#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:38:38 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227289 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/58/4035881.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_4035881 loop_ _publ_author_name 'Ji, Kai-Long' 'Fan, Yao-Yue' 'Ge, Zhan-Peng' 'Sheng, Li' 'Xu, You-Kai' 'Gan, Li-She' 'Li, Jing-Ya' 'Yue, Jian-Min' _publ_section_title ; Maximumins A-D, Rearranged Labdane-Type Diterpenoids with Four Different Carbon Skeletons from Amomum maximum. ; _journal_issue 1 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 282 _journal_page_last 288 _journal_paper_doi 10.1021/acs.joc.8b02665 _journal_volume 84 _journal_year 2019 _chemical_absolute_configuration rmad _chemical_formula_moiety 'C19 H26 O3' _chemical_formula_sum 'C19 H26 O3' _chemical_formula_weight 302.40 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2018-04-11 _audit_creation_method ; Olex2 1.2 (compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.36880(10) _cell_length_b 12.2935(2) _cell_length_c 21.2458(4) _cell_measurement_reflns_used 7886 _cell_measurement_temperature 170(2) _cell_measurement_theta_max 54.75 _cell_measurement_theta_min 3.615 _cell_volume 1663.44(5) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 169.99 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_unetI/netI 0.0361 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 10236 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 54.847 _diffrn_reflns_theta_min 3.620 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.408 _exptl_absorpt_correction_T_max 0.7508 _exptl_absorpt_correction_T_min 0.4957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1523 before and 0.0897 after correction. The Ratio of minimum to maximum transmission is 0.6602. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.207 _exptl_crystal_description prism _exptl_crystal_F_000 656 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.162 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.054 _refine_ls_abs_structure_details ; Flack x determined using 1153 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.03(13) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 202 _refine_ls_number_reflns 3118 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.095 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0423 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.3788P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1025 _refine_ls_wR_factor_ref 0.1062 _reflns_Friedel_coverage 0.704 _reflns_Friedel_fraction_full 0.983 _reflns_Friedel_fraction_max 0.981 _reflns_number_gt 2917 _reflns_number_total 3118 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo8b02665_si_003.cif _cod_data_source_block mjl18129_0m _cod_database_code 4035881 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.996 _shelx_estimated_absorpt_t_min 0.953 _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 C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C5(H5), C8(H8) 2.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C11(H11A,H11B) 2.c Aromatic/amide H refined with riding coordinates: C14(H14), C15(H15), C16(H16) 2.d Idealised Me refined as rotating group: C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C) ; _shelx_res_file ; TITL mjl18129_0m_a.res in P2(1)2(1)2(1) mjl18129_0m.res created by SHELXL-2016/6 at 12:15:34 on 11-Apr-2018 REM Old TITL mjl18129_0m in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.112, Rweak 0.020, Alpha 0.003, Orientation as input REM Flack x = 0.231 ( 0.101 ) from Parsons' quotients REM Formula found by SHELXT: C19 O3 CELL 1.34139 6.3688 12.2935 21.2458 90 90 90 ZERR 4 0.0001 0.0002 0.0004 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H O DISP C 0.0148 0.007 57.7477 DISP H -0 0 0.6481 DISP O 0.0412 0.025 193.9543 UNIT 76 104 12 L.S. 4 PLAN 20 SIZE 0.01 0.03 0.12 TEMP -103.16 BOND $H list 4 fmap 2 ACTA OMIT 0 6 0 REM REM REM WGHT 0.052200 0.378800 FVAR 1.03004 O1 3 0.834330 0.340823 0.634912 11.00000 0.05308 0.02958 = 0.03714 0.00499 0.00488 0.00724 O2 3 0.509008 0.139601 0.595700 11.00000 0.02470 0.04732 = 0.05027 -0.00182 0.00451 -0.00113 O3 3 1.006614 0.106381 0.477716 11.00000 0.04914 0.04514 = 0.04233 -0.00206 0.01516 0.00434 C1 1 0.616133 0.127495 0.786850 11.00000 0.03317 0.02404 = 0.03741 -0.00311 0.00065 -0.00351 AFIX 23 H1A 2 0.572562 0.092705 0.746906 11.00000 -1.20000 H1B 2 0.750743 0.094380 0.800113 11.00000 -1.20000 AFIX 0 C2 1 0.449575 0.106365 0.837195 11.00000 0.03982 0.02744 = 0.03965 -0.00009 0.00321 -0.01020 AFIX 23 H2A 2 0.438956 0.027029 0.844526 11.00000 -1.20000 H2B 2 0.311812 0.131910 0.821465 11.00000 -1.20000 AFIX 0 C3 1 0.497339 0.163008 0.899783 11.00000 0.03911 0.02980 = 0.03629 0.00399 0.00511 -0.00348 AFIX 23 H3A 2 0.626487 0.131059 0.917970 11.00000 -1.20000 H3B 2 0.380728 0.148735 0.929468 11.00000 -1.20000 AFIX 0 C4 1 0.527347 0.287330 0.893432 11.00000 0.02649 0.02719 = 