#------------------------------------------------------------------------------ #$Date: 2020-02-01 02:10:45 +0200 (Sat, 01 Feb 2020) $ #$Revision: 247418 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557203.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_1557203 loop_ _publ_author_name 'Wang, Rong' 'Fan, Run-Zhu' 'Ni, Fu-Qiang' 'Sang, Jun' 'Xie, Xing-Lin' 'Luo, Si-Yuan' 'Tang, Gui-Hua' 'Yin, Sheng' _publ_section_title ; 19-nor-, 20-nor-, and tetranor-Halimane-Type Furanoditerpenoids from Croton crassifolius ; _journal_name_full 'Journal of Natural Products' _journal_paper_doi 10.1021/acs.jnatprod.9b00634 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C21 H26 O6' _chemical_formula_sum 'C21 H26 O6' _chemical_formula_weight 374.42 _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 2019-05-17 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.03150(10) _cell_length_b 8.3527(2) _cell_length_c 27.8078(5) _cell_measurement_reflns_used 12478 _cell_measurement_temperature 99.99(10) _cell_measurement_theta_max 77.1990 _cell_measurement_theta_min 5.5090 _cell_volume 1865.48(6) _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 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 99.99(10) _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.979 _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 -123.00 -32.00 0.50 0.06 -- -46.62 -23.00 -42.00 182 2 \w -173.00 -70.00 0.50 0.50 -- -100.00-127.00 -98.00 206 3 \w -173.00 -83.00 0.50 0.50 -- -100.00-101.00 156.00 180 4 \w -176.00 -85.00 0.50 0.50 -- -100.00 -23.00 -42.00 182 5 \w 34.00 110.00 0.50 0.50 -- 107.00-101.00 156.00 152 6 \w -95.00 -11.00 0.50 0.06 -- -46.62 125.00 -90.00 168 7 \w 15.00 95.00 0.50 0.06 -- 46.62-125.00 0.00 160 8 \w 34.00 125.00 0.50 0.50 -- 107.00 -61.00 -30.00 182 9 \w 83.00 178.00 0.50 0.50 -- 107.00 77.00-120.00 190 10 \w 34.00 125.00 0.50 0.50 -- 107.00 -61.00 120.00 182 11 \w 34.00 109.00 0.50 0.50 -- 107.00 -94.00 90.00 150 12 \w 76.00 178.00 0.50 0.50 -- 107.00 125.00 30.00 204 13 \w 32.00 123.00 0.50 0.50 -- 107.00 -30.00 120.00 182 14 \w -119.00 -23.00 0.50 0.06 -- -46.62 -77.00 90.00 192 15 \w -120.00 -52.00 0.50 0.06 -- -46.62 -38.00-120.00 136 16 \w -119.00 -23.00 0.50 0.06 -- -46.62 -77.00-180.00 192 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0462454000 _diffrn_orient_matrix_UB_12 0.1551835000 _diffrn_orient_matrix_UB_13 0.0268555000 _diffrn_orient_matrix_UB_21 0.0367915000 _diffrn_orient_matrix_UB_22 0.0826500000 _diffrn_orient_matrix_UB_23 -0.0483989000 _diffrn_orient_matrix_UB_31 -0.1823293000 _diffrn_orient_matrix_UB_32 0.0558313000 _diffrn_orient_matrix_UB_33 -0.0030418000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_unetI/netI 0.0251 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.979 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 18993 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.971 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 77.516 _diffrn_reflns_theta_min 3.178 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.800 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74926 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 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 1.333 _exptl_crystal_description block _exptl_crystal_F_000 800 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.197 _refine_diff_density_min -0.171 _refine_diff_density_rms 0.041 _refine_ls_abs_structure_details ; Flack x determined using 1502 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.07(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 248 _refine_ls_number_reflns 3856 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0359 _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^)+(0.0507P)^2^+0.5131P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0938 _refine_ls_wR_factor_ref 0.0945 _reflns_Friedel_coverage 0.711 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.960 _reflns_number_gt 3733 _reflns_number_total 3856 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file np9b00634_si_005.cif _cod_data_source_block wangr_190424_2 _cod_database_code 1557203 _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 0.924 _shelx_estimated_absorpt_t_min 0.795 _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 71.98 _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, All O(H) groups 2.a Ternary CH refined with riding coordinates: C11(H11), C4(H4), C2(H2) 2.b Secondary CH2 refined with riding coordinates: C9(H9A,H9B), C8(H8A,H8B), C12(H12A,H12B), C3(H3A,H3B), C7(H7A,H7B) 2.c Aromatic/amide H refined with riding coordinates: C16(H16), C19(H19), C17(H17) 2.d Idealised Me refined as rotating group: C27(H27A,H27B,H27C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C) 2.e Idealised tetrahedral OH refined as rotating group: O25(H25) ; _shelx_res_file ; TITL wangr_190424_2_a.res in P2(1)2(1)2(1) wangr_190424_2.res created by SHELXL-2016/6 at 09:44:29 on 17-May-2019 REM Old TITL wangr_190424_2 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1): R1 0.107, Rweak 0.028, Alpha 0.001 REM 0.498 for 26 systematic absences, Orientation as input REM Flack x = -0.019 ( 0.106 ) from 1530 Parsons' quotients REM Formula found by SHELXT: C21 O6 CELL 1.54184 8.0315 8.3527 27.8078 90 90 90 ZERR 4 0.0001 0.0002 0.0005 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 UNIT 84 104 24 L.S. 4 PLAN 5 SIZE 0.3 0.2 0.1 BOND $h htab conf LIST 6 fmap 2 acta REM REM REM WGHT 0.050700 0.513100 FVAR 0.63899 O14 3 0.601277 0.545302 0.488248 11.00000 0.02105 0.03899 = 0.02615 -0.00182 0.00027 -0.00018 O20 3 0.700273 0.409153 0.425632 11.00000 0.02296 0.03432 = 0.03140 0.00139 0.00138 0.00396 O22 3 -0.007311 0.543604 0.318706 11.00000 0.01963 0.04896 = 0.02389 -0.00406 -0.00036 0.00343 O18 3 0.385665 0.661555 0.634328 11.00000 0.03489 0.05082 = 0.02587 -0.00740 0.00341 -0.00521 O24 3 0.052650 