#------------------------------------------------------------------------------ #$Date: 2020-05-06 00:40:03 +0300 (Wed, 06 May 2020) $ #$Revision: 251780 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/80/1558008.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_1558008 loop_ _publ_author_name 'Ma, Lie-Feng' 'Chen, Meng-Jia' 'Liang, Dong-E' 'Shi, Lin-Mei' 'Ying, You-Min' 'Shan, Wei-Guang' 'Li, Guo-Qiang' 'Zhan, Zha-Jun' _publ_section_title ; Streptomyces albogriseolus SY67903 Produces Eunicellin Diterpenoids Structurally Similar to Terpenes of the Gorgonian Muricella sibogae, the Bacterial Source ; _journal_name_full 'Journal of Natural Products' _journal_paper_doi 10.1021/acs.jnatprod.0c00147 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C21 H30 O5, C H4 O' _chemical_formula_sum 'C22 H34 O6' _chemical_formula_weight 394.49 _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 mixed _atom_sites_solution_primary dual _audit_creation_date 2020-04-09 _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 9.2746(3) _cell_length_b 10.2656(3) _cell_length_c 22.5834(7) _cell_measurement_reflns_used 9889 _cell_measurement_temperature 170(2) _cell_measurement_theta_max 72.25 _cell_measurement_theta_min 4.31 _cell_volume 2150.15(12) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 170.0 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_unetI/netI 0.0191 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 37206 _diffrn_reflns_point_group_measured_fraction_full 0.988 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 72.254 _diffrn_reflns_theta_min 4.732 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.711 _exptl_absorpt_correction_T_max 0.7536 _exptl_absorpt_correction_T_min 0.5800 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1535 before and 0.0539 after correction. The Ratio of minimum to maximum transmission is 0.7696. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.219 _exptl_crystal_description block _exptl_crystal_F_000 856 _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.32 _refine_diff_density_max 0.244 _refine_diff_density_min -0.192 _refine_diff_density_rms 0.052 _refine_ls_abs_structure_details ; Flack x determined using 1791 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 262 _refine_ls_number_reflns 4205 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.109 