 0.441332 0.488029 11.00000 -1.20000 AFIX 0 C1 1 -0.472635 0.354074 0.477139 11.00000 0.03518 0.03446 = 0.04110 0.00429 0.01408 0.00591 AFIX 43 H1 2 -0.511264 0.375134 0.500925 11.00000 -1.20000 AFIX 0 C2 1 -0.538673 0.322956 0.445675 11.00000 0.02877 0.04737 = 0.05695 0.00299 0.00487 0.00158 AFIX 93 H2A 2 -0.504573 0.301033 0.421097 11.00000 -1.20000 H2B 2 -0.620729 0.322281 0.447405 11.00000 -1.20000 AFIX 0 C21B 1 -0.136646 0.061898 0.394659 11.00000 0.01787 0.02141 = 0.03589 0.00636 0.00246 -0.00129 C22B 1 -0.174694 -0.019461 0.364925 11.00000 0.02067 0.02312 = 0.03698 0.00557 -0.00072 -0.00129 C23B 1 -0.126910 -0.132974 0.364193 11.00000 0.03449 0.02086 = 0.04413 -0.00036 -0.00007 0.00095 AFIX 43 H23B 2 -0.152140 -0.187362 0.343651 11.00000 -1.20000 AFIX 0 C24B 1 -0.042859 -0.167277 0.393178 11.00000 0.03554 0.01611 = 0.05024 0.00553 0.00122 0.00526 AFIX 43 H24B 2 -0.011426 -0.245171 0.392422 11.00000 -1.20000 AFIX 0 C25B 1 -0.004221 -0.089109 0.423242 11.00000 0.02299 0.02506 = 0.04281 0.00939 0.00172 0.00081 C26B 1 -0.051330 0.024094 0.423111 11.00000 0.02348 0.02143 = 0.03494 0.00337 0.00180 -0.00280 AFIX 43 H26B 2 -0.024266 0.078589 0.443356 11.00000 -1.20000 AFIX 0 O27B 3 -0.262439 0.000314 0.336807 11.00000 0.02858 0.02230 = 0.04801 0.00025 -0.01177 0.00013 AFIX 147 H27B 2 -0.277416 0.073260 0.335762 11.00000 -1.50000 AFIX 0 C28B 1 0.089074 -0.124224 0.454877 11.00000 0.03077 0.03411 = 0.04695 0.01291 -0.00260 0.00450 AFIX 23 H28C 2 0.062655 -0.104129 0.482162 11.00000 -1.20000 H28D 2 0.101138 -0.211168 0.453814 11.00000 -1.20000 AFIX 0 C29B 1 0.201119 -0.062919 0.448346 11.00000 0.02637 0.05233 = 0.05086 0.01508 -0.00314 0.00135 AFIX 43 H29B 2 0.243845 -0.084942 0.425572 11.00000 -1.20000 AFIX 0 C30B 1 0.243694 0.020373 0.472670 11.00000 0.04533 0.05600 = 0.08111 0.02015 -0.02194 -0.00991 AFIX 93 H30C 2 0.202509 0.043871 0.495636 11.00000 -1.20000 H30D 2 0.315619 0.057014 0.467265 11.00000 -1.20000 AFIX 0 PART 2 C19B 1 0.056462 0.360235 0.481170 -21.00000 0.03841 AFIX 43 H19B 2 -0.004302 0.363637 0.499655 -21.00000 -1.20000 AFIX 0 C20B 1 0.149089 0.302469 0.492985 -21.00000 0.08241 AFIX 93 H20C 2 0.212441 0.296370 0.475654 -21.00000 -1.20000 H20D 2 0.153662 0.266207 0.518981 -21.00000 -1.20000 AFIX 0 C18B 1 0.035692 0.420748 0.442346 -21.00000 0.02751 AFIX 23 H18C 2 0.024228 0.506612 0.447168 -21.00000 -1.20000 H18D 2 -0.036071 0.389180 0.428714 -21.00000 -1.20000 AFIX 0 HKLF 4 REM reardk3_a.res in P2(1)/n REM wR2 = 0.1651, GooF = S = 1.089, Restrained GooF = 1.091 for all data REM R1 = 0.0707 for 6588 Fo > 4sig(Fo) and 0.0916 for all 8478 data REM 556 parameters refined using 4 restraints END WGHT 0.0422 6.1801 REM Highest difference peak 0.351, deepest hole -0.276, 1-sigma level 0.057 Q1 1 0.1354 0.0179 0.3317 11.00000 0.05 0.35 Q2 1 0.6223 0.8863 0.4377 11.00000 0.05 0.29 Q3 1 -0.2062 0.4009 0.3191 11.00000 0.05 0.25 Q4 1 -0.1593 0.1245 0.3975 11.00000 0.05 0.25 Q5 1 -0.1772 -0.0061 0.4008 11.00000 0.05 0.23 ; _shelx_res_checksum 88485 _shelx_hkl_file ; 0 0 2 1465.70 11.99 0 0 -2 1399.44 15.52 0 0 -3 -0.43 1.04 0 0 -3 1.33 0.96 0 0 3 0.48 0.44 0 0 -4 4974.19 42.92 0 0 -4 4940.01 44.84 0 0 -5 0.34 1.78 0 0 -5 1.15 1.85 0 0 5 -0.29 0.89 0 0 -6 2190.44 37.32 0 0 6 2144.21 24.05 0 0 -7 0.97 2.60 0 0 -7 1.24 2.84 0 0 7 -0.68 1.62 0 0 -8 3825.49 58.33 0 0 8 3801.70 36.55 0 0 -8 3810.11 56.98 0 0 -9 4.38 4.16 0 0 9 12.15 5.20 0 0 -9 -4.85 6.48 0 0 10 -2.09 2.26 0 0 -10 0.61 2.42 0 0 -11 0.69 2.65 0 0 -11 1.35 3.01 0 0 11 0.64 1.45 0 0 12 48.08 6.08 0 0 -12 40.89 8.96 0 0 -12 35.34 6.79 0 0 13 -1.10 2.88 0 0 -13 0.81 3.89 0 0 -14 12.88 6.92 0 0 14 12.19 2.54 0 0 15 0.14 2.93 0 0 -15 4.25 5.93 0 0 -16 3.76 7.00 0 0 16 25.16 6.83 0 0 -17 2.46 5.93 0 0 17 18.60 7.15 0 0 18 22.98 4.09 0 0 -18 18.81 7.01 0 0 19 -1.97 2.42 0 0 -19 -1.16 4.89 0 0 20 1.19 2.42 0 0 -20 1.79 4.69 0 0 21 0.49 2.38 0 0 -21 0.51 4.60 0 0 22 39.81 7.18 0 0 -22 33.55 7.14 0 0 22 31.72 4.12 0 0 -22 41.21 9.92 0 0 23 -1.59 3.35 0 0 -23 -2.41 2.22 0 0 -23 1.36 2.76 0 0 -23 -0.33 4.45 0 0 23 3.84 2.15 0 0 -24 122.27 18.93 0 0 24 131.88 9.22 0 0 -24 139.31 13.54 0 0 24 151.20 15.68 0 0 -24 173.12 11.48 0 0 24 142.21 8.95 0 0 -25 0.93 3.68 0 0 25 0.75 3.38 0 0 -25 -6.95 2.64 0 0 -25 -1.85 7.19 0 0 25 -2.51 2.42 0 0 25 -2.84 2.46 0 0 -26 366.85 25.75 0 0 26 385.72 14.38 0 0 26 402.23 25.94 0 0 -26 332.42 33.75 0 0 -26 445.75 19.20 0 0 26 483.62 17.10 0 0 -27 2.11 1.92 0 0 -27 3.00 4.08 0 0 27 5.65 3.56 0 0 -27 -1.46 7.07 0 0 28 -0.41 1.97 0 0 -28 3.23 5.10 0 0 -28 -8.84 7.62 0 0 -29 3.84 7.86 0 0 29 0.54 1.86 0 0 -29 -0.23 3.40 0 0 -30 7.91 4.20 0 0 30 6.79 1.82 0 0 31 5.68 2.98 0 0 -31 2.99 4.43 0 0 32 68.84 7.12 0 0 -32 55.47 10.68 0 0 33 -3.26 2.44 0 0 -33 -2.08 3.22 0 0 34 38.14 4.58 0 0 35 0.29 1.56 0 0 36 47.12 4.68 0 0 37 26.98 4.08 0 0 38 30.66 3.47 0 0 39 1.19 1.20 0 -1 0 -0.47 0.50 0 1 0 -0.18 0.49 0 1 0 -0.35 0.91 0 1 -1 58.12 3.59 0 -1 -1 65.23 4.25 0 1 -1 59.17 3.25 0 -1 -1 63.70 2.95 0 1 1 67.92 3.69 0 1 1 63.06 4.19 0 1 -1 61.90 4.34 0 -1 1 68.34 3.01 0 1 -2 2465.32 23.92 0 1 -2 2522.41 31.61 0 1 2 2558.22 27.78 0 -1 -2 2539.97 28.20 0 -1 2 2522.13 21.31 0 -1 -2 2572.16 19.86 0 -1 -3 659.18 15.55 0 1 -3 670.02 13.66 0 1 3 677.92 7.17 0 -1 3 673.64 12.12 0 -1 -3 694.12 11.82 0 1 -4 874.13 17.16 0 -1 -4 859.64 14.88 0 -1 -4 899.45 19.85 0 1 5 835.95 11.29 0 1 -5 843.32 19.00 0 -1 -5 858.09 21.35 0 -1 -5 857.37 16.80 0 -1 5 846.21 16.17 0 -1 -6 996.39 19.91 0 1 6 1006.02 14.07 0 -1 -6 992.10 25.90 0 -1 6 1022.08 19.39 0 -1 7 3.98 2.53 0 1 -7 1.90 2.38 0 1 7 3.95 1.33 0 -1 -7 4.59 2.50 0 -1 -7 4.78 3.02 0 -1 8 40.24 7.26 0 1 8 40.86 5.21 0 -1 9 1583.94 28.10 0 1 -9 1537.54 38.28 0 1 9 1524.69 22.75 0 -1 -9 1532.31 40.33 0 -1 10 39.32 4.74 0 1 10 37.08 3.97 0 -1 -10 40.75 6.90 0 1 -10 33.26 6.46 0 1 11 65.52 5.87 0 -1 -11 57.64 7.42 0 -1 11 60.80 6.31 0 1 -11 54.65 9.36 0 -1 -11 68.59 9.44 0 1 -12 3.98 3.06 0 1 12 15.05 4.01 0 -1 -12 2.51 3.28 0 -1 12 19.34 5.79 0 -1 13 33.05 4.85 0 1 13 35.23 4.41 0 -1 -13 31.25 7.05 0 -1 -13 26.43 5.97 0 1 -13 25.39 7.33 0 1 14 17.32 2.81 0 1 -14 9.20 6.43 0 -1 -14 18.61 5.64 0 -1 14 18.32 5.26 0 -1 -15 113.96 17.10 0 -1 -15 128.70 13.72 0 1 -15 119.21 16.91 0 -1 15 146.94 10.20 0 1 15 141.04 8.91 0 1 16 55.91 6.28 0 -1 -16 38.53 8.18 0 1 -16 41.97 11.48 0 -1 16 46.44 6.86 0 1 -17 7.33 8.29 0 1 17 29.08 7.33 0 -1 17 33.69 9.76 0 -1 -17 18.44 8.62 0 -1 18 67.13 8.90 0 -1 -18 54.39 8.09 0 1 -18 56.49 14.21 0 -1 -18 53.18 11.05 0 1 18 70.97 8.11 0 -1 -19 14.31 6.29 0 -1 -19 19.46 9.56 0 1 19 20.19 5.05 0 -1 19 15.76 4.89 0 1 -19 14.15 8.30 0 1 -20 -4.10 6.71 0 1 20 -0.55 2.60 0 -1 20 1.23 2.77 0 -1 -20 -0.78 4.92 0 -1 21 104.16 11.67 0 -1 -21 89.89 15.38 0 1 -21 108.71 16.63 0 1 -21 86.26 20.30 0 1 21 105.66 10.74 0 -1 -22 63.77 8.84 0 -1 -22 70.18 12.98 0 1 22 53.79 3.50 0 1 22 83.83 9.94 0 1 -22 81.61 15.53 0 1 -22 70.64 9.94 0 -1 22 90.86 12.25 0 1 -23 201.82 17.07 0 -1 -23 214.30 23.37 0 1 23 240.15 17.42 0 -1 23 248.24 19.88 0 1 23 240.69 10.46 0 1 -23 245.43 13.86 0 -1 23 217.74 9.59 0 -1 -23 204.81 15.87 0 1 -23 222.93 25.38 0 1 23 225.63 11.14 0 1 -24 47.05 13.44 0 1 24 36.73 5.60 0 -1 24 76.20 6.95 0 -1 -24 46.44 12.60 0 1 24 72.43 8.23 0 1 -24 50.16 9.55 0 -1 24 59.37 10.98 0 -1 -24 46.23 10.11 0 1 -24 49.90 6.26 0 1 25 147.00 9.59 0 1 -25 130.56 11.19 0 1 -25 121.63 19.80 0 -1 -25 132.54 13.12 0 -1 25 137.21 7.39 0 -1 -25 110.93 18.89 0 -1 25 138.43 15.95 0 1 25 147.74 8.24 0 1 -25 119.81 13.65 0 -1 -26 3.38 7.02 0 1 -26 1.66 4.64 0 -1 -26 2.84 4.23 0 1 26 14.63 5.41 0 1 26 11.22 4.73 0 -1 26 12.81 3.86 0 -1 26 16.18 6.55 0 1 -26 1.07 7.30 0 1 -26 25.18 8.37 0 1 -27 38.33 5.94 0 1 27 45.89 5.35 0 1 27 69.61 6.57 0 -1 -27 37.61 12.63 0 -1 27 40.16 9.18 0 -1 -27 45.33 8.54 0 1 -27 36.78 12.27 0 1 -27 39.77 9.27 0 -1 27 56.28 5.66 0 1 28 55.14 6.41 0 -1 28 53.35 11.00 0 1 28 52.99 6.40 0 1 -28 37.73 13.29 0 -1 -28 47.91 9.42 0 1 -28 41.08 9.31 0 -1 -28 40.56 12.29 0 -1 28 50.27 5.42 0 -1 -29 46.59 16.22 0 -1 29 46.37 11.84 0 1 29 32.66 4.95 0 1 -29 15.13 8.33 0 -1 -29 24.99 7.46 0 1 29 28.45 4.94 0 1 -29 18.85 6.55 0 -1 29 24.30 5.03 0 -1 -30 120.85 14.00 0 1 30 127.61 8.50 0 1 -30 103.49 14.43 0 -1 30 109.50 7.55 0 -1 -31 0.92 4.38 0 -1 31 4.85 2.53 0 1 -31 0.84 3.53 0 1 31 -1.36 2.46 0 -1 -32 30.82 7.21 0 1 32 43.03 6.44 0 -1 32 25.75 3.90 0 -1 -33 29.31 8.03 0 -1 33 37.49 4.00 0 1 33 36.30 4.57 0 -1 -34 -0.51 2.66 0 -1 34 1.40 1.48 0 1 34 0.79 1.88 0 -1 -35 4.02 2.93 0 -1 35 1.22 1.54 0 1 35 0.18 1.70 0 -1 36 4.94 1.73 0 1 36 4.33 1.87 0 1 37 63.88 5.49 0 1 38 2.82 1.36 0 1 39 -0.50 1.08 0 -2 0 366.77 8.82 0 2 0 333.32 13.70 0 2 0 328.49 10.34 0 2 1 61.67 6.18 0 2 1 68.81 5.00 0 -2 -1 61.25 6.16 0 2 -1 63.01 4.64 0 2 -1 52.60 4.77 0 2 -1 59.09 6.31 0 -2 -1 73.94 3.83 0 -2 1 65.81 4.26 0 -2 -2 119.26 3.85 0 2 -2 127.14 6.89 0 -2 2 130.90 6.22 0 -2 -2 126.86 6.13 0 2 2 131.98 8.78 0 2 -2 128.42 7.42 0 -2 -2 129.27 8.99 0 2 -2 118.26 9.13 0 2 -3 2895.28 34.53 0 -2 3 2701.07 29.48 0 -2 -3 2732.51 29.14 0 2 3 2794.72 40.66 0 2 -3 2761.07 44.34 0 -2 -3 2838.46 41.31 0 2 -3 2872.03 35.15 0 -2 4 94.03 6.44 0 2 4 98.79 8.56 0 -2 -4 102.35 6.18 0 -2 -4 93.78 8.17 0 2 -4 97.63 6.98 0 -2 -5 2527.04 40.46 0 2 5 2518.55 42.05 0 2 -5 2560.94 36.31 0 2 -6 84.54 7.25 0 -2 -6 117.97 10.10 0 2 6 93.71 3.81 0 -2 6 103.21 9.52 0 -2 -6 76.81 5.96 0 -2 -7 151.18 9.13 0 -2 7 171.39 9.94 0 2 -7 152.07 10.29 0 -2 -7 184.65 15.12 0 2 7 187.34 5.85 0 -2 -8 0.75 2.92 0 -2 -8 1.88 2.37 0 2 -8 2.15 1.93 0 -2 8 3.77 1.70 0 2 8 -0.33 1.66 0 -2 -9 142.35 11.91 0 -2 9 130.93 9.30 0 2 9 138.70 6.21 0 -2 -9 125.69 9.52 0 2 -9 121.75 11.19 0 2 10 404.92 11.46 0 -2 -10 389.77 17.79 0 -2 -10 415.75 21.13 0 -2 10 401.35 16.35 0 2 -10 396.06 20.76 0 -2 11 57.52 7.89 0 2 11 60.68 5.85 0 -2 -11 37.64 6.21 0 2 -11 41.66 7.70 0 -2 -12 66.13 8.22 0 -2 12 