0.602553 0.241793 11.00000 0.02772 0.07382 = 0.02372 0.00075 -0.00257 0.00938 O25 3 0.237571 0.265714 0.295616 11.00000 0.03458 0.04786 = 0.03370 -0.01391 -0.00116 -0.00874 AFIX 147 H25 2 0.155593 0.208639 0.291737 11.00000 -1.50000 AFIX 0 C5 1 0.305282 0.493506 0.345294 11.00000 0.01914 0.03200 = 0.02513 -0.00248 0.00108 0.00505 C9 1 0.441105 0.722389 0.388993 11.00000 0.02867 0.02618 = 0.02882 -0.00207 -0.00022 0.00072 AFIX 23 H9A 2 0.549972 0.721665 0.404094 11.00000 -1.20000 H9B 2 0.366455 0.782991 0.409501 11.00000 -1.20000 AFIX 0 C13 1 0.582004 0.464546 0.446407 11.00000 0.02334 0.02840 = 0.02342 0.00315 -0.00203 -0.00006 C15 1 0.425617 0.600841 0.556972 11.00000 0.02120 0.03440 = 0.02848 -0.00235 -0.00202 0.00025 C10 1 0.378159 0.552060 0.385075 11.00000 0.02035 0.02498 = 0.02665 -0.00144 -0.00016 0.00431 C8 1 0.453894 0.805216 0.340439 11.00000 0.02966 0.02865 = 0.03095 0.00224 0.00365 0.00253 AFIX 23 H8A 2 0.471245 0.919147 0.344971 11.00000 -1.20000 H8B 2 0.547707 0.762677 0.322568 11.00000 -1.20000 AFIX 0 C1 1 0.398462 0.455143 0.431416 11.00000 0.02158 0.02691 = 0.02436 0.00036 -0.00092 0.00079 C6 1 0.275539 0.597228 0.300420 11.00000 0.02109 0.04079 = 0.02333 -0.00110 0.00017 0.00391 C11 1 0.445427 0.619695 0.503954 11.00000 0.02320 0.02969 = 0.02794 -0.00089 0.00047 0.00208 AFIX 13 H11 2 0.447212 0.733860 0.495844 11.00000 -1.20000 AFIX 0 C16 1 0.401360 0.455579 0.583756 11.00000 0.03398 0.03737 = 0.02862 0.00073 -0.00182 0.00333 AFIX 43 H16 2 0.401365 0.351865 0.571591 11.00000 -1.20000 AFIX 0 C4 1 0.241859 0.321499 0.344144 11.00000 0.02450 0.03593 = 0.02802 -0.00800 -0.00086 -0.00098 AFIX 13 H4 2 0.127901 0.320513 0.356738 11.00000 -1.20000 AFIX 0 C21 1 0.097030 0.578917 0.282727 11.00000 0.02591 0.04316 = 0.02200 -0.00241 0.00147 0.00759 C19 1 0.414980 0.720565 0.589587 11.00000 0.03028 0.04028 = 0.03026 -0.00473 0.00183 -0.00448 AFIX 43 H19 2 0.426221 0.828736 0.582358 11.00000 -1.20000 AFIX 0 C2 1 0.339990 0.277368 0.427199 11.00000 0.02368 0.02694 = 0.03550 0.00273 -0.00015 -0.00180 AFIX 13 H2 2 0.222165 0.276214 0.436354 11.00000 -1.20000 AFIX 0 C12 1 0.310235 0.535942 0.474445 11.00000 0.02106 0.03390 = 0.02711 -0.00139 -0.00028 0.00024 AFIX 23 H12A 2 0.228905 0.613102 0.463139 11.00000 -1.20000 H12B 2 0.253445 0.456446 0.493876 11.00000 -1.20000 AFIX 0 C3 1 0.347610 0.216533 0.375871 11.00000 0.02887 0.02658 = 0.03745 -0.00336 0.00208 -0.00085 AFIX 23 H3A 2 0.461915 0.217793 0.364614 11.00000 -1.20000 H3B 2 0.307410 0.107115 0.374536 11.00000 -1.20000 AFIX 0 C7 1 0.294382 0.776975 0.312821 11.00000 0.02876 0.03558 = 0.02925 0.00576 0.00136 0.00803 AFIX 23 H7A 2 0.295633 0.839476 0.283424 11.00000 -1.20000 H7B 2 0.200145 0.811585 0.332001 11.00000 -1.20000 AFIX 0 C17 1 0.378645 0.499012 0.629873 11.00000 0.03080 0.04500 = 0.02928 0.00335 -0.00068 -0.00129 AFIX 43 H17 2 0.360684 0.428221 0.655161 11.00000 -1.20000 AFIX 0 C27 1 0.394545 0.554615 0.258997 11.00000 0.02442 0.05075 = 0.02752 -0.00308 0.00143 0.00512 AFIX 137 H27A 2 0.507459 0.571560 0.269115 11.00000 -1.50000 H27B 2 0.370809 0.621367 0.231743 11.00000 -1.50000 H27C 2 0.379624 0.444330 0.250287 11.00000 -1.50000 AFIX 0 C23 1 -0.180295 0.527050 0.305692 11.00000 0.02044 0.06172 = 0.03187 -0.00875 -0.00381 0.00376 AFIX 137 H23A 2 -0.193385 0.436626 0.284720 11.00000 -1.50000 H23B 2 -0.216913 0.622261 0.289503 11.00000 -1.50000 H23C 2 -0.245725 0.511245 0.334190 11.00000 -1.50000 AFIX 0 C26 1 0.428736 0.164552 0.461972 11.00000 0.03776 0.03198 = 0.04103 0.00799 -0.00060 0.00042 AFIX 137 H26A 2 0.541551 0.148985 0.451566 11.00000 -1.50000 H26B 2 0.372093 0.063364 0.462581 11.00000 -1.50000 H26C 2 0.428367 0.210370 0.493632 11.00000 -1.50000 AFIX 0 HKLF 4 REM wangr_190424_2_a.res in P2(1)2(1)2(1) REM R1 = 0.0359 for 3733 Fo > 4sig(Fo) and 0.0371 for all 3856 data REM 248 parameters refined using 0 restraints END WGHT 0.0507 0.5131 REM Instructions for potential hydrogen bonds EQIV $1 -x, y-1/2, -z+1/2 HTAB O25 O24_$1 EQIV $2 -x+1/2, -y+1, z+1/2 HTAB C17 O24_$2 EQIV $3 -x, y+1/2, -z+1/2 HTAB C23 O25_$3 REM Highest difference peak 0.197, deepest hole -0.171, 1-sigma level 0.041 Q1 1 0.3740 0.4954 0.6698 11.00000 0.05 0.20 Q2 1 0.3918 0.4877 0.4029 11.00000 0.05 0.16 Q3 1 0.0504 0.5384 0.3524 11.00000 0.05 0.16 Q4 1 -0.1987 0.6620 0.2768 11.00000 0.05 0.16 Q5 1 0.4267 0.6085 0.5360 11.00000 0.05 0.15 ; _shelx_res_checksum 68101 _shelx_hkl_file ; 0 0 2 2.98 0.47 0 0 -2 2.54 0.49 0 0 3 0.69 0.45 0 0 -3 0.04 0.54 0 0 4 189.73 7.66 0 0 4 182.79 7.19 0 0 -4 192.67 7.57 0 0 -5 2.03 1.13 0 0 5 0.30 1.13 0 0 5 -0.39 0.81 0 0 6 1.61 1.16 0 0 -6 1.51 1.26 0 0 6 0.91 1.49 0 0 -7 2.86 1.60 0 0 7 -0.43 1.71 0 0 7 -0.08 1.12 0 0 8 229.63 9.75 0 0 8 223.44 10.38 0 0 -8 234.04 10.50 0 0 -9 0.42 1.46 0 0 9 -0.14 1.54 0 0 9 0.10 1.14 0 0 -10 19.42 2.77 0 0 10 17.59 2.86 0 0 10 16.94 2.30 0 0 -11 -0.54 1.74 0 0 11 -0.13 1.21 0 0 11 0.84 1.65 0 0 -12 152.85 9.20 0 0 12 153.83 8.99 0 0 12 153.97 8.30 0 0 13 0.32 1.51 0 0 -13 0.23 1.92 0 0 13 -0.20 1.96 0 0 14 623.58 26.77 0 0 14 656.98 26.25 0 0 15 0.23 1.76 0 0 -15 -0.56 2.16 0 0 15 1.35 1.57 0 0 -16 1113.02 37.73 0 0 16 1155.29 43.31 0 0 16 1139.76 42.59 0 0 17 2.13 2.19 0 0 17 0.69 1.61 0 0 -17 0.27 0.68 0 0 18 201.49 12.18 0 0 -18 204.17 7.74 0 0 18 209.07 12.03 0 0 19 0.30 1.74 0 0 -19 0.13 0.74 0 0 -19 0.29 0.85 0 0 20 5.21 2.39 0 0 -20 3.64 1.06 0 0 -20 3.74 1.04 0 0 -21 0.92 0.98 0 0 -21 -0.31 0.97 0 0 21 0.63 1.75 0 0 21 0.31 0.86 0 0 -22 165.85 11.93 0 0 -22 192.12 7.58 0 0 22 183.95 7.33 0 0 -22 188.00 7.53 0 0 -23 1.04 1.11 0 0 23 0.15 1.03 0 0 -23 1.04 1.83 0 0 -23 -0.06 1.08 0 0 24 78.60 3.83 0 0 -24 77.11 3.94 0 0 -24 74.63 3.92 0 0 -25 -0.30 1.14 0 0 -25 0.37 1.14 0 0 25 -0.10 1.12 0 0 26 83.63 4.14 0 0 -26 88.24 4.40 0 0 -26 89.06 4.32 0 0 -27 0.45 1.04 0 0 27 0.15 1.12 0 0 -27 0.49 1.21 0 0 28 18.06 1.75 0 0 -28 17.42 