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0301 _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^)+(0.0529P)^2^+0.3346P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0897 _refine_ls_wR_factor_ref 0.0898 _reflns_Friedel_coverage 0.749 _reflns_Friedel_fraction_full 0.991 _reflns_Friedel_fraction_max 0.990 _reflns_number_gt 4196 _reflns_number_total 4205 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file np0c00147_si_003.cif _cod_data_source_block 191119_hm183_17_0m _cod_database_code 1558008 _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 0.804 _shelx_estimated_absorpt_t_min 0.722 _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 C(H,H,H,H) groups, All O(H) groups 2. Restrained distances O6-H6A 0.84 with sigma of 0.02 3.a Ternary CH refined with riding coordinates: C1(H1A), C8(H8), C10(H10), C14(H14), C18(H18) 3.b Secondary CH2 refined with riding coordinates: C4(H4A,H4B), C5(H5A,H5B), C9(H9A,H9B), C12(H12A,H12B), C13(H13A,H13B) 3.c Aromatic/amide H refined with riding coordinates: C2(H2A), C6(H6) 3.d X=CH2 refined with riding coordinates: C17(H17A,H17B) 3.e Idealised Me refined as rotating group: C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B, H22C) 3.f Idealised tetrahedral OH refined as rotating group: O1(H1), O2(H2) ; _shelx_res_file ; TITL 191119_hm183_17_0m_a.res in P2(1)2(1)2(1) 191119_hm183_17_0m.res created by SHELXL-2016/6 at 15:01:42 on 09-Apr-2020 REM Old TITL 191119_HM183_17_0m in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.124, Rweak 0.034, Alpha 0.005, Orientation as input REM Flack x = 0.113 ( 0.031 ) from Parsons' quotients REM Formula found by SHELXT: C21 O7 CELL 1.54178 9.2746 10.2656 22.5834 90 90 90 ZERR 4 0.0003 0.0003 0.0007 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 88 136 24 DFIX 0.84 O6 H6a L.S. 20 0 0 PLAN 20 SIZE 0.32 0.36 0.49 TEMP -103.15 BOND $H htab list 4 fmap 2 53 acta REM REM REM WGHT 0.052900 0.334600 FVAR 1.40264 O1 3 0.766153 0.705118 0.254642 11.00000 0.05208 0.03911 = 0.02300 0.00810 -0.00071 -0.01080 AFIX 147 H1 2 0.769433 0.785950 0.249019 11.00000 -1.50000 AFIX 0 O2 3 0.509782 0.619755 0.255905 11.00000 0.04870 0.08149 = 0.02543 -0.00589 -0.00450 -0.02076 AFIX 147 H2 2 0.590235 0.649285 0.245340 11.00000 -1.50000 AFIX 0 O3 3 0.380275 0.606664 0.337112 11.00000 0.03182 0.04429 = 0.03195 -0.00400 -0.00589 -0.00270 O4 3 0.500504 0.639031 0.592532 11.00000 