63.21 7.19 0 2 12 72.59 5.56 0 -2 -12 64.39 9.83 0 2 -12 65.40 10.10 0 -2 -13 243.77 16.12 0 -2 13 251.78 14.17 0 2 13 260.92 11.11 0 2 -13 245.11 20.75 0 -2 -13 197.27 15.58 0 -2 14 24.14 4.03 0 2 -14 28.07 8.17 0 -2 -14 29.22 6.51 0 2 14 25.19 3.13 0 2 -15 0.86 4.22 0 -2 -15 -2.04 3.93 0 2 15 6.55 3.71 0 2 16 236.78 13.11 0 -2 16 229.76 16.45 0 2 -16 187.06 21.76 0 -2 -16 182.40 17.03 0 -2 -16 200.20 20.85 0 -2 17 50.78 7.24 0 2 -17 49.61 12.17 0 -2 -17 41.42 8.90 0 2 17 59.62 6.76 0 2 18 13.45 3.78 0 -2 18 11.86 4.41 0 2 -18 9.60 5.83 0 -2 -18 7.05 4.43 0 -2 -18 14.00 4.93 0 -2 19 6.49 3.96 0 -2 -19 -1.57 5.91 0 -2 -19 7.70 5.11 0 2 19 3.32 2.30 0 2 -19 0.38 6.38 0 -2 -20 3.13 5.25 0 -2 20 3.59 3.83 0 2 -20 5.38 4.95 0 -2 -20 4.46 4.32 0 -2 -21 24.59 5.59 0 2 -21 7.61 3.92 0 -2 21 31.28 7.55 0 2 -21 26.85 12.01 0 2 -21 27.99 7.89 0 -2 -21 25.82 8.20 0 2 -22 60.44 7.87 0 -2 -22 38.06 6.70 0 2 22 43.67 5.01 0 2 22 57.98 6.50 0 -2 22 51.46 9.51 0 2 -22 35.09 13.21 0 2 -22 29.44 7.53 0 -2 -22 33.73 10.85 0 -2 -22 58.58 18.53 0 -2 -23 124.32 17.89 0 2 -23 144.91 21.28 0 2 -23 106.86 25.05 0 -2 23 152.66 16.44 0 -2 -23 129.08 12.16 0 2 23 130.41 7.82 0 2 23 139.98 9.43 0 2 -23 113.33 13.23 0 2 24 195.14 10.82 0 2 -24 228.55 27.63 0 2 -24 244.69 14.64 0 2 -24 193.66 17.75 0 -2 24 239.39 21.14 0 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1.76 0 6 36 -1.34 1.15 0 6 -36 -1.52 1.66 0 6 -37 2.27 1.26 0 7 0 -2.27 5.32 0 7 0 3.06 2.85 0 -7 0 0.13 4.04 0 -7 1 19.16 7.76 0 7 1 12.95 4.32 0 7 1 17.94 8.56 0 7 -1 18.24 8.29 0 -7 -1 14.70 6.91 0 7 -1 14.77 4.59 0 7 -2 6.76 3.82 0 -7 -2 5.24 4.77 0 -7 2 4.18 3.72 0 7 2 7.01 6.92 0 7 2 6.94 4.63 0 7 -2 10.73 7.47 0 7 -3 114.47 18.55 0 -7 -3 117.69 16.71 0 -7 3 127.04 18.33 0 7 -3 116.65 12.41 0 7 3 116.68 13.40 0 7 3 117.38 18.32 0 7 4 104.27 12.73 0 -7 4 111.55 16.56 0 7 -4 110.73 12.30 0 -7 -4 108.91 16.62 0 7 4 103.05 17.75 0 7 5 3.88 4.71 0 7 -5 6.28 3.44 0 -7 5 4.61 3.98 0 -7 -5 5.03 3.68 0 -7 5 1.50 2.94 0 7 5 12.93 6.18 0 -7 -6 407.58 32.44 0 7 6 422.51 35.08 0 -7 6 368.97 22.14 0 7 -6 427.03 24.91 0 7 6 388.33 25.86 0 7 7 31.59 7.48 0 7 -7 51.07 6.67 0 7 7 49.39 14.66 0 7 -7 36.67 7.70 0 -7 -7 44.04 13.88 0 -7 7 38.37 7.71 0 7 -8 310.08 22.64 0 7 8 314.06 31.21 0 7 8 285.10 23.46 0 7 -8 342.98 15.35 0 -7 8 283.39 20.00 0 -7 -8 332.59 28.62 0 -7 -9 16.57 8.01 0 7 -9 16.00 3.73 0 7 -9 10.47 4.92 0 -7 -9 15.64 3.89 0 7 9 15.87 9.03 0 -7 9 11.33 5.05 0 7 -10 48.23 9.36 0 7 -10 66.72 7.72 0 7 10 51.30 14.69 0 -7 10 40.78 8.70 0 -7 -10 44.89 6.08 0 -7 -10 50.01 12.60 0 -7 -11 295.99 14.53 0 -7 11 273.60 21.02 0 -7 -11 287.22 28.25 0 7 -11 291.58 15.25 0 7 -11 279.60 24.56 0 7 11 283.38 31.63 0 -7 -12 50.43 12.22 0 7 -12 45.86 10.46 0 -7 12 45.12 9.37 0 -7 -12 48.87 6.12 0 7 -12 46.07 6.13 0 7 12 58.32 15.37 0 7 13 25.95 10.61 0 -7 -13 27.44 5.11 0 -7 -13 25.84 10.72 0 -7 13 18.66 5.54 0 7 -13 29.22 6.15 0 7 -13 25.10 8.40 0 7 -14 104.35 17.97 0 7 14 127.52 21.98 0 -7 -14 107.65 17.58 0 -7 -14 117.38 9.59 0 7 -14 114.91 9.96 0 -7 14 120.44 14.67 0 7 -15 37.25 10.32 0 7 15 20.76 11.44 0 -7 -15 21.46 4.72 0 -7 -15 15.27 9.44 0 -7 15 18.94 7.41 0 -7 -16 34.88 13.84 0 -7 -16 50.07 8.38 0 7 -16 30.19 5.88 0 -7 16 36.95 9.44 0 7 16 40.01 14.23 0 7 16 33.49 6.20 0 -7 17 12.00 4.91 0 7 -17 14.27 3.09 0 -7 -17 12.02 3.31 0 7 17 21.51 10.17 0 -7 -17 7.74 8.12 0 7 17 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29 0.88 2.06 0 7 29 5.42 1.81 0 7 -29 4.33 2.93 0 7 30 7.29 2.04 0 7 -30 7.68 3.26 0 -7 -30 6.51 3.35 0 7 30 11.99 2.75 0 7 -31 3.99 2.91 0 7 31 1.82 1.78 0 7 31 0.17 1.42 0 -7 -31 -1.42 1.72 0 7 32 8.91 1.90 0 7 32 11.61 2.46 0 -7 -32 9.58 3.27 0 7 -32 12.91 3.86 0 7 -33 29.44 4.69 0 -7 -33 26.54 4.48 0 7 33 38.62 4.01 0 7 -34 4.22 1.75 0 7 34 3.83 1.40 0 7 -35 28.87 3.52 0 -8 0 780.50 23.84 0 8 0 751.18 51.59 0 -8 0 757.47 47.85 0 8 1 140.90 23.00 0 -8 -1 131.58 9.94 0 -8 1 157.56 22.58 0 8 -1 136.37 28.50 0 -8 -1 148.39 21.33 0 8 -2 45.48 13.43 0 8 2 47.75 13.75 0 -8 2 50.83 12.48 0 8 -2 48.21 5.96 0 -8 -2 52.56 13.32 0 -8 -2 37.97 5.41 0 -8 3 33.33 9.47 0 8 3 32.67 11.76 0 -8 -3 36.00 5.51 0 8 -3 31.43 5.08 0 -8 -3 34.21 10.56 0 8 -4 200.65 12.49 0 -8 -4 197.45 23.87 0 -8 4 213.67 25.91 0 -8 -4 188.58 12.04 0 8 4 204.10 26.60 0 8 5 42.20 16.63 0 -8 -5 32.35 13.10 0 -8 -5 36.27 7.60 0 8 -5 35.10 6.28 0 -8 5 35.46 13.09 0 -8 6 491.56 38.15 0 -8 -6 439.20 19.13 0 -8 -6 538.96 40.13 0 8 -6 497.75 19.75 0 8 6 446.89 40.74 0 -8 7 6.49 8.67 0 8 -7 3.57 3.70 0 -8 -7 7.42 4.31 0 -8 -7 3.35 1.86 0 8 7 5.39 8.28 0 8 8 19.32 9.60 0 8 -8 13.98 4.11 0 -8 8 16.81 7.39 0 -8 -8 16.15 6.46 0 -8 -8 15.59 3.85 0 8 9 114.14 20.44 0 -8 -9 113.86 9.56 0 -8 9 124.43 20.13 0 8 -9 120.71 10.32 0 -8 -9 124.48 18.81 0 -8 -10 18.96 4.88 0 8 10 18.83 10.20 0 8 -10 16.31 4.74 0 -8 -10 16.81 7.83 0 8 11 100.67 20.99 0 -8 11 78.34 11.70 0 -8 -11 98.85 17.08 0 8 -11 108.63 9.90 0 -8 -11 105.19 10.49 0 -8 -12 25.94 11.50 0 8 -12 32.69 7.11 0 -8 -12 24.80 4.98 0 8 12 26.93 12.19 0 -8 12 18.65 6.62 0 -8 13 172.73 18.83 0 8 -13 235.62 14.58 0 -8 -13 208.36 27.27 0 -8 -13 214.04 13.40 0 8 13 227.36 30.94 0 8 -14 5.04 3.95 0 -8 -14 3.16 3.98 0 -8 -14 0.61 2.08 0 -8 14 -2.71 4.35 0 8 14 5.07 7.33 0 8 15 5.08 8.42 0 -8 -15 6.47 3.33 0 8 -15 0.47 2.73 0 -8 15 -2.89 4.16 0 8 15 -1.04 2.42 0 -8 -15 -4.05 6.27 0 -8 -16 74.71 8.71 0 8 16 66.98 7.54 0 -8 -16 73.28 17.40 0 8 -16 68.89 8.62 0 8 16 73.54 18.81 0 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-29 45.35 6.09 0 8 -29 43.02 6.13 0 8 30 0.59 1.19 0 -8 -30 -1.04 2.03 0 8 -30 2.79 2.14 0 8 -31 4.14 2.55 0 8 31 5.22 1.88 0 8 -32 1.96 1.65 0 8 -33 3.27 1.76 0 -9 0 -4.22 7.23 0 -9 0 1.93 3.16 0 9 0 -5.30 7.74 0 -9 1 14.23 8.85 0 -9 1 15.87 4.48 0 9 1 12.54 8.96 0 -9 -1 23.47 7.20 0 -9 -1 16.33 11.04 0 -9 -2 94.42 17.81 0 -9 2 96.67 18.77 0 9 2 90.03 20.12 0 -9 2 88.75 8.37 0 -9 -2 88.97 8.83 0 -9 3 34.28 12.01 0 -9 -3 34.07 10.43 0 9 3 36.78 13.37 0 -9 -3 34.91 5.25 0 9 4 43.57 15.76 0 9 -4 43.41 6.21 0 -9 -4 38.47 11.13 0 -9 4 44.50 13.31 0 -9 -4 37.18 6.01 0 9 -5 271.86 15.40 0 -9 5 281.03 31.12 0 -9 -5 267.77 15.32 0 9 5 245.75 34.63 0 -9 -5 269.09 29.91 0 9 -6 81.44 9.17 0 -9 6 82.20 19.71 0 -9 -6 78.73 17.65 0 9 6 96.18 24.12 0 -9 -6 87.44 8.79 0 -9 7 11.86 7.03 0 9 -7 15.85 4.48 0 -9 -7 9.55 3.47 0 9 7 12.37 9.18 0 -9 -7 11.52 7.29 0 -9 -8 7.67 4.62 0 -9 8 2.23 5.55 0 9 8 11.67 13.17 0 -9 -8 2.23 5.62 0 9 -8 2.64 3.64 0 9 9 432.48 43.49 0 -9 -9 444.55 19.08 0 -9 -9 420.74 38.05 0 9 -9 446.46 20.33 0 -9 9 446.52 39.24 0 -9 10 4.53 5.72 0 -9 -10 9.43 6.43 0 -9 -10 23.34 7.35 0 9 10 5.65 7.52 0 9 -10 13.78 5.31 0 -9 -11 25.58 5.07 0 9 -11 33.74 6.04 0 9 11 29.96 11.46 0 -9 -11 30.87 10.43 0 -9 11 31.60 10.65 0 9 -12 8.37 3.78 0 -9 -12 8.44 6.44 0 -9 12 9.51 4.61 0 9 12 9.29 7.77 0 -9 -12 10.04 4.10 0 -9 -13 294.23 33.24 0 9 -13 322.17 17.66 0 -9 -13 325.81 16.91 0 -9 13 326.72 33.25 0 9 -14 10.01 3.58 0 -9 -14 11.78 3.64 0 9 14 4.72 2.52 0 9 -15 3.15 2.99 0 -9 -15 3.28 2.93 0 9 15 1.72 2.12 0 9 15 5.01 2.39 0 9 16 180.49 11.80 0 9 -16 204.67 15.31 0 9 16 207.27 13.19 0 -9 -16 179.83 13.46 0 -9 -17 0.77 1.82 0 9 17 -1.65 3.53 0 9 -17 0.91 2.79 0 9 17 -2.89 3.15 0 9 -18 61.92 9.04 0 -9 -18 63.26 8.43 0 9 18 50.95 6.36 0 9 18 52.31 6.71 0 9 -19 27.88 6.00 0 9 19 18.17 3.70 0 9 19 22.20 4.56 0 -9 -19 30.24 5.50 0 9 20 6.94 2.62 0 9 20 14.65 4.35 0 -9 -20 7.92 3.22 0 9 -20 7.10 3.61 0 9 -21 103.81 10.34 0 9 21 100.01 8.28 0 9 21 90.91 7.57 0 -9 -21 96.62 9.66 0 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-8 1.59 1.85 0 10 -9 18.91 6.47 0 -10 -9 21.55 5.76 0 10 -10 73.18 9.25 0 -10 -10 75.49 9.23 0 -10 -11 41.31 6.52 0 10 -11 44.69 6.63 0 10 -12 5.14 3.24 0 10 12 6.50 3.58 0 10 13 25.44 5.06 0 10 13 26.75 5.34 0 -10 -13 24.28 5.19 0 10 -13 34.71 6.32 0 10 -14 125.93 11.18 0 -10 -14 120.48 10.21 0 10 14 119.35 9.85 0 10 14 101.57 9.10 0 10 15 6.53 2.33 0 -10 -15 2.60 2.05 0 10 15 4.07 2.97 0 10 -15 5.34 3.45 0 -10 -16 10.26 3.53 0 10 16 12.09 3.28 0 10 -16 9.52 3.98 0 10 16 11.46 4.00 0 10 -17 7.64 3.39 0 -10 -17 9.36 3.11 0 10 17 18.35 3.83 0 10 17 9.89 3.66 0 10 -18 41.36 6.79 0 10 18 38.32 5.53 0 -10 -18 38.63 5.86 0 10 18 31.49 4.66 0 10 -19 12.66 3.54 0 10 19 11.70 3.08 0 10 19 12.20 3.77 0 -10 -19 11.36 4.08 0 10 -20 17.50 4.28 0 10 20 15.78 3.87 0 10 20 15.05 3.31 0 -10 -20 16.14 3.93 0 10 -21 89.03 8.68 0 10 21 80.48 7.05 0 -10 -21 89.14 8.45 0 10 21 75.09 6.41 0 -10 -22 64.78 6.87 0 10 -22 63.07 7.30 0 10 22 66.59 6.06 0 10 22 49.89 5.10 0 10 -23 29.55 5.37 0 -10 -23 28.27 4.77 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158.94 12.10 6 5 6 161.58 11.20 6 5 7 312.80 15.09 -6 5 -7 285.93 27.98 6 -5 7 260.68 14.48 6 5 7 289.81 15.20 6 5 7 293.69 14.38 6 5 8 18.36 7.38 6 -5 8 16.25 4.85 6 5 8 17.56 7.06 6 5 8 -1.74 3.61 6 -5 8 2.02 2.26 6 5 8 19.67 6.33 -6 5 -8 1.28 3.02 6 5 9 194.37 11.94 6 -5 9 167.55 10.83 -6 5 -9 196.24 23.33 6 -5 9 173.41 12.16 6 5 9 185.63 9.63 6 5 9 181.87 11.91 6 5 9 200.04 11.06 6 -5 9 187.55 10.80 6 5 10 31.94 5.07 6 -5 10 21.62 3.89 6 5 10 23.54 3.94 6 -5 10 25.10 4.98 6 5 10 25.59 4.04 6 5 10 25.94 4.95 -6 5 -10 27.70 9.40 6 5 11 8.58 3.53 6 -5 11 21.44 5.44 6 5 11 4.51 2.36 6 -5 11 6.87 3.58 6 5 11 12.83 4.61 6 5 11 8.70 3.67 -6 5 -11 4.59 5.65 6 5 12 66.11 7.52 6 -5 12 53.29 7.01 -6 5 -12 54.37 13.04 6 -5 12 49.87 5.75 6 5 12 67.73 7.36 6 5 12 59.91 9.60 6 5 12 54.16 7.04 6 5 13 -6.78 3.91 6 -5 13 -4.01 2.93 6 5 13 3.12 7.54 6 5 13 -8.56 4.37 6 -5 13 0.48 2.58 6 5 13 -3.05 3.14 -6 5 -13 -1.24 3.99 6 5 14 32.45 5.28 6 -5 14 23.68 5.30 6 -5 14 32.33 5.98 6 5 14 25.39 4.71 6 5 14 22.51 4.78 6 5 14 24.68 5.25 -6 5 -14 23.68 9.14 6 5 15 2.37 2.88 6 -5 15 -1.74 2.71 6 5 15 -1.79 2.79 6 -5 15 0.27 2.38 6 5 15 -0.56 2.47 6 5 15 -1.55 3.00 -6 5 -15 -0.87 4.54 -6 5 -16 3.51 5.18 6 -5 16 8.54 4.40 6 5 16 4.61 4.22 6 -5 16 1.19 1.95 