1.87 0 0 -28 15.82 1.69 0 0 -29 -0.14 0.95 0 0 -29 -0.44 1.07 0 0 29 0.50 1.02 0 0 30 8.48 1.26 0 0 -30 7.21 1.14 0 0 -30 7.49 1.34 0 0 31 0.41 0.88 0 0 -31 0.50 0.94 0 0 32 30.59 1.79 0 0 -32 26.75 1.85 0 0 33 -0.46 0.62 0 0 -33 0.13 0.67 0 0 34 2.87 0.61 0 0 -34 3.27 0.66 0 1 0 0.87 0.57 0 -1 0 1.22 0.77 0 1 0 0.69 0.41 0 1 0 0.69 0.43 0 1 1 175.09 6.22 0 1 -1 153.33 6.03 0 -1 -1 166.34 6.28 0 -1 1 169.09 6.85 0 1 -1 162.20 5.74 0 -1 2 2179.62 69.42 0 -1 -2 2147.80 68.81 0 -1 -2 1991.24 68.15 0 -1 3 568.35 21.63 0 -1 -3 620.56 21.07 0 1 -4 602.08 21.31 0 -1 -4 606.00 21.45 0 1 5 252.64 10.31 0 1 -5 266.49 10.34 0 -1 -5 260.00 10.50 0 1 6 4244.97 139.34 0 1 -6 4218.21 139.17 0 -1 -6 4168.15 139.44 0 1 -7 1010.86 34.63 0 -1 7 937.08 33.62 0 1 7 1017.36 34.80 0 -1 -7 1012.63 35.02 0 1 8 16.22 2.20 0 -1 8 18.20 2.98 0 -1 8 12.68 1.59 0 -1 -8 15.20 2.23 0 1 8 12.51 1.88 0 -1 9 473.24 17.59 0 -1 9 487.06 20.06 0 1 9 483.23 18.64 0 -1 -9 509.85 19.22 0 1 9 437.13 17.85 0 -1 10 249.06 12.43 0 -1 -10 258.47 11.70 0 1 10 240.74 11.19 0 -1 10 231.23 10.14 0 1 10 229.73 10.49 0 -1 11 829.35 32.88 0 1 11 827.87 30.77 0 -1 -11 929.20 32.51 0 1 11 844.69 31.41 0 -1 11 813.24 30.17 0 1 12 441.21 18.58 0 -1 -12 512.53 20.57 0 1 12 479.21 19.48 0 -1 12 487.38 20.93 0 -1 12 443.16 18.16 0 -1 13 164.15 10.36 0 -1 -13 177.71 10.38 0 1 13 158.18 8.67 0 1 13 169.52 9.41 0 1 -14 28.17 3.53 0 -1 -14 31.90 4.51 0 1 14 27.75 3.51 0 1 14 29.70 3.80 0 -1 14 34.19 4.77 0 1 15 83.61 6.68 0 -1 -15 99.39 7.95 0 1 15 71.17 5.83 0 -1 15 79.73 7.22 0 1 -15 89.40 6.55 0 1 16 133.25 8.60 0 1 -16 134.90 8.58 0 -1 16 129.07 9.50 0 1 16 103.67 7.32 0 -1 -16 145.74 9.97 0 -1 -16 117.69 4.80 0 1 -16 118.55 4.84 0 -1 17 81.52 7.83 0 -1 -17 91.03 8.11 0 1 -17 98.02 7.25 0 1 17 91.70 7.25 0 1 17 72.49 6.07 0 1 -17 82.87 3.72 0 -1 -17 83.60 3.70 0 -1 -18 69.97 3.33 0 1 -18 78.91 6.73 0 1 18 70.74 6.61 0 1 -18 72.92 3.51 0 1 -18 69.25 3.48 0 -1 -18 74.54 7.71 0 1 18 62.19 5.67 0 1 -18 70.94 3.37 0 -1 18 73.90 7.43 0 1 -19 13.09 3.01 0 -1 -19 16.46 4.36 0 1 19 14.13 3.42 0 1 -19 13.01 1.49 0 -1 -19 16.16 1.46 0 1 -19 15.67 1.45 0 -1 19 16.44 3.97 0 -1 -20 523.41 18.41 0 -1 20 509.40 25.32 0 -1 20 524.70 18.23 0 -1 -20 600.88 27.77 0 1 -20 523.50 18.59 0 1 20 528.08 18.23 0 1 -20 518.88 18.41 0 1 -20 522.73 24.04 0 1 20 552.55 24.99 0 -1 21 177.39 6.80 0 1 21 161.79 11.67 0 1 -21 157.08 11.11 0 1 -21 166.54 7.05 0 -1 -21 173.69 6.96 0 1 21 171.67 6.76 0 1 -21 175.18 7.00 0 -1 21 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5.51 0 5 6 61.00 2.81 0 5 -6 58.04 2.83 0 -5 7 152.03 11.79 0 5 7 136.14 8.85 0 5 7 148.30 5.87 0 5 7 148.75 9.52 0 5 -7 146.17 10.37 0 5 -7 162.10 5.98 0 -5 -7 178.08 11.46 0 -5 -8 130.48 9.85 0 -5 8 108.40 10.02 0 5 8 111.45 7.88 0 5 8 102.39 4.42 0 5 8 116.26 8.31 0 5 -8 117.48 4.59 0 5 -8 122.93 9.23 0 5 9 123.73 8.97 0 -5 -9 137.98 10.25 0 5 9 120.55 4.88 0 5 -9 127.61 4.98 0 -5 9 125.88 11.15 0 5 -9 143.11 10.11 0 5 9 124.70 8.72 0 5 -9 120.18 5.11 0 -5 10 6.11 3.72 0 5 -10 3.71 0.93 0 5 10 4.58 2.10 0 5 10 2.59 0.71 0 5 10 4.38 2.25 0 5 -10 4.17 0.82 0 5 -10 4.15 0.92 0 5 -10 3.99 2.40 0 -5 -10 5.80 2.82 0 5 11 124.46 9.25 0 -5 11 106.82 4.66 0 5 11 118.62 4.67 0 5 -11 115.31 5.01 0 -5 -11 129.99 10.32 0 5 -11 136.63 10.06 0 -5 11 133.11 11.66 0 5 11 141.92 9.83 0 5 -11 118.85 5.02 0 5 -11 124.31 4.77 0 5 -12 26.94 1.96 0 5 -12 28.43 1.70 0 5 -12 26.74 4.63 0 5 12 30.14 4.83 0 -5 -12 23.77 4.76 0 -5 12 28.49 1.74 0 5 12 32.04 4.82 0 -5 12 28.69 5.99 0 5 -12 29.58 2.06 0 5 -13 282.98 15.92 0 5 13 248.17 15.21 0 5 13 285.19 15.71 0 -5 13 272.03 18.20 0 -5 13 244.10 9.22 0 -5 -13 308.85 17.34 0 5 -13 250.72 9.56 0 5 -13 255.62 9.63 0 5 -14 36.76 2.40 0 -5 14 23.81 5.98 0 5 -14 34.36 2.26 0 5 -14 31.46 5.11 0 5 14 28.01 4.87 0 -5 -14 42.62 6.40 0 5 14 38.34 5.54 0 -5 14 31.04 1.94 0 5 -15 625.47 28.26 0 -5 -15 614.40 20.67 0 5 -15 598.56 20.86 0 -5 15 575.71 20.40 0 5 15 567.70 27.99 0 -5 -15 641.21 29.82 0 5 15 619.39 28.09 0 -5 15 640.30 32.00 0 5 -15 578.61 20.73 0 5 -16 85.51 4.16 0 -5 -16 84.20 3.92 0 -5 16 76.80 3.61 0 5 -16 77.29 3.92 0 5 16 73.48 8.10 0 -5 -16 91.38 9.43 0 -5 16 65.01 9.52 0 5 16 75.86 8.07 0 5 -16 72.89 7.93 0 5 -17 32.99 2.49 0 5 -17 33.62 5.36 0 5 -17 31.17 2.28 0 -5 17 35.54 2.12 0 -5 -17 36.62 2.37 0 5 17 30.78 5.50 0 -5 -17 34.97 6.13 0 5 17 36.94 5.84 0 5 18 4.90 2.82 0 5 18 5.85 3.02 0 -5 -18 6.04 3.39 0 5 -18 7.06 1.48 0 -5 18 5.41 1.03 0 5 -18 6.56 2.79 0 5 -18 4.87 1.23 0 -5 -18 6.02 1.30 0 -5 -19 14.96 1.68 0 5 19 9.98 3.56 0 -5 -19 14.01 4.12 0 5 -19 13.45 1.59 0 5 -19 9.53 3.16 0 -5 19 12.09 4.66 0 5 -19 13.31 1.76 0 5 19 9.42 3.46 0 -5 -20 113.21 11.43 0 -5 20 97.61 11.29 0 -5 -20 110.54 4.84 0 5 -20 101.70 4.76 0 5 -20 101.94 4.98 0 5 20 96.06 9.78 0 5 -21 9.35 1.39 0 -5 -21 11.06 1.57 0 5 -21 9.55 1.63 0 5 -22 312.95 12.06 0 -5 -22 340.11 11.94 0 5 -22 304.44 11.74 0 -5 23 51.83 3.09 0 5 -23 51.76 3.16 0 -5 -23 52.81 3.01 0 5 -23 47.98 2.82 0 -5 24 18.25 1.86 0 5 -24 18.61 1.93 0 -5 -24 17.31 1.73 0 -5 25 2.90 1.18 0 5 -25 3.28 1.20 0 -5 -25 3.40 1.17 0 5 -26 6.08 1.31 0 5 -26 4.88 1.01 0 -5 -26 8.18 1.26 0 -5 26 6.72 1.24 0 5 -27 31.35 2.09 0 -5 -27 30.85 1.99 0 -5 27 31.17 2.01 0 -5 28 1.17 0.79 0 -5 -28 1.08 0.77 0 -5 29 38.53 1.98 0 -5 -29 41.51 2.06 0 -5 30 14.28 0.95 0 -5 -30 16.70 1.10 0 6 0 207.81 7.62 0 6 0 178.75 7.46 0 -6 0 194.30 12.68 0 -6 1 6.15 2.81 0 6 1 1.52 0.90 0 -6 -1 3.58 2.51 0 -6 1 1.06 2.02 0 6 -1 0.56 0.74 0 6 1 2.59 0.96 0 -6 2 18.56 4.17 0 6 2 21.18 1.69 0 -6 2 22.49 4.73 0 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0 32.17 4.62 -2 5 0 23.93 4.14 -2 5 0 26.24 1.73 2 -5 0 30.64 4.36 -2 5 -1 17.48 1.58 2 5 1 16.19 2.93 -2 5 -1 13.86 2.36 -2 -5 1 24.77 4.13 -2 5 -1 15.01 3.40 2 -5 -1 23.62 3.85 2 -5 -2 63.84 6.24 -2 -5 2 54.73 6.82 2 5 2 53.77 5.27 -2 5 -2 54.85 2.95 -2 5 -2 56.65 5.99 