0.04453 0.05341 = 0.03075 -0.01170 0.00405 0.01787 O5 3 0.711280 0.534686 0.596193 11.00000 0.03493 0.03785 = 0.02191 -0.00246 -0.00191 0.00530 C1 1 0.707431 0.431708 0.415748 11.00000 0.01850 0.01819 = 0.02074 -0.00041 0.00072 0.00041 AFIX 13 H1A 2 0.621489 0.467875 0.394660 11.00000 -1.20000 AFIX 0 C2 1 0.691177 0.465168 0.480388 11.00000 0.02158 0.01717 = 0.02211 0.00181 -0.00028 -0.00112 AFIX 43 H2A 2 0.759499 0.428450 0.506915 11.00000 -1.20000 AFIX 0 C3 1 0.589237 0.541947 0.503922 11.00000 0.02180 0.01665 = 0.02394 0.00034 0.00119 -0.00243 C4 1 0.461768 0.597849 0.470651 11.00000 0.02179 0.02409 = 0.02769 -0.00415 -0.00099 0.00321 AFIX 23 H4A 2 0.378537 0.602073 0.498031 11.00000 -1.20000 H4B 2 0.435990 0.537022 0.438323 11.00000 -1.20000 AFIX 0 C5 1 0.485098 0.734975 0.443568 11.00000 0.03842 0.02183 = 0.02729 -0.00330 -0.00361 0.00977 AFIX 23 H5A 2 0.396605 0.761699 0.422275 11.00000 -1.20000 H5B 2 0.501899 0.798327 0.475892 11.00000 -1.20000 AFIX 0 C6 1 0.610724 0.738728 0.401429 11.00000 0.03568 0.01538 = 0.02984 0.00167 -0.00718 0.00111 AFIX 43 H6 2 0.695308 0.779634 0.416165 11.00000 -1.20000 AFIX 0 C7 1 0.620196 0.692494 0.346002 11.00000 0.03370 0.01835 = 0.02596 0.00284 -0.00433 -0.00085 C8 1 0.768315 0.678691 0.317516 11.00000 0.03653 0.02704 = 0.02248 0.00415 -0.00159 -0.00902 AFIX 13 H8 2 0.835932 0.741318 0.336990 11.00000 -1.20000 AFIX 0 C9 1 0.827258 0.540178 0.325608 11.00000 0.02939 0.03034 = 0.02225 -0.00016 0.00430 -0.00396 AFIX 23 H9A 2 0.922489 0.533172 0.306063 11.00000 -1.20000 H9B 2 0.761233 0.477259 0.306412 11.00000 -1.20000 AFIX 0 C10 1 0.842813 0.505569 0.391989 11.00000 0.02159 0.02235 = 0.02218 -0.00161 0.00164 -0.00188 AFIX 13 H10 2 0.847105 0.590143 0.413891 11.00000 -1.20000 AFIX 0 C11 1 0.982529 0.434837 0.405332 11.00000 0.02126 0.03067 = 0.02706 -0.00279 0.00429 0.00052 C12 1 0.983659 0.290774 0.392974 11.00000 0.02232 0.03301 = 0.04316 -0.00807 0.00081 0.00560 AFIX 23 H12A 2 1.074696 0.252509 0.407853 11.00000 -1.20000 H12B 2 0.979265 0.276046 0.349688 11.00000 -1.20000 AFIX 0 C13 1 0.855819 0.223379 0.422715 11.00000 0.02532 0.02256 = 0.03674 -0.00296 -0.00225 0.00451 AFIX 23 H13A 2 0.864327 0.232084 0.466233 11.00000 -1.20000 H13B 2 0.857025 0.129412 0.412866 11.00000 -1.20000 AFIX 0 C14 1 0.713172 0.283394 0.402149 11.00000 0.02276 0.01871 = 0.02357 -0.00219 0.00042 0.00173 AFIX 13 H14 2 0.711441 