6 5 16 6.48 3.32 6 5 16 7.55 4.14 6 -5 17 33.41 6.09 -6 5 -17 48.21 13.09 6 -5 17 50.15 7.18 6 5 17 55.99 6.38 6 5 17 53.51 6.78 6 5 17 46.98 6.42 6 5 18 20.60 6.10 6 -5 18 16.79 4.40 6 5 18 19.09 4.75 6 5 18 25.04 5.68 6 -5 19 11.51 3.80 6 5 19 4.51 3.15 6 -5 19 11.41 3.51 6 5 19 10.76 3.61 6 5 19 10.29 3.25 6 -5 20 12.14 5.34 6 -5 20 6.96 3.81 6 5 20 13.75 4.76 6 5 20 9.47 4.04 6 5 21 1.70 2.51 6 -5 21 3.14 2.11 6 5 21 -2.20 2.90 6 5 21 3.19 2.15 6 -5 22 104.99 9.26 6 -5 22 72.05 8.14 6 5 22 89.74 8.09 6 5 22 85.84 8.07 6 5 22 92.88 8.43 6 5 23 -4.50 3.15 6 -5 23 -0.07 2.86 6 -5 23 0.02 1.73 6 5 23 1.11 2.20 6 5 23 -2.34 2.59 6 -5 24 -0.36 2.20 6 5 24 0.32 2.36 6 -5 24 0.18 1.73 6 5 24 2.24 2.65 6 -5 25 -1.28 2.36 6 -5 25 -0.37 1.42 6 5 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2.00 6 -6 -22 52.14 5.42 6 -6 -22 62.27 8.05 6 -6 -21 15.72 3.73 6 -6 -21 19.60 6.32 -6 6 20 -0.82 2.60 6 -6 -20 3.68 1.75 6 -6 -20 3.21 2.50 -6 6 19 135.79 8.40 6 -6 -19 120.37 8.57 6 -6 -19 140.89 12.45 6 -6 -18 29.16 5.36 -6 6 18 28.46 3.99 6 -6 -18 31.86 4.53 6 -6 -18 29.12 5.38 6 -6 -17 -1.76 2.41 -6 -6 17 -1.49 3.22 -6 6 17 7.69 3.22 6 6 -17 1.99 5.34 6 -6 -17 4.31 3.96 -6 -6 16 22.18 6.68 -6 6 16 23.91 3.45 6 -6 -16 27.26 5.47 6 6 -16 26.47 11.12 6 -6 -16 23.39 4.96 -6 -6 15 60.82 10.54 6 6 -15 67.58 17.40 6 -6 -15 64.08 8.07 6 -6 -15 68.45 8.01 -6 -6 14 74.31 11.78 6 6 -14 85.05 19.36 -6 6 14 71.62 19.07 6 -6 -14 91.16 10.26 6 -6 -14 60.38 7.97 -6 -6 13 64.57 11.02 6 6 -13 66.47 16.42 6 -6 -13 71.00 8.73 -6 6 13 63.73 17.24 6 -6 -13 76.90 7.74 -6 -6 12 43.81 8.86 6 6 -12 49.92 14.07 -6 6 12 36.27 12.85 6 -6 -12 45.34 6.84 -6 -6 11 -1.02 5.78 6 6 -11 11.31 7.71 -6 6 11 16.44 9.25 6 -6 -11 7.04 2.43 -6 -6 10 63.39 11.18 6 6 -10 64.24 17.23 -6 6 10 62.47 15.96 6 -6 -10 61.78 8.30 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70.10 15.83 -6 6 0 74.51 15.74 6 -6 0 61.23 7.00 6 6 1 56.49 6.56 6 -6 1 58.19 7.27 -6 -6 -1 67.39 13.16 6 6 1 59.29 6.91 6 6 1 66.03 14.69 -6 6 -1 61.78 14.92 6 -6 1 55.40 6.82 6 -6 2 23.10 4.81 6 -6 2 24.22 5.25 6 6 2 17.15 4.53 -6 6 -2 23.31 9.01 6 6 2 14.83 4.47 6 6 3 22.73 5.13 6 -6 3 23.85 4.79 -6 6 -3 27.53 9.44 6 6 3 26.00 4.93 6 6 4 3.30 3.61 6 -6 4 0.78 2.21 -6 6 -4 -0.98 3.49 6 6 4 0.00 2.68 6 6 5 10.77 4.26 6 -6 5 6.41 3.51 -6 6 -5 4.21 4.42 6 6 5 7.20 4.36 6 6 6 46.77 7.43 6 6 6 36.57 5.55 6 -6 6 41.81 6.55 -6 6 -6 41.69 11.50 6 6 7 4.80 2.74 6 -6 7 10.04 3.27 -6 6 -7 13.44 7.95 6 6 7 7.54 2.53 6 6 8 15.51 4.41 6 6 8 34.42 5.71 6 -6 8 15.68 4.13 -6 6 -8 15.21 6.90 6 6 8 23.38 5.97 6 6 9 452.11 18.15 6 -6 9 463.47 19.42 -6 6 -9 475.80 38.01 6 6 9 442.47 15.75 6 6 9 485.18 20.35 6 6 10 7.09 4.68 6 -6 10 0.23 2.01 6 -6 10 3.82 2.92 6 6 10 8.76 3.93 6 6 10 1.30 2.83 -6 6 -10 -0.80 3.85 6 6 11 49.08 6.08 6 -6 11 43.52 6.38 6 -6 11 33.13 5.22 6 6 11 48.76 4.96 6 6 11 55.76 7.76 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5.72 2.94 6 -6 22 3.19 2.07 6 6 22 5.86 3.90 6 6 22 6.06 4.38 6 6 23 20.97 4.54 6 -6 23 13.64 3.96 6 -6 23 15.62 3.25 6 6 23 15.45 3.35 6 6 23 15.03 3.50 6 -6 24 46.24 6.14 6 -6 24 40.85 4.78 6 6 24 49.21 6.04 6 6 24 44.68 5.51 6 6 24 50.34 5.71 6 -6 25 12.05 3.24 6 6 25 12.19 3.28 6 6 25 12.58 2.96 6 -6 26 1.95 2.32 6 6 26 1.41 2.06 6 6 26 -0.35 1.55 6 -6 27 10.70 3.12 6 6 27 16.99 3.46 6 6 27 11.93 2.97 6 -6 28 2.27 2.28 6 6 28 1.98 1.97 6 6 28 -0.88 1.43 6 -6 29 2.03 1.85 6 6 29 6.94 2.45 6 6 29 4.19 1.78 6 -6 30 13.95 2.84 6 6 30 21.62 2.74 6 -6 31 4.05 1.54 6 6 31 3.04 1.30 6 -6 32 5.61 1.49 6 -7 -31 0.51 1.17 -6 7 30 5.01 1.34 6 -7 -30 5.15 2.02 -6 7 29 64.49 4.42 6 -7 -29 57.93 6.41 -6 7 28 33.33 3.31 6 -7 -28 22.42 4.71 -6 7 27 1.50 1.47 6 -7 -27 2.32 1.82 -6 7 26 2.25 1.34 6 -7 -26 6.23 2.92 -6 7 25 7.77 2.36 6 -7 -25 2.95 2.45 -6 7 24 75.60 5.81 6 -7 -24 69.29 8.08 -6 7 23 16.89 2.84 6 -7 -23 18.34 2.89 6 -7 -23 17.55 4.44 -6 7 22 50.30 5.01 6 -7 -22 42.17 4.48 6 -7 -22 44.67 6.94 -6 7 21 20.29 3.52 6 -7 -21 11.36 2.52 6 -7 -21 12.65 4.45 -6 7 20 22.46 3.39 6 -7 -20 15.00 2.82 6 -7 -20 14.14 4.50 -6 7 19 18.88 2.96 6 -7 -19 22.69 3.41 6 -7 -19 24.20 5.29 -6 7 18 154.81 8.82 6 -7 -18 135.51 8.71 6 -7 -18 137.99 10.63 6 -7 -18 157.64 12.75 6 -7 -17 31.49 5.12 -6 7 17 24.88 3.23 6 -7 -17 29.03 4.12 6 -7 -17 29.38 5.26 -6 7 16 49.08 5.29 6 -7 -16 43.18 7.04 6 -7 -16 49.79 7.96 -6 7 15 98.50 6.53 6 -7 -15 95.60 9.83 6 -7 -15 106.64 9.81 6 -7 -14 -0.11 3.49 6 -7 -14 1.53 2.07 6 7 -13 132.11 24.19 6 -7 -13 147.44 11.84 6 7 -12 34.89 11.42 6 -7 -12 39.52 6.81 -6 7 12 43.80 14.76 6 7 -11 39.45 12.59 6 -7 -11 41.66 6.08 -6 7 11 43.13 14.07 6 7 -10 3.22 5.04 -6 7 10 1.66 5.23 6 7 -9 137.52 23.92 -6 7 9 147.14 25.34 6 -7 -9 169.88 12.05 -6 -7 8 3.06 5.50 6 7 -8 4.94 6.06 -6 7 8 6.41 7.30 6 -7 -8 2.93 2.76 -6 -7 7 15.03 7.95 6 7 -7 15.09 8.98 -6 7 7 15.42 10.20 6 -7 -7 18.48 4.40 -6 -7 6 75.50 15.68 6 7 -6 87.40 17.72 -6 7 6 85.67 18.23 6 -7 -6 77.24 8.12 -6 7 5 35.81 13.25 6 -7 -5 29.38 5.97 -6 -7 5 27.11 9.97 6 7 -5 33.91 11.29 6 -7 -5 26.80 6.12 6 -7 -4 34.96 5.49 -6 7 4 41.12 13.89 -6 -7 4 37.42 12.46 6 7 -4 43.65 8.77 6 7 -4 39.67 12.50 6 -7 -4 39.25 6.55 6 -7 -3 40.16 5.96 -6 7 3 41.79 13.85 -6 -7 3 29.22 10.06 6 7 -3 38.81 6.39 6 7 -3 33.58 11.20 6 -7 -3 33.83 6.17 6 -7 -2 14.63 4.62 6 -7 -2 19.76 5.02 -6 7 2 26.32 11.75 -6 -7 2 15.61 7.91 6 7 -2 15.63 4.63 6 7 -2 15.03 7.21 6 -7 -1 7.64 3.97 -6 -7 1 3.77 3.87 -6 7 1 7.64 7.57 6 -7 -1 5.93 3.16 6 7 -1 -4.04 4.01 6 7 -1 3.26 4.27 6 -7 0 8.68 3.63 -6 -7 0 5.58 4.78 -6 7 0 2.53 3.27 6 -7 0 8.61 3.22 6 7 0 6.20 5.20 6 -7 1 15.78 4.78 6 -7 1 11.12 3.88 -6 7 -1 16.73 8.61 6 7 1 6.90 3.88 -6 7 -2 55.67 14.15 6 -7 2 48.25 6.42 6 7 2 56.84 8.06 6 -7 2 67.83 7.95 -6 7 -3 40.12 13.93 6 -7 3 43.45 7.29 6 7 3 54.00 8.98 6 -7 3 47.46 8.93 6 -7 4 414.82 18.87 6 7 4 348.61 15.96 -6 7 -4 394.87 36.11 6 -7 4 376.39 17.61 6 7 4 381.28 19.19 6 7 5 128.31 9.65 -6 7 -5 149.82 24.17 6 -7 5 137.64 11.11 6 7 5 157.12 11.91 6 7 6 46.98 5.98 6 -7 6 55.59 7.21 -6 7 -6 49.62 13.48 6 7 6 50.41 7.01 6 7 7 25.82 5.69 6 -7 7 24.36 5.33 6 7 7 28.54 5.97 6 7 7 34.06 7.55 -6 7 -7 29.65 10.19 6 -7 8 377.87 17.03 -6 7 -8 423.37 36.69 6 7 8 403.05 16.20 6 7 8 441.06 20.41 6 -7 9 283.98 14.80 -6 7 -9 314.18 33.10 6 7 9 287.40 13.43 6 7 9 350.60 17.93 6 -7 10 192.33 12.35 -6 7 -10 208.02 26.51 6 7 10 189.94 11.08 6 7 10 205.16 13.81 6 -7 11 54.67 6.74 6 7 11 66.28 7.28 6 7 11 61.41 7.96 6 -7 11 57.38 6.58 6 -7 12 6.87 2.75 6 -7 12 3.74 2.81 6 7 12 -0.81 2.57 6 7 12 4.42 5.74 6 -7 13 113.71 8.97 6 -7 13 85.04 8.02 6 7 13 87.76 7.43 6 7 13 94.96 8.88 6 -7 14 87.58 8.00 6 -7 14 101.08 8.89 6 7 14 114.41 9.52 6 7 14 97.55 9.44 6 -7 15 61.19 6.76 6 -7 15 61.70 6.71 6 7 15 51.44 5.64 6 7 15 64.19 7.70 6 -7 16 5.75 2.48 6 -7 16 7.86 2.78 6 7 16 11.38 5.00 6 7 16 7.82 2.90 6 -7 17 23.97 4.40 6 7 17 17.00 3.23 6 7 17 19.74 3.84 6 -7 18 1.51 2.55 6 7 18 0.61 2.23 6 7 18 -1.12 1.87 6 7 18 0.16 2.51 6 -7 19 5.41 2.78 6 7 19 5.94 3.82 6 7 19 7.40 3.01 6 7 19 6.03 3.56 6 -7 20 1.01 2.49 6 7 20 3.12 2.25 6 7 20 3.25 2.67 6 7 20 -0.89 2.61 6 -7 21 5.48 2.67 6 7 21 3.49 2.41 6 7 21 5.48 2.35 6 7 21 3.41 2.50 6 -7 22 31.51 4.82 6 7 22 38.64 5.28 6 7 22 30.12 3.97 6 7 22 30.73 4.62 6 -7 23 0.38 1.82 6 7 23 5.19 2.77 6 7 23 6.26 2.37 6 7 23 5.62 2.95 6 -7 24 4.49 2.58 6 7 24 2.97 2.06 6 7 24 2.70 2.02 6 7 24 2.50 2.23 6 -7 25 3.40 2.12 6 7 25 6.03 2.45 6 7 25 7.86 2.37 6 -7 26 8.07 2.56 6 7 26 7.61 2.47 6 7 26 7.53 2.42 6 -7 27 1.59 1.38 6 7 27 1.51 1.63 6 -7 28 3.27 2.06 6 7 28 5.58 2.00 6 -7 29 -0.06 1.25 6 7 29 -0.04 1.26 6 -7 30 3.24 1.33 6 -8 -29 2.39 1.82 6 -8 -28 3.62 2.00 6 -8 -27 6.86 2.86 6 -8 -26 8.61 2.87 6 -8 -25 3.85 2.69 6 -8 -24 21.43 4.43 6 -8 -23 3.07 2.53 6 -8 -22 1.87 2.40 6 -8 -21 -0.40 2.26 6 -8 -20 43.81 6.95 6 -8 -19 124.04 7.15 6 -8 -19 138.15 11.16 6 -8 -18 39.94 4.40 6 -8 -18 39.42 5.61 6 -8 -18 46.95 6.67 6 -8 -17 5.18 3.04 6 -8 -17 3.99 2.83 6 -8 -17 3.68 3.90 6 -8 -16 143.06 8.33 6 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3.23 6 8 4 16.55 5.32 6 -8 5 36.25 5.49 6 8 5 48.82 8.40 6 -8 5 31.09 6.54 6 -8 6 137.65 9.76 6 8 6 159.65 12.83 6 -8 6 166.53 12.14 6 -8 7 15.43 6.04 6 -8 7 12.93 3.50 6 8 7 7.39 2.40 6 8 7 11.31 3.30 6 -8 8 12.72 3.15 6 8 8 11.96 3.55 6 8 8 8.79 3.17 6 8 9 41.66 7.55 6 8 9 25.17 9.13 6 8 10 -7.27 3.61 6 8 10 16.43 5.68 6 8 11 56.01 5.95 6 8 11 62.62 7.30 6 -8 11 50.31 6.20 6 8 12 74.15 7.58 6 8 12 74.87 9.65 6 8 13 -0.74 2.63 6 8 13 -2.05 3.03 6 8 14 28.74 4.85 6 8 14 22.15 4.99 6 -8 15 3.78 1.73 6 8 15 11.86 3.40 6 8 15 8.96 3.06 6 -8 16 12.13 3.20 6 8 16 7.68 2.71 6 8 16 10.11 3.92 6 -8 17 20.22 3.86 6 8 17 25.04 4.26 6 8 17 24.37 5.05 6 -8 18 6.76 2.63 6 8 18 9.90 2.69 6 8 18 12.28 3.74 6 -8 19 9.45 3.25 6 8 19 8.37 2.86 6 8 19 8.97 3.04 6 -8 20 0.82 2.19 6 8 20 2.54 2.37 6 8 20 0.00 2.38 6 -8 21 8.71 2.58 6 8 21 13.54 3.18 6 8 21 12.75 3.38 6 8 22 7.48 2.90 6 -8 22 5.42 2.47 6 8 22 7.42 2.63 6 -8 23 16.17 2.97 6 8 23 19.85 3.31 6 8 23 21.97 3.53 6 -8 24 1.08 1.37 6 8 24 4.55 1.80 6 8 24 3.40 1.76 6 -8 25 5.88 2.22 6 8 25 3.97 1.85 6 -8 26 9.46 1.97 6 8 26 16.82 2.50 6 -8 27 0.55 1.04 6 8 27 1.37 1.07 6 -9 -26 1.77 1.55 6 -9 -25 8.26 2.74 6 -9 -24 -0.18 1.47 6 -9 -23 12.56 3.00 6 -9 -22 15.13 4.39 6 -9 -21 1.10 1.56 6 -9 -20 -0.52 1.90 6 -9 -19 1.13 1.82 6 -9 -18 1.39 2.92 6 -9 -18 1.44 2.27 6 -9 -17 52.67 6.30 6 -9 -17 68.98 7.56 6 -9 -16 6.24 3.20 6 -9 -16 6.58 3.49 6 -9 -15 25.67 4.73 6 -9 -15 28.53 5.39 6 -9 -14 46.01 6.63 6 -9 -14 63.40 7.10 6 -9 -13 14.15 3.63 6 -9 -13 22.65 5.20 6 -9 -12 5.88 3.57 6 -9 -11 48.54 7.94 6 -9 -10 1.17 3.30 6 -9 -9 5.87 3.37 6 -9 -8 15.42 3.96 6 -9 -7 1.34 2.93 6 -9 -6 98.05 10.01 6 -9 -5 71.77 9.24 6 -9 -4 22.54 5.65 6 9 -4 15.93 5.30 6 -9 -3 16.22 4.59 6 9 -3 17.88 4.73 6 9 -2 43.27 6.79 6 -9 -2 46.05 6.47 6 9 -1 19.89 4.72 6 -9 -1 34.05 6.20 6 -9 0 9.08 5.07 6 9 0 -0.69 3.50 6 -9 1 