2 -5 -3 70.79 6.73 -2 5 -3 62.01 3.22 -2 -5 3 61.10 3.01 -2 5 -3 66.66 3.09 2 5 3 59.72 5.68 -2 -5 3 69.06 7.58 -2 -5 4 94.96 4.17 -2 -5 4 89.00 8.85 2 5 4 91.76 7.37 -2 5 -4 94.41 4.34 -2 5 -4 99.55 4.18 -2 -5 5 277.70 10.35 2 -5 -5 316.85 16.32 2 5 5 297.60 15.21 -2 -5 5 309.35 17.80 -2 5 -5 267.66 10.50 -2 5 -5 298.05 10.35 -2 -5 6 88.93 9.06 2 -5 -6 97.75 8.19 2 5 6 90.22 7.50 -2 -5 6 79.62 3.82 -2 5 -6 85.59 4.04 -2 5 -6 90.94 3.83 -2 -5 7 73.85 3.37 2 -5 -7 75.20 7.27 -2 -5 7 68.35 3.42 2 5 7 69.37 6.73 -2 5 -7 67.45 3.55 -2 5 -7 76.93 3.37 -2 -5 7 88.49 8.89 -2 -5 7 73.25 3.46 -2 -5 8 161.90 6.50 2 5 8 169.39 11.20 -2 -5 8 167.52 6.48 2 -5 -8 195.27 12.19 -2 -5 8 160.08 6.57 2 5 8 161.65 6.34 -2 5 -8 168.56 6.36 -2 5 -8 155.24 6.64 -2 -5 8 178.11 13.35 -2 -5 9 71.94 3.46 -2 -5 9 71.60 3.47 -2 -5 9 67.12 3.50 2 5 9 75.46 7.30 2 -5 -9 76.34 7.51 2 5 9 71.53 3.28 -2 5 -9 73.19 3.30 -2 5 -9 66.85 3.57 -2 -5 9 81.51 9.02 -2 5 -10 5.00 1.17 -2 -5 10 2.97 1.00 -2 -5 10 4.36 1.06 -2 -5 10 5.36 1.06 2 5 10 4.66 0.88 2 -5 -10 3.67 2.65 2 5 10 4.51 2.55 -2 5 -10 4.72 0.84 -2 -5 10 3.39 3.38 -2 -5 11 103.59 4.67 -2 -5 11 106.74 4.62 2 -5 -11 116.52 9.73 -2 5 -11 101.28 4.78 -2 5 -11 108.19 4.37 2 5 11 104.31 4.34 -2 -5 11 104.28 4.84 2 5 11 110.70 9.43 -2 -5 11 121.92 11.25 -2 5 -11 96.39 4.42 -2 -5 12 96.05 4.52 2 5 12 104.57 9.16 -2 5 -12 99.43 4.08 -2 -5 12 97.72 4.42 -2 -5 12 89.90 4.59 -2 5 -12 96.78 4.62 -2 5 -12 98.62 4.36 2 -5 -12 112.49 9.70 -2 -5 12 101.74 10.67 -2 -5 13 21.44 1.78 2 -5 -13 26.29 5.15 -2 -5 13 22.29 1.90 -2 5 -13 22.62 1.49 -2 5 -13 20.80 1.76 -2 5 -13 22.89 1.99 2 5 13 19.56 4.21 -2 -5 14 726.82 24.27 -2 5 -14 678.50 24.28 -2 -5 14 688.89 24.03 2 -5 -14 714.83 23.96 -2 5 -14 669.95 24.05 2 5 14 744.98 32.59 2 -5 -14 704.77 32.57 -2 -5 15 17.07 1.84 2 -5 -15 23.12 4.90 -2 5 -15 18.93 1.82 2 5 15 18.52 4.41 -2 5 -15 18.01 1.88 -2 -5 15 19.21 1.69 -2 -5 15 18.61 5.28 2 -5 -15 18.86 1.70 2 -5 -16 10.11 1.34 2 -5 -16 8.75 3.50 -2 -5 16 11.17 1.58 -2 5 -16 9.01 1.43 -2 -5 16 9.46 1.34 2 5 16 6.93 3.57 -2 5 -16 9.62 1.50 -2 -5 16 14.39 4.95 -2 -5 17 4.35 1.07 2 -5 -17 3.82 2.81 2 5 17 3.53 2.67 -2 5 -17 3.68 1.20 -2 -5 17 3.69 1.29 -2 5 -17 3.64 1.28 2 -5 -17 5.82 1.17 -2 -5 17 6.11 3.80 2 -5 -18 177.19 14.14 -2 5 -18 184.01 7.58 -2 -5 18 182.49 7.28 -2 5 -18 178.95 7.46 2 -5 -18 186.78 7.31 -2 -5 18 165.73 14.54 2 5 18 170.91 13.43 -2 -5 18 180.08 7.58 2 -5 -19 29.16 5.85 -2 5 -19 29.39 2.30 2 -5 -19 30.04 2.15 -2 5 -19 28.71 2.34 -2 -5 19 21.12 5.42 2 5 19 23.66 4.97 -2 -5 19 28.46 2.09 -2 5 -20 56.98 3.33 2 -5 -20 58.18 3.18 -2 5 -20 57.96 3.36 -2 -5 20 56.60 3.12 -2 5 -21 68.29 3.66 2 -5 -21 65.56 3.43 -2 -5 21 62.60 3.38 -2 5 -21 73.92 3.75 -2 5 -22 38.21 2.86 -2 5 -22 38.46 2.58 2 -5 -22 36.03 2.38 -2 5 -22 37.56 2.55 -2 -5 23 10.22 1.58 2 -5 -23 11.01 1.39 -2 5 -23 11.13 1.72 -2 5 -23 11.48 1.56 -2 5 -23 10.10 1.52 -2 5 -24 10.89 1.49 2 -5 -24 12.67 1.39 -2 -5 24 11.69 1.52 -2 5 -24 11.66 1.49 -2 5 -24 11.62 1.62 -2 -5 25 87.78 3.97 -2 5 -25 79.56 3.94 -2 5 -25 85.32 3.96 2 -5 -25 85.45 3.81 -2 5 -25 84.78 3.93 -2 -5 26 13.00 1.39 -2 5 -26 11.08 1.28 -2 5 -26 12.77 1.40 2 -5 -26 15.46 1.31 -2 5 -27 15.08 1.35 2 -5 -27 15.82 1.24 -2 -5 27 14.51 1.31 -2 -5 28 8.58 1.00 2 -5 -28 9.01 0.89 -2 5 -28 8.94 1.04 -2 5 -29 52.74 2.35 -2 -5 29 56.27 2.38 2 -6 27 3.00 0.61 2 6 -27 2.42 0.65 -2 -6 -26 5.77 0.74 2 -6 26 8.64 0.98 2 6 -26 9.26 1.01 -2 -6 -26 8.72 0.87 2 -6 25 5.23 0.99 -2 -6 -25 4.77 0.78 2 6 -25 6.64 1.04 -2 -6 -25 5.92 0.89 -2 -6 -24 16.98 1.33 2 6 -24 16.16 1.51 -2 -6 -24 18.24 1.41 2 6 -23 61.11 3.13 -2 -6 -23 61.87 2.98 2 6 -22 -0.15 1.06 -2 -6 -22 0.97 0.88 2 6 -21 13.86 1.64 -2 -6 -21 12.17 1.39 -2 -6 -20 9.43 1.32 2 6 -20 9.35 1.50 -2 -6 -19 12.81 1.48 2 6 -19 13.61 1.69 2 6 -18 57.24 3.37 -2 -6 -18 63.10 3.22 -2 -6 -17 82.24 3.92 2 6 -17 79.66 4.12 2 6 -16 109.87 5.13 -2 -6 -16 111.42 4.92 -2 -6 -15 6.62 3.54 -2 6 15 9.56 3.35 2 6 -15 8.34 1.49 2 6 -15 8.08 3.19 -2 -6 -15 9.57 1.34 2 -6 15 8.27 4.34 2 -6 14 117.12 12.24 2 6 -14 116.59 10.89 -2 -6 -14 131.30 11.60 -2 -6 -14 134.02 5.43 -2 6 14 106.37 10.21 2 6 -14 129.66 5.64 2 6 -14 120.90 5.00 -2 -6 -13 4.13 2.77 -2 6 13 0.41 1.72 2 6 -13 1.17 0.71 2 6 -13 2.28 1.20 2 6 -13 0.45 2.23 2 -6 13 1.72 3.01 -2 6 12 63.37 3.16 2 6 -12 65.66 8.07 2 6 -12 78.06 3.79 -2 -6 -12 75.15 8.60 2 6 -12 77.67 3.45 -2 6 12 71.73 7.86 2 -6 12 67.66 9.28 -2 6 11 82.02 3.76 -2 -6 -11 92.75 4.10 -2 6 11 78.27 8.10 2 6 -11 82.16 4.11 2 6 -11 91.01 3.96 -2 -6 -11 90.91 9.35 -2 -6 -10 243.92 8.62 -2 6 10 182.67 13.18 -2 6 10 212.95 8.29 -2 -6 -10 252.00 15.90 2 6 -10 219.07 8.43 2 -6 10 198.40 15.80 2 6 -10 223.15 8.62 -2 -6 -9 59.51 3.10 -2 6 9 48.58 6.06 -2 -6 -9 62.37 7.61 2 6 -9 58.40 3.11 2 6 -9 61.28 3.09 2 -6 9 57.93 7.98 -2 6 9 54.99 2.89 -2 6 8 129.59 5.52 -2 -6 -8 141.22 5.71 -2 6 8 109.91 9.27 -2 -6 -8 138.98 11.35 2 6 -8 146.14 5.78 2 6 -8 137.47 5.70 2 6 -8 151.76 12.04 2 -6 8 112.95 11.48 -2 -6 -7 62.89 3.17 -2 6 7 47.61 5.68 -2 -6 -7 61.31 7.44 2 6 -7 58.19 3.07 -2 6 7 61.79 3.10 2 6 -7 64.04 7.84 2 -6 7 58.49 7.87 2 6 -7 66.12 3.27 -2 -6 -6 52.85 6.85 -2 -6 -6 49.65 2.78 2 6 -6 54.89 2.91 2 6 -6 45.15 6.64 2 -6 6 41.33 6.57 -2 6 6 53.06 2.80 -2 -6 -5 43.45 2.57 -2 -6 -5 40.33 5.97 2 -6 5 37.06 6.12 2 6 -5 51.87 2.81 -2 6 5 48.55 2.65 -2 -6 -4 2.91 0.95 -2 -6 -4 -0.40 2.52 -2 6 4 2.40 0.95 -2 6 4 3.49 1.17 2 6 -4 3.83 1.08 2 -6 4 1.99 2.52 2 -6 4 0.41 2.33 -2 -6 -3 61.21 7.16 2 -6 3 50.27 6.54 -2 -6 -3 52.67 2.82 2 6 -3 52.15 2.90 -2 6 3 50.79 3.04 -2 6 3 49.89 2.79 -2 -6 -2 47.14 6.49 -2 6 2 49.00 2.96 -2 -6 -2 48.93 2.71 -2 6 2 48.85 2.75 2 -6 2 53.53 6.63 -2 -6 -1 103.06 9.14 -2 -6 -1 86.24 3.98 -2 6 1 86.89 4.29 -2 6 1 83.56 3.99 2 -6 1 98.21 8.85 -2 -6 0 4.02 0.99 -2 -6 0 4.72 2.54 2 -6 0 8.39 2.93 -2 6 0 3.45 1.14 2 6 0 5.79 1.16 -2 6 0 2.56 0.99 2 6 1 90.38 4.19 