0.274960 0.358041 11.00000 -1.20000 AFIX 0 C15 1 0.593551 0.577090 0.568041 11.00000 0.02580 0.01934 = 0.02537 0.00085 0.00379 -0.00246 C16 1 0.493515 0.636767 0.313629 11.00000 0.03616 0.02885 = 0.02580 0.00177 -0.00589 -0.00043 C17 1 1.095885 0.497177 0.426335 11.00000 0.02463 0.04313 = 0.04561 -0.00855 0.00014 -0.00125 AFIX 93 H17A 2 1.182552 0.451020 0.434244 11.00000 -1.20000 H17B 2 1.090861 0.588233 0.433554 11.00000 -1.20000 AFIX 0 C18 1 0.578781 0.211568 0.425097 11.00000 0.02720 0.02067 = 0.02768 -0.00104 0.00310 -0.00201 AFIX 13 H18 2 0.569862 0.229105 0.468499 11.00000 -1.20000 AFIX 0 C19 1 0.587030 0.064030 0.416208 11.00000 0.03612 0.02073 = 0.05565 0.00295 0.00608 -0.00173 AFIX 137 H19A 2 0.598325 0.044722 0.373964 11.00000 -1.50000 H19B 2 0.498254 0.023559 0.430886 11.00000 -1.50000 H19C 2 0.669795 0.029290 0.438081 11.00000 -1.50000 AFIX 0 C20 1 0.441778 0.259791 0.394902 11.00000 0.02368 0.02418 = 0.05493 -0.00226 -0.00249 -0.00400 AFIX 137 H20A 2 0.428069 0.352478 0.403636 11.00000 -1.50000 H20B 2 0.358885 0.210280 0.409655 11.00000 -1.50000 H20C 2 0.450319 0.247612 0.352005 11.00000 -1.50000 AFIX 0 C21 1 0.723277 0.567199 0.658136 11.00000 0.04754 0.05262 = 0.02153 -0.00189 -0.00241 -0.00206 AFIX 137 H21A 2 0.699902 0.659458 0.663809 11.00000 -1.50000 H21B 2 0.822037 0.550684 0.671617 11.00000 -1.50000 H21C 2 0.656042 0.513544 0.681067 11.00000 -1.50000 AFIX 0 O6 3 0.189634 0.458103 0.267991 11.00000 0.04814 0.03772 = 0.03273 -0.00396 -0.00668 -0.00368 C22 1 0.161186 0.545497 0.221539 11.00000 0.04391 0.06492 = 0.03523 0.01005 -0.00215 -0.00626 AFIX 137 H22A 2 0.119864 0.497961 0.187950 11.00000 -1.50000 H22B 2 0.251159 0.587616 0.209242 11.00000 -1.50000 H22C 2 0.092698 0.611856 0.235033 11.00000 -1.50000 AFIX 0 H6A 2 0.235590 0.501555 0.291411 11.00000 -1.50000 HKLF 4 REM 191119_hm183_17_0m_a.res in P2(1)2(1)2(1) REM R1 = 0.0301 for 4196 Fo > 4sig(Fo) and 0.0302 for all 4205 data REM 262 parameters refined using 1 restraints END WGHT 0.0529 0.3346 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, y+1/2, -z+1/2 HTAB O1 O6_$1 HTAB O2 O1 EQIV $2 x+1/2, -y+3/2, -z+1 HTAB C8 O4_$2 HTAB C22 O2 HTAB O6 O3 REM Highest difference peak 0.244, deepest hole -0.192, 1-sigma level 0.052 Q1 1 0.7768 0.4635 0.4022 11.00000 0.05 0.24 Q2 1 0.9132 0.4710 0.4025 11.00000 0.05 0.22 Q3 1 0.7830 0.2573 0.4123 11.00000 0.05 0.21 Q4 1 0.6440 