14.94 5.70 6 9 1 10.23 4.21 6 9 2 44.50 7.55 6 -9 2 66.45 8.14 6 9 3 25.10 6.75 6 -9 3 48.71 8.87 6 9 4 96.26 10.68 6 -9 4 94.80 10.56 6 9 5 14.98 5.69 6 -9 5 34.48 7.29 6 9 6 75.90 8.39 6 -9 6 76.63 8.23 6 -9 7 10.35 5.13 6 9 7 6.67 3.84 6 -9 8 11.45 4.55 6 9 8 14.88 3.42 6 9 8 15.32 4.76 6 -9 9 11.47 4.59 6 9 9 6.46 2.07 6 9 9 17.91 5.32 6 9 10 50.69 6.30 6 9 10 52.12 6.92 6 -9 10 39.51 5.56 6 -9 10 34.83 6.17 6 -9 11 0.01 2.27 6 -9 11 0.49 2.19 6 9 11 3.43 2.30 6 9 11 -2.31 3.66 6 9 12 15.36 3.31 6 9 12 14.13 4.18 6 9 13 44.13 5.00 6 9 13 47.95 6.62 6 9 14 21.22 3.55 6 9 14 25.15 4.96 6 9 15 33.91 4.55 6 9 15 39.02 5.93 6 9 16 5.98 2.23 6 9 16 7.59 3.06 6 9 17 6.75 2.40 6 9 17 7.23 3.05 6 9 18 34.01 4.08 6 9 18 35.19 5.07 6 9 19 18.68 3.31 6 9 19 10.74 3.33 6 9 20 8.55 2.48 6 9 20 4.94 2.40 6 9 21 36.29 3.89 6 9 21 30.60 3.91 6 9 22 7.50 2.12 6 9 22 5.34 2.18 6 -9 23 14.09 2.46 6 9 23 13.87 2.45 6 9 23 14.66 2.53 6 -9 24 10.06 2.08 6 9 24 7.20 1.63 6 9 25 4.99 1.41 6 -10 -23 5.47 1.92 6 -10 -22 1.07 1.48 6 -10 -21 0.46 1.54 6 -10 -20 43.98 5.17 6 -10 -19 1.05 1.58 6 -10 -18 2.07 1.99 6 -10 -17 9.67 2.88 6 -10 -17 5.63 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2.59 8.50 7 0 -14 -0.17 4.52 7 0 -14 4.83 2.55 7 0 -14 3.15 5.36 7 0 -14 2.55 2.96 7 0 -13 89.59 15.50 7 0 -13 83.78 14.92 7 0 -13 88.98 6.60 7 0 -13 87.26 8.09 7 0 -12 0.64 10.31 7 0 -12 1.15 1.82 7 0 -12 -2.57 5.01 7 0 -12 -3.14 3.54 7 0 -11 762.61 42.08 7 0 -11 775.28 43.27 7 0 -11 761.34 19.93 7 0 -11 868.59 25.40 7 0 -10 -0.25 3.91 7 0 -10 0.89 4.16 7 0 -10 -3.72 3.44 7 0 -9 129.84 17.10 7 0 -9 126.36 16.77 7 0 -8 5.82 8.16 -7 0 8 -2.22 4.13 7 0 -8 -1.72 3.58 7 0 -7 263.14 23.32 7 0 -7 255.21 22.92 -7 0 7 230.47 19.90 7 0 -6 1.26 5.14 7 0 -6 -0.35 3.52 -7 0 6 -1.41 2.37 7 0 -5 35.59 9.02 -7 0 5 30.47 7.24 -7 0 4 2.27 2.24 7 0 -4 -0.51 3.15 -7 0 3 18.56 4.93 7 0 -3 22.36 6.93 -7 0 2 0.72 2.39 7 0 -2 1.28 3.24 -7 0 1 9.05 3.52 7 0 -1 12.11 4.88 -7 0 0 -1.56 3.15 7 0 0 1.83 2.66 -7 0 -1 47.19 7.88 7 0 1 44.47 8.36 -7 0 -2 3.58 4.38 7 0 2 2.33 3.69 -7 0 -3 460.80 26.12 -7 0 -4 1.24 3.04 -7 0 -5 115.00 13.43 -7 0 -6 1.48 3.15 7 0 7 32.25 6.33 7 0 7 36.72 5.41 -7 0 -7 23.99 6.39 7 0 8 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5.57 -7 7 15 25.20 3.73 7 -7 -15 16.46 4.71 7 -7 -14 41.79 7.02 -7 7 14 40.74 4.24 7 -7 -14 42.73 6.82 7 -7 -13 127.83 11.31 7 -7 -13 132.90 10.82 7 -7 -12 9.73 4.52 7 -7 -12 4.24 4.25 7 -7 -11 185.39 14.40 7 -7 -11 195.60 12.76 7 -7 -10 11.88 3.93 7 -7 -10 13.16 4.18 7 -7 -9 74.87 10.42 7 -7 -9 64.85 8.53 7 7 -8 239.08 31.20 7 -7 -8 248.22 17.42 7 -7 -8 265.72 14.76 7 7 -7 1.80 5.61 7 -7 -7 15.43 6.95 -7 7 6 32.17 13.05 7 7 -6 21.81 10.33 7 -7 -6 15.26 4.82 7 -7 -5 33.36 5.46 -7 7 5 39.93 14.53 7 7 -5 33.67 14.75 7 -7 -5 35.62 6.06 7 -7 -4 172.97 10.98 7 7 -4 181.05 12.59 7 7 -4 155.80 23.27 7 -7 -4 184.20 11.98 -7 7 4 186.05 27.09 7 -7 -3 73.93 7.71 7 7 -3 50.75 15.44 7 7 -3 48.43 6.69 7 -7 -3 60.22 8.42 -7 7 3 74.57 18.65 7 -7 -2 3.89 3.49 -7 7 2 19.14 11.38 7 -7 -2 12.34 3.63 7 7 -2 6.07 4.26 7 7 -2 11.84 8.82 7 -7 -1 54.30 6.53 7 7 -1 56.32 7.77 7 -7 -1 53.94 6.89 -7 7 1 58.47 15.11 7 -7 0 4.69 3.72 7 -7 0 6.11 3.52 -7 7 0 0.03 3.69 7 7 0 1.46 2.92 7 -7 1 0.13 2.17 7 -7 1 1.90 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2.70 7 7 14 8.68 3.57 7 -7 15 55.66 6.34 7 -7 15 76.57 7.08 7 7 15 72.66 6.66 7 7 15 74.63 8.17 7 -7 16 28.05 5.09 7 -7 16 28.16 4.58 7 7 16 30.28 4.60 7 7 16 25.00 5.92 7 -7 17 2.90 1.92 7 -7 17 0.08 1.61 7 7 17 -3.55 2.75 7 7 17 -2.70 2.52 7 -7 18 21.46 3.68 7 -7 18 11.69 3.22 7 7 18 17.55 3.66 7 7 18 10.65 2.64 7 7 18 16.33 3.52 7 -7 19 61.12 6.47 7 -7 19 53.37 5.58 7 7 19 56.05 5.66 7 7 19 64.56 7.00 7 7 19 49.43 5.49 7 -7 20 10.91 2.94 7 7 20 22.36 3.72 7 7 20 20.51 3.68 7 7 20 19.43 3.97 7 -7 21 11.09 2.79 7 7 21 15.66 3.27 7 7 21 14.04 2.70 7 7 21 15.12 3.39 7 -7 22 6.51 2.28 7 7 22 5.81 1.84 7 7 22 7.06 2.00 7 7 22 10.01 2.74 7 -7 23 0.45 1.53 7 7 23 -0.03 1.51 7 7 23 1.35 1.84 7 -7 24 55.14 5.63 7 7 24 61.86 5.82 7 -7 25 1.55 1.42 7 7 25 1.78 1.50 7 -7 26 2.12 1.35 7 7 26 1.75 1.31 7 -7 27 5.11 1.59 7 -8 -27 2.54 1.33 7 -8 -26 7.94 2.80 7 -8 -25 21.33 3.46 7 -8 -24 48.94 5.83 7 -8 -23 1.43 1.80 7 -8 -22 2.54 1.74 7 -8 -21 -0.41 1.05 7 -8 -21 -1.73 2.25 7 -8 -20 16.56 2.60 7 -8 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4 30.77 7.44 7 -8 5 -0.23 2.48 7 -8 5 -2.75 3.59 7 -8 5 -0.99 1.94 7 8 5 -5.22 5.14 7 -8 6 22.29 5.04 7 -8 6 19.25 4.14 7 -8 6 23.70 4.46 7 8 6 22.99 6.49 7 -8 7 3.31 4.06 7 -8 7 2.42 2.75 7 -8 7 -1.78 1.62 7 8 7 6.05 7.02 7 -8 8 60.39 6.32 7 8 8 66.92 8.70 7 -8 8 57.62 6.86 7 -8 8 56.39 7.02 7 -8 9 59.08 6.07 7 8 9 72.58 8.69 7 -8 9 58.45 6.72 7 -8 9 78.22 8.18 7 -8 10 54.39 5.58 7 8 10 61.61 8.33 7 -8 10 44.11 5.50 7 -8 10 64.15 7.54 7 -8 11 3.86 3.05 7 -8 11 1.78 1.79 7 8 11 -5.04 2.94 7 8 11 -0.27 2.77 7 -8 12 97.51 7.21 7 8 12 93.76 7.41 7 8 12 107.33 9.77 7 -8 12 78.28 7.90 7 -8 13 19.59 4.29 7 8 13 24.62 3.96 7 8 13 23.06 4.31 7 8 14 67.10 6.11 7 8 14 68.89 7.47 7 8 15 62.07 5.71 7 8 15 64.01 7.23 7 8 16 14.25 3.44 7 8 16 11.61 3.22 7 8 17 30.23 4.08 7 8 17 34.08 5.33 7 -8 18 -1.81 2.00 7 8 18 0.83 1.51 7 8 18 -0.39 2.02 7 -8 19 14.83 2.83 7 8 19 24.28 3.27 7 8 19 25.41 4.16 7 -8 20 -1.91 1.57 7 8 20 0.03 1.36 7 8 20 -1.60 2.08 7 -8 21 10.31 2.30 7 -8 21 3.99 1.62 7 -8 22 4.47 1.56 7 -8 22 3.03 1.57 7 8 22 1.58 1.35 7 8 22 2.26 1.64 7 -8 23 3.57 1.21 7 8 23 7.42 2.11 7 -8 24 17.73 2.31 7 8 24 24.80 2.78 7 8 25 0.12 0.94 7 -9 -24 2.11 1.46 7 -9 -23 2.05 1.82 7 -9 -22 19.83 3.51 7 -9 -21 3.62 2.35 7 -9 -20 11.61 3.05 7 -9 -19 10.37 2.86 7 -9 -18 1.22 1.44 7 -9 -18 1.03 1.53 7 -9 -17 5.31 1.59 7 -9 -17 10.18 3.22 7 -9 -17 4.61 2.25 7 -9 -16 19.94 2.74 7 -9 -16 15.60 4.30 7 -9 -16 20.41 4.00 7 -9 -15 36.57 3.99 7 -9 -15 33.12 5.11 7 -9 -15 44.89 5.76 7 -9 -14 7.65 2.75 7 -9 -14 11.98 2.84 7 -9 -14 10.41 3.71 7 -9 -13 6.71 3.61 7 -9 -13 5.88 2.90 7 -9 -12 1.63 2.43 7 -9 -12 1.09 2.59 7 -9 -11 2.46 2.95 7 -9 -11 3.43 2.49 7 -9 -10 58.70 7.44 7 -9 -10 33.84 6.66 7 -9 -9 8.25 4.02 7 -9 -9 11.01 4.47 7 -9 -8 61.58 8.04 7 -9 -8 70.31 7.45 7 -9 -7 21.51 6.01 7 -9 -7 29.11 5.99 7 -9 -6 117.44 11.35 7 -9 -6 130.20 10.01 7 -9 -5 22.12 6.48 7 -9 -5 17.79 5.34 7 -9 -4 25.31 6.60 7 9 -3 119.01 9.76 7 -9 -3 106.39 10.09 7 9 -2 8.83 3.47 7 -9 -2 22.61 6.22 7 9 -1 39.85 6.67 7 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7 9 21 14.30 2.56 7 -10 -20 18.84 3.11 7 -10 -19 10.86 2.91 7 -10 -18 7.47 2.67 7 -10 -17 -0.92 1.67 7 -10 -17 1.46 1.45 7 -10 -16 9.48 2.62 7 -10 -16 9.37 2.33 7 -10 -15 6.76 2.43 7 -10 -15 5.01 1.96 7 -10 -14 48.00 5.43 7 -10 -14 21.33 3.74 7 -10 -13 9.22 2.86 7 -10 -13 9.43 2.59 7 -10 -12 0.25 2.08 7 -10 -12 0.39 0.96 7 -10 -12 0.71 1.81 7 -10 -11 1.45 2.17 7 -10 -11 6.15 3.38 7 -10 -10 142.94 9.96 7 -10 -10 178.28 10.66 7 -10 -9 14.27 5.65 7 -10 -9 23.53 5.33 7 -10 -8 7.79 3.19 7 -10 -8 11.56 3.54 7 -10 -7 23.28 4.65 7 -10 -7 30.36 4.73 7 -10 -6 11.29 3.71 7 -10 -6 13.77 3.82 7 -10 -5 3.49 2.89 7 -10 -5 8.72 3.96 7 -10 -4 55.85 6.62 7 -10 -4 45.66 6.40 7 -10 -3 18.66 4.58 7 -10 -3 25.71 5.20 7 10 -2 44.44 5.85 7 -10 -2 58.14 6.86 7 -10 -2 55.28 6.03 7 -10 -1 10.82 3.57 7 -10 -1 11.32 3.58 7 -10 0 -0.45 2.30 7 10 0 1.48 2.75 7 -10 0 2.36 2.18 7 -10 1 13.45 3.49 7 -10 1 13.97 3.49 7 10 1 14.01 4.26 7 -10 2 5.09 3.08 7 -10 2 4.96 3.40 7 10 2 -0.65 3.36 7 -10 3 2.26 2.40 7 -10 3 2.74 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16.56 7.80 8 4 -11 16.47 4.72 -8 4 11 15.02 7.15 8 -4 -11 13.97 4.25 -8 -4 10 16.60 7.46 8 -4 -10 10.50 3.21 8 4 -10 14.47 8.49 8 4 -10 19.58 5.82 -8 4 10 11.47 7.42 8 -4 -10 13.83 4.82 -8 -4 9 409.64 33.45 8 -4 -9 369.59 16.94 8 4 -9 424.34 37.73 8 4 -9 429.31 19.74 8 -4 -9 468.28 23.43 -8 4 9 424.02 40.31 -8 -4 8 -1.90 7.44 8 -4 -8 4.09 2.71 8 4 -8 4.36 7.47 8 4 -8 4.25 3.32 -8 4 8 5.18 7.93 8 -4 -8 3.94 3.72 -8 -4 7 129.03 18.22 8 4 -7 106.56 9.17 8 -4 -7 112.27 9.22 8 4 -7 134.09 21.36 8 4 -7 111.58 9.36 8 -4 -7 120.65 12.02 -8 4 7 135.45 22.30 -8 -4 6 80.12 15.61 8 4 -6 59.10 10.30 8 -4 -6 57.88 7.34 8 4 -6 72.59 8.17 8 4 -6 62.54 14.80 8 4 -6 64.46 8.40 8 -4 -6 64.37 9.46 -8 4 6 54.57 15.66 -8 -4 5 82.88 16.04 8 4 -5 73.59 8.56 8 -4 -5 66.27 7.48 8 4 -5 74.38 8.35 8 4 -5 63.28 13.61 8 4 -5 79.68 9.34 8 -4 -5 66.27 9.43 -8 4 5 74.03 16.22 8 -4 -4 -1.53 3.84 -8 4 4 6.60 8.33 -8 -4 4 -7.41 7.44 8 4 -4 4.75 4.27 8 -4 -4 2.25 3.56 8 4 -4 11.25 5.95 8 4 -4 3.14 5.22 8 4 -4 4.63 4.24 8 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10.70 -8 4 -5 138.81 20.44 8 -4 5 126.07 11.32 8 4 5 139.19 10.44 8 4 5 127.41 9.51 8 -4 5 141.24 10.50 8 4 6 -1.71 3.06 8 -4 6 -0.34 2.69 8 -4 6 1.91 3.52 8 4 6 -4.69 3.58 -8 4 -6 -0.50 4.61 8 4 6 1.85 3.06 8 -4 6 1.60 2.50 8 4 7 8.24 4.36 8 -4 7 10.65 3.95 8 -4 7 3.37 3.17 8 4 7 11.98 5.36 -8 4 -7 5.42 6.47 8 4 7 10.16 3.60 8 -4 7 6.44 2.96 8 4 8 0.72 2.64 8 -4 8 0.07 2.94 8 -4 8 2.19 2.89 8 4 8 1.34 3.25 -8 4 -8 1.79 5.14 8 4 8 -0.21 2.76 8 -4 8 2.45 2.03 8 4 9 17.57 3.93 8 -4 9 13.42 3.83 8 -4 9 17.86 5.36 8 4 9 19.28 4.27 8 4 9 16.64 4.09 -8 4 -9 21.54 9.45 8 4 9 12.75 2.14 8 -4 9 19.75 4.10 8 4 10 17.11 5.16 8 -4 10 19.25 5.21 8 -4 10 9.34 4.19 8 4 10 14.83 3.69 8 4 10 16.49 4.47 -8 4 -10 16.14 7.85 8 4 11 -2.04 2.87 8 -4 11 1.71 2.56 8 -4 11 1.09 2.23 8 4 11 6.89 5.75 8 4 11 1.29 4.18 -8 4 -11 -2.00 4.84 8 4 12 44.62 6.75 8 -4 12 35.31 6.67 8 -4 12 40.23 6.13 8 4 12 49.08 6.88 8 4 12 40.70 6.31 -8 4 -12 44.62 12.13 8 4 13 82.45 8.77 8 -4 13 70.37 8.67 8 -4 13 104.22 10.20 8 4 13 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8 6 -7 35.34 15.16 8 -6 -7 18.09 4.16 8 -6 -6 394.14 17.02 8 6 -6 370.44 37.10 8 -6 -6 347.97 20.94 8 -6 -6 389.16 16.91 8 -6 -5 20.35 8.13 8 -6 -5 44.94 8.32 8 6 -5 39.31 7.84 8 6 -5 32.47 15.32 8 -6 -5 34.40 7.22 -8 6 5 51.71 21.08 8 -6 -4 38.05 7.30 8 -6 -4 