2 6 1 83.93 6.90 -2 -6 1 85.39 4.02 -2 6 -1 86.69 4.32 2 -6 -1 103.83 9.10 -2 -6 1 104.51 9.23 -2 -6 2 44.43 2.64 2 -6 -2 60.73 6.95 2 6 2 51.96 2.83 2 6 2 45.64 5.14 -2 -6 2 57.26 6.90 -2 6 -2 48.24 2.92 2 -6 -3 53.87 6.65 -2 -6 3 50.63 2.76 -2 6 -3 46.36 2.91 2 6 3 53.16 2.85 2 6 3 39.90 5.05 -2 6 -3 49.01 2.76 -2 -6 3 46.20 6.49 -2 -6 4 2.91 3.26 2 -6 -4 3.93 2.37 -2 -6 4 1.25 2.45 2 6 4 3.95 1.09 2 6 4 2.88 2.15 -2 -6 4 3.98 1.02 -2 6 -4 2.44 0.92 -2 6 -4 1.78 1.03 2 -6 -5 52.92 6.76 -2 -6 5 47.12 2.69 2 6 5 49.11 2.74 2 6 5 45.22 5.49 -2 -6 5 42.86 7.11 -2 6 -5 46.92 2.89 -2 6 -5 46.87 2.68 -2 -6 6 51.04 2.81 2 -6 -6 51.85 6.70 2 6 6 48.09 5.86 2 6 6 47.87 2.75 -2 6 -6 49.09 2.97 -2 -6 6 53.14 7.81 -2 6 -6 47.86 2.73 -2 -6 7 61.01 3.21 -2 -6 7 57.72 3.02 2 6 7 54.44 6.38 2 -6 -7 60.71 7.35 -2 6 -7 64.61 3.19 -2 -6 7 58.47 8.35 2 6 7 66.02 3.21 -2 6 -7 59.25 3.39 -2 -6 8 134.59 5.65 -2 -6 8 135.98 12.47 2 -6 -8 141.97 11.47 -2 -6 8 135.45 5.76 2 6 8 137.75 5.67 2 6 8 149.12 10.70 -2 6 -8 133.46 5.96 -2 6 -8 141.19 5.69 -2 -6 9 56.91 3.08 2 6 9 54.87 6.55 2 6 9 61.30 3.04 -2 6 -9 59.36 3.35 2 -6 -9 61.48 7.57 -2 -6 9 60.36 8.57 -2 6 -9 61.93 3.06 -2 -6 9 54.83 3.10 -2 6 -10 231.19 8.95 -2 -6 10 208.18 8.74 2 6 10 231.74 8.51 -2 -6 10 221.65 8.64 2 -6 -10 225.63 15.28 2 6 10 216.21 14.18 -2 -6 10 211.13 8.58 -2 -6 10 231.88 17.00 -2 6 -10 241.16 8.53 -2 -6 11 87.48 10.36 -2 -6 11 81.27 4.16 -2 -6 11 83.27 4.11 -2 6 -11 96.97 4.06 2 6 11 90.26 8.74 2 -6 -11 100.54 9.78 2 6 11 93.12 4.01 -2 6 -11 93.61 4.50 -2 -6 12 77.25 3.73 -2 6 -12 75.99 3.47 -2 6 -12 79.38 4.04 -2 -6 12 70.86 3.80 2 6 12 73.76 3.45 2 -6 -12 74.38 8.64 -2 -6 12 79.48 9.89 2 6 12 84.71 8.43 -2 -6 13 4.62 3.80 -2 -6 13 1.64 1.10 2 6 13 0.41 2.01 -2 -6 13 1.38 0.95 2 -6 -13 0.92 2.41 -2 6 -13 2.07 0.75 -2 6 -13 2.80 1.24 -2 6 -14 121.97 4.95 -2 -6 14 126.89 5.40 -2 -6 14 124.26 5.61 2 6 14 123.04 10.75 2 -6 -14 140.41 5.51 -2 6 -14 122.91 5.27 -2 6 -14 126.93 5.71 2 -6 -14 121.88 11.36 -2 -6 14 113.62 12.23 2 -6 -15 3.77 3.30 -2 -6 15 7.09 1.42 2 -6 -15 11.01 1.37 -2 6 -15 9.16 1.30 2 6 15 6.31 2.94 -2 6 -15 9.60 1.54 -2 -6 15 6.36 3.97 -2 -6 15 10.42 1.33 -2 -6 16 113.36 5.02 2 -6 -16 107.29 4.79 -2 6 -16 102.89 4.69 -2 6 -16 107.97 5.02 -2 -6 16 103.97 4.72 -2 -6 17 83.54 4.10 -2 -6 17 81.24 3.84 -2 6 -17 83.49 4.16 -2 6 -17 75.14 3.82 2 -6 -17 83.72 3.95 -2 6 -18 66.61 3.49 -2 -6 18 60.10 3.12 -2 6 -18 56.70 3.15 2 -6 -18 60.27 3.19 -2 -6 18 59.18 3.34 -2 -6 19 11.93 1.57 -2 -6 19 13.87 1.42 -2 6 -19 10.35 1.47 2 -6 -19 12.48 1.45 -2 6 -19 11.59 1.55 -2 -6 20 8.49 1.42 -2 6 -20 9.28 1.43 -2 6 -20 9.18 1.29 2 -6 -20 9.50 1.34 -2 -6 20 9.26 1.22 -2 -6 21 13.11 1.52 -2 6 -21 12.95 1.87 2 -6 -21 10.06 1.31 -2 6 -21 11.86 1.48 -2 6 -21 9.02 1.30 -2 -6 22 0.56 0.99 -2 6 -22 0.85 1.25 -2 6 -22 0.74 0.88 -2 6 -22 0.57 0.94 2 -6 -22 0.92 0.85 -2 6 -23 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108.57 9.28 -5 5 7 103.16 9.99 -5 5 7 122.13 4.97 -5 -5 -7 111.90 5.13 -5 5 7 123.10 5.40 5 5 -7 104.91 10.24 -5 5 7 122.97 13.19 -5 5 6 62.08 7.55 -5 5 6 70.15 3.39 -5 -5 -6 67.14 3.55 5 5 -6 77.61 7.76 -5 5 6 74.82 3.80 5 5 -6 65.11 7.96 -5 5 6 69.84 9.93 -5 5 5 12.35 4.55 -5 5 5 16.74 1.51 -5 5 5 9.61 3.24 -5 -5 -5 13.17 1.53 5 5 -5 12.71 3.38 -5 5 5 14.46 1.68 5 5 -5 13.99 3.89 -5 5 4 83.12 8.61 -5 5 4 85.15 3.99 -5 -5 -4 89.05 4.22 5 5 -4 74.52 7.94 -5 5 4 88.14 4.32 5 5 -4 90.00 9.04 -5 5 4 86.09 10.77 -5 5 3 104.20 9.73 -5 5 3 132.44 5.33 -5 -5 -3 125.32 5.50 5 5 -3 114.16 9.98 -5 5 3 123.31 5.57 -5 5 3 119.98 12.95 -5 5 2 66.58 7.53 -5 5 2 74.72 3.62 -5 -5 -2 83.00 3.94 5 5 -2 68.31 7.66 -5 5 2 75.10 3.90 -5 5 2 66.09 9.68 -5 5 1 52.25 2.84 -5 5 1 44.65 6.07 -5 -5 -1 52.20 2.99 5 5 -1 42.36 6.12 -5 5 1 47.34 2.93 -5 5 1 51.11 8.38 -5 5 0 112.65 4.99 -5 5 0 105.27 9.40 -5 5 0 107.19 4.93 -5 -5 0 119.80 5.24 5 5 0 108.55 9.94 -5 5 0 126.87 5.37 -5 5 0 119.06 12.77 -5 5 -1 45.94 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-16 5.75 0.83 -8 -3 -15 4.61 0.57 8 3 -15 10.67 1.07 -8 3 14 53.24 2.27 -8 -3 -14 35.22 1.83 -8 3 13 8.97 1.08 -8 -3 -13 5.66 0.71 -8 3 12 10.95 1.25 -8 -3 -12 7.94 0.84 -8 3 11 21.03 1.65 -8 -3 -11 17.41 1.24 -8 3 10 96.44 4.14 -8 -3 -10 84.13 3.63 -8 3 9 15.27 1.56 -8 -3 -9 12.56 1.13 -8 3 8 80.14 3.80 -8 -3 -8 71.77 3.28 -8 -3 -8 78.10 3.64 -8 3 7 16.11 1.68 -8 -3 -7 15.01 1.23 -8 -3 -7 15.39 1.52 -8 3 6 46.32 2.83 -8 -3 -6 43.47 2.30 -8 -3 -6 48.74 2.68 -8 3 5 3.61 1.22 -8 -3 -5 2.74 0.76 -8 -3 -5 3.25 1.08 -8 3 4 15.47 1.79 -8 -3 -4 12.91 1.22 -8 -3 -4 15.27 1.56 -8 3 3 149.78 5.87 -8 -3 -3 143.08 5.78 -8 -3 -3 155.83 6.18 -8 3 2 37.02 2.14 -8 -3 -2 36.05 2.10 -8 -3 -2 39.00 2.42 -8 3 1 19.34 1.65 -8 3 1 23.05 1.64 -8 -3 -1 24.29 1.66 -8 -3 -1 26.38 1.96 -8 3 0 46.69 2.67 -8 -3 0 49.44 2.56 -8 3 0 48.51 2.56 -8 -3 0 55.30 2.94 -8 3 -1 23.22 1.88 -8 -3 1 20.81 1.61 -8 3 -1 25.83 1.70 -8 -3 1 24.65 1.95 -8 -3 2 35.16 2.02 -8 3 -2 37.61 2.42 -8 -3 2 39.71 2.23 -8 3 -2 36.93 2.15 -8 -3 2 43.69 2.55 -8 3 -3 149.19 6.09 -8 -3 3 143.06 5.72 -8 3 -3 150.67 5.73 -8 -3 3 158.63 6.16 -8 -3 4 10.62 1.19 -8 3 -4 11.12 1.51 -8 3 -4 9.72 1.10 -8 -3 4 12.33 1.49 -8 -3 5 2.66 0.85 -8 3 -5 2.34 1.16 -8 3 -5 3.25 0.79 -8 -3 5 3.36 1.11 -8 -3 6 41.38 2.32 -8 3 -6 44.84 2.75 -8 3 -6 40.20 2.20 -8 -3 6 45.03 2.64 -8 -3 7 15.04 1.38 -8 3 -7 17.34 1.80 -8 3 -7 14.55 1.23 -8 -3 7 16.60 1.65 -8 -3 8 66.65 3.31 -8 3 -8 78.85 3.82 -8 3 -8 69.17 3.17 -8 -3 8 79.56 3.69 -8 -3 9 12.74 1.29 -8 3 -9 13.35 1.65 -8 3 -9 11.14 1.07 -8 -3 9 13.09 1.46 -8 -3 10 84.26 3.77 -8 3 -10 99.23 4.29 -8 -3 10 94.07 4.05 -8 -3 11 20.07 1.53 -8 3 -11 24.50 1.99 -8 -3 11 21.43 1.71 -8 -3 12 9.61 1.12 -8 3 -12 7.06 0.82 -8 -3 12 9.40 1.20 -8 -3 13 7.28 1.02 -8 3 -13 6.68 0.76 -8 -3 14 51.57 2.21 -8 3 -14 31.27 1.69 -8 -3 15 8.39 0.95 -8 3 -15 10.50 1.29 -8 -3 16 4.29 0.74 -8 3 -16 5.83 1.04 -8 -3 17 7.96 0.81 -8 3 -17 8.41 1.06 -8 -3 18 49.25 2.12 -8 3 -18 49.21 2.31 -8 -3 19 4.11 0.50 -8 3 -19 3.29 0.61 -8 -4 -17 2.76 0.45 -8 -4 -16 56.07 2.25 8 4 -16 49.34 2.23 -8 -4 -15 35.51 1.74 8 4 -15 34.77 1.77 -8 -4 -14 26.06 1.53 8 4 -14 27.76 1.62 -8 -4 -13 48.00 2.32 8 4 -13 48.56 2.39 -8 -4 -12 10.54 1.07 -8 -4 -11 10.98 1.14 -8 -4 -10 0.88 0.77 -8 -4 -9 -0.08 0.23 -8 -4 -9 4.29 0.93 -8 -4 -8 -0.02 0.31 -8 -4 -8 25.36 1.57 -8 -4 -7 0.26 0.47 -8 -4 -7 2.59 0.94 -8 -4 -6 44.63 2.13 -8 -4 -6 52.46 2.65 -8 -4 -5 5.65 0.77 -8 -4 -5 7.74 1.17 -8 -4 -4 36.22 1.84 -8 -4 -3 32.58 1.73 -8 -4 -2 5.46 0.83 -8 -4 -1 48.48 2.28 -8 -4 0 12.27 1.05 -8 -4 1 48.07 2.25 -8 -4 2 4.94 0.77 -8 4 -2 4.64 0.92 -8 -4 3 31.38 1.31 -8 4 -3 31.00 1.67 -8 -4 4 33.36 1.30 -8 4 -4 34.23 1.78 -8 -4 5 4.64 0.69 -8 4 -5 6.86 1.16 -8 4 -6 45.50 2.48 -8 -4 6 49.20 2.65 -8 -4 7 0.29 0.32 -8 4 -7 2.06 1.00 -8 -4 7 1.99 0.99 -8 4 -8 23.26 1.61 -8 -4 8 26.37 1.71 -8 -4 9 2.11 0.60 -8 4 -9 4.55 1.06 -8 -4 9 2.71 0.95 -8 -4 10 0.30 0.53 -8 4 -10 1.40 0.96 -8 -4 10 0.38 0.83 -8 -4 11 7.81 0.84 -8 4 -11 9.91 1.27 -8 -4 12 7.49 0.80 -8 4 -12 8.88 1.20 -8 -4 12 11.13 1.17 -8 -4 13 32.76 1.69 -8 4 -13 45.64 2.27 -8 -4 14 18.14 1.10 -8 4 -14 22.98 1.53 -8 -4 15 23.07 1.23 -8 4 -15 31.86 1.70 8 5 -14 27.70 1.34 -8 -5 -13 21.59 1.14 8 5 -13 20.68 1.21 -8 -5 -12 3.09 0.57 8 5 -12 3.00 0.69 -8 -5 -11 17.07 1.11 -8 -5 -10 61.24 2.67 -8 -5 -9 10.93 0.74 8 5 -9 10.42 0.84 -8 -5 -8 0.98 0.42 -8 -5 -8 1.93 0.70 -8 -5 -7 9.85 0.80 -8 -5 -7 12.61 1.13 -8 -5 -6 12.34 0.92 -8 -5 -6 14.98 1.23 -8 -5 -5 4.86 0.67 -8 -5 -5 7.14 1.00 -8 -5 -4 0.37 0.52 -8 -5 -4 1.59 0.82 -8 -5 -3 5.58 0.74 -8 -5 -3 7.68 1.05 -8 -5 -2 8.56 0.86 -8 -5 -2 12.10 1.24 -8 -5 -1 6.15 0.78 -8 -5 -1 8.52 1.15 -8 -5 0 0.54 0.55 -8 -5 0 0.57 0.82 -8 -5 1 6.70 0.78 -8 -5 1 8.82 1.17 -8 -5 2 9.42 0.87 -8 -5 2 12.59 1.29 -8 -5 3 4.89 0.66 -8 -5 3 5.33 1.04 -8 -5 4 0.04 0.47 -8 -5 4 1.26 0.85 -8 -5 5 6.97 1.07 -8 -5 5 4.53 0.61 -8 -5 6 15.53 1.30 -8 -5 6 13.42 0.80 -8 5 -7 7.78 0.90 -8 -5 7 9.85 1.16 -8 -5 7 9.53 0.71 -8 -5 8 1.32 0.38 -8 5 -8 1.14 0.65 -8 -5 8 2.62 0.85 -8 5 -9 13.75 1.01 -8 -5 9 16.11 1.23 -8 5 -10 42.15 2.03 -8 5 -11 13.32 1.04 -8 5 -12 2.09 0.58 -8 -6 -6 11.88 0.83 8 6 -6 11.57 0.84 -8 -6 -5 7.18 0.71 -8 -6 -4 18.73 1.08 8 6 -4 11.43 0.89 -8 -6 -3 3.94 0.64 8 6 -3 2.86 0.57 -8 -6 -2 5.09 0.53 -8 -6 -2 6.75 0.77 -8 -6 -1 12.16 0.77 8 6 -1 9.62 0.87 -8 -6 0 0.49 0.38 -8 -6 0 0.86 0.59 8 6 0 0.90 0.52 -8 -6 1 11.75 0.75 8 6 1 10.65 0.90 -8 -6 2 6.18 0.79 8 6 2 4.18 0.64 -8 -6 2 5.19 0.51 -8 -6 3 4.06 0.70 8 6 3 2.61 0.56 -8 -6 4 18.43 1.22 -8 -6 5 7.54 0.79 -8 -6 6 11.57 0.91 -9 0 0 -1.36 0.82 -9 0 1 2.39 0.94 -9 0 1 2.98 0.91 -9 0 -1 2.14 0.79 -9 0 2 52.72 2.82 -9 0 2 56.91 2.78 -9 0 -2 56.86 2.75 -9 0 3 66.39 3.26 -9 0 3 66.37 3.15 -9 0 -3 69.35 3.14 -9 0 4 61.47 3.17 -9 0 4 66.05 3.08 -9 0 -4 68.73 3.07 -9 0 5 144.22 5.94 -9 0 -5 153.81 5.80 -9 0 6 0.75 0.88 -9 0 -6 1.65 1.24 -9 0 -6 0.51 0.67 -9 0 7 2.67 0.95 -9 0 -7 1.57 1.23 -9 0 -7 1.40 0.70 -9 0 8 33.06 2.01 -9 0 -8 28.59 1.72 -9 0 9 0.80 0.85 -9 0 -9 0.80 0.60 -9 0 -10 51.33 2.79 -9 0 -10 44.49 2.22 -9 0 -11 0.59 0.97 -9 0 -11 1.13 0.57 -9 0 -12 6.75 1.19 -9 0 -12 3.43 0.65 -9 0 -13 12.57 0.94 -9 0 14 10.99 0.95 -9 0 -14 5.11 0.64 -9 0 15 11.26 0.85 -9 0 -15 4.36 0.53 -9 0 16 8.48 0.64 -9 0 -16 2.58 0.40 -9 1 15 32.60 1.27 -9 -1 -15 11.54 0.83 -9 1 14 11.80 0.91 -9 -1 -14 4.95 0.58 -9 -1 -13 4.81 0.61 -9 -1 -13 6.67 0.60 -9 1 12 15.13 1.21 -9 -1 -12 12.99 0.86 -9 1 11 2.14 0.81 -9 -1 -11 1.83 0.58 -9 -1 -11 2.19 0.52 -9 1 10 9.99 1.14 -9 -1 -10 8.24 0.87 -9 -1 -10 7.71 0.77 -9 -1 -9 10.66 0.98 -9 -1 -9 11.02 0.91 -9 -1 -8 0.31 0.59 -9 -1 -8 0.80 0.57 -9 -1 -7 0.57 0.60 -9 -1 -7 1.33 0.58 -9 -1 -6 35.40 1.93 -9 -1 -6 34.56 1.82 -9 1 5 31.52 2.09 -9 -1 -5 31.16 1.82 -9 -1 -5 31.50 1.72 -9 1 4 1.45 0.97 -9 -1 -4 0.55 0.66 -9 -1 -4 1.07 0.63 -9 1 3 6.16 1.13 -9 -1 -3 6.75 0.95 -9 -1 -3 6.79 0.85 -9 1 3 5.23 0.91 -9 -1 -2 6.18 0.85 -9 1 2 5.97 0.93 -9 -1 -2 5.28 0.92 -9 1 1 72.72 3.28 -9 -1 -1 71.47 3.25 -9 -1 -1 72.88 3.11 -9 -1 0 2.26 0.80 -9 1 0 0.62 0.77 -9 -1 0 1.95 0.72 -9 -1 1 68.50 3.16 -9 -1 1 70.47 3.21 -9 1 -1 72.79 3.22 -9 -1 1 70.42 3.05 -9 -1 2 5.62 0.98 -9 -1 2 7.41 1.00 -9 1 -2 6.06 0.93 -9 -1 2 6.30 0.82 -9 -1 3 5.54 0.98 -9 1 -3 5.06 1.26 -9 -1 3 5.61 0.94 -9 1 -3 5.05 0.88 -9 -1 3 5.17 0.78 -9 -1 4 1.62 0.82 -9 1 -4 1.92 1.10 -9 1 -4 1.18 0.70 -9 -1 4 -0.27 0.41 -9 -1 5 29.96 1.62 -9 1 -5 30.63 1.96 -9 1 -5 26.98 1.43 -9 -1 6 35.13 2.09 -9 1 -6 39.23 2.43 -9 1 -6 35.06 1.95 -9 -1 7 0.89 0.80 -9 1 -7 1.65 1.12 -9 1 -7 0.92 0.63 -9 -1 8 0.94 0.83 -9 1 -8 1.12 1.03 -9 1 -8 1.16 0.61 -9 -1 9 11.08 1.17 -9 1 -9 13.28 1.49 -9 1 -9 8.42 0.91 -9 -1 10 9.73 1.05 -9 1 -10 6.30 0.82 -9 -1 11 1.96 0.78 -9 1 -11 1.34 0.54 -9 -1 12 15.27 1.18 -9 1 -12 17.01 1.45 -9 -1 13 7.94 0.86 -9 1 -13 4.97 0.62 -9 -1 14 10.31 0.88 -9 1 -14 12.33 1.10 -9 1 -15 34.15 1.49 -9 1 -15 11.90 0.82 -9 -2 -13 4.79 0.52 -9 -2 -13 16.37 0.84 -9 -2 -12 4.47 0.56 -9 -2 -12 13.04 0.83 -9 2 11 12.81 1.07 -9 -2 -11 16.20 1.00 -9 2 10 14.69 1.22 -9 -2 -10 14.64 1.03 -9 2 9 34.56 1.90 -9 -2 -9 33.03 1.67 -9 2 8 32.31 1.92 -9 -2 -8 34.35 1.72 -9 -2 -7 29.13 1.66 -9 -2 -7 36.31 1.83 -9 -2 -6 9.48 0.92 -9 -2 -6 11.90 1.06 -9 -2 -5 11.66 1.03 -9 -2 -5 14.73 1.17 -9 -2 -4 20.11 1.37 -9 -2 -4 23.61 1.51 -9 -2 -3 24.29 1.56 -9 -2 -3 28.67 1.69 -9 2 2 86.95 3.72 -9 -2 -2 88.45 3.71 -9 -2 -2 93.53 3.82 -9 2 1 93.05 3.89 -9 -2 -1 93.84 3.89 -9 -2 -1 96.24 3.96 -9 -2 0 7.68 0.96 -9 -2 0 8.68 1.02 -9 2 0 5.17 0.87 -9 -2 1 89.13 3.82 -9 2 -1 93.74 3.84 -9 -2 1 95.43 3.91 -9 2 -2 93.14 2.94 -9 -2 2 86.53 2.65 -9 2 -2 84.77 2.61 -9 -2 2 90.97 2.75 -9 -2 3 24.74 1.47 -9 2 -3 28.26 1.85 -9 2 -3 23.01 1.53 -9 -2 3 28.77 1.68 -9 -2 4 22.25 1.40 -9 2 -4 22.82 1.71 -9 2 -4 21.66 1.42 -9 -2 4 23.02 1.50 -9 -2 5 12.56 1.08 -9 2 -5 14.43 1.44 -9 2 -5 11.85 1.04 -9 -2 5 12.24 1.11 -9 -2 6 9.41 0.99 -9 2 -6 13.01 1.38 -9 2 -6 8.63 0.91 -9 -2 6 11.73 1.04 -9 -2 7 33.22 1.79 -9 2 -7 30.02 1.69 -9 -2 7 33.83 1.76 -9 -2 8 31.34 1.69 -9 2 -8 33.03 2.02 -9 2 -8 27.10 1.56 -9 -2 8 30.02 1.59 -9 -2 9 30.43 1.60 -9 2 -9 34.57 2.01 -9 -2 10 12.00 0.98 -9 2 -10 14.19 1.37 -9 -2 11 12.56 0.98 -9 2 -11 16.36 1.32 -9 -2 12 12.34 0.90 -9 2 -12 5.27 0.58 -9 -2 13 13.76 0.87 -9 2 -13 5.68 0.54 -9 -2 14 40.87 1.76 -9 -3 -12 42.44 1.83 -9 -3 -11 18.38 1.08 9 3 -11 15.48 1.02 -9 -3 -10 31.16 1.58 -9 -3 -9 26.64 1.46 -9 -3 -8 7.31 0.78 -9 -3 -8 2.24 0.39 -9 -3 -7 9.97 0.91 -9 -3 -7 3.56 0.49 -9 -3 -6 15.20 0.99 -9 -3 -6 31.12 1.51 -9 -3 -5 11.82 0.87 -9 -3 -5 21.40 1.30 -9 -3 -4 1.16 0.45 -9 -3 -4 2.71 0.72 -9 -3 -3 6.69 0.69 -9 -3 -3 11.37 1.04 -9 -3 -2 1.70 0.71 -9 -3 -1 28.50 1.71 -9 -3 0 9.62 1.04 -9 -3 1 26.61 1.66 -9 -3 2 1.66 0.71 -9 3 -3 6.98 0.71 -9 -3 3 11.27 1.06 -9 3 -4 1.40 0.72 -9 3 -4 1.91 0.49 -9 -3 4 2.95 0.74 -9 3 -5 18.43 1.29 -9 -3 5 19.54 1.30 -9 3 -6 23.79 1.45 -9 -3 6 26.93 1.43 -9 3 -7 8.53 0.98 -9 -3 7 7.57 0.84 -9 3 -8 4.59 0.83 -9 -3 8 5.00 0.70 -9 3 -9 25.62 1.58 -9 3 -10 26.71 1.59 -9 3 -11 14.49 1.10 -9 3 -12 35.04 1.71 9 4 -9 1.33 0.49 -9 -4 -4 21.86 1.33 -9 -4 -3 6.95 0.83 -9 -4 -2 4.08 0.74 -9 -4 -1 20.33 1.32 -9 -4 0 4.69 0.77 -9 -4 1 21.04 1.36 -9 -4 2 2.78 0.68 -9 -4 3 5.92 0.80 -9 -4 4 20.77 1.30 -9 -4 5 5.51 0.72 -9 -4 6 1.78 0.57 -9 -4 7 16.56 1.06 -10 0 -4 1.38 0.38 -10 0 -5 0.66 0.31 -10 0 -6 0.22 0.27 0 0 0 0.00 0.00 TITL wangr_190424_2 in P2(1)2(1)2(1) REM P2(1)2(1)2(1) (#19 in standard setting) CELL 1.54184 8.031468 8.352738 27.807791 90.0000 90.0000 90.0000 ZERR 8.00 0.000120 0.000148 0.000456 0.0000 0.0000 0.0000 LATT -1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N O UNIT 88.00 80.00 8.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 46232 _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 1.533 _oxdiff_exptl_absorpt_empirical_full_min 0.716 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 O14 O 0.60128(18) 0.54530(19) 0.48825(5) 0.0287(3) Uani 1 1 d . O20 O 0.70027(19) 0.40915(19) 0.42563(5) 0.0296(3) Uani 1 1 d . O22 O -0.00731(18) 0.5436(2) 0.31871(5) 0.0308(4) Uani 1 1 d . O18 O 0.3857(2) 0.6616(2) 0.63433(6) 0.0372(4) Uani 1 1 d . O24 O 0.0526(2) 0.6026(3) 0.24179(6) 0.0418(4) Uani 1 1 d . O25 O 0.2376(2) 0.2657(2) 0.29562(6) 0.0387(4) Uani 1 1 d . H25 H 0.155593 0.208639 0.291737 0.058 Uiso 1 1 calc GR C5 C 0.3053(2) 0.4935(3) 0.34529(7) 0.0254(4) Uani 1 1 d . C9 C 0.4411(3) 0.7224(3) 0.38899(8) 0.0279(4) Uani 1 1 d . H9A H 0.549972 0.721665 0.404094 0.033 Uiso 1 1 calc R H9B H 0.366455 0.782991 0.409501 0.033 Uiso 1 1 calc R C13 C 0.5820(3) 0.4645(3) 0.44641(7) 0.0251(4) Uani 1 1 d . C15 C 0.4256(3) 0.6008(3) 0.55697(8) 0.0280(4) Uani 1 1 d . C10 C 0.3782(2) 0.5521(2) 0.38508(7) 0.0240(4) Uani 1 1 d . C8 C 0.4539(3) 0.8052(3) 0.34044(8) 0.0298(5) Uani 1 1 d . H8A H 0.471245 0.919147 0.344971 0.036 Uiso 1 1 calc R H8B H 0.547707 0.762677 0.322568 0.036 Uiso 1 1 calc R C1 C 0.3985(3) 0.4551(2) 0.43142(7) 0.0243(4) Uani 1 1 d . C6 C 0.2755(3) 0.5972(3) 0.30042(7) 0.0284(4) Uani 1 1 d . C11 C 0.4454(3) 0.6197(3) 0.50395(8) 0.0269(4) Uani 1 1 d . H11 H 0.447212 0.733860 0.495844 0.032 Uiso 1 1 calc R C16 C 0.4014(3) 0.4556(3) 0.58376(8) 0.0333(5) Uani 1 1 d . H16 H 0.401365 0.351865 0.571591 0.040 Uiso 1 1 calc R C4 C 0.2419(3) 0.3215(3) 0.34414(8) 0.0295(5) Uani 1 1 d . H4 H 0.127901 0.320513 0.356738 0.035 Uiso 1 1 calc R C21 C 0.0970(3) 0.5789(3) 0.28273(7) 0.0304(5) Uani 1 1 d . C19 C 0.4150(3) 0.7206(3) 0.58959(8) 0.0336(5) Uani 1 1 d . H19 H 0.426221 0.828736 0.582358 0.040 Uiso 1 1 calc R C2 C 0.3400(3) 0.2774(3) 0.42720(8) 0.0287(4) Uani 1 1 d . H2 H 0.222165 0.276214 0.436354 0.034 Uiso 1 1 calc R C12 C 0.3102(3) 0.5359(3) 0.47445(7) 0.0274(4) Uani 1 1 d . H12A H 0.228905 0.613102 0.463139 0.033 Uiso 1 1 calc R H12B H 0.253445 0.456446 0.493876 0.033 Uiso 1 1 calc R C3 C 0.3476(3) 0.2165(3) 0.37587(8) 0.0310(5) Uani 1 1 d . H3A H 0.461915 0.217793 0.364614 0.037 Uiso 1 1 calc R H3B H 0.307410 0.107115 0.374536 0.037 Uiso 1 1 calc R C7 C 0.2944(3) 0.7770(3) 0.31282(8) 0.0312(5) Uani 1 1 d . H7A H 0.295633 0.839476 0.283424 0.037 Uiso 1 1 calc R H7B H 0.200145 0.811585 0.332001 0.037 Uiso 1 1 calc R C17 C 0.3786(3) 0.4990(3) 0.62987(8) 0.0350(5) Uani 1 1 d . H17 H 0.360684 0.428221 0.655161 0.042 Uiso 1 1 calc R C27 C 0.3945(3) 0.5546(3) 0.25900(8) 0.0342(5) Uani 1 1 d . H27A H 0.507459 0.571560 0.269115 0.051 Uiso 1 1 calc GR H27B H 0.370809 0.621367 0.231743 0.051 Uiso 1 1 calc GR H27C H 0.379624 0.444330 0.250287 0.051 Uiso 1 1 calc GR C23 C -0.1803(3) 0.5271(4) 0.30569(9) 0.0380(6) Uani 1 1 d . H23A H -0.193385 0.436626 0.284720 0.057 Uiso 1 1 calc GR H23B H -0.216913 0.622261 0.289503 0.057 Uiso 1 1 calc GR H23C H -0.245725 0.511245 0.334190 0.057 Uiso 1 1 calc GR C26 C 0.4287(3) 0.1646(3) 0.46197(9) 0.0369(5) Uani 1 1 d . H26A H 0.541551 0.148985 0.451566 0.055 Uiso 1 1 calc GR H26B H 0.372093 0.063364 0.462581 0.055 Uiso 1 1 calc GR H26C H 0.428367 0.210370 0.493632 0.055 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 O14 0.0210(7) 0.0390(8) 0.0261(7) -0.0018(6) 0.0003(6) -0.0002(6) O20 0.0230(7) 0.0343(8) 0.0314(7) 0.0014(6) 0.0014(6) 0.0040(6) O22 0.0196(7) 0.0490(9) 0.0239(7) -0.0041(7) -0.0004(5) 0.0034(6) O18 0.0349(9) 0.0508(10) 0.0259(7) -0.0074(7) 0.0034(7) -0.0052(8) O24 0.0277(8) 0.0738(13) 0.0237(8) 0.0007(8) -0.0026(6) 0.0094(8) O25 0.0346(9) 0.0479(10) 0.0337(8) -0.0139(7) -0.0012(7) -0.0087(8) C5 0.0191(9) 0.0320(11) 0.0251(9) -0.0025(8) 0.0011(8) 0.0050(8) C9 0.0287(10) 0.0262(10) 0.0288(10) -0.0021(8) -0.0002(8) 0.0007(8) C13 0.0233(10) 0.0284(10) 0.0234(9) 0.0031(7) -0.0020(8) -0.0001(8) C15 0.0212(9) 0.0344(11) 0.0285(10) -0.0023(8) -0.0020(8) 0.0003(8) C10 