0.03022 -0.00252 -0.00006 -0.00171 C5 1 0.689907 0.303418 0.840998 11.00000 0.02097 0.02178 = 0.03235 -0.00143 -0.00552 -0.00067 AFIX 13 H5 2 0.817508 0.264891 0.856976 11.00000 -1.20000 AFIX 0 C6 1 0.769000 0.417714 0.825440 11.00000 0.02707 0.02324 = 0.03756 -0.00201 0.00107 -0.00202 AFIX 23 H6A 2 0.863437 0.445063 0.858899 11.00000 -1.20000 H6B 2 0.650330 0.469005 0.820435 11.00000 -1.20000 AFIX 0 C7 1 0.888761 0.403477 0.762846 11.00000 0.02301 0.02333 = 0.03952 0.00031 -0.00049 -0.00294 AFIX 23 H7A 2 1.039946 0.419213 0.768719 11.00000 -1.20000 H7B 2 0.832284 0.453354 0.730416 11.00000 -1.20000 AFIX 0 C8 1 0.856460 0.283560 0.742796 11.00000 0.01794 0.02432 = 0.03369 0.00142 -0.00172 0.00115 AFIX 13 H8 2 0.972651 0.239698 0.761720 11.00000 -1.20000 AFIX 0 C9 1 0.864093 0.267474 0.671987 11.00000 0.02060 0.02703 = 0.03642 0.00066 0.00026 0.00305 C10 1 0.647752 0.249750 0.776046 11.00000 0.01916 0.02279 = 0.03171 -0.00167 -0.00160 -0.00108 C11 1 0.919266 0.153854 0.649699 11.00000 0.02949 0.02722 = 0.03539 -0.00212 -0.00677 0.00710 AFIX 23 H11A 2 1.070103 0.140581 0.657935 11.00000 -1.20000 H11B 2 0.838010 0.100508 0.674703 11.00000 -1.20000 AFIX 0 C12 1 0.876579 0.134617 0.581216 11.00000 0.02481 0.02275 = 0.03537 0.00109 -0.00197 -0.00011 C13 1 0.659992 0.131758 0.559334 11.00000 0.02605 0.02736 = 0.03573 0.00140 -0.00160 0.00077 C14 1 0.639157 0.118191 0.491860 11.00000 0.04356 0.03291 = 0.03913 -0.00068 -0.01083 0.00030 AFIX 43 H14 2 0.503484 0.117206 0.473286 11.00000 -1.20000 AFIX 0 C15 1 0.808137 0.107121 0.455755 11.00000 0.06173 0.03660 = 0.03528 -0.00116 -0.00212 0.00394 AFIX 43 H15 2 0.787756 0.099233 0.411696 11.00000 -1.20000 AFIX 0 C16 1 1.033090 0.121237 0.540685 11.00000 0.03211 0.02965 = 0.04215 -0.00179 0.00497 0.00221 AFIX 43 H16 2 1.172409 0.122088 0.556653 11.00000 -1.20000 AFIX 0 C18 1 0.621204 0.332093 0.954742 11.00000 0.03906 0.03908 = 0.03419 -0.00330 -0.00304 -0.00099 AFIX 137 H18A 2 0.760154 0.299963 0.961603 11.00000 -1.50000 H18B 2 0.529008 0.313548 0.990080 11.00000 -1.50000 H18C 2 0.634362 0.411341 0.951681 11.00000 -1.50000 AFIX 0 C19 1 0.316296 0.344242 0.883064 11.00000 0.02595 0.03985 = 0.04037 -0.00462 0.00248 0.00230 AFIX 137 H19A 2 0.340697 0.420253 0.871245 11.00000 -1.50000 H19B 2 0.233882 0.341551 0.921986 11.00000 -1.50000 H19C 2 0.239237 0.307345 0.849326 11.00000 -1.50000 AFIX 0 C20 1 0.462476 0.297457 0.738983 11.00000 0.02090 0.03791 = 0.03579 -0.00097 -0.00280 0.00172 AFIX 137 H20A 2 0.330391 0.276401 0.759268 11.00000 -1.50000 H20B 2 0.465043 0.269478 0.695798 11.00000 -1.50000 H20C 2 0.473711 0.376951 0.738222 11.00000 -1.50000 AFIX 0 HKLF 4 REM mjl18129_0m_a.res in P2(1)2(1)2(1) REM R1 = 0.0423 for 2917 Fo > 4sig(Fo) and 0.0460 for all 3118 data REM 202 parameters refined using 0 restraints END WGHT 0.0521 0.3778 REM Highest difference peak 0.162, deepest hole -0.225, 1-sigma level 0.054 Q1 1 0.7433 0.2657 0.7578 11.00000 0.05 0.16 Q2 1 0.0606 0.4275 0.9784 11.00000 0.05 0.16 Q3 1 0.6597 0.1278 0.6653 11.00000 0.05 0.16 Q4 1 0.6604 0.3615 0.6554 11.00000 0.05 0.16 Q5 1 0.8191 0.2382 0.8636 11.00000 0.05 0.15 Q6 1 0.7799 0.1302 0.7069 11.00000 0.05 0.15 Q7 1 0.6577 0.1570 0.9746 11.00000 0.05 0.15 Q8 1 0.0080 0.3505 0.9343 11.00000 0.05 0.14 Q9 1 0.5869 0.3195 0.6038 11.00000 0.05 0.14 Q10 1 0.8678 0.1193 0.7987 11.00000 0.05 0.14 Q11 1 0.9161 0.1239 0.8071 11.00000 0.05 0.14 Q12 1 0.1548 0.2547 0.8753 11.00000 0.05 0.14 Q13 1 0.3693 0.1398 0.5694 11.00000 0.05 0.14 Q14 1 1.0611 0.2175 0.8195 11.00000 0.05 0.14 Q15 1 0.5612 0.2791 0.7634 11.00000 0.05 0.14 Q16 1 0.8723 0.3531 0.9617 11.00000 0.05 0.14 Q17 1 1.0904 0.1639 0.6940 11.00000 0.05 0.13 Q18 1 1.0125 0.2513 0.8935 11.00000 0.05 0.13 Q19 1 0.9146 0.1221 0.4119 11.00000 0.05 0.13 Q20 1 0.3202 0.2217 0.4786 11.00000 0.05 0.13 ; _shelx_res_checksum 17302 _shelx_hkl_file ; 1 0 0 -0.0101 0.54506 6 -1 0 0 0.29159 0.67917 6 -2 0 0 2397.12 96.4250 6 -2 0 0 2052.57 96.6100 1 -3 0 0 0.11057 1.13319 6 -3 0 0 -1.5275 1.38224 1 -4 0 0 271.053 14.3763 1 -4 0 0 298.200 13.7488 6 -5 0 0 -0.5721 1.43195 6 5 0 0 3.59569 2.14923 3 -5 0 0 1.20760 2.07026 1 6 0 0 981.253 47.2908 3 -6 0 0 1077.31 47.7480 1 -7 0 0 1.51985 2.33396 1 0 -1 0 0.00727 0.33333 3 1 -1 0 13.3047 1.22909 6 -1 1 0 12.9297 1.43110 6 1 1 0 14.4300 1.19786 3 -1 -1 0 14.8516 1.28682 6 1 1 0 12.7229 1.25179 6 -2 1 0 913.146 38.9528 6 -2 -1 0 862.005 39.1903 1 -3 1 0 -0.2321 1.21973 6 -3 1 0 1.06741 1.46837 1 -3 -1 0 0.54777 1.03629 6 -3 -1 0 0.46414 1.70483 1 4 -1 0 24.1734 3.57311 3 -4 1 0 27.1609 2.91778 6 -4 1 0 22.5219 3.27312 1 -4 -1 0 32.2364 2.86499 6 -4 -1 0 29.0898 3.65417 1 -5 1 0 119.832 6.91271 6 5 -1 0 100.599 7.59103 3 -5 -1 0 116.145 7.90474 1 -5 1 0 109.813 7.82891 1 -6 1 0 0.76306 2.69400 1 -6 -1 0 1.78506 2.41235 1 -6 1 0 2.77795 2.04282 6 6 -1 0 2.08459 2.86563 3 -7 -1 0 3.69335 2.37741 1 -7 1 0 0.24298 2.23423 1 -1 2 0 162.205 7.58767 6 -2 2 0 113.397 6.06623 1 -2 -2 0 110.194 