0.2407 0.4074 11.00000 0.05 0.19 Q5 1 0.5757 0.6446 0.3357 11.00000 0.05 0.18 Q6 1 0.6816 0.6957 0.3287 11.00000 0.05 0.17 Q7 1 0.6245 0.5717 0.6670 11.00000 0.05 0.16 Q8 1 0.6089 0.6599 0.3737 11.00000 0.05 0.15 Q9 1 0.9140 0.2557 0.4079 11.00000 0.05 0.15 Q10 1 0.7966 0.4611 0.4995 11.00000 0.05 0.15 Q11 1 0.1316 0.5989 0.3230 11.00000 0.05 0.15 Q12 1 0.8874 0.3806 0.4651 11.00000 0.05 0.15 Q13 1 0.3651 0.4971 0.5356 11.00000 0.05 0.15 Q14 1 0.6340 0.4872 0.3603 11.00000 0.05 0.14 Q15 1 0.6357 0.5008 0.3036 11.00000 0.05 0.14 Q16 1 0.6134 0.5410 0.3135 11.00000 0.05 0.14 Q17 1 0.6553 0.8459 0.3336 11.00000 0.05 0.14 Q18 1 1.1163 0.3558 0.3232 11.00000 0.05 0.14 Q19 1 1.1370 0.3207 0.3206 11.00000 0.05 0.14 Q20 1 0.3912 0.5753 0.4826 11.00000 0.05 0.14 ; _shelx_res_checksum 33919 _shelx_hkl_file ; -2 0 0 536.55 20.10 -2 0 0 552.34 20.50 2 0 0 536.95 20.30 2 0 0 466.15 21.30 -3 0 0 2.10 1.10 3 0 0 3.90 0.90 3 0 0 2.80 0.90 4 0 0 2191.78 84.09 4 0 0 2142.49 84.39 -4 0 0 2300.97 84.59 4 0 0 2260.87 84.59 5 0 0 1.70 1.20 5 0 0 5.20 1.40 -5 0 0 4.20 1.80 6 0 0 387.46 18.30 6 0 0 389.46 17.40 -7 0 0 9.10 2.40 -7 0 0 -0.70 1.40 -7 0 0 2.40 2.50 -7 0 0 2.40 7.20 7 0 0 0.30 1.50 7 0 0 0.20 1.30 -8 0 0 427.16 18.90 -8 0 0 474.45 19.60 -8 0 0 424.46 24.40 8 0 0 426.86 21.40 -8 0 0 379.96 39.80 -8 0 0 502.85 22.10 -8 0 0 443.66 19.40 8 0 0 417.86 21.60 -9 0 0 0.10 1.60 -9 0 0 2.80 2.70 -9 0 0 2.00 1.80 -9 0 0 7.90 2.20 -9 0 0 5.40 8.60 -9 0 0 0.30 1.70 9 0 0 1.60 0.90 -10 0 0 1634.94 62.09 -10 0 0 1655.73 61.59 -10 0 0 1620.84 63.29 -10 0 0 1585.94 61.39 -10 0 0 1539.25 61.09 -11 0 0 -0.90 1.30 11 0 0 -0.50 1.20 -11 0 0 0.40 1.00 -11 0 0 1.30 1.00 -11 0 0 0.30 4.30 -11 0 0 0.90 1.00 -11 0 0 -0.50 0.90 0 1 0 5.40 0.60 -2 -1 0 465.95 18.30 2 -1 0 484.65 18.60 2 -1 0 474.45 18.80 2 1 0 456.05 17.70 2 1 0 461.75 17.50 2 1 0 451.05 17.40 -2 1 0 450.25 18.30 4 -1 0 1751.92 66.69 4 -1 0 1741.43 66.09 -4 -1 0 1726.73 65.89 4 1 0 1724.43 65.29 4 1 0 1671.03 65.09 4 1 0 1800.12 64.99 -4 1 0 1629.44 65.39 -5 -1 0 449.66 19.40 5 -1 0 427.26 19.10 5 -1 0 460.95 20.10 5 1 0 457.55 18.80 -5 1 0 408.56 18.30 5 1 0 414.36 17.90 6 -1 0 1278.37 54.19 -6 -1 0 1291.37 53.39 6 -1 0 1385.26 53.29 6 1 0 1417.36 51.99 6 1 0 1321.27 52.99 -7 -1 0 172.78 10.30 -7 -1 0 134.69 7.70 7 -1 0 140.09 8.80 7 -1 0 138.49 10.10 -7 -1 0 154.88 9.20 -7 -1 0 156.98 8.80 -7 -1 0 149.19 8.20 -7 1 