0.0204(9) 0.0250(10) 0.0266(9) -0.0014(8) -0.0002(8) 0.0043(8) C8 0.0297(11) 0.0286(11) 0.0310(10) 0.0022(8) 0.0036(9) 0.0025(9) C1 0.0216(9) 0.0269(10) 0.0244(9) 0.0004(8) -0.0009(7) 0.0008(8) C6 0.0211(10) 0.0408(12) 0.0233(9) -0.0011(9) 0.0002(7) 0.0039(9) C11 0.0232(10) 0.0297(10) 0.0279(10) -0.0009(8) 0.0005(8) 0.0021(8) C16 0.0340(12) 0.0374(12) 0.0286(10) 0.0007(9) -0.0018(9) 0.0033(10) C4 0.0245(10) 0.0359(12) 0.0280(10) -0.0080(8) -0.0009(8) -0.0010(9) C21 0.0259(11) 0.0432(12) 0.0220(9) -0.0024(9) 0.0015(8) 0.0076(10) C19 0.0303(11) 0.0403(12) 0.0303(10) -0.0047(9) 0.0018(9) -0.0045(10) C2 0.0237(10) 0.0269(10) 0.0355(11) 0.0027(9) -0.0002(8) -0.0018(8) C12 0.0211(10) 0.0339(11) 0.0271(10) -0.0014(8) -0.0003(8) 0.0002(8) C3 0.0289(11) 0.0266(10) 0.0374(12) -0.0034(9) 0.0021(9) -0.0008(8) C7 0.0288(11) 0.0356(12) 0.0292(10) 0.0058(9) 0.0014(9) 0.0080(9) C17 0.0308(11) 0.0450(13) 0.0293(10) 0.0033(10) -0.0007(9) -0.0013(10) C27 0.0244(10) 0.0507(14) 0.0275(10) -0.0031(10) 0.0014(8) 0.0051(10) C23 0.0204(10) 0.0617(16) 0.0319(11) -0.0087(11) -0.0038(8) 0.0038(11) C26 0.0378(13) 0.0320(11) 0.0410(12) 0.0080(10) -0.0006(11) 0.0004(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C13 O14 C11 111.72(16) C21 O22 C23 115.90(17) C19 O18 C17 106.56(19) C4 O25 H25 109.5 C10 C5 C6 122.0(2) C10 C5 C4 120.38(19) C4 C5 C6 117.51(18) H9A C9 H9B 107.8 C10 C9 H9A 109.0 C10 C9 H9B 109.0 C10 C9 C8 112.72(18) C8 C9 H9A 109.0 C8 C9 H9B 109.0 O14 C13 C1 111.65(17) O20 C13 O14 120.90(19) O20 C13 C1 127.45(19) C16 C15 C11 128.0(2) C19 C15 C11 126.3(2) C19 C15 C16 105.6(2) C5 C10 C9 123.15(19) C5 C10 C1 123.17(19) C9 C10 C1 113.64(17) C9 C8 H8A 109.9 C9 C8 H8B 109.9 H8A C8 H8B 108.3 C7 C8 C9 108.83(18) C7 C8 H8A 109.9 C7 C8 H8B 109.9 C13 C1 C2 110.98(17) C13 C1 C12 101.99(16) C10 C1 C13 107.70(17) C10 C1 C2 114.06(17) C10 C1 C12 111.84(17) C12 C1 C2 109.60(17) C5 C6 C7 110.52(17) C5 C6 C27 112.38(18) C21 C6 C5 110.59(18) C21 C6 C7 105.15(18) C21 C6 C27 108.64(17) C27 C6 C7 109.30(19) O14 C11 C15 109.96(17) O14 C11 H11 109.4 O14 C11 C12 104.63(16) C15 C11 H11 109.4 C15 C11 C12 113.96(18) C12 C11 H11 109.4 C15 C16 H16 126.7 C17 C16 C15 106.5(2) C17 C16 H16 126.7 O25 C4 C5 109.59(19) O25 C4 H4 108.2 O25 C4 C3 112.16(19) C5 C4 H4 108.2 C3 C4 C5 110.36(17) C3 C4 H4 108.2 O22 C21 C6 111.72(17) O24 C21 O22 123.7(2) O24 C21 C6 124.4(2) O18 C19 H19 124.6 C15 C19 O18 110.9(2) C15 C19 H19 124.6 C1 C2 H2 106.3 C3 C2 C1 112.16(18) C3 C2 H2 106.3 C3 C2 C26 111.75(19) C26 C2 C1 113.51(18) C26 C2 H2 106.3 C1 C12 H12A 110.4 C1 C12 H12B 110.4 C11 C12 C1 106.82(17) C11 C12 H12A 110.4 C11 C12 H12B 110.4 H12A C12 H12B 108.6 C4 C3 C2 109.49(18) C4 C3 H3A 109.8 C4 C3 H3B 109.8 C2 C3 H3A 109.8 C2 C3 H3B 109.8 H3A C3 H3B 108.2 C8 C7 C6 110.32(18) C8 C7 H7A 109.6 C8 C7 H7B 109.6 C6 C7 H7A 109.6 C6 C7 H7B 109.6 H7A C7 H7B 108.1 O18 C17 H17 124.8 C16 C17 O18 110.4(2) C16 C17 H17 124.8 C6 C27 H27A 109.5 C6 C27 H27B 109.5 C6 C27 H27C 109.5 H27A C27 H27B 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 O22 C23 H23A 109.5 O22 C23 H23B 109.5 O22 C23 H23C 109.5 H23A C23 H23B 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 C2 C26 H26A 109.5 C2 C26 H26B 109.5 C2 C26 H26C 109.5 H26A C26 H26B 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O14 C13 1.354(3) O14 C11 1.464(3) O20 C13 1.204(3) O22 C21 1.338(3) O22 C23 1.442(3) O18 C19 1.359(3) O18 C17 1.364(3) O24 C21 1.209(3) O25 H25 0.8200 O25 C4 1.428(3) C5 C10 1.344(3) C5 C6 1.538(3) C5 C4 1.525(3) C9 H9A 0.9700 C9 H9B 0.9700 C9 C10 1.514(3) C9 C8 1.521(3) C13 C1 1.534(3) C15 C11 1.491(3) C15 C16 1.437(3) C15 C19 1.353(3) C10 C1 1.531(3) C8 H8A 0.9700 C8 H8B 0.9700 C8 C7 1.512(3) C1 C2 1.562(3) C1 C12 1.546(3) C6 C21 1.523(3) C6 C7 1.548(3) C6 C27 1.539(3) C11 H11 0.9800 C11 C12 1.530(3) C16 H16 0.9300 C16 C17 1.345(3) C4 H4 0.9800 C4 C3 1.506(3) C19 H19 0.9300 C2 H2 0.9800 C2 C3 1.516(3) C2 C26 1.527(3) C12 H12A 0.9700 C12 H12B 0.9700 C3 H3A 0.9700 C3 H3B 0.9700 C7 H7A 0.9700 C7 H7B 0.9700 C17 H17 0.9300 C27 H27A 0.9600 C27 H27B 0.9600 C27 H27C 0.9600 C23 H23A 0.9600 C23 H23B 0.9600 C23 H23C 0.9600 C26 H26A 0.9600 C26 H26B 0.9600 C26 H26C 0.9600 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 O14 C13 C1 C10 114.00(18) O14 C13 C1 C2 -120.51(19) O14 C13 C1 C12 -3.8(2) O14 C11 C12 C1 -17.9(2) O20 C13 C1 C10 -66.5(3) O20 C13 C1 C2 59.0(3) O20 C13 C1 C12 175.7(2) O25 C4 C3 C2 -177.21(18) C5 C10 C1 C13 128.3(2) C5 C10 C1 C2 4.7(3) C5 C10 C1 C12 -120.4(2) C5 C6 C21 O22 28.6(3) C5 C6 C21 O24 -155.5(2) C5 C6 C7 C8 48.9(2) C5 C4 C3 C2 60.3(2) C9 C10 C1 C13 -54.2(2) C9 C10 C1 C2 -177.85(17) C9 C10 C1 C12 57.1(2) C9 C8 C7 C6 -65.9(2) C13 O14 C11 C15 138.96(18) C13 O14 C11 C12 16.2(2) C13 C1 C2 C3 -96.6(2) C13 C1 C2 C26 31.3(3) C13 C1 C12 C11 13.3(2) C15 C11 C12 C1 -138.05(19) C15 C16 C17 O18 0.4(3) C10 C5 C6 C21 -131.5(2) C10 C5 C6 C7 -15.5(3) C10 C5 C6 C27 106.9(2) C10 C5 C4 O25 -155.18(19) C10 C5 C4 C3 -31.2(3) C10 C9 C8 C7 47.4(2) C10 C1 C2 C3 25.3(2) C10 C1 C2 C26 153.11(19) C10 C1 C12 C11 -101.53(19) C8 C9 C10 C5 -14.6(3) C8 C9 C10 C1 167.89(17) C1 C2 C3 C4 -57.8(2) C6 C5 C10 C9 -1.6(3) C6 C5 C10 C1 175.63(18) C6 C5 C4 O25 27.4(2) C6 C5 C4 C3 151.42(19) C11 O14 C13 O20 172.60(19) C11 O14 C13 C1 -7.9(2) C11 C15 C16 C17 -175.8(2) C11 C15 C19 O18 175.6(2) C16 C15 C11 O14 -66.3(3) C16 C15 C11 C12 50.8(3) C16 C15 C19 O18 -0.2(3) C4 C5 C10 C9 -178.88(18) C4 C5 C10 C1 -1.6(3) C4 C5 C6 C21 45.9(2) C4 C5 C6 C7 161.87(18) C4 C5 C6 C27 -75.7(2) C21 C6 C7 C8 168.25(17) C19 O18 C17 C16 -0.5(3) C19 C15 C11 O14 118.9(2) C19 C15 C11 C12 -124.0(2) C19 C15 C16 C17 -0.1(2) C2 C1 C12 C11 130.97(18) C12 C1 C2 C3 151.53(18) C12 C1 C2 C26 -80.6(2) C7 C6 C21 O22 -90.8(2) C7 C6 C21 O24 85.1(3) C17 O18 C19 C15 0.4(3) C27 C6 C21 O22 152.3(2) C27 C6 C21 O24 -31.8(3) C27 C6 C7 C8 -75.3(2) C23 O22 C21 O24 2.9(3) C23 O22 C21 C6 178.8(2) C26 C2 C3 C4 173.47(19)