41.51 6.24 8 6 -4 40.50 7.19 8 6 -4 44.16 13.02 8 -6 -4 39.22 5.83 -8 6 4 54.72 16.86 8 -6 -3 90.92 8.97 8 6 -3 86.71 8.72 8 6 -3 95.42 18.33 8 -6 -3 94.11 10.55 8 -6 -3 88.81 8.03 -8 6 3 113.19 21.03 8 -6 -2 12.88 4.07 8 -6 -2 6.09 4.33 8 -6 -2 20.57 5.59 8 6 -2 4.62 3.82 8 6 -2 12.55 12.34 8 6 -1 117.74 9.89 8 -6 -1 138.45 10.67 8 6 -1 130.99 11.02 8 6 -1 137.41 22.20 8 -6 -1 153.09 12.57 8 -6 -1 131.30 9.63 -8 6 1 146.08 23.04 8 -6 0 13.77 3.82 8 -6 0 10.77 4.62 8 6 0 7.50 3.94 8 -6 0 25.14 5.41 -8 6 0 29.08 11.04 8 6 0 3.44 3.33 8 -6 1 11.68 4.16 8 -6 1 7.40 3.93 8 6 1 14.58 6.45 8 -6 1 13.31 4.33 -8 6 -1 24.30 11.67 8 6 1 11.82 5.20 8 6 2 128.88 11.23 -8 6 -2 150.64 23.50 8 -6 2 128.21 10.66 8 6 2 130.24 11.39 8 -6 2 149.05 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7 21 4.02 1.99 8 -7 -21 3.46 1.93 8 -7 -21 -1.62 1.78 -8 7 20 4.83 2.04 8 -7 -20 3.39 1.66 8 -7 -20 3.65 2.20 -8 7 19 -1.84 1.68 8 -7 -19 -0.97 1.62 8 -7 -19 0.40 1.69 -8 7 18 1.18 1.91 8 -7 -18 3.07 2.33 8 -7 -18 1.17 2.44 8 -7 -18 4.70 2.78 -8 7 17 17.24 2.95 8 -7 -17 19.50 3.55 8 -7 -17 15.13 3.61 8 -7 -17 18.69 3.89 -8 7 16 13.20 2.94 8 -7 -16 14.75 3.07 8 -7 -16 11.98 3.53 8 -7 -16 13.68 3.98 -8 7 15 -3.99 2.91 8 -7 -15 1.70 1.82 8 -7 -15 -0.94 2.89 -8 7 14 221.47 9.67 8 -7 -14 234.11 14.59 8 -7 -14 235.22 13.28 -8 7 13 121.47 6.69 8 -7 -13 121.64 10.93 8 -7 -13 113.75 9.53 8 -7 -12 33.38 6.77 8 -7 -12 38.41 5.97 8 -7 -11 95.39 10.38 8 -7 -11 102.87 8.95 8 -7 -10 102.88 10.83 8 -7 -10 92.35 8.73 8 -7 -9 145.73 12.96 8 -7 -9 141.10 10.57 8 -7 -8 2.41 4.81 8 -7 -8 8.11 4.70 8 -7 -7 -12.04 5.71 8 -7 -7 -0.71 2.27 8 -7 -6 19.55 4.66 8 -7 -6 19.05 3.65 8 -7 -5 4.32 4.02 8 -7 -5 2.82 2.30 8 -7 -4 33.01 5.57 8 7 -4 40.26 8.18 8 -7 -4 43.80 9.73 8 -7 -4 32.05 5.37 8 -7 -3 6.56 3.21 8 7 -3 9.83 5.08 8 -7 -3 7.43 3.39 8 -7 -2 8.04 5.10 8 -7 -2 7.99 4.27 8 7 -2 -0.98 3.99 8 -7 -2 10.19 4.42 8 -7 -1 24.78 6.60 8 -7 -1 16.55 4.26 8 7 -1 29.11 7.72 8 -7 -1 20.93 5.57 8 -7 0 10.01 4.31 8 -7 0 11.92 6.19 8 -7 0 10.07 4.04 8 7 0 23.99 7.27 8 -7 1 88.36 8.86 8 7 1 87.71 10.35 8 -7 1 91.53 9.98 8 -7 1 92.75 8.53 8 -7 2 77.57 8.55 8 7 2 74.32 9.04 8 -7 2 91.48 9.43 8 -7 2 95.32 9.13 8 -7 3 11.34 4.12 8 -7 3 10.08 4.65 8 -7 3 6.09 4.17 8 7 3 11.93 6.48 8 -7 4 17.98 3.83 8 -7 4 13.85 3.63 8 -7 4 18.62 3.98 8 7 4 5.69 3.29 8 -7 5 4.68 2.56 8 -7 5 4.84 2.38 8 7 5 6.28 3.55 8 -7 5 6.93 3.50 8 7 5 4.47 3.09 8 -7 6 28.13 5.04 8 -7 6 25.94 4.55 8 7 6 32.06 6.36 8 -7 6 23.44 5.11 8 7 6 38.77 6.68 8 -7 7 -1.60 2.09 8 -7 7 3.94 2.96 8 7 7 5.64 5.09 8 -7 7 3.21 3.00 8 7 7 5.13 5.59 8 -7 8 1.23 1.74 8 7 8 1.56 2.64 8 -7 8 0.62 2.20 8 7 8 2.68 3.77 8 -7 8 1.00 1.97 8 -7 9 32.19 5.42 8 7 9 32.41 5.20 8 7 9 43.17 6.73 8 -7 9 34.88 5.05 8 -7 9 43.07 5.36 8 7 10 47.16 6.06 8 -7 10 49.95 6.04 8 -7 10 47.96 5.52 8 -7 10 58.23 6.06 8 -7 11 9.91 2.68 8 7 11 3.96 2.59 8 -7 11 8.92 2.69 8 7 11 9.45 4.05 8 7 12 37.69 5.21 8 -7 12 32.23 4.72 8 7 12 39.86 8.22 8 -7 12 37.67 5.12 8 -7 13 4.53 1.98 8 -7 13 4.58 2.33 8 7 13 6.58 3.07 8 -7 14 20.77 3.61 8 7 14 22.35 4.35 8 -7 14 22.51 3.80 8 -7 15 106.53 7.83 8 -7 15 136.45 8.81 8 7 15 137.36 8.09 8 7 15 143.42 10.46 8 -7 15 141.12 8.63 8 -7 16 16.60 3.28 8 -7 16 17.75 3.36 8 7 16 18.93 3.16 8 7 16 20.60 4.38 8 -7 17 8.43 2.27 8 -7 17 13.11 3.14 8 7 17 10.09 2.21 8 7 17 10.27 3.65 8 -7 18 33.58 4.34 8 -7 18 21.01 3.50 8 7 18 37.00 4.19 8 7 18 36.95 4.94 8 -7 19 9.49 2.33 8 -7 19 7.24 1.97 8 7 19 9.41 2.13 8 7 19 6.64 2.75 8 -7 20 1.55 1.21 8 -7 20 2.46 1.37 8 7 20 -0.04 1.21 8 7 20 0.19 1.91 8 -7 21 10.67 2.57 8 7 21 12.31 2.55 8 7 21 5.06 2.59 8 -7 22 8.72 1.76 8 7 22 12.20 2.66 8 -7 23 6.99 1.81 8 7 23 15.55 2.87 8 -7 24 17.42 2.44 8 -8 -23 2.56 1.44 8 -8 -22 16.73 3.46 8 -8 -22 7.52 3.73 8 -8 -21 44.71 3.55 8 -8 -21 46.36 5.12 8 -8 -20 42.14 3.85 8 -8 -20 45.55 5.43 8 -8 -19 14.18 2.41 8 -8 -19 9.96 3.10 8 -8 -18 1.94 1.52 8 -8 -18 1.43 1.85 8 -8 -18 5.08 2.19 8 -8 -17 3.13 2.35 8 -8 -17 0.99 1.58 8 -8 -16 17.81 2.94 8 -8 -16 14.91 3.61 8 -8 -16 15.41 3.39 8 -8 -15 23.20 3.49 8 -8 -15 23.10 4.21 8 -8 -15 24.76 4.65 8 -8 -14 47.97 6.46 8 -8 -14 57.40 6.39 8 -8 -13 8.59 3.52 8 -8 -13 16.98 4.13 8 -8 -12 4.41 2.92 8 -8 -12 7.00 2.84 8 -8 -11 119.47 10.64 8 -8 -11 130.22 9.66 8 -8 -10 126.66 11.30 8 -8 -10 121.26 9.81 8 -8 -9 13.59 5.21 8 -8 -9 4.72 3.36 8 -8 -8 82.90 9.52 8 -8 -8 81.38 8.25 8 -8 -7 44.13 8.12 8 -8 -7 41.59 6.40 8 -8 -6 71.94 9.79 8 -8 -6 85.60 8.12 8 -8 -5 33.07 6.73 8 -8 -5 33.92 5.29 8 -8 -4 2.56 3.46 8 8 -4 -1.27 2.82 8 -8 -4 5.95 2.78 8 -8 -3 9.79 3.99 8 8 -3 5.48 3.68 8 -8 -3 7.77 2.89 8 -8 -2 3.45 4.74 8 8 -2 3.01 3.12 8 -8 -2 1.31 2.54 8 -8 -1 0.90 2.98 8 8 -1 5.87 4.16 8 -8 -1 2.87 2.91 8 -8 0 36.85 6.45 8 -8 0 28.33 4.67 8 8 0 36.65 6.70 8 -8 0 40.03 5.54 8 -8 1 34.99 5.90 8 -8 1 25.62 4.67 8 8 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23.24 4.83 9 6 2 19.56 4.85 9 -6 2 30.08 4.88 9 6 3 18.91 6.59 9 -6 3 20.27 5.28 9 6 3 21.13 5.53 9 -6 3 18.02 4.28 9 6 4 68.97 8.87 9 -6 4 59.32 7.60 9 6 4 67.24 8.49 9 -6 4 66.57 7.39 9 6 5 8.86 4.23 9 -6 5 5.40 4.09 9 6 5 11.21 5.25 9 -6 5 1.84 2.77 9 6 6 10.48 5.08 9 -6 6 11.56 3.94 9 6 6 17.67 5.86 9 -6 6 11.04 3.47 9 6 7 122.15 15.31 9 -6 7 139.04 10.66 9 -6 7 139.05 9.73 9 -6 8 6.06 4.02 9 6 8 3.22 3.15 9 -6 9 29.10 5.32 9 6 9 40.73 7.04 9 -6 9 32.28 4.48 9 6 10 27.51 5.80 9 -6 10 21.50 4.50 9 6 10 32.35 6.50 9 6 11 5.43 2.90 9 -6 11 3.23 2.30 9 6 11 5.40 4.24 9 6 12 0.18 2.12 9 -6 12 -0.41 1.75 9 6 12 -1.51 2.89 9 6 13 4.74 2.41 9 -6 13 0.13 1.58 9 -6 13 4.99 2.65 9 6 13 4.15 3.51 9 6 14 -0.73 1.96 9 -6 14 0.10 1.69 9 -6 14 0.53 1.70 9 6 14 1.61 3.09 9 6 15 274.19 12.51 9 -6 15 279.02 13.66 9 6 15 284.20 14.21 9 6 16 15.10 3.13 9 -6 16 12.38 3.05 9 -6 16 16.26 3.60 9 6 16 14.35 3.83 9 -6 17 6.96 2.45 9 -6 17 12.37 2.92 9 6 17 11.23 3.05 9 -6 18 59.42 5.64 9 -6 18 63.76 5.98 9 6 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62.43 7.45 10 -4 1 76.69 8.87 10 4 1 64.96 7.28 10 4 1 63.91 6.59 10 -4 1 74.86 8.05 10 4 2 4.12 3.29 10 -4 2 5.34 3.42 10 4 2 -5.37 5.14 10 4 2 2.12 3.15 10 -4 2 7.58 3.06 10 4 3 16.90 6.25 10 -4 3 9.98 3.97 10 4 3 9.91 3.57 10 4 3 24.54 5.38 10 -4 3 9.98 3.25 10 4 4 183.37 13.52 10 -4 4 180.35 12.60 10 4 4 167.48 11.65 10 4 4 163.83 10.70 10 -4 4 169.17 10.87 10 4 5 102.23 10.16 10 -4 5 93.38 10.57 10 4 5 111.27 9.83 10 4 5 91.44 8.07 10 -4 5 95.79 8.37 10 4 6 21.67 5.78 10 -4 6 14.97 3.44 10 -4 6 7.52 4.21 10 4 6 13.79 5.54 10 4 6 7.25 3.35 10 -4 6 7.56 3.03 10 4 7 5.27 5.17 10 -4 7 -5.44 2.59 10 -4 7 0.14 2.92 10 4 7 1.97 3.80 10 -4 7 -0.19 1.62 10 4 8 172.81 13.18 10 -4 8 156.75 10.67 10 -4 8 211.10 13.66 10 4 8 210.89 12.77 10 -4 8 167.27 9.61 10 4 9 162.17 12.20 10 -4 9 147.11 10.35 10 -4 9 190.24 13.01 10 4 9 187.99 12.39 10 -4 9 154.79 8.94 10 4 10 66.86 7.66 10 -4 10 81.18 8.71 10 4 10 86.02 8.26 10 4 11 37.93 6.66 10 -4 11 35.67 5.51 10 -4 11 32.91 5.96 10 4 11 51.81 7.27 10 4 12 52.41 6.85 10 -4 12 47.21 6.08 10 -4 12 61.00 7.53 10 4 12 67.20 7.71 10 4 13 10.51 6.39 10 -4 13 4.83 2.61 10 -4 13 3.67 2.18 10 4 13 7.69 3.89 10 4 14 1.55 2.64 10 -4 14 1.70 2.24 10 -4 14 3.53 2.76 10 4 14 5.24 3.38 10 4 15 23.68 4.48 10 -4 15 18.40 4.21 10 -4 15 19.88 4.56 10 4 15 20.78 4.23 10 4 16 24.39 4.19 10 -4 16 21.14 3.98 10 -4 16 24.69 4.57 10 4 16 23.65 4.01 10 4 17 37.18 5.10 10 -4 17 36.25 5.21 10 -4 17 26.26 4.31 10 4 17 37.06 5.33 10 4 18 81.70 6.80 10 -4 18 64.74 6.25 10 -4 18 79.41 7.31 10 4 18 73.29 6.57 10 4 19 1.98 1.89 10 -4 19 4.01 2.59 10 -4 19 2.97 2.44 10 4 19 8.12 3.17 10 4 20 -1.32 1.67 10 -4 20 -1.18 1.67 10 -4 20 1.59 1.74 10 4 20 -2.30 2.68 10 4 21 -2.16 1.61 10 -4 21 -2.35 1.63 10 4 21 0.32 2.12 10 -4 22 4.02 2.06 10 -4 22 3.60 1.76 10 4 22 4.78 2.32 10 -4 23 3.69 1.55 10 -4 23 1.79 1.31 10 -4 24 1.19 1.03 10 -4 24 1.63 1.10 10 -4 25 5.22 1.90 10 -4 25 6.08 1.54 -10 5 26 14.55 1.90 10 -5 -26 15.93 2.24 -10 5 25 19.82 2.61 10 -5 -25 14.67 2.28 -10 5 24 41.26 3.71 10 -5 -24 34.07 3.50 -10 5 23 17.15 2.58 10 -5 -23 12.88 2.55 -10 5 22 -0.51 1.66 10 -5 -22 4.15 1.82 -10 5 21 119.01 6.48 10 -5 -21 126.08 7.05 -10 5 20 20.26 3.23 10 -5 -20 19.65 3.14 -10 5 19 5.62 1.89 10 -5 -19 8.29 2.11 10 -5 -19 6.87 2.03 -10 5 18 0.82 1.60 10 -5 -18 3.25 2.02 10 -5 -18 0.01 1.64 10 -5 -17 1.39 1.65 10 -5 -17 1.89 1.91 10 -5 -16 13.27 3.12 10 -5 -16 11.05 3.19 10 -5 -15 12.13 3.14 10 -5 -15 12.01 3.64 10 -5 -14 0.90 1.60 10 -5 -14 -3.38 3.16 10 -5 -13 82.08 7.13 10 -5 -13 72.07 8.18 10 -5 -12 21.57 5.55 10 -5 -11 7.52 3.33 10 -5 -10 36.44 6.76 10 5 -9 28.39 5.80 10 -5 -9 23.29 5.16 10 5 -8 -3.62 4.90 10 -5 -8 1.55 2.90 10 5 -7 0.52 3.78 10 -5 -7 7.50 4.55 10 -5 -6 11.82 3.97 10 5 -6 15.60 5.78 10 -5 -6 8.18 4.49 10 -5 -5 121.48 9.61 10 5 -5 117.99 9.39 10 5 -5 102.65 10.32 10 -5 -5 101.11 10.05 10 -5 -4 44.94 7.21 10 5 -4 34.59 5.69 10 5 -4 34.65 6.25 10 -5 -4 30.45 6.17 10 -5 -3 30.28 5.60 10 5 -3 29.19 5.42 10 5 -3 24.96 4.65 10 -5 -3 21.66 5.04 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13 2 11 23.65 3.43 13 -2 11 20.24 2.66 13 -2 11 29.02 3.16 13 2 12 -0.22 1.45 13 -2 12 0.95 0.83 13 2 13 5.06 1.60 13 -2 13 3.78 1.16 13 2 14 0.60 1.02 -13 3 16 14.52 1.85 13 -3 -14 0.20 1.32 13 -3 -13 24.77 2.58 13 -3 -13 13.15 2.49 13 -3 -12 18.72 3.00 13 -3 -11 7.11 2.31 13 -3 -10 48.10 4.86 13 -3 -9 74.31 6.28 13 -3 -8 76.00 6.32 13 3 -7 37.33 5.32 13 -3 -7 31.98 4.38 13 3 -6 41.73 5.08 13 -3 -6 43.07 4.70 13 -3 -5 25.53 3.81 13 3 -5 26.60 4.59 13 3 -4 72.51 6.53 13 -3 -4 80.67 6.30 13 3 -3 7.60 2.78 13 -3 -3 1.03 1.49 13 -3 -2 29.38 3.58 13 -3 -1 4.02 1.78 13 -3 0 11.18 2.53 13 -3 1 0.42 1.40 13 -3 2 2.74 1.48 13 -3 2 -0.66 1.40 13 -3 3 2.31 1.38 13 -3 3 2.50 1.31 13 3 4 1.63 2.03 13 -3 4 3.17 1.31 13 -3 4 0.85 1.10 13 3 5 5.83 3.10 13 -3 5 5.00 1.80 13 3 6 1.46 2.17 13 -3 6 0.68 1.11 13 3 7 1.15 2.03 13 -3 7 2.44 1.50 13 3 8 8.60 2.61 13 -3 8 9.62 