6.10070 1 -3 2 0 317.311 15.4820 1 -3 -2 0 317.250 15.3163 1 -4 2 0 227.886 11.9536 1 -4 -2 0 216.215 11.7836 1 -4 2 0 225.439 11.3520 6 -5 -2 0 27.4468 3.90261 1 -5 2 0 30.2514 3.60225 6 5 -2 0 28.1210 4.10304 3 -6 2 0 316.251 17.6524 1 -6 2 0 336.539 16.7503 6 6 -2 0 333.773 17.8512 3 -6 -2 0 340.302 17.6110 1 -7 2 0 146.868 9.59317 1 -7 -2 0 144.467 9.35146 1 0 -3 0 2.60549 0.83364 5 0 -3 0 2.51827 1.04879 3 1 3 0 80.2143 4.12189 3 -1 -3 0 76.5382 4.39199 1 -1 -3 0 74.8242 3.98902 5 -2 -3 0 22.1544 2.80099 1 -2 3 0 29.9930 2.76179 6 -2 -3 0 30.5340 2.40126 5 -2 3 0 29.3301 2.96398 1 -3 -3 0 24.8503 3.12371 1 -3 3 0 26.6603 3.25495 1 3 -3 0 31.9219 3.84447 3 -3 3 0 26.7484 3.03611 6 -4 -3 0 80.9303 5.86548 1 4 -3 0 79.6138 6.44815 3 -4 3 0 81.7747 7.11871 6 -4 3 0 78.8505 5.98008 1 5 -3 0 5.60758 2.92537 3 -5 -3 0 0.08895 1.88941 1 -5 3 0 3.61335 2.06532 6 -5 3 0 2.44482 2.22004 1 -6 3 0 57.4052 5.21745 6 6 -3 0 60.6179 6.50723 3 6 -3 0 49.4668 3.54081 5 -6 3 0 55.9629 6.01636 1 -6 -3 0 44.6827 5.42317 1 -7 3 0 16.3454 5.49802 1 -7 -3 0 8.24463 2.78137 1 -1 -4 0 622.143 27.0569 1 -1 4 0 627.162 26.9471 6 -1 -4 0 568.081 26.7047 5 -2 -4 0 1033.85 48.1603 1 -2 4 0 1121.32 48.2123 6 -2 4 0 1116.43 48.4675 1 -2 -4 0 1091.76 47.8145 5 -3 4 0 5.10275 1.74898 6 -3 -4 0 1.67635 1.72915 1 3 -4 0 8.84898 2.42180 3 -4 4 0 23.7915 3.82902 1 4 -4 0 22.8781 3.63049 3 -4 4 0 22.9257 3.25336 6 -4 -4 0 28.3465 3.93682 1 -5 4 0 33.0569 4.29090 6 5 -4 0 28.2165 4.80762 3 -5 -4 0 32.4496 4.44232 1 5 -4 0 32.6043 2.86983 5 -5 4 0 38.4649 5.13944 1 -6 4 0 14.0682 3.12649 6 6 -4 0 19.9147 2.19830 5 7 -4 0 195.039 10.2557 2 -7 -4 0 217.040 13.4978 1 -1 -5 0 2318.60 100.290 5 -1 -5 0 2325.02 99.9156 2 1 -5 0 2290.58 100.293 5 2 -5 0 10.6957 2.43698 3 -2 -5 0 8.07552 1.97602 1 2 -5 0 9.77253 1.42275 5 -2 5 0 8.95861 1.66683 6 -2 -5 0 6.06021 1.56189 5 -3 -5 0 1.29855 1.75820 1 -3 5 0 1.88473 1.92668 1 -3 5 0 4.82075 2.01116 6 3 -5 0 2.90309 1.10339 5 -3 -5 0 1.73419 1.32568 5 3 -5 0 1.29737 2.20122 3 -4 -5 0 20.7121 3.18790 1 -4 5 0 20.3047 3.49142 1 4 -5 0 17.1064 3.66449 3 -4 5 0 26.9735 3.79875 6 -5 5 0 894.102 43.1814 6 5 -5 0 936.198 41.5748 5 -5 5 0 907.059 43.7736 1 5 -5 0 969.188 44.5437 3 -5 -5 0 968.863 43.1924 1 -6 -5 0 17.4951 3.68168 1 -6 5 0 21.5765 5.04083 6 6 -5 0 27.5631 6.47267 3 6 -5 0 23.4808 2.62192 5 -6 5 0 21.4473 4.32697 1 7 -5 0 0.07239 1.77249 2 -1 -6 0 721.270 31.9342 5 -1 6 0 745.490 32.1555 6 -1 -6 0 716.183 31.4383 2 1 -6 0 683.294 31.7257 5 2 -6 0 61.3314 5.28284 3 -2 -6 0 67.9914 4.21144 3 -2 6 0 72.1343 4.86041 6 -2 -6 0 64.2778 4.41095 5 2 -6 0 60.8811 3.93522 5 -3 -6 0 57.8757 4.24596 5 -3 6 0 50.0273 5.08902 1 -3 -6 0 57.4409 4.86118 1 -3 6 0 52.3778 4.79263 6 3 -6 0 49.4892 3.63928 5 3 -6 0 53.9222 5.45911 3 -4 -6 0 1.14298 2.37356 1 4 -6 0 2.54852 1.31892 5 -4 6 0 0.32925 2.18506 6 4 -6 0 1.10734 2.66924 3 -4 6 0 0.04383 2.17260 1 -5 6 0 37.3153 5.16619 1 5 -6 0 42.8650 3.64983 5 -5 6 0 40.2104 5.28778 6 5 -6 0 35.1850 5.30576 3 -6 6 0 19.3824 3.95609 1 -6 6 0 14.3100 3.51212 6 6 -6 0 19.2492 6.57314 3 7 -6 0 3.94718 1.98248 2 -1 7 0 2193.85 93.4515 6 -1 -7 0 2168.56 93.2451 5 1 -7 0 2076.39 93.7659 3 -1 -7 0 2159.98 92.6508 2 1 -7 0 2081.35 93.0193 5 -2 7 0 12.9665 2.80049 6 -2 -7 0 15.9501 2.17251 3 2 -7 0 13.9548 2.03360 5 -2 -7 0 16.4059 2.51477 5 3 -7 0 110.527 6.21309 5 3 -7 0 101.849 8.10405 3 -3 7 0 106.650 7.41000 6 -3 7 0 122.475 9.98201 1 4 -7 0 1.55498 2.84807 3 -4 7 0 6.99145 2.96301 1 -4 7 0 4.93113 2.83220 6 5 -7 0 154.899 8.89085 5 -5 7 0 167.753 11.2733 1 5 -7 0 179.773 11.9662 3 -5 7 0 161.574 10.8316 6 -6 7 0 8.42904 3.69838 1 0 -8 0 2808.35 121.024 2 0 -8 0 2813.97 121.797 3 0 -8 0 2749.76 121.517 5 -1 -8 0 134.564 7.10728 3 1 -8 0 120.450 6.92340 5 -1 -8 0 120.031 7.12281 5 -1 8 0 120.635 7.27805 6 1 -8 0 116.182 7.73437 3 -2 8 0 232.638 12.7257 6 2 -8 0 245.123 13.4060 3 -2 -8 0 236.515 12.0060 3 2 -8 0 255.550 12.1159 5 -3 8 0 805.610 39.1015 6 3 -8 0 874.783 37.9303 5 -3 8 0 900.482 40.1841 1 3 -8 0 791.190 39.4964 3 -4 8 0 327.942 18.0818 6 4 -8 0 342.703 18.7065 3 4 -8 0 342.684 16.3356 5 -4 8 0 328.111 18.5424 1 -5 8 0 703.436 35.8167 1 5 -8 0 789.166 37.0851 3 -5 8 0 717.891 35.9852 6 5 -8 0 744.342 33.6600 5 -6 8 0 58.3941 7.35028 1 6 -8 0 62.5208 4.99844 5 6 -8 0 75.3326 5.41339 2 0 -9 0 3.78305 1.38902 2 0 -9 0 0.97255 1.76867 5 0 -9 0 1.48714 1.66890 3 0 9 0 0.14236 1.67288 6 -1 9 0 32.4255 3.98556 6 1 -9 0 41.0388 3.71596 5 1 -9 0 42.9481 4.24825 2 -1 -9 0 38.3560 3.80447 3 -1 -9 0 34.3840 2.96747 2 -1 -9 0 43.9435 4.27767 5 1 -9 0 39.3756 4.76356 3 -2 9 0 35.9141 4.43238 6 -2 -9 0 32.9781 3.65461 3 -2 -9 0 36.5176 4.08518 5 2 -9 0 45.5330 5.49410 3 2 -9 0 42.7138 4.02180 5 3 -9 0 85.8407 7.74276 3 -3 -9 0 91.0949 6.42815 5 -3 9 0 92.2723 8.41660 1 -3 9 0 85.5534 7.17614 6 4 -9 0 14.2126 2.69993 5 4 -9 0 8.08779 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13.7812 1 -4 -1 -4 271.578 15.2130 