0 126.79 8.40 7 1 0 152.08 9.20 -7 1 0 148.09 8.80 7 1 0 154.48 7.80 -7 1 0 153.08 10.30 -7 1 0 138.09 7.70 -7 1 0 114.89 20.90 -8 -1 0 514.65 22.30 -8 -1 0 526.35 24.50 8 -1 0 490.45 21.00 -8 -1 0 428.56 42.80 8 -1 0 515.15 25.60 8 -1 0 577.44 24.70 -8 -1 0 537.65 22.10 -8 1 0 534.55 24.80 -8 1 0 516.45 21.70 -8 1 0 529.75 23.20 8 1 0 535.65 24.00 -8 1 0 538.25 22.40 -9 -1 0 54.39 4.50 -9 -1 0 62.79 5.00 -9 -1 0 62.09 6.40 -9 -1 0 50.79 16.70 -9 -1 0 69.89 7.60 9 -1 0 55.69 3.70 -9 -1 0 57.59 4.80 -9 1 0 42.00 15.00 -9 1 0 58.19 5.30 -9 1 0 55.49 4.50 -9 1 0 57.49 6.70 -9 1 0 62.89 5.10 -9 1 0 58.99 4.90 -10 -1 0 5.40 1.80 -10 -1 0 3.00 7.00 -10 -1 0 3.80 1.50 10 -1 0 1.90 1.20 -10 -1 0 2.50 1.50 -10 -1 0 3.50 2.30 -10 1 0 1.40 1.60 -10 1 0 1.60 2.20 10 1 0 1.50 1.10 -10 1 0 2.10 6.30 -10 1 0 2.50 1.50 -10 1 0 2.00 1.60 -10 1 0 2.40 1.60 -11 -1 0 81.59 4.00 -11 -1 0 80.59 5.20 11 -1 0 82.89 4.30 -11 -1 0 82.99 4.20 -11 -1 0 82.59 4.30 -11 -1 0 73.99 12.10 -11 1 0 82.79 4.20 -11 1 0 82.59 4.20 -11 1 0 90.09 5.40 -11 1 0 66.59 4.90 -11 1 0 78.99 11.10 -11 1 0 82.29 5.20 0 2 0 4753.22 176.58 -4 -2 0 2122.89 82.49 4 -2 0 2222.78 83.99 4 -2 0 2108.99 83.09 4 2 0 2089.49 81.09 -4 2 0 2177.98 82.69 4 2 0 2310.57 80.79 4 2 0 2152.08 80.89 -5 -2 0 12.20 2.50 5 -2 0 10.70 2.30 5 -2 0 7.00 2.20 -5 2 0 8.70 2.10 5 2 0 13.20 1.60 5 2 0 10.20 1.60 5 2 0 10.60 1.20 -6 -2 0 438.06 20.20 6 -2 0 408.36 20.00 6 -2 0 463.15 21.80 6 2 0 450.15 18.90 6 2 0 425.86 17.40 -7 -2 0 902.91 34.90 -7 -2 0 885.41 35.60 7 -2 0 934.51 39.00 -7 -2 0 894.01 34.80 7 -2 0 806.52 33.40 7 -2 0 871.71 36.70 -7 2 0 764.42 56.59 -7 2 0 832.42 35.40 -7 2 0 818.92 34.40 7 2 0 894.41 35.30 8 -2 0 1297.47 50.19 -8 -2 0 1323.67 51.09 8 -2 0 1335.57 53.59 -8 -2 0 1373.26 52.29 -8 -2 0 1309.07 53.19 -8 -2 0 1318.57 51.39 -8 -2 0 1369.16 51.39 8 -2 0 1235.08 55.49 -8 2 0 1241.18 50.99 -8 2 0 1313.37 52.29 -8 2 0 1265.57 50.59 -8 2 0 1337.87 53.99 8 2 0 1272.97 51.79 -9 -2 0 937.61 36.60 -9 -2 0 963.30 37.50 -9 -2 0 786.22 59.09 -9 -2 0 963.80 37.00 -9 -2 0 935.81 38.60 -9 -2 0 937.01 37.00 -9 2 0 983.30 37.20 -9 2 0 895.71 36.20 -9 2 0 921.31 39.10 -9 2 0 920.81 36.60 -10 -2 0 337.17 13.90 -10 -2 0 302.07 13.90 -10 -2 0 325.17 13.80 -10 -2 0 328.27 15.30 10 -2 0 342.37 14.20 -10 -2 0 329.07 14.00 -10 2 0 314.77 15.60 -10 2 0 344.17 14.30 -10 2 0 322.77 13.60 -10 2 0 310.87 14.60 -10 2 0 312.27 