1.99 13 3 9 5.25 2.29 13 -3 9 1.62 1.43 13 -3 10 21.52 2.61 13 3 10 13.37 2.42 13 3 11 9.62 2.16 13 -3 11 11.14 1.92 13 3 12 7.22 1.80 13 -3 12 7.92 1.51 13 3 13 -1.14 1.05 -13 4 13 0.03 0.87 13 -4 -13 1.14 1.12 13 -4 -12 1.16 1.13 13 -4 -11 1.54 0.86 13 -4 -11 1.97 1.21 13 -4 -10 6.97 1.56 13 -4 -10 3.84 1.85 13 -4 -9 9.81 1.76 13 -4 -9 9.40 2.44 13 -4 -8 10.58 1.82 13 -4 -8 8.74 2.33 13 -4 -7 11.11 2.34 13 -4 -6 13.94 2.51 13 -4 -5 5.10 2.43 13 -4 -4 1.80 1.93 13 -4 -3 3.71 1.56 13 -4 -2 20.46 3.25 13 -4 -1 39.49 4.22 13 -4 0 14.12 2.64 13 -4 1 3.75 1.49 13 -4 2 75.61 4.73 13 -4 3 27.34 2.92 13 -4 4 24.56 3.07 13 -4 5 57.75 4.23 13 -4 6 1.61 1.16 13 -4 7 1.86 0.95 13 -4 8 1.40 0.97 13 -4 9 1.22 0.84 13 -4 10 1.56 0.88 13 -5 -10 2.77 1.40 13 -5 -9 -1.56 1.39 13 -5 -8 23.06 2.86 13 -5 -7 41.30 3.81 13 -5 -6 -0.76 1.23 13 -5 -5 2.83 1.37 13 -5 -4 1.01 1.07 13 -5 -3 28.07 3.04 13 -5 -2 19.71 2.82 13 -5 -1 162.33 6.93 13 -5 0 58.67 4.11 13 -5 1 2.38 1.34 14 0 -10 -0.79 1.43 14 0 -9 -2.60 1.37 14 0 -8 5.28 1.91 14 0 -7 -1.64 1.74 14 0 -6 -1.53 1.42 14 0 -5 5.91 2.11 14 0 -4 65.93 4.95 14 0 -3 0.31 1.10 14 0 -2 5.47 1.73 14 0 -1 7.06 1.79 14 0 0 61.68 4.33 14 0 1 2.50 1.22 14 -1 -10 -0.25 1.16 14 1 -9 3.11 1.61 14 -1 -9 2.18 1.45 14 1 -8 -1.02 1.38 14 -1 -8 0.59 1.16 14 1 -7 1.49 1.35 14 -1 -7 1.82 1.31 14 1 -6 1.38 1.61 14 -1 -6 2.62 1.28 14 1 -5 30.78 3.71 14 -1 -5 32.45 3.49 14 -1 -4 21.09 2.89 14 1 -4 18.77 2.96 14 1 -3 0.95 1.30 14 -1 -3 0.90 1.12 14 -1 -2 14.84 2.56 14 1 -2 14.83 2.62 14 1 -1 81.10 5.04 14 -1 -1 81.49 4.87 14 1 0 8.33 1.88 14 -1 0 8.44 1.74 14 -1 1 4.63 1.45 14 -2 -8 2.59 1.46 14 -2 -7 0.23 1.10 14 -2 -6 48.57 4.17 14 -2 -5 13.37 2.15 14 -2 -4 2.08 1.22 14 -2 -3 22.87 2.72 14 -2 -2 57.39 4.02 14 -2 -1 -2.12 1.09 0 0 0 0.00 0.00 TITL REARDK3 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 11.525337 11.264050 33.022222 90.0000 92.5450 90.0000 ZERR 8.00 0.000295 0.000343 0.001009 0.0000 0.0025 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H O UNIT 216.00 208.00 24.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 79798 _olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount' _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 2.151 _oxdiff_exptl_absorpt_empirical_full_min 0.648 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1A O 0.60017(16) 0.17097(19) 0.30613(7) 0.0406(5) Uani 1 1 d . . . . . C2A C 0.4954(2) 0.1661(2) 0.31196(9) 0.0297(6) Uani 1 1 d . . . . . C3A C 0.4510(2) 0.1161(2) 0.34885(9) 0.0308(6) Uani 1 1 d . . . . . H3A H 0.503176 0.076590 0.367424 0.037 Uiso 1 1 calc R U . . . C4A C 0.3389(2) 0.1241(2) 0.35731(9) 0.0293(6) Uani 1 1 d . . . . . H4A H 0.314090 0.082819 0.380478 0.035 Uiso 1 1 calc R U . . . C5A C 0.2486(2) 0.1940(2) 0.33270(9) 0.0276(6) Uani 1 1 d . . . . . C6A C 0.3041(2) 0.2643(2) 0.29847(8) 0.0264(6) Uani 1 1 d . . . . . H6A H 0.243684 0.282096 0.276646 0.032 Uiso 1 1 calc R U . . . C7A C 0.4083(2) 0.2078(2) 0.27997(9) 0.0282(6) Uani 1 1 d . . . . . H7AA H 0.382395 0.139543 0.262990 0.034 Uiso 1 1 calc R U . . . H7AB H 0.445375 0.266223 0.262252 0.034 Uiso 1 1 calc R U . . . C8A C 0.1451(2) 0.1141(3) 0.31893(11) 0.0401(8) Uani 1 1 d . . . . . H8AA H 0.100467 0.094102 0.342935 0.048 Uiso 1 1 calc R U . . . H8AB H 0.093143 0.159997 0.300066 0.048 Uiso 1 1 calc R U . . . C9A C 0.1777(3) 0.0027(3) 0.29877(10) 0.0362(7) Uani 1 1 d . . . . . H9A H 0.210808 0.008824 0.273014 0.043 Uiso 1 1 calc R U . . . C10A C 0.1646(3) -0.1032(3) 0.31362(10) 0.0389(7) Uani 1 1 d . . . . . H10A H 0.131764 -0.112897 0.339298 0.047 Uiso 1 1 calc R U . . . H10B H 0.187730 -0.170734 0.298779 0.047 Uiso 1 1 calc R U . . . O11A O 0.34532(15) 0.37596(16) 0.31724(5) 0.0256(4) Uani 1 1 d . . . . . C12A C 0.2787(2) 0.3944(2) 0.34985(8) 0.0231(5) Uani 1 1 d . . . . . C13A C 0.2140(2) 0.2956(2) 0.35972(8) 0.0261(6) Uani 1 1 d . . . . . C14A C 0.1419(2) 0.2996(2) 0.39216(9) 0.0306(6) Uani 1 1 d . . . . . H14A H 0.096540 0.232517 0.398761 0.037 Uiso 1 1 calc R U . . . C15A C 0.1369(2) 0.4035(3) 0.41503(9) 0.0308(6) Uani 1 1 d D . . . . C16A C 0.2060(2) 0.4995(2) 0.40501(8) 0.0272(6) Uani 1 1 d . . . . . H16A H 0.203551 0.569177 0.421173 0.033 Uiso 1 1 calc R U . . . C17A C 0.2792(2) 0.4982(2) 0.37216(8) 0.0232(5) Uani 1 1 d . . . . . C18A C 0.0653(4) 0.4077(4) 0.45277(15) 0.0358(11) Uani 0.849(9) 1 d D . P A 1 H18A H 0.068088 0.489297 0.463957 0.043 Uiso 0.849(9) 1 calc R U P A 1 H18B H -0.016650 0.389492 0.444939 0.043 Uiso 0.849(9) 1 calc R U P A 1 C19A C 0.1068(5) 0.3227(4) 0.48506(14) 0.0386(10) Uani 0.849(9) 1 d D . P A 1 H19A H 0.106914 0.240768 0.478265 0.046 Uiso 0.849(9) 1 calc R U P A 1 C20A C 0.1426(3) 0.3514(4) 0.52161(13) 0.0469(13) Uani 0.849(9) 1 d D . P A 1 H20A H 0.143942 0.432368 0.529685 0.056 Uiso 0.849(9) 1 calc R U P A 1 H20B H 0.167556 0.291441 0.540264 0.056 Uiso 0.849(9) 1 calc R U P A 1 C21A C 0.3564(2) 0.5993(2) 0.36326(8) 0.0232(5) Uani 1 1 d . . . . . C22A C 0.3558(2) 0.6542(2) 0.32547(8) 0.0246(5) Uani 1 1 d . . . . . C23A C 0.4305(2) 0.7482(2) 0.31847(8) 0.0276(6) Uani 1 1 d . . . . . H23A H 0.428882 0.785541 0.292652 0.033 Uiso 1 1 calc R U . . . C24A C 0.5075(2) 0.7876(2) 0.34905(9) 0.0278(6) Uani 1 1 d . . . . . H24A H 0.558936 0.851273 0.343984 0.033 Uiso 1 1 calc R U . . . C25A C 0.5097(2) 0.7342(2) 0.38722(9) 0.0277(6) Uani 1 1 d . . . . . C26A C 0.4343(2) 0.6415(2) 0.39380(8) 0.0254(5) Uani 1 1 d . . . . . H26A H 0.435236 0.605180 0.419785 0.030 Uiso 1 1 calc R U . . . O27A O 0.27995(17) 0.62417(17) 0.29385(6) 0.0295(4) Uani 1 1 d . . . . . H27A H 0.246999 0.559829 0.299119 0.044 Uiso 1 1 calc R U . . . C28A C 0.5898(2) 0.7805(3) 0.42124(10) 0.0355(7) Uani 1 1 d . . . . . H28A H 0.611063 0.714597 0.439982 0.043 Uiso 1 1 calc R U . . . H28B H 0.661984 0.810962 0.409827 0.043 Uiso 1 1 calc R U . . . C29A C 0.5329(3) 0.8781(3) 0.44435(9) 0.0386(7) Uani 1 1 d . . . . . H29A H 0.466809 0.858290 0.459187 0.046 Uiso 1 1 calc R U . . . C30A C 0.5684(3) 0.9886(3) 0.44536(11) 0.0492(9) Uani 1 1 d . . . . . H30A H 0.634147 1.011450 0.430859 0.059 Uiso 1 1 calc R U . . . H30B H 0.528327 1.045872 0.460583 0.059 Uiso 1 1 calc R U . . . O1B O 0.09597(15) 0.45143(18) 0.27827(6) 0.0333(5) Uani 1 1 d . . . . . C2B C -0.0010(2) 0.4548(2) 0.29231(8) 0.0262(6) Uani 1 1 d . . . . . C3B C -0.0273(2) 0.5372(2) 0.32488(9) 0.0305(6) Uani 1 1 d . . . . . H3B H 0.029867 0.593414 0.333681 0.037 Uiso 1 1 calc R U . . . C4B C -0.1287(2) 0.5359(2) 0.34257(8) 0.0288(6) Uani 1 1 d . . . . . H4B H -0.140931 0.594606 0.362579 0.035 Uiso 1 1 calc R U . . . C5B C -0.2256(2) 0.4493(2) 0.33359(8) 0.0249(5) Uani 1 1 d . . . . . C6B C -0.1906(2) 0.3494(2) 0.30459(8) 0.0226(5) Uani 1 1 d . . . . . H6B H -0.261744 0.321085 0.289077 0.027 Uiso 1 1 calc R U . . . C7B C -0.0992(2) 0.3808(2) 0.27474(8) 0.0250(5) Uani 1 1 d . . . . . H7BA H -0.066929 0.306379 0.263932 0.030 Uiso 1 1 calc R U . . . H7BB H -0.137035 0.424370 0.251710 0.030 Uiso 1 1 calc R U . . . C8B C -0.3381(2) 0.5137(3) 0.31908(9) 0.0306(6) Uani 1 1 d . . . . . H8BA H -0.403312 0.456455 0.318567 0.037 Uiso 1 1 calc R U . . . H8BB H -0.355378 0.576939 0.338755 0.037 Uiso 1 1 calc R U . . . C9B C -0.3304(2) 0.5677(3) 0.27799(9) 0.0333(6) Uani 1 1 d . . . . . H9B H -0.273807 0.627789 0.274616 0.040 Uiso 1 1 calc R U . . . C10B C -0.3960(3) 0.5380(3) 0.24639(10) 0.0427(8) Uani 1 1 d . . . . . H10C H -0.453515 0.478255 0.248665 0.051 Uiso 1 1 calc R U . . . H10D H -0.386283 0.576180 0.221113 0.051 Uiso 1 1 calc R U . . . O11B O -0.14533(15) 0.25189(15) 0.33032(5) 0.0238(4) Uani 1 1 d . . . . . C12B C -0.1912(2) 0.2672(2) 0.36763(8) 0.0225(5) Uani 1 1 d . . . . . C13B C -0.2405(2) 0.3788(2) 0.37234(8) 0.0237(5) Uani 1 1 d . . . . . C14B C -0.2883(2) 0.4104(2) 0.40836(8) 0.0279(6) Uani 1 1 d . . . . . H14B H -0.323027 0.486241 0.411225 0.033 Uiso 1 1 calc R U . . . C15B C -0.2852(2) 0.3299(3) 0.44062(8) 0.0273(6) Uani 1 1 d . . . . . C16B C -0.2345(2) 0.2192(2) 0.43517(8) 0.0267(6) Uani 1 1 d . . . . . H16B H -0.231169 0.165283 0.457321 0.032 Uiso 1 1 calc R U . . . C17B C -0.1877(2) 0.1832(2) 0.39839(8) 0.0243(5) Uani 1 1 d . . . . . C3 C -0.3416(2) 0.3601(3) 0.47973(9) 0.0331(6) Uani 1 1 d . . . . . H3C H -0.312296 0.304779 0.501101 0.040 Uiso 1 1 calc R U . . . H3D H -0.317883 0.441332 0.488029 0.040 Uiso 1 1 calc R U . . . C1 C -0.4726(3) 0.3541(3) 0.47714(10) 0.0365(7) Uani 1 1 d . . . . . H1 H -0.511264 0.375134 0.500925 0.044 Uiso 1 1 calc R U . . . C2 C -0.5387(3) 0.3230(3) 0.44568(11) 0.0443(8) Uani 1 1 d . . . . . H2A H -0.504573 0.301033 0.421097 0.053 Uiso 1 1 calc R U . . . H2B H -0.620729 0.322281 0.447405 0.053 Uiso 1 1 calc R U . . . C21B C -0.1366(2) 0.0619(2) 0.39466(8) 0.0250(5) Uani 1 1 d . . . . . C22B C -0.1747(2) -0.0195(2) 0.36493(8) 0.0270(6) Uani 1 1 d . . . . . C23B C -0.1269(3) -0.1330(3) 0.36419(9) 0.0332(6) Uani 1 1 d . . . . . H23B H -0.152140 -0.187362 0.343651 0.040 Uiso 1 1 calc R U . . . C24B C -0.0429(3) -0.1673(3) 0.39318(9) 0.0340(6) Uani 1 1 d . . . . . H24B H -0.011426 -0.245171 0.392422 0.041 Uiso 1 1 calc R U . . . C25B C -0.0042(2) -0.0891(3) 0.42324(9) 0.0303(6) Uani 1 1 d . . . . . C26B C -0.0513(2) 0.0241(2) 0.42311(8) 0.0266(6) Uani 1 1 d . . . . . H26B H -0.024266 0.078589 0.443356 0.032 Uiso 1 1 calc R U . . . O27B O -0.26244(17) 0.00031(18) 0.33681(6) 0.0334(5) Uani 1 1 d . . . . . H27B H -0.277416 0.073260 0.335762 0.050 Uiso 1 1 calc R U . . . C28B C 0.0891(2) -0.1242(3) 0.45488(10) 0.0374(7) Uani 1 1 d . . . . . H28C H 0.062655 -0.104129 0.482162 0.045 Uiso 1 1 calc R U . . . H28D H 0.101138 -0.211168 0.453814 0.045 Uiso 1 1 calc R U . . . C29B C 0.2011(3) -0.0629(3) 0.44835(11) 0.0433(8) Uani 1 1 d . . . . . H29B H 0.243845 -0.084942 0.425572 0.052 Uiso 1 1 calc R U . . . C30B C 0.2437(3) 0.0204(4) 0.47267(14) 0.0615(11) Uani 1 1 d . . . . . H30C H 0.202509 0.043871 0.495636 0.074 Uiso 1 1 