6 4 -1 4 268.675 13.5803 3 -4 1 -4 266.717 13.7599 1 4 -1 -4 291.613 12.6745 5 -4 -1 4 298.771 15.0554 1 -4 1 -4 304.317 15.3198 6 5 -1 4 21.9408 2.98418 3 -5 1 4 24.1455 2.86250 6 -5 1 4 24.0102 4.80526 1 -5 1 -4 21.3149 3.11362 6 5 -1 -4 24.9450 2.30946 2 -5 1 -4 18.7972 2.78488 1 -5 -1 4 20.8165 4.14283 1 -6 -1 -4 122.949 7.41772 1 -6 1 4 117.351 9.23079 1 6 -1 -4 105.735 8.82787 3 -6 -1 4 121.107 9.11939 1 -6 1 -4 103.385 7.15619 1 -7 -1 4 23.5035 4.05292 1 0 2 -4 358.846 15.7804 6 0 -2 -4 340.841 15.9045 5 0 2 -4 353.787 16.0981 4 0 -2 -4 377.886 16.0760 2 -1 -2 -4 770.251 34.6940 5 1 -2 4 751.095 34.5577 3 -1 2 4 843.620 35.1069 1 -1 -2 -4 837.607 34.7317 2 1 -2 -4 808.302 34.4339 2 -1 2 -4 778.393 34.6850 6 1 -2 -4 743.931 34.3574 5 -2 -2 -4 622.728 26.0661 5 -2 -2 -4 569.713 25.7239 1 -2 2 4 580.336 26.4955 1 -2 -2 -4 579.580 25.9567 2 -2 2 4 606.037 25.7586 6 -2 -2 4 550.557 26.3474 1 2 -2 -4 549.743 25.3611 5 -2 2 -4 585.146 26.0670 6 -3 -2 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120.202 8.92484 1 -5 4 -4 119.020 8.31385 6 5 -4 -4 117.809 6.76110 5 5 -4 -4 130.071 7.15158 2 6 -4 4 33.2197 3.60355 5 -6 4 4 40.4125 4.69794 6 -6 4 -4 32.1143 4.54343 6 6 -4 -4 43.9685 3.78406 2 -6 -4 4 31.6436 4.87848 1 6 -4 -4 41.2551 6.19103 3 -7 4 4 57.0753 6.42447 1 -7 -4 4 70.7503 7.45853 1 0 -5 -4 61.2568 3.67082 2 0 -5 4 63.9857 4.02967 3 0 5 -4 61.5790 3.67233 6 0 -5 4 64.1577 3.54932 5 0 -5 -4 63.6073 3.96129 5 1 -5 4 10.0110 1.91536 3 1 5 -4 6.52160 1.35020 4 -1 -5 -4 7.19017 1.50834 2 -1 -5 -4 9.17109 1.88842 5 1 -5 -4 4.59198 1.95755 3 -1 -5 4 5.25846 1.77272 1 -1 -5 4 7.54639 1.22964 5 1 -5 -4 5.41100 1.24192 2 1 -5 -4 6.12129 1.31175 5 -1 -5 4 7.17864 1.69371 3 -1 5 -4 6.93743 1.72676 6 -2 -5 -4 1387.83 61.6844 2 2 -5 4 1360.78 62.1555 3 -2 -5 -4 1457.20 62.0433 5 -2 -5 4 1454.37 61.4329 5 2 -5 -4 1417.11 61.4910 5 -2 -5 4 1407.51 62.2906 1 -2 5 -4 1375.04 62.1785 6 -3 5 4 176.030 10.3994 1 -3 5 4 176.257 9.31143 6 -3 -5 -4 172.795 9.09712 5 3 -5 4 161.516 9.36176 3 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5 -2 6 -4 524.071 25.7212 6 -2 -6 4 573.615 25.0810 5 -2 -6 4 562.900 25.6245 3 2 -6 -4 534.205 25.0538 5 3 -6 4 358.973 17.5690 3 -3 -6 -4 357.403 17.1289 5 -3 6 -4 330.151 17.3798 6 3 -6 -4 359.366 16.2796 5 -3 -6 4 337.377 15.9095 5 -3 6 -4 337.835 17.0617 1 -3 -6 4 360.882 17.5302 1 -4 6 4 108.755 8.93725 1 4 -6 4 103.686 7.69092 3 -4 6 4 105.888 7.48488 6 4 -6 -4 104.669 5.95224 5 -4 6 -4 97.7333 7.50553 6 -4 6 -4 90.9419 6.69238 1 -4 -6 4 104.509 7.64357 1 4 -6 -4 104.225 8.49052 3 5 -6 4 368.472 17.2363 5 -5 6 4 340.480 18.4545 6 -5 6 4 363.925 20.3855 1 5 -6 -4 354.183 16.7913 5 -5 6 -4 324.755 18.5657 6 5 -6 -4 384.549 17.4194 2 6 -6 4 137.061 7.90526 5 6 -6 -4 141.072 8.11145 2 -6 -6 4 152.238 10.0148 1 -7 6 4 48.0009 5.80157 1 7 -6 -4 61.8023 5.86300 2 0 7 -4 999.256 46.4151 6 0 -7 -4 1105.07 46.3859 2 0 -7 -4 1015.98 46.7567 3 0 -7 4 1090.47 46.8141 3 0 -7 4 1051.69 46.3064 5 0 -7 -4 1051.31 46.6953 5 1 7 -4 444.342 19.9490 6 1 -7 4 447.017 20.7121 3 -1 -7 -4 416.707 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279.817 21.1941 1 5 -7 -4 283.509 14.4553 5 -6 7 4 11.9707 4.51881 1 6 -7 4 7.81906 2.18452 5 6 -7 -4 7.47134 2.41737 2 0 -8 4 420.173 19.5304 3 0 -8 -4 401.246 19.4173 3 0 -8 -4 421.905 18.9935 2 0 -8 4 423.059 19.0237 5 0 8 -4 384.997 19.0694 6 0 -8 -4 411.806 19.4711 5 -1 -8 -4 93.6333 5.24929 3 -1 -8 -4 92.9111 5.37080 2 1 -8 4 93.6270 6.23355 3 1 8 -4 80.2660 5.10394 6 -1 8 4 96.4451 6.18478 6 1 -8 4 80.6012 5.25161 5 -1 -8 -4 94.4669 6.37991 5 -1 -8 4 83.4070 5.35893 5 -1 -8 4 83.9391 5.84423 3 1 -8 -4 77.0622 6.33906 3 1 -8 -4 72.8747 7.46433 5 1 -8 -4 94.8895 5.47209 2 -2 8 4 67.8066 5.75155 6 -2 -8 -4 70.1725 4.74649 2 2 -8 4 71.5796 4.73828 5 -2 -8 -4 78.2630 5.79366 5 2 -8 4 74.0195 6.02932 3 -2 8 -4 71.9708 5.63665 6 2 -8 -4 74.7384 4.97566 2 -2 -8 4 69.8220 5.33030 3 2 -8 -4 73.5189 5.07891 5 -2 -8 4 70.5180 4.91650 5 2 -8 -4 62.9152 6.39829 3 -3 -8 -4 148.696 8.82142 5 3 -8 4 141.706 9.31622 3 -3 8 4 142.078 9.20340 6 3 -8 4 140.241 7.76830 5 3 -8 -4 150.700 7.95362 2 -3 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-1 -6 -20 95.0272 7.44741 2 -1 -6 -20 75.9428 6.26643 4 -1 6 20 93.3696 6.97982 1 -1 6 -20 79.3888 7.54980 4 1 -6 -20 89.9864 6.50684 4 1 -6 -20 94.2096 7.30367 2 2 6 -20 28.8319 4.24679 4 -2 -6 -20 37.4156 5.50308 2 2 -6 -20 25.4706 3.47662 4 -2 6 -20 25.3636 4.39503 4 -3 -6 -20 16.4281 4.81588 2 3 6 -20 14.3148 3.09035 4 3 -6 -20 12.5010 3.08302 4 3 -6 -20 8.11868 4.37491 2 0 -7 -20 50.5722 5.09177 4 0 7 -20 56.7313 6.61569 4 0 -7 -20 67.0770 6.40522 2 1 7 -20 12.0375 3.23560 4 -1 7 20 12.3557 3.32207 1 1 -7 20 19.5715 4.83582 5 -1 7 -20 16.2716 3.80342 4 1 -7 -20 15.6693 3.29705 4 -2 -7 -20 52.3837 6.17131 2 -2 7 20 69.2479 7.02844 1 2 7 -20 53.3352 6.31948 4 2 -7 20 58.9570 5.70272 5 2 -7 -20 61.8527 5.15797 4 2 -7 -20 53.7462 5.83012 2 -3 7 20 26.0581 