13.70 -11 -2 0 254.47 20.50 -11 -2 0 274.27 11.60 11 -2 0 270.67 11.30 -11 -2 0 258.27 10.80 -11 2 0 263.87 11.70 -11 2 0 267.97 10.80 -11 2 0 263.47 11.90 -11 2 0 259.87 17.30 -11 2 0 285.57 11.10 -11 2 0 262.17 11.00 0 3 0 9.40 1.40 1 -3 0 12.20 1.90 -1 -3 0 9.30 1.40 -1 -3 0 10.00 0.90 -1 3 0 12.70 1.70 1 3 0 11.30 1.30 -1 3 0 12.50 1.70 1 3 0 12.70 1.30 2 -3 0 5709.83 209.38 2 3 0 5474.05 206.88 2 3 0 5761.82 206.98 2 3 0 5417.36 206.78 3 -3 0 879.21 36.00 3 -3 0 884.21 35.40 -3 -3 0 868.91 34.50 3 3 0 855.41 32.50 -3 3 0 894.91 35.00 -3 3 0 866.11 35.20 4 -3 0 63.49 5.30 4 -3 0 77.59 6.00 -4 -3 0 68.19 4.80 -4 3 0 68.39 5.20 4 3 0 76.29 3.20 -5 -3 0 435.96 19.70 5 -3 0 411.16 21.20 5 -3 0 436.36 20.40 5 3 0 439.26 17.60 -5 3 0 447.96 19.90 5 3 0 480.35 17.60 -5 3 0 447.96 20.00 -6 -3 0 496.05 22.60 6 -3 0 515.75 24.90 6 -3 0 514.75 23.30 6 3 0 495.45 20.20 -6 3 0 472.35 21.60 -7 -3 0 504.85 21.40 7 -3 0 507.35 25.60 -7 -3 0 527.35 24.80 -7 -3 0 526.45 21.50 -7 -3 0 509.15 21.20 -7 -3 0 512.85 22.10 7 -3 0 516.65 23.90 7 -3 0 467.95 20.10 -7 -3 0 527.45 23.20 -7 -3 0 505.45 23.60 -7 3 0 454.15 20.80 -7 3 0 453.95 20.50 7 3 0 506.45 20.30 -7 3 0 484.05 22.10 -8 -3 0 507.45 22.90 -8 -3 0 503.45 21.20 -8 -3 0 522.45 21.90 -8 -3 0 497.85 20.90 8 -3 0 466.15 20.00 -8 -3 0 498.15 21.20 -8 3 0 494.75 22.10 -8 3 0 496.65 23.50 -8 3 0 468.65 20.60 -8 3 0 481.95 20.40 -9 -3 0 37.90 4.80 -9 -3 0 33.10 3.60 -9 -3 0 32.40 3.60 -9 -3 0 20.80 11.20 -9 -3 0 29.20 4.10 -9 3 0 41.40 4.20 -9 3 0 25.70 14.40 -9 3 0 29.40 3.30 -9 3 0 36.60 4.10 -9 3 0 35.60 5.30 -9 3 0 36.20 3.60 -10 -3 0 1.50 6.20 -10 -3 0 1.70 1.20 10 -3 0 0.90 1.20 -10 -3 0 5.40 1.50 -10 -3 0 1.50 1.80 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210.88 11.30 -6 4 0 215.18 10.20 7 -4 0 1426.26 62.29 -7 -4 0 1571.94 56.99 -7 -4 0 1495.25 58.19 -7 -4 0 1514.85 60.79 -7 -4 0 1503.95 56.59 -7 -4 0 1432.36 56.69 -7 4 0 1363.46 55.99 -7 4 0 1362.36 55.69 -8 -4 0 648.24 51.49 -8 -4 0 758.12 32.40 -8 -4 0 807.12 31.20 -8 -4 0 807.12 31.00 -8 -4 0 813.72 31.20 -8 -4 0 792.72 31.00 -8 4 0 740.03 31.90 -8 4 0 807.52 33.80 -8 4 0 744.93 30.30 -8 4 0 758.32 30.50 -9 -4 0 289.97 29.80 -9 -4 0 330.97 14.10 9 -4 0 326.47 14.40 -9 -4 0 334.17 14.20 -9 -4 0 332.27 15.30 -9 -4 0 337.97 14.20 -9 4 0 325.97 13.70 -9 4 0 336.67 15.20 -9 4 0 330.67 13.80 -9 4 0 308.67 16.10 -10 -4 0 13.70 1.90 -10 -4 0 