calc R U . . . H30D H 0.315619 0.057014 0.467265 0.074 Uiso 1 1 calc R U . . . C19B C 0.056(2) 0.360(2) 0.4812(6) 0.038(6) Uiso 0.151(9) 1 d D . P A 2 H19B H -0.004302 0.363637 0.499655 0.046 Uiso 0.151(9) 1 calc R U P A 2 C20B C 0.149(3) 0.302(4) 0.4930(15) 0.082(15) Uiso 0.151(9) 1 d D . P A 2 H20C H 0.212441 0.296370 0.475654 0.099 Uiso 0.151(9) 1 calc R U P A 2 H20D H 0.153662 0.266207 0.518981 0.099 Uiso 0.151(9) 1 calc R U P A 2 C18B C 0.0357(17) 0.421(2) 0.4423(6) 0.028(7) Uiso 0.151(9) 1 d D . P A 2 H18C H 0.024228 0.506612 0.447168 0.033 Uiso 0.151(9) 1 calc R U P A 2 H18D H -0.036071 0.389180 0.428714 0.033 Uiso 0.151(9) 1 calc R U P A 2 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 O1A 0.0179(9) 0.0349(12) 0.0683(15) 0.0077(10) -0.0048(9) 0.0004(9) C2A 0.0231(13) 0.0172(13) 0.0480(17) -0.0046(11) -0.0083(11) 0.0018(10) C3A 0.0275(13) 0.0202(14) 0.0435(16) 0.0011(11) -0.0112(11) 0.0028(11) C4A 0.0297(14) 0.0167(13) 0.0409(16) 0.0007(11) -0.0056(11) -0.0003(11) C5A 0.0206(12) 0.0175(13) 0.0441(16) 0.0000(11) -0.0067(11) 0.0000(10) C6A 0.0251(12) 0.0190(13) 0.0341(14) -0.0054(11) -0.0088(10) 0.0036(10) C7A 0.0224(12) 0.0249(14) 0.0367(15) -0.0053(11) -0.0049(10) 0.0048(11) C8A 0.0246(14) 0.0232(15) 0.071(2) -0.0060(14) -0.0121(14) -0.0018(12) C9A 0.0331(15) 0.0360(17) 0.0395(17) -0.0075(13) 0.0016(12) -0.0077(13) C10A 0.0440(17) 0.0220(15) 0.0502(19) -0.0029(13) -0.0023(14) -0.0021(13) O11A 0.0283(9) 0.0179(9) 0.0306(10) -0.0025(7) -0.0006(7) -0.0015(7) C12A 0.0200(11) 0.0201(13) 0.0288(13) 0.0011(10) -0.0016(9) -0.0002(10) C13A 0.0224(12) 0.0168(13) 0.0386(15) 0.0003(11) -0.0046(10) -0.0003(10) C14A 0.0212(12) 0.0210(14) 0.0497(17) 0.0042(12) 0.0031(11) -0.0031(11) C15A 0.0238(13) 0.0273(15) 0.0416(16) 0.0019(12) 0.0061(11) 0.0003(11) C16A 0.0265(13) 0.0205(13) 0.0346(15) -0.0019(11) 0.0019(11) 0.0002(11) C17A 0.0224(12) 0.0170(12) 0.0300(14) 0.0015(10) -0.0021(10) 0.0010(10) C18A 0.027(2) 0.036(2) 0.045(3) 0.005(2) 0.007(2) 0.0012(17) C19A 0.036(3) 0.033(2) 0.048(3) 0.0047(19) 0.011(2) -0.001(2) C20A 0.035(2) 0.053(3) 0.053(3) 0.005(2) 0.0077(17) 0.0041(18) C21A 0.0221(12) 0.0168(12) 0.0307(13) -0.0009(10) -0.0001(10) 0.0005(10) C22A 0.0234(12) 0.0202(13) 0.0299(13) -0.0033(10) -0.0009(10) 0.0021(10) C23A 0.0295(13) 0.0198(13) 0.0336(14) 0.0020(11) 0.0031(11) -0.0002(11) C24A 0.0238(12) 0.0173(13) 0.0423(16) -0.0011(11) 0.0034(11) -0.0023(10) C25A 0.0230(12) 0.0215(14) 0.0383(15) -0.0035(11) -0.0012(11) -0.0004(11) C26A 0.0253(12) 0.0197(13) 0.0312(14) -0.0011(10) 0.0010(10) -0.0005(10) O27A 0.0337(10) 0.0227(10) 0.0314(10) 0.0029(8) -0.0054(8) -0.0055(8) C28A 0.0280(14) 0.0325(16) 0.0456(17) -0.0007(13) -0.0053(12) -0.0105(12) C29A 0.0381(16) 0.0394(18) 0.0380(17) -0.0023(13) -0.0023(13) -0.0101(14) C30A 0.055(2) 0.042(2) 0.050(2) -0.0058(16) -0.0057(16) -0.0110(17) O1B 0.0196(9) 0.0305(11) 0.0500(12) 0.0088(9) 0.0043(8) 0.0006(8) C2B 0.0207(12) 0.0200(13) 0.0377(15) 0.0086(11) -0.0014(10) -0.0006(10) C3B 0.0278(13) 0.0222(14) 0.0410(16) 0.0002(11) -0.0039(11) -0.0047(11) C4B 0.0334(14) 0.0188(13) 0.0340(15) 0.0003(11) -0.0009(11) 0.0013(11) C5B 0.0235(12) 0.0171(13) 0.0342(14) 0.0008(10) 0.0012(10) 0.0031(10) C6B 0.0194(11) 0.0164(12) 0.0318(14) 0.0011(10) -0.0012(10) 0.0006(10) C7B 0.0214(12) 0.0226(13) 0.0312(14) 0.0010(10) 0.0020(10) -0.0008(10) C8B 0.0241(13) 0.0269(15) 0.0410(16) 0.0045(12) 0.0037(11) 0.0094(11) C9B 0.0270(14) 0.0276(15) 0.0454(17) 0.0101(12) 0.0027(12) 0.0066(12) C10B 0.0402(17) 0.0427(19) 0.0446(18) 0.0090(15) -0.0045(14) 0.0067(15) O11B 0.0239(9) 0.0170(9) 0.0306(9) 0.0023(7) 0.0029(7) 0.0027(7) C12B 0.0182(11) 0.0196(13) 0.0295(13) -0.0002(10) 0.0006(9) -0.0015(10) C13B 0.0202(12) 0.0166(12) 0.0343(14) 0.0020(10) 0.0002(10) -0.0001(10) C14B 0.0246(13) 0.0217(13) 0.0371(15) -0.0019(11) 0.0000(11) 0.0026(11) C15B 0.0213(12) 0.0283(14) 0.0321(14) -0.0018(11) -0.0010(10) -0.0022(11) C16B 0.0223(12) 0.0248(14) 0.0328(14) 0.0027(11) -0.0012(10) -0.0026(11) C17B 0.0175(11) 0.0199(13) 0.0353(14) 0.0017(11) -0.0010(10) -0.0014(10) C3 0.0351(15) 0.0318(16) 0.0323(15) -0.0005(12) 0.0014(11) 0.0013(13) C1 0.0352(15) 0.0345(17) 0.0411(17) 0.0043(13) 0.0141(13) 0.0059(13) C2 0.0288(15) 0.047(2) 0.057(2) 0.0030(16) 0.0049(14) 0.0016(14) C21B 0.0179(11) 0.0214(13) 0.0359(14) 0.0064(11) 0.0025(10) -0.0013(10) C22B 0.0207(12) 0.0231(14) 0.0370(15) 0.0056(11) -0.0007(10) -0.0013(11) C23B 0.0345(15) 0.0209(14) 0.0441(17) -0.0004(12) -0.0001(12) 0.0009(12) C24B 0.0355(15) 0.0161(13) 0.0502(18) 0.0055(12) 0.0012(13) 0.0053(12) C25B 0.0230(13) 0.0251(14) 0.0428(16) 0.0094(12) 0.0017(11) 0.0008(11) C26B 0.0235(12) 0.0214(13) 0.0349(14) 0.0034(11) 0.0018(10) -0.0028(11) O27B 0.0286(10) 0.0223(10) 0.0480(12) 0.0003(9) -0.0118(8) 0.0001(8) C28B 0.0308(15) 0.0341(17) 0.0469(18) 0.0129(13) -0.0026(13) 0.0045(13) C29B 0.0264(14) 0.052(2) 0.0509(19) 0.0151(16) -0.0031(13) 0.0014(14) C30B 0.045(2) 0.056(2) 0.081(3) 0.020(2) -0.0219(19) -0.0099(18) 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 7 -4 -1 0.1748 -7 1 1 0.2071 -1 -7 1 0.0482 1 7 -1 0.0482 0 2 21 0.0197 0 -2 -21 0.0197 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 O1A C2A C3A 122.1(3) . . ? O1A C2A C7A 120.4(3) . . ? C3A C2A C7A 117.5(2) . . ? C2A C3A H3A 119.1 . . ? C4A C3A C2A 121.8(3) . . ? C4A C3A H3A 119.1 . . ? C3A C4A H4A 117.6 . . ? C3A C4A C5A 124.8(3) . . ? C5A C4A H4A 117.6 . . ? C4A C5A C6A 111.3(2) . . ? C4A C5A C8A 111.0(2) . . ? C4A C5A C13A 105.7(2) . . ? C6A C5A C8A 115.0(2) . . ? C13A C5A C6A 100.0(2) . . ? C13A C5A C8A 113.1(2) . . ? C5A C6A H6A 109.5 . . ? C7A C6A C5A 116.3(2) . . ? C7A C6A H6A 109.5 . . ? O11A C6A C5A 105.5(2) . . ? O11A C6A H6A 109.5 . . ? O11A C6A C7A 106.4(2) . . ? C2A C7A C6A 111.5(2) . . ? C2A C7A H7AA 109.3 . . ? C2A C7A H7AB 109.3 . . ? C6A C7A H7AA 109.3 . . ? C6A C7A H7AB 109.3 . . ? H7AA C7A H7AB 108.0 . . ? C5A C8A H8AA 108.6 . . ? C5A C8A H8AB 108.6 . . ? H8AA C8A H8AB 107.6 . . ? C9A C8A C5A 114.7(2) . . ? C9A C8A H8AA 108.6 . . ? C9A C8A H8AB 108.6 . . ? C8A C9A H9A 117.5 . . ? C10A C9A C8A 125.0(3) . . ? C10A C9A H9A 117.5 . . ? C9A C10A H10A 120.0 . . ? C9A C10A H10B 120.0 . . ? H10A C10A H10B 120.0 . . ? C12A O11A C6A 106.22(19) . . ? O11A C12A C13A 113.0(2) . . ? O11A C12A C17A 124.0(2) . . ? C17A C12A C13A 122.9(2) . . ? C12A C13A C5A 108.0(2) . . ? C14A C13A C5A 131.5(2) . . ? C14A C13A C12A 120.2(3) . . ? C13A C14A H14A 120.4 . . ? C13A C14A C15A 119.1(3) . . ? C15A C14A H14A 120.4 . . ? C14A C15A C18A 120.4(3) . . ? C14A C15A C18B 118.7(11) . . ? C16A C15A C14A 119.0(3) . . ? C16A C15A C18A 120.4(3) . . ? C16A C15A C18B 120.3(11) . . ? C15A C16A H16A 118.5 . . ? C15A C16A C17A 123.1(3) . . ? C17A C16A H16A 118.5 . . ? C12A C17A C16A 115.6(2) . . ? C12A C17A C21A 122.2(2) . . ? C16A C17A C21A 122.1(2) . . ? C15A C18A H18A 108.9 . . ? C15A C18A H18B 108.9 . . ? H18A C18A H18B 107.7 . . ? C19A C18A C15A 113.3(3) . . ? C19A C18A H18A 108.9 . . ? C19A C18A H18B 108.9 . . ? C18A C19A H19A 117.2 . . ? C20A C19A C18A 125.5(5) . . ? C20A C19A H19A 117.2 . . ? C19A C20A H20A 120.0 . . ? C19A C20A H20B 120.0 . . ? H20A C20A H20B 120.0 . . ? C22A C21A C17A 122.6(2) . . ? C22A C21A C26A 118.2(2) . . ? C26A C21A C17A 119.2(2) . . ? C23A C22A C21A 120.5(2) . . ? O27A C22A C21A 123.4(2) . . ? O27A C22A C23A 116.0(2) . . ? C22A C23A H23A 119.9 . . ? C24A C23A C22A 120.2(3) . . ? C24A C23A H23A 119.9 . . ? C23A C24A H24A 119.8 . . ? C23A C24A C25A 120.3(3) . . ? C25A C24A H24A 119.8 . . ? C24A C25A C28A 120.5(3) . . ? C26A C25A C24A 118.8(2) . . ? C26A C25A C28A 120.7(3) . . ? C21A C26A H26A 119.0 . . ? C25A C26A C21A 121.9(3) . . ? C25A C26A H26A 119.0 . . ? C22A O27A H27A 109.5 . . ? C25A C28A H28A 109.4 . . ? C25A C28A H28B 109.4 . . ? H28A C28A H28B 108.0 . . ? C29A C28A C25A 111.2(2) . . ? C29A C28A H28A 109.4 . . ? C29A C28A H28B 109.4 . . ? C28A C29A H29A 117.8 . . ? C30A C29A C28A 124.3(3) . . ? C30A C29A H29A 117.8 . . ? C29A C30A H30A 120.0 . . ? C29A C30A H30B 120.0 . . ? H30A C30A H30B 120.0 . . ? O1B C2B C3B 121.2(2) . . ? O1B C2B C7B 121.3(3) . . ? C3B C2B C7B 117.3(2) . . ? C2B C3B H3B 119.0 . . ? C4B C3B C2B 122.1(3) . . ? C4B C3B H3B 119.0 . . ? C3B C4B H4B 117.2 . . ? C3B C4B C5B 125.5(3) . . ? C5B C4B H4B 117.2 . . ? C4B C5B C6B 112.5(2) . . ? C4B C5B C8B 111.3(2) . . ? C4B C5B C13B 106.5(2) . . ? C6B C5B C8B 112.9(2) . . ? C13B C5B C6B 100.6(2) . . ? C13B C5B C8B 112.4(2) . . ? C5B C6B H6B 108.6 . . ? C7B C6B C5B 116.3(2) . . ? C7B C6B H6B 108.6 . . ? O11B C6B C5B 106.4(2) . . ? O11B C6B H6B 108.6 . . ? O11B C6B C7B 108.14(19) . . ? C2B C7B C6B 114.3(2) . . ? C2B C7B H7BA 108.7 . . ? C2B C7B H7BB 108.7 . . ? C6B C7B H7BA 108.7 . . ? C6B C7B H7BB 108.7 . . ? H7BA C7B H7BB 107.6 . . ? C5B C8B H8BA 109.0 . . ? C5B C8B H8BB 109.0 . . ? H8BA C8B H8BB 107.8 . . ? C9B C8B C5B 113.0(2) . . ? C9B C8B H8BA 109.0 . . ? C9B C8B H8BB 109.0 . . ? C8B C9B H9B 117.7 . . ? C10B C9B C8B 124.5(3) . . ? C10B C9B H9B 117.7 . . ? C9B C10B H10C 120.0 . . ? C9B C10B H10D 120.0 . . ? H10C C10B H10D 120.0 . . ? C12B O11B C6B 106.51(18) . . ? O11B C12B C13B 112.9(2) . . ? O11B C12B C17B 124.9(2) . . ? C17B C12B C13B 122.2(2) . . ? C12B C13B C5B 108.4(2) . . ? C14B C13B C5B 130.9(2) . . ? C14B C13B C12B 120.7(2) . . ? C13B C14B H14B 120.3 . . ? C13B C14B C15B 119.5(3) . . ? C15B C14B H14B 120.3 . . ? C14B C15B C3 120.5(3) . . ? C16B C15B C14B 118.6(3) . . ? C16B C15B C3 120.8(3) . . ? C15B C16B H16B 118.4 . . ? C15B C16B C17B 123.2(3) . . ? C17B C16B H16B 118.4 . . ? C12B C17B C16B 115.8(2) . . ? C12B C17B C21B 124.2(2) . . ? C16B C17B C21B 120.1(2) . . ? C15B C3 H3C 108.7 . . ? C15B C3 H3D 108.7 . . ? H3C C3 H3D 107.6 . . ? C1 C3 C15B 114.1(2) . . ? C1 C3 H3C 108.7 . . ? C1 C3 H3D 108.7 . . ? C3 C1 H1 116.5 . . ? C2 C1 C3 127.0(3) . . ? C2 C1 H1 116.5 . . ? C1 C2 H2A 120.0 . . ? C1 C2 H2B 120.0 . . ? H2A C2 H2B 120.0 . . ? C22B C21B C17B 123.0(2) . . ? C26B C21B C17B 119.4(2) . . ? C26B C21B C22B 117.5(2) . . ? C23B C22B C21B 120.1(2) . . ? O27B C22B C21B 124.9(2) . . ? O27B C22B C23B 114.9(2) . . ? C22B C23B H23B 119.7 . . ? C24B C23B C22B 120.6(3) . . ? C24B C23B H23B 119.7 . . ? C23B C24B H24B 119.7 . . ? C25B C24B C23B 120.7(3) . . ? C25B C24B H24B 119.7 . . ? C24B C25B C26B 118.0(3) . . ? C24B C25B C28B 121.5(3) . . ? C26B C25B C28B 120.5(3) . . ? C21B C26B H26B 118.4 . . ? C25B C26B C21B 123.2(3) . . ? C25B C26B H26B 118.4 . . ? C22B O27B H27B 109.5 . . ? C25B C28B H28C 109.2 . . ? C25B C28B H28D 109.2 . . ? H28C C28B H28D 107.9 . . ? C29B C28B C25B 111.8(2) . . ? C29B C28B H28C 109.2 . . ? C29B C28B H28D 109.2 . . ? C28B C29B H29B 118.5 . . ? C30B C29B C28B 123.0(4) . . ? C30B C29B H29B 118.5 . . ? C29B C30B H30C 120.0 . . ? C29B C30B H30D 120.0 . . ? H30C C30B H30D 120.0 . . ? C20B C19B H19B 116.6 . . ? C20B C19B C18B 127(3) . . ? C18B C19B H19B 116.6 . . ? C19B C20B H20C 120.0 . . ? C19B C20B H20D 120.0 . . ? H20C C20B H20D 120.0 . . ? C15A C18B H18C 109.4 . . ? C15A C18B H18D 109.4 . . ? C19B C18B C15A 111.2(17) . . ? C19B C18B H18C 109.4 . . ? C19B C18B H18D 109.4 . . ? H18C C18B H18D 108.0 . . ? 