4.31015 1 3 -7 -20 25.7706 3.57146 2 0 -8 -20 22.1577 3.56258 4 0 -8 -20 15.7975 3.32512 2 0 8 -20 25.1711 4.09932 4 1 8 -20 3.63933 3.16993 4 -1 8 20 13.2671 3.73647 1 -1 -8 -20 9.45438 3.18550 2 1 -8 -20 7.15677 2.53144 4 1 -8 -20 9.14565 3.26280 2 -1 8 -20 5.38037 3.39978 4 2 8 -20 12.9723 5.57779 4 2 -8 20 24.5509 2.97967 5 -2 8 20 18.9040 3.51137 1 -2 -8 -20 19.0046 3.83829 2 2 -8 -20 17.2409 2.96133 4 2 -8 -20 16.9265 3.32011 2 0 -9 -20 24.3196 3.76000 2 -1 -9 -20 36.6776 4.42997 2 1 -9 -20 34.2730 4.47132 2 0 0 -21 1.98204 3.38484 2 0 0 -21 0.58853 2.90054 4 -1 0 -21 145.518 9.73278 2 1 0 -21 141.235 9.39376 4 -1 0 -21 145.399 9.63521 4 1 0 -21 139.436 8.96899 2 2 0 -21 4.83966 2.79163 4 -2 0 -21 3.83581 3.07104 4 -3 0 21 12.2309 3.66898 1 -3 0 -21 8.55102 2.89823 4 3 0 -21 6.42407 2.76449 4 4 0 -21 -2.9529 2.28911 4 -4 0 21 0.32473 3.02787 1 0 -1 -21 182.914 11.1352 2 0 -1 -21 175.593 10.9303 4 0 1 -21 173.246 11.2086 4 0 1 -21 202.693 12.2767 2 1 1 -21 43.8427 5.42508 4 1 1 -21 39.3270 4.43420 2 -1 -1 -21 33.3389 4.99800 2 1 -1 -21 36.1334 4.85650 2 -1 1 -21 40.6707 5.37780 4 1 -1 -21 35.5508 4.77905 4 2 1 -21 20.9278 4.01849 4 2 1 -21 22.3139 3.24920 2 2 -1 -21 18.7359 3.29554 2 -2 1 -21 23.8712 4.48983 4 2 -1 -21 15.0578 3.26710 4 -3 1 21 5.73452 3.58883 1 3 1 -21 6.44910 3.07616 4 -3 -1 -21 4.85159 2.85629 4 -3 1 -21 2.97472 2.69484 4 3 -1 -21 5.01479 2.81318 4 4 1 -21 7.88709 2.80586 4 -4 -1 21 12.7922 3.38897 1 0 2 -21 19.4782 3.75859 4 0 -2 -21 21.7717 3.83163 4 0 -2 -21 23.0480 4.00515 2 -1 -2 -21 61.2893 6.22740 2 1 2 -21 51.3041 5.97770 4 -1 -2 -21 56.6835 5.69295 4 -1 2 -21 49.1924 5.95975 4 1 -2 -21 50.3210 5.48293 4 1 -2 -21 56.1960 5.66926 2 -2 -2 -21 13.7286 3.82901 2 -2 -2 -21 15.1845 3.66636 4 2 2 -21 16.2767 3.81302 4 2 -2 -21 17.1584 3.80395 4 -2 2 -21 9.83930 3.55675 4 2 -2 -21 16.8796 3.38024 2 -3 -2 -21 34.5440 4.23334 4 3 2 -21 48.0074 5.42340 4 3 -2 -21 51.9680 5.29367 4 3 -2 -21 45.0027 4.80705 2 -3 2 -21 32.2105 4.73490 4 4 2 -21 11.0397 3.04933 4 -4 2 21 17.7255 3.85321 1 -4 -2 21 16.7577 4.13005 1 4 -2 -21 20.6384 3.39276 4 0 -3 -21 19.8214 3.67983 4 0 -3 -21 15.3094 3.48709 2 1 3 -21 6.85543 3.19886 4 -1 -3 -21 2.97272 2.66174 4 -1 -3 -21 -0.7871 2.90554 2 1 -3 -21 2.58976 2.82459 2 -1 3 -21 8.57433 3.47963 4 1 -3 -21 8.13927 3.15275 4 -2 -3 -21 16.9860 3.67566 4 -2 -3 -21 17.9597 3.87398 2 2 3 -21 23.6853 4.22499 4 -2 3 -21 14.2235 3.61751 4 2 -3 -21 19.9596 3.53606 2 2 -3 -21 23.1528 3.85351 4 -3 3 21 15.5350 3.54076 1 -3 -3 -21 8.23759 4.92245 4 3 3 -21 16.7189 3.42712 4 -3 3 -21 9.18090 3.49326 4 3 -3 -21 11.2624 2.87460 2 3 -3 -21 11.9665 3.12888 4 -4 3 21 4.21844 2.89727 1 4 3 -21 0.28433 2.47307 4 4 -3 -21 3.35110 2.44516 4 0 -4 -21 19.6151 3.99603 2 0 4 -21 19.9278 4.34313 4 -1 -4 -21 26.1227 4.14688 2 -1 -4 -21 30.2356 3.95252 4 1 -4 -21 29.2550 4.38811 2 1 -4 -21 36.3580 4.42285 4 -2 -4 -21 6.01323 3.14294 2 2 4 -21 10.8777 3.33794 4 -2 -4 -21 13.5257 3.08428 4 2 -4 -21 10.3359 2.84130 2 2 -4 -21 13.9893 3.28563 4 3 4 -21 31.4118 4.55587 4 -3 4 21 24.2695 4.53553 1 3 -4 -21 27.4609 3.67123 4 3 -4 -21 34.2586 5.98458 2 -3 4 -21 19.0681 3.96259 4 -4 4 21 40.4757 5.10986 1 4 -4 -21 42.2183 4.56472 4 0 5 -21 71.0822 6.93462 4 0 -5 -21 67.7934 6.52594 2 0 -5 -21 62.2323 5.72019 4 -1 -5 -21 66.4374 6.50979 2 -1 -5 -21 44.9026 5.05479 4 1 5 -21 53.5139 6.36163 4 -1 5 -21 55.2039 6.39365 4 1 -5 -21 62.4014 5.40155 4 1 -5 -21 52.8007 5.78729 2 2 5 -21 2.07970 2.57644 4 -2 -5 -21 0.67298 2.99619 2 2 -5 -21 -2.6222 2.19328 4 -2 5 -21 -0.2829 2.54684 4 2 -5 -21 -1.7187 2.20115 2 -3 5 21 55.9452 6.31210 1 3 -5 -21 66.4109 5.52513 2 3 -5 -21 72.4067 7.48300 4 0 6 -21 39.6369 5.40688 4 0 -6 -21 40.0859 4.30426 4 1 6 -21 30.0817 4.31600 4 -1 -6 -21 40.8463 5.04691 2 -1 -6 -21 25.1187 3.77618 4 1 -6 -21 36.3340 4.80549 2 1 -6 -21 33.8356 4.04063 4 -1 6 -21 30.1534 4.47579 4 -2 6 21 79.6843 6.75635 1 -2 -6 -21 67.4656 6.74277 2 2 6 -21 70.0309 8.93023 4 2 -6 -21 77.2347 5.92681 4 -2 6 -21 64.4412 6.94485 4 2 -6 -21 70.1181 6.39583 2 3 6 -21 35.8431 4.56134 4 3 -6 -21 48.0695 4.84928 2 3 -6 -21 37.4435 4.45243 4 0 -7 -21 7.47388 4.91551 4 0 7 -21 3.69704 3.11035 4 0 -7 -21 0.74035 2.93333 2 -1 -7 -21 35.7923 4.85940 2 1 7 -21 31.6633 6.76113 4 1 -7 -21 21.7640 3.57555 2 -1 7 -21 30.6208 4.65804 4 2 7 -21 4.72443 3.03648 4 -2 7 21 10.8243 3.48025 1 -2 -7 -21 10.0775 3.38039 2 2 -7 21 9.73999 2.26332 5 2 -7 -21 3.97705 3.09961 2 0 -8 -21 55.3238 5.73479 2 0 8 -21 53.5611 5.73302 4 -1 -8 -21 1.83475 2.36804 2 1 8 -21 -2.7605 2.74051 4 1 -8 -21 -1.1712 2.39518 4 1 -8 -21 4.42641 2.75418 2 0 0 -22 23.2379 3.89736 2 0 0 -22 19.3181 3.78883 4 1 0 -22 2.54796 2.72891 4 1 0 -22 1.35531 2.24059 2 -1 0 -22 2.03141 3.05557 4 2 0 -22 12.2401 3.01115 2 2 0 -22 18.0447 3.46711 4 -2 0 -22 10.5896 3.85105 4 -3 0 -22 13.0817 3.27219 4 3 0 -22 11.2778 3.02517 4 4 0 -22 18.8159 3.34500 4 0 -1 -22 -3.8282 2.40930 4 0 1 -22 1.25668 2.65232 4 0 -1 -22 0.49122 2.68766 2 -1 -1 -22 40.5611 5.08074 4 1 1 -22 36.6557 4.72598 4 1 1 -22 32.3504 4.20974 2 -1 -1 -22 32.4312 4.42500 2 1 -1 -22 37.3099 4.58609 4 -1 1 -22 36.2383 5.21824 4 1 -1 -22 46.2923 5.07437 2 -2 -1 -22 9.27448 2.97701 4 2 1 -22 8.23244 3.36798 4 -2 1 -22 8.54777 3.23670 4 2 -1 -22 9.91442 2.65003 2 2 -1 -22 9.09598 2.94686 4 3 1 -22 31.2533 4.17053 4 3 -1 -22 31.8427 3.98697 4 -3 1 -22 24.0428 4.04513 4 4 1 -22 32.3777 3.99523 4 4 -1 -22 42.3953 4.70017 4 0 -2 -22 -1.2927 2.25895 4 0 -2 -22 2.30656 2.79096 2 0 2 -22 -0.3803 2.58551 4 -1 -2 -22 16.9661 3.31958 4 1 2 -22 10.5718 3.35325 4 1 -2 -22 18.5120 3.70368 2 1 -2 -22 12.2736 3.19214 4 -1 2 -22 15.0917 3.81627 4 -2 -2 -22 18.4148 4.30958 2 2 2 -22 16.1903 3.64043 4 2 -2 -22 15.3270 3.48388 4 -2 2 -22 14.2665 4.03453 4 3 2 -22 3.38197 2.77061 4 -3 -2 -22 6.51306 2.89205 4 3 -2 -22 -1.3962 2.57304 4 3 -2 -22 3.42680 2.52709 2 -3 2 -22 5.06867 3.23758 4 0 -3 -22 -0.1213 2.31309 4 0 -3 -22 3.23805 3.03273 2 0 3 -22 0.86953 2.80622 4 1 3 -22 49.8800 5.61958 4 -1 -3 -22 36.2591 4.50531 4 -1 -3 -22 37.8315 4.84704 2 1 -3 -22 41.8576 5.06448 4 -2 -3 -22 12.5654 3.18231 4 2 3 -22 13.8325 3.28206 4 -2 -3 -22 16.2046 3.75329 2 2 -3 -22 20.9417 3.61647 2 -2 3 -22 17.1624 4.25981 4 2 -3 -22 9.51451 2.86523 4 -3 3 -22 0.34895 3.77828 4 3 -3 -22 -2.8804 2.64260 2 0 -4 -22 7.61212 3.05011 2 0 -4 -22 6.40644 2.70073 4 -1 -4 -22 18.8722 3.84482 2 1 4 -22 14.9230 3.82780 4 1 -4 -22 15.8334 3.67967 2 -1 4 -22 13.7874 3.80136 4 1 -4 -22 11.1588 3.25164 4 2 4 -22 18.3367 3.55756 4 -2 -4 -22 26.0337 5.80934 4 2 -4 -22 11.2920 3.15857 2 -2 4 -22 17.1749 4.23560 4 2 -4 -22 17.7384 3.37283 4 3 4 -22 2.46652 2.54246 4 3 -4 -22 9.33195 2.61180 2 3 -4 -22 6.56764 2.75523 4 0 5 -22 5.63466 2.78118 4 0 -5 -22 5.21415 3.12265 2 0 -5 -22 5.31899 2.70070 4 1 5 -22 -1.0427 2.51092 4 -1 -5 -22 0.25790 2.47230 4 -1 -5 -22 2.80104 3.10126 2 -1 5 -22 -2.5885 2.40875 4 1 -5 -22 2.21358 2.50418 4 1 -5 -22 -2.1265 2.55117 2 -2 -5 -22 15.0634 3.53246 2 2 5 -22 5.87718 3.40675 4 2 -5 -22 12.6922 3.21307 4 -2 5 -22 19.9671 4.25967 4 2 -5 -22 9.79658 3.39660 2 3 5 -22 9.78297 2.84431 4 3 -5 -22 11.2994 2.71851 4 3 -5 -22 4.93916 2.62513 2 0 -6 -22 -0.3134 3.85768 4 0 -6 -22 -2.8386 2.73406 2 0 6 -22 0.79968 2.62625 4 -1 -6 -22 2.62107 3.01429 2 1 6 -22 3.91808 2.99856 4 -1 -6 -22 8.04628 3.21856 4 -1 6 -22 -2.3702 2.57418 4 1 -6 -22 2.14708 2.63881 2 1 -6 -22 3.38252 2.89188 4 2 6 -22 62.7239 5.91598 4 -2 -6 -22 72.7500 6.29855 2 -2 6 -22 66.3806 6.64728 4 2 -6 -22 60.9401 5.58871 4 2 -6 -22 78.7238 5.98539 2 0 -7 -22 -0.6437 2.60731 4 0 7 -22 2.16346 2.43257 4 -1 -7 -22 109.882 7.90358 2 1 7 -22 103.188 7.74523 4 -1 7 -22 99.7958 7.88564 4 1 -7 -22 107.440 7.02694 4 1 -7 -22 119.586 7.89939 2 0 0 -23 -3.1936 2.34209 2 0 0 -23 2.03086 2.59985 4 1 0 -23 14.0199 2.94297 2 1 0 -23 16.1769 3.75298 4 -1 0 -23 18.6028 4.07792 4 -2 0 -23 106.996 7.99343 4 -3 0 -23 18.0373 3.45952 4 0 -1 -23 0.09080 2.51804 2 0 -1 -23 2.80488 2.86814 4 -1 -1 -23 12.6378 3.35994 4 -1 -1 -23 14.2793 3.83553 2 1 1 -23 9.62156 3.24887 4 1 -1 -23 10.5708 2.93959 2 1 -1 -23 6.29491 3.29782 4 -1 1 -23 13.0400 3.51407 4 2 1 -23 6.04389 2.97989 4 -2 -1 -23 4.25034 2.76281 4 2 -1 -23 4.31537 2.70723 4 2 -1 -23 -0.5611 2.97307 2 -2 1 -23 0.22987 2.87271 4 3 1 -23 27.3219 3.96352 4 3 -1 -23 30.2242 4.18849 4 0 2 -23 1.22208 2.91603 4 0 -2 -23 0.90577 2.64803 2 0 -2 -23 5.08813 2.82983 4 1 2 -23 24.9533 4.35146 4 -1 -2 -23 29.7092 4.51476 2 -1 -2 -23 23.9245 3.96576 4 1 -2 -23 24.1482 3.91534 2 1 -2 -23 28.6475 4.17981 4 -1 2 -23 30.5849 4.66104 4 2 2 -23 -0.1754 2.46235 4 -2 -2 -23 2.46139 2.50126 4 2 -2 -23 4.43286 2.74466 2 -2 2 -23 -1.6918 2.90891 4 2 -2 -23 0.06717 2.23234 4 3 2 -23 61.0879 5.46565 4 3 -2 -23 61.7124 5.68794 4 -3 2 -23 54.5950 5.70123 4 0 3 -23 -2.1724 2.81777 4 0 -3 -23 0.68895 2.62568 4 0 -3 -23 1.73586 2.73833 2 1 3 -23 5.13879 3.27038 4 -1 -3 -23 12.2215 3.42261 2 -1 -3 -23 4.96458 2.61456 4 1 -3 -23 8.16737 2.90840 4 1 -3 -23 7.93483 2.91184 2 2 3 -23 -2.0390 2.61925 4 -2 -3 -23 3.49385 2.59929 4 -2 3 -23 -0.4976 2.76778 4 2 -3 -23 0.30576 2.28775 4 2 -3 -23 -1.5701 2.47148 2 3 3 -23 18.0571 3.29006 4 -3 3 -23 14.1679 3.48537 4 3 -3 -23 14.6273 3.19874 4 3 -3 -23 22.7998 4.93406 2 0 -4 -23 88.4352 7.01122 2 0 -4 -23 77.4941 6.35042 4 0 4 -23 83.8718 7.23119 4 1 4 -23 25.1368 4.01586 4 -1 -4 -23 27.7085 4.36996 2 -1 -4 -23 33.8099 4.54876 4 1 -4 -23 26.7148 3.59609 4 1 -4 -23 32.1674 4.55059 2 -1 4 -23 29.9293 4.69287 4 2 4 -23 53.2128 5.72608 4 2 -4 -23 61.7021 5.70049 2 2 -4 -23 63.0711 6.51833 4 0 -5 -23 -1.5073 2.72091 2 0 5 -23 2.88193 2.50671 4 -1 -5 -23 -1.2692 2.48607 4 -1 -5 -23 6.07820 3.69025 2 1 5 -23 1.11498 3.34802 4 -1 5 -23 1.31635 3.42229 4 1 -5 -23 3.20514 3.03050 4 1 -5 -23 7.62386 4.64800 2 -2 -5 -23 7.33512 2.56625 2 2 5 -23 15.1131 3.32366 4 2 -5 -23 10.8447 2.77080 4 -2 5 -23 2.92481 2.83268 4 0 6 -23 46.4850 