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 O1A C2A 1.233(3) . ? C2A C3A 1.456(4) . ? C2A C7A 1.500(4) . ? C3A H3A 0.9500 . ? C3A C4A 1.337(4) . ? C4A H4A 0.9500 . ? C4A C5A 1.512(4) . ? C5A C6A 1.542(4) . ? C5A C8A 1.547(4) . ? C5A C13A 1.515(4) . ? C6A H6A 1.0000 . ? C6A C7A 1.511(4) . ? C6A O11A 1.472(3) . ? C7A H7AA 0.9900 . ? C7A H7AB 0.9900 . ? C8A H8AA 0.9900 . ? C8A H8AB 0.9900 . ? C8A C9A 1.477(4) . ? C9A H9A 0.9500 . ? C9A C10A 1.301(4) . ? C10A H10A 0.9500 . ? C10A H10B 0.9500 . ? O11A C12A 1.366(3) . ? C12A C13A 1.387(4) . ? C12A C17A 1.382(4) . ? C13A C14A 1.385(4) . ? C14A H14A 0.9500 . ? C14A C15A 1.395(4) . ? C15A C16A 1.392(4) . ? C15A C18A 1.526(5) . ? C15A C18B 1.519(16) . ? C16A H16A 0.9500 . ? C16A C17A 1.403(4) . ? C17A C21A 1.483(4) . ? C18A H18A 0.9900 . ? C18A H18B 0.9900 . ? C18A C19A 1.496(7) . ? C19A H19A 0.9500 . ? C19A C20A 1.299(6) . ? C20A H20A 0.9500 . ? C20A H20B 0.9500 . ? C21A C22A 1.392(4) . ? C21A C26A 1.403(4) . ? C22A C23A 1.391(4) . ? C22A O27A 1.374(3) . ? C23A H23A 0.9500 . ? C23A C24A 1.387(4) . ? C24A H24A 0.9500 . ? C24A C25A 1.396(4) . ? C25A C26A 1.382(4) . ? C25A C28A 1.514(4) . ? C26A H26A 0.9500 . ? O27A H27A 0.8400 . ? C28A H28A 0.9900 . ? C28A H28B 0.9900 . ? C28A C29A 1.506(4) . ? C29A H29A 0.9500 . ? C29A C30A 1.310(5) . ? C30A H30A 0.9500 . ? C30A H30B 0.9500 . ? O1B C2B 1.229(3) . ? C2B C3B 1.463(4) . ? C2B C7B 1.502(4) . ? C3B H3B 0.9500 . ? C3B C4B 1.330(4) . ? C4B H4B 0.9500 . ? C4B C5B 1.502(4) . ? C5B C6B 1.542(4) . ? C5B C8B 1.543(3) . ? C5B C13B 1.522(4) . ? C6B H6B 1.0000 . ? C6B C7B 1.515(4) . ? C6B O11B 1.470(3) . ? C7B H7BA 0.9900 . ? C7B H7BB 0.9900 . ? C8B H8BA 0.9900 . ? C8B H8BB 0.9900 . ? C8B C9B 1.493(4) . ? C9B H9B 0.9500 . ? C9B C10B 1.305(4) . ? C10B H10C 0.9500 . ? C10B H10D 0.9500 . ? O11B C12B 1.373(3) . ? C12B C13B 1.391(4) . ? C12B C17B 1.387(4) . ? C13B C14B 1.380(4) . ? C14B H14B 0.9500 . ? C14B C15B 1.398(4) . ? C15B C16B 1.392(4) . ? C15B C3 1.511(4) . ? C16B H16B 0.9500 . ? C16B C17B 1.410(4) . ? C17B C21B 1.495(4) . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C3 C1 1.510(4) . ? C1 H1 0.9500 . ? C1 C2 1.308(5) . ? C2 H2A 0.9500 . ? C2 H2B 0.9500 . ? C21B C22B 1.399(4) . ? C21B C26B 1.396(4) . ? C22B C23B 1.393(4) . ? C22B O27B 1.361(3) . ? C23B H23B 0.9500 . ? C23B C24B 1.386(4) . ? C24B H24B 0.9500 . ? C24B C25B 1.386(4) . ? C25B C26B 1.386(4) . ? C25B C28B 1.518(4) . ? C26B H26B 0.9500 . ? O27B H27B 0.8400 . ? C28B H28C 0.9900 . ? C28B H28D 0.9900 . ? C28B C29B 1.489(4) . ? C29B H29B 0.9500 . ? C29B C30B 1.316(5) . ? C30B H30C 0.9500 . ? C30B H30D 0.9500 . ? C19B H19B 0.9500 . ? C19B C20B 1.295(19) . ? C19B C18B 1.462(18) . ? C20B H20C 0.9500 . ? C20B H20D 0.9500 . ? C18B H18C 0.9900 . ? C18B H18D 0.9900 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O27A H27A O1B 0.84 2.21 2.907(3) 140.3 . yes O27B H27B O1A 0.84 2.01 2.662(3) 134.0 1_455 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1A C2A C3A C4A 171.6(3) . . . . ? O1A C2A C7A C6A -145.4(3) . . . . ? C2A C3A C4A C5A -6.1(4) . . . . ? C3A C2A C7A C6A 37.0(3) . . . . ? C3A C4A C5A C6A -4.9(4) . . . . ? C3A C4A C5A C8A 124.6(3) . . . . ? C3A C4A C5A C13A -112.5(3) . . . . ? C4A C5A C6A C7A 32.7(3) . . . . ? C4A C5A C6A O11A -84.9(2) . . . . ? C4A C5A C8A C9A -51.1(4) . . . . ? C4A C5A C13A C12A 96.1(3) . . . . ? C4A C5A C13A C14A -77.5(3) . . . . ? C5A C6A C7A C2A -48.5(3) . . . . ? C5A C6A O11A C12A -24.7(2) . . . . ? C5A C8A C9A C10A 112.4(4) . . . . ? C5A C13A C14A C15A 171.9(3) . . . . ? C6A C5A C8A C9A 76.4(3) . . . . ? C6A C5A C13A C12A -19.6(3) . . . . ? C6A C5A C13A C14A 166.9(3) . . . . ? C6A O11A C12A C13A 12.4(3) . . . . ? C6A O11A C12A C17A -170.5(2) . . . . ? C7A C2A C3A C4A -10.9(4) . . . . ? C7A C6A O11A C12A -148.8(2) . . . . ? C8A C5A C6A C7A -94.6(3) . . . . ? C8A C5A C6A O11A 147.7(2) . . . . ? C8A C5A C13A C12A -142.4(2) . . . . ? C8A C5A C13A C14A 44.1(4) . . . . ? O11A C6A C7A C2A 68.6(3) . . . . ? O11A C12A C13A C5A 5.4(3) . . . . ? O11A C12A C13A C14A 179.9(2) . . . . ? O11A C12A C17A C16A -179.0(2) . . . . ? O11A C12A C17A C21A -2.0(4) . . . . ? C12A C13A C14A C15A -1.0(4) . . . . ? C12A C17A C21A C22A 56.9(4) . . . . ? C12A C17A C21A C26A -122.5(3) . . . . ? C13A C5A C6A C7A 144.0(2) . . . . ? C13A C5A C6A O11A 26.3(2) . . . . ? C13A C5A C8A C9A -169.6(3) . . . . ? C13A C12A C17A C16A -2.3(4) . . . . ? C13A C12A C17A C21A 174.7(2) . . . . ? C13A C14A C15A C16A -1.1(4) . . . . ? C13A C14A C15A C18A -175.5(3) . . . . ? C13A C14A C15A C18B 163.0(9) . . . . ? C14A C15A C16A C17A 1.6(4) . . . . ? C14A C15A C18A C19A 62.1(5) . . . . ? C14A C15A C18B C19B 83(2) . . . . ? C15A C16A C17A C12A 0.1(4) . . . . ? C15A C16A C17A C21A -176.9(2) . . . . ? C15A C18A C19A C20A 120.2(5) . . . . ? C16A C15A C18A C19A -112.2(4) . . . . ? C16A C15A C18B C19B -113.0(18) . . . . ? C16A C17A C21A C22A -126.3(3) . . . . ? C16A C17A C21A C26A 54.3(3) . . . . ? C17A C12A C13A C5A -171.6(2) . . . . ? C17A C12A C13A C14A 2.8(4) . . . . ? C17A C21A C22A C23A -179.5(2) . . . . ? C17A C21A C22A O27A 3.5(4) . . . . ? C17A C21A C26A C25A 179.0(2) . . . . ? C18A C15A C16A C17A 176.0(3) . . . . ? C21A C22A C23A C24A 0.6(4) . . . . ? C22A C21A C26A C25A -0.4(4) . . . . ? C22A C23A C24A C25A -0.7(4) . . . . ? C23A C24A C25A C26A 0.3(4) . . . . ? C23A C24A C25A C28A -177.3(3) . . . . ? C24A C25A C26A C21A 0.3(4) . . . . ? C24A C25A C28A C29A 87.7(3) . . . . ? C25A C28A C29A C30A -114.6(3) . . . . ? C26A C21A C22A C23A 0.0(4) . . . . ? C26A C21A C22A O27A -177.0(2) . . . . ? C26A C25A C28A C29A -89.8(3) . . . . ? O27A C22A C23A C24A 177.8(2) . . . . ? C28A C25A C26A C21A 177.9(3) . . . . ? O1B C2B C3B C4B -174.7(3) . . . . ? O1B C2B C7B C6B 153.0(2) . . . . ? C2B C3B C4B C5B 3.0(4) . . . . ? C3B C2B C7B C6B -31.3(3) . . . . ? C3B C4B C5B C6B 6.9(4) . . . . ? C3B C4B C5B C8B -121.0(3) . . . . ? C3B C4B C5B C13B 116.2(3) . . . . ? C4B C5B C6B C7B -29.1(3) . . . . ? C4B C5B C6B O11B 91.4(2) . . . . ? C4B C5B C8B C9B 69.5(3) . . . . ? C4B C5B C13B C12B -103.7(2) . . . . ? C4B C5B C13B C14B 73.9(3) . . . . ? C5B C6B C7B C2B 41.4(3) . . . . ? C5B C6B O11B C12B 22.4(2) . . . . ? C5B C8B C9B C10B 117.9(3) . . . . ? C5B C13B C14B C15B -176.2(3) . . . . ? C6B C5B C8B C9B -58.1(3) . . . . ? C6B C5B C13B C12B 13.8(3) . . . . ? C6B C5B C13B C14B -168.7(3) . . . . ? C6B O11B C12B C13B -13.9(3) . . . . ? C6B O11B C12B C17B 167.6(2) . . . . ? C7B C2B C3B C4B 9.5(4) . . . . ? C7B C6B O11B C12B 148.0(2) . . . . ? C8B C5B C6B C7B 98.0(3) . . . . ? C8B C5B C6B O11B -141.6(2) . . . . ? C8B C5B C13B C12B 134.2(2) . . . . ? C8B C5B C13B C14B -48.2(4) . . . . ? O11B C6B C7B C2B -78.1(3) . . . . ? O11B C12B C13B C5B -0.6(3) . . . . ? O11B C12B C13B C14B -178.5(2) . . . . ? O11B C12B C17B C16B 176.7(2) . . . . ? O11B C12B C17B C21B -2.2(4) . . . . ? C12B C13B C14B C15B 1.1(4) . . . . ? C12B C17B C21B C22B -57.7(4) . . . . ? C12B C17B C21B C26B 125.8(3) . . . . ? C13B C5B C6B C7B -142.0(2) . . . . ? C13B C5B C6B O11B -21.5(2) . . . . ? C13B C5B C8B C9B -171.2(2) . . . . ? C13B C12B C17B C16B -1.7(4) . . . . ? C13B C12B C17B C21B 179.5(2) . . . . ? C13B C14B C15B C16B -0.5(4) . . . . ? C13B C14B C15B C3 -177.2(2) . . . . ? C14B C15B C16B C17B -1.2(4) . . . . ? C14B C15B C3 C1 74.3(3) . . . . ? C15B C16B C17B C12B 2.2(4) . . . . ? C15B C16B C17B C21B -178.8(2) . . . . ? C15B C3 C1 C2 2.0(5) . . . . ? C16B C15B C3 C1 -102.3(3) . . . . ? C16B C17B C21B C22B 123.5(3) . . . . ? C16B C17B C21B C26B -53.0(3) . . . . ? C17B C12B C13B C5B 177.9(2) . . . . ? C17B C12B C13B C14B 0.1(4) . . . . ? C17B C21B C22B C23B -177.2(3) . . . . ? C17B C21B C22B O27B -1.3(4) . . . . ? C17B C21B C26B C25B 176.2(2) . . . . ? C3 C15B C16B C17B 175.5(2) . . . . ? C21B C22B C23B C24B 1.1(4) . . . . ? C22B C21B C26B C25B -0.5(4) . . . . ? C22B C23B C24B C25B -0.4(5) . . . . ? C23B C24B C25B C26B -0.6(4) . . . . ? C23B C24B C25B C28B -179.0(3) . . . . ? C24B C25B C26B C21B 1.1(4) . . . . ? C24B C25B C28B C29B 108.4(3) . . . . ? C25B C28B C29B C30B 109.9(4) . . . . ? C26B C21B C22B C23B -0.6(4) . . . . ? C26B C21B C22B O27B 175.3(2) . . . . ? C26B C25B C28B C29B -70.0(4) . . . . ? O27B C22B C23B C24B -175.2(3) . . . . ? C28B C25B C26B C21B 179.5(3) . . . . ? C20B C19B C18B C15A 3(4) . . . . ? C18B C15A C16A C17A -162.3(10) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 6.9922 -3.9979 -1.0166 -0.2626 0.9149 0.5166 -6.9978 0.9993 1.0070 0.1539 -0.5815 -0.7293 -1.0126 -6.9971 0.9781 -0.1986 0.7224 -0.6118 1.0126 6.9971 -0.9781 0.1986 -0.7224 0.6118 0.0135 1.9924 21.0070 1.0107 0.0616 0.1076 -0.0135 -1.9924 -21.0070 -1.0107 -0.0616 -0.1076