5.50083 4 0 -6 -23 49.5241 5.34639 2 1 6 -23 0.62732 2.42649 4 -1 -6 -23 2.53790 2.71346 2 1 -6 -23 3.76122 2.18353 4 -1 6 -23 0.45391 2.49406 4 1 -6 -23 -1.8711 2.63052 2 0 0 -24 21.2291 4.13449 4 -1 0 -24 13.6405 3.42351 4 1 0 -24 22.1119 4.03829 4 -2 0 -24 82.8845 6.55884 4 2 0 -24 65.2526 7.55134 4 0 -1 -24 23.4193 3.91229 4 0 -1 -24 20.0874 3.55467 2 0 1 -24 16.8403 3.64778 4 1 1 -24 10.9885 3.35144 4 -1 -1 -24 17.2262 3.65652 4 1 -1 -24 10.1288 3.14681 4 1 -1 -24 7.94694 3.49071 2 -2 -1 -24 16.2694 3.44471 4 2 -1 -24 14.9240 3.16717 2 -2 1 -24 24.4887 4.11577 4 0 -2 -24 5.57445 3.05450 2 0 -2 -24 3.06579 2.64814 4 0 2 -24 7.63665 3.04931 4 -1 -2 -24 4.77501 2.78679 2 -1 -2 -24 7.69316 3.20342 4 1 2 -24 4.39687 2.65963 4 1 -2 -24 1.90715 2.65294 4 2 2 -24 16.9515 3.34215 4 -2 -2 -24 21.4730 3.43630 4 2 -2 -24 18.7813 3.18270 2 -2 2 -24 21.7678 4.07780 4 0 3 -24 68.3077 6.86449 4 0 -3 -24 67.7413 7.51312 4 0 -3 -24 79.5633 6.60592 2 1 3 -24 2.37981 4.20691 4 -1 -3 -24 7.24330 3.67497 2 -1 -3 -24 5.45060 2.81547 4 1 -3 -24 4.29384 2.74861 2 1 -3 -24 6.25587 4.36592 4 -1 3 -24 5.73499 3.64687 4 -2 -3 -24 26.3688 3.70111 4 2 3 -24 35.1291 4.46080 4 -2 3 -24 31.4818 4.40047 4 2 -3 -24 28.6812 3.63461 2 0 -4 -24 34.5624 4.73415 2 0 4 -24 28.0132 5.35256 4 0 -4 -24 24.7466 3.71818 4 -1 -4 -24 7.21350 3.05658 2 -1 -4 -24 4.82968 2.82172 4 1 4 -24 11.2903 3.50273 4 1 -4 -24 10.1553 3.14516 2 1 -4 -24 5.80311 2.79553 4 -1 4 -24 4.91827 3.19976 4 2 4 -24 2.66031 2.52280 4 2 -4 -24 2.50523 2.38987 4 -2 4 -24 0.68801 2.56749 4 2 -4 -24 -0.9083 2.19464 2 0 -5 -24 -0.1812 2.24962 2 0 -5 -24 -2.4964 2.11389 4 0 5 -24 -4.4251 2.22317 4 -1 -5 -24 33.2023 4.43916 2 -1 -5 -24 17.5264 3.92417 4 1 5 -24 28.4920 4.23591 4 1 -5 -24 24.6227 3.87166 2 1 -5 -24 25.3779 3.66897 4 -1 5 -24 18.9286 3.68955 4 0 0 -25 1.27290 2.66917 4 1 0 -25 2.44765 2.53068 4 -1 0 -25 3.76829 2.74218 4 -2 0 -25 3.10622 2.57049 4 2 0 -25 1.59628 2.39343 4 0 1 -25 -1.2642 2.42543 4 0 -1 -25 0.10680 2.70604 4 -1 -1 -25 13.3883 3.50077 4 1 -1 -25 11.3460 3.01181 2 -1 1 -25 15.8002 3.33898 4 0 2 -25 5.75389 3.16964 4 0 -2 -25 10.1063 2.75259 2 0 -2 -25 7.32603 2.82373 4 -1 -2 -25 32.2204 4.17865 4 1 2 -25 33.3178 4.21251 4 1 -2 -25 32.8527 3.98950 4 0 3 -25 28.7224 4.23197 4 0 -3 -25 34.2610 4.22762 2 0 -3 -25 34.0518 4.18775 4 -1 -3 -25 2.44769 2.38214 2 -1 -3 -25 8.65945 2.60379 4 1 3 -25 5.06854 2.66845 4 1 -3 -25 3.14772 2.42557 2 1 -3 -25 3.50243 2.62471 4 -1 3 -25 4.19350 2.82812 4 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7508 _exptl_absorpt_correction_T_min 0.4957 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 1.34180 6.368 12.292 21.238 90.017 90.005 89.994 ) ; _shelx_hkl_checksum 40586 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn O1 O 0.8343(3) 0.34082(14) 0.63491(8) 0.0399(5) Uani 1 1 d . O2 O 0.5090(3) 0.13960(15) 0.59570(9) 0.0408(5) Uani 1 1 d . O3 O 1.0066(3) 0.10638(16) 0.47772(9) 0.0455(5) Uani 1 1 d . C1 C 0.6161(4) 0.12749(19) 0.78685(11) 0.0315(6) Uani 1 1 d . H1A H 0.572562 0.092705 0.746906 0.038 Uiso 1 1 calc R H1B H 0.750743 0.094380 0.800113 0.038 Uiso 1 1 calc R C2 C 0.4496(4) 0.1064(2) 0.83719(12) 0.0356(6) Uani 1 1 d . H2A H 0.438956 0.027029 0.844526 0.043 Uiso 1 1 calc R H2B H 0.311812 0.131910 0.821465 0.043 Uiso 1 1 calc R C3 C 0.4973(5) 0.16301(19) 0.89978(11) 0.0351(6) Uani 1 1 d . H3A H 0.626487 0.131059 0.917970 0.042 Uiso 1 1 calc R H3B H 0.380728 0.148735 0.929468 0.042 Uiso 1 1 calc R C4 C 0.5273(4) 0.28733(18) 0.89343(11) 0.0280(5) Uani 1 1 d . C5 C 0.6899(4) 0.30342(17) 0.84100(11) 0.0250(5) Uani 1 1 d . H5 H 0.817508 0.264891 0.856976 0.030 Uiso 1 1 calc R C6 C 0.7690(4) 0.41771(18) 0.82544(12) 0.0293(5) Uani 1 1 d . H6A H 0.863437 0.445063 0.858899 0.035 Uiso 1 1 calc R H6B H 0.650330 0.469005 0.820435 0.035 Uiso 1 1 calc R C7 C 0.8888(4) 0.40348(18) 0.76285(11) 0.0286(5) Uani 1 1 d . H7A H 1.039946 0.419213 0.768719 0.034 Uiso 1 1 calc R H7B H 0.832284 0.453354 0.730416 0.034 Uiso 1 1 calc R C8 C 0.8565(4) 0.28356(17) 0.74280(11) 0.0253(5) Uani 1 1 d . H8 H 0.972651 0.239698 0.761720 0.030 Uiso 1 1 calc R C9 C 0.8641(4) 0.26747(18) 0.67199(11) 0.0280(5) Uani 1 1 d . C10 C 0.6478(4) 0.24975(17) 0.77605(10) 0.0246(5) Uani 1 1 d . C11 C 0.9193(4) 0.15385(19) 0.64970(11) 0.0307(5) Uani 1 1 d . H11A H 1.070103 0.140581 0.657935 0.037 Uiso 1 1 calc R H11B H 0.838010 0.100508 0.674703 0.037 Uiso 1 1 calc R C12 C 0.8766(4) 0.13462(18) 0.58122(11) 0.0276(5) Uani 1 1 d . C13 C 0.6600(4) 0.13176(18) 0.55933(11) 0.0297(5) Uani 1 1 d . C14 C 0.6392(5) 0.1182(2) 0.49186(12) 0.0385(6) Uani 1 1 d . H14 H 0.503484 0.117206 0.473286 0.046 Uiso 1 1 calc R C15 C 0.8081(5) 0.1071(2) 0.45576(13) 0.0445(7) Uani 1 1 d . H15 H 0.787756 0.099233 0.411696 0.053 Uiso 1 1 calc R C16 C 1.0331(4) 0.12124(19) 0.54069(12) 0.0346(6) Uani 1 1 d . H16 H 1.172409 0.122088 0.556653 0.042 Uiso 1 1 calc R C18 C 0.6212(4) 0.3321(2) 0.95474(12) 0.0374(6) Uani 1 1 d . H18A H 0.760154 0.299963 0.961603 0.056 Uiso 1 1 calc GR H18B H 0.529008 0.313548 0.990080 0.056 Uiso 1 1 calc GR H18C H 0.634362 0.411341 0.951681 0.056 Uiso 1 1 calc GR C19 C 0.3163(4) 0.3442(2) 0.88306(12) 0.0354(6) Uani 1 1 d . H19A H 0.340697 0.420253 0.871245 0.053 Uiso 1 1 calc GR H19B H 0.233882 0.341551 0.921986 0.053 Uiso 1 1 calc GR H19C H 0.239237 0.307345 0.849326 0.053 Uiso 1 1 calc GR C20 C 0.4625(4) 0.2975(2) 0.73898(12) 0.0315(5) Uani 1 1 d . H20A H 0.330391 0.276401 0.759268 0.047 Uiso 1 1 calc GR H20B H 0.465043 0.269478 0.695798 0.047 Uiso 1 1 calc GR H20C H 0.473711 0.376951 0.738222 0.047 Uiso 1 1 calc GR loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0531(12) 0.0296(8) 0.0371(9) 0.0050(7) 0.0049(9) 0.0072(9) O2 0.0247(9) 0.0473(11) 0.0503(10) -0.0018(8) 0.0045(9) -0.0011(8) O3 0.0491(12) 0.0451(11) 0.0423(10) -0.0021(8) 0.0152(10) 0.0043(10) C1 0.0332(13) 0.0240(11) 0.0374(13) -0.0031(9) 0.0007(11) -0.0035(10) C2 0.0398(15) 0.0274(12) 0.0396(14) -0.0001(10) 0.0032(12) -0.0102(11) C3 0.0391(14) 0.0298(12) 0.0363(13) 0.0040(10) 0.0051(12) -0.0035(11) C4 0.0265(12) 0.0272(11) 0.0302(11) -0.0025(9) -0.0001(10) -0.0017(10) C5 0.0210(11) 0.0218(10) 0.0324(12) -0.0014(9) -0.0055(10) -0.0007(9) C6 0.0271(13) 0.0232(11) 0.0376(13) -0.0020(10) 0.0011(10) -0.0020(9) C7 0.0230(12) 0.0233(11) 0.0395(13) 0.0003(9) -0.0005(10) -0.0029(9) C8 0.0179(11) 0.0243(11) 0.0337(12) 0.0014(9) -0.0017(10) 0.0012(8) C9 0.0206(11) 0.0270(11) 0.0364(12) 0.0007(10) 0.0003(10) 0.0031(9) C10 0.0192(11) 0.0228(10) 0.0317(12) -0.0017(9) -0.0016(10) -0.0011(9) C11 0.0295(12) 0.0272(11) 0.0354(12) -0.0021(9) -0.0068(10) 0.0071(10) C12 0.0248(12) 0.0228(10) 0.0354(12) 0.0011(9) -0.0020(10) -0.0001(9) C13 0.0261(12) 0.0274(11) 0.0357(12) 0.0014(10) -0.0016(11) 0.0008(10) C14 0.0436(16) 0.0329(12) 0.0391(14) -0.0007(11) -0.0108(13) 0.0003(12) C15 0.0617(19) 0.0366(14) 0.0353(14) -0.0012(11) -0.0021(14) 0.0039(14) C16 0.0321(13) 0.0296(12) 0.0422(13) -0.0018(10) 0.0050(12) 0.0022(11) C18 0.0391(15) 0.0391(13) 0.0342(13) -0.0033(11) -0.0030(12) -0.0010(12) C19 0.0260(12) 0.0398(13) 0.0404(14) -0.0046(11) 0.0025(11) 0.0023(11) C20 0.0209(12) 0.0379(13) 0.0358(13) -0.0010(10) -0.0028(10) 0.0017(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0148 0.0070 '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 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C15 O3 C16 117.1(2) H1A C1 H1B 108.0 C2 C1 H1A 109.4 C2 C1 H1B 109.4 C2 C1 C10 111.25(19) C10 C1 H1A 109.4 C10 C1 H1B 109.4 C1 C2 H2A 109.0 C1 C2 H2B 109.0 C1 C2 C3 113.1(2) H2A C2 H2B 107.8 C3 C2 H2A 109.0 C3 C2 H2B 109.0 C2 C3 H3A 108.9 C2 C3 H3B 108.9 C2 C3 C4 113.47(19) H3A C3 H3B 107.7 C4 C3 H3A 108.9 C4 C3 H3B 108.9 C5 C4 C3 105.92(19) C5 C4 C18 107.89(19) C18 C4 C3 109.2(2) C19 C4 C3 110.8(2) C19 C4 C5 115.41(19) C19 C4 C18 107.5(2) C4 C5 H5 103.9 C4 C5 C10 118.29(19) C6 C5 C4 119.87(19) C6 C5 H5 103.9 C6 C5 C10 104.79(18) C10 C5 H5 103.9 C5 C6 H6A 110.9 C5 C6 H6B 110.9 C5 C6 C7 104.18(18) H6A C6 H6B 108.9 C7 C6 H6A 110.9 C7 C6 H6B 110.9 C6 C7 H7A 110.5 C6 C7 H7B 110.5 C6 C7 C8 106.23(18) H7A C7 H7B 108.7 C8 C7 H7A 110.5 C8 C7 H7B 110.5 C7 C8 H8 107.7 C7 C8 C10 104.01(18) C9 C8 C7 113.11(19) C9 C8 H8 107.7 C9 C8 C10 116.16(19) C10 C8 H8 107.7 O1 C9 C8 122.8(2) O1 C9 C11 121.2(2) C11 C9 C8 115.91(19) C1 C10 C5 107.82(18) C1 C10 C8 116.12(18) C1 C10 C20 110.5(2) C5 C10 C8 98.15(17) C20 C10 C5 115.24(19) C20 C10 C8 108.70(18) C9 C11 H11A 108.8 C9 C11 H11B 108.8 H11A C11 H11B 107.7 C12 C11 C9 114.0(2) C12 C11 H11A 108.8 C12 C11 H11B 108.8 C13 C12 C11 119.0(2) C16 C12 C11 120.9(2) C16 C12 C13 120.1(2) O2 C13 C12 122.3(2) O2 C13 C14 123.7(2) C14 C13 C12 113.9(2) C13 C14 H14 119.7 C15 C14 C13 120.6(3) C15 C14 H14 119.7 O3 C15 H15 117.9 C14 C15 O3 124.1(3) C14 C15 H15 117.9 O3 C16 H16 117.9 C12 C16 O3 124.1(2) C12 C16 H16 117.9 C4 C18 H18A 109.5 C4 C18 H18B 109.5 C4 C18 H18C 109.5 H18A C18 H18B 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C4 C19 H19A 109.5 C4 C19 H19B 109.5 C4 C19 H19C 109.5 H19A C19 H19B 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C10 C20 H20A 109.5 C10 C20 H20B 109.5 C10 C20 H20C 109.5 H20A C20 H20B 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C9 1.212(3) O2 C13 1.237(3) O3 C15 1.347(4) O3 C16 1.361(3) C1 H1A 0.9900 C1 H1B 0.9900 C1 C2 1.529(4) C1 C10 1.534(3) C2 H2A 0.9900 C2 H2B 0.9900 C2 C3 1.532(3) C3 H3A 0.9900 C3 H3B 0.9900 C3 C4 1.546(3) C4 C5 1.534(3) C4 C18 1.535(3) C4 C19 1.531(3) C5 H5 1.0000 C5 C6 1.529(3) C5 C10 1.553(3) C6 H6A 0.9900 C6 H6B 0.9900 C6 C7 1.543(3) C7 H7A 0.9900 C7 H7B 0.9900 C7 C8 1.548(3) C8 H8 1.0000 C8 C9 1.518(3) C8 C10 1.562(3) C9 C11 1.516(3) C10 C20 1.535(3) C11 H11A 0.9900 C11 H11B 0.9900 C11 C12 1.499(3) C12 C13 1.456(3) C12 C16 1.327(3) C13 C14 1.449(3) C14 H14 0.9500 C14 C15 1.329(4) C15 H15 0.9500 C16 H16 0.9500 C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C20 H20A 0.9800 C20 H20B 0.9800 C20 H20C 0.9800