11.30 1.90 -10 -4 0 10.80 9.20 10 -4 0 12.70 2.10 -10 -4 0 14.40 1.80 -10 -4 0 11.30 2.10 -10 4 0 13.70 2.50 -10 4 0 12.60 1.90 -10 4 0 11.40 1.60 -10 4 0 10.80 2.50 -10 4 0 11.80 2.00 0 -5 0 0.10 0.90 0 -5 0 1.90 1.10 0 5 0 1.80 1.30 0 5 0 0.90 1.10 1 -5 0 4553.34 167.68 1 -5 0 4426.26 166.68 -1 -5 0 4326.47 166.98 1 -5 0 4184.28 168.08 -1 5 0 4537.55 167.98 -1 5 0 4579.44 167.78 1 5 0 4495.45 167.18 1 5 0 4587.24 166.88 2 -5 0 4.80 1.70 -2 -5 0 4.90 1.60 2 -5 0 3.30 2.00 2 5 0 1.90 1.00 -2 5 0 2.20 1.50 2 5 0 4.80 1.20 3 -5 0 499.35 24.20 3 -5 0 518.55 23.30 -3 -5 0 530.55 22.20 -3 5 0 518.25 23.20 -3 5 0 516.75 23.40 3 5 0 530.45 21.40 -4 -5 0 1241.98 50.19 4 -5 0 1240.38 51.69 4 -5 0 1293.27 53.49 -4 5 0 1298.87 50.19 -4 5 0 1225.88 49.30 -4 5 0 1309.87 51.59 5 -5 0 3.10 1.90 -5 -5 0 11.40 2.80 -5 5 0 3.90 2.50 -5 5 0 4.10 1.60 -5 5 0 0.90 1.20 -5 5 0 3.70 2.20 -6 -5 0 193.08 9.70 6 -5 0 176.48 9.10 6 -5 0 172.98 13.30 6 -5 0 168.28 11.80 -6 -5 0 213.28 10.60 -6 -5 0 203.48 10.60 -6 -5 0 199.98 11.40 -6 -5 0 198.58 25.70 -6 5 0 163.08 8.60 -6 5 0 204.88 12.80 -6 5 0 181.68 10.10 -7 -5 0 21.40 3.10 7 -5 0 27.00 3.10 -7 -5 0 25.90 4.10 -7 5 0 22.50 3.80 -7 5 0 21.10 2.50 -8 -5 0 12.40 2.30 8 -5 0 9.90 2.00 -8 -5 0 8.60 1.90 -8 -5 0 7.50 8.60 -8 -5 0 6.40 2.50 -8 -5 0 17.00 3.10 -8 5 0 7.90 1.70 -8 5 0 6.80 3.10 -9 -5 0 353.56 14.80 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130.49 7.40 -6 -7 0 138.99 7.70 -6 -7 0 160.38 19.00 -6 7 0 133.29 6.90 -6 7 0 136.89 7.10 -7 -7 0 281.77 12.60 7 -7 0 268.57 12.50 -7 -7 0 277.37 23.40 -7 -7 0 272.87 11.60 -7 -7 0 292.67 13.30 7 -7 0 266.27 11.90 -7 -7 0 271.17 11.70 -7 -7 0 278.37 12.60 -7 7 0 275.67 11.40 8 -7 0 14.50 2.20 8 -7 0 18.10 2.00 -8 -7 0 13.80 2.00 -8 -7 0 15.60 2.30 -8 -7 0 14.70 6.40 -8 -7 0 21.20 3.20 9 -7 0 7.80 1.70 -9 7 0 5.80 1.40 0 -8 0 315.77 14.40 0 -8 0 329.97 13.80 0 -8 0 317.67 13.30 0 8 0 333.07 14.80 0 8 0 337.47 14.90 0 8 0 324.67 16.90 -1 -8 0 356.36 18.30 1 -8 0 377.86 18.30 -1 -8 0 364.56 16.20 1 -8 0 367.96 15.90 1 -8 0 371.96 15.10 -1 -8 0 358.46 14.60 1 -8 0 378.66 15.90 -1 8 0 386.66 19.20 -1 8 0 364.56 19.00 -2 -8 0 2347.47 84.89 2 -8 0 2235.18 83.69 -2 -8 0 2141.39 83.99 2 -8 0 2230.78 84.09 -2 -8 0 2346.97 84.09 2 -8 0 2206.58 83.49 -2 -8 0 2135.59 83.99 -2 -8 0 2146.69 84.79 2 -8 0 2129.79 83.59 -2 8 0 2341.37 85.29 -2 8 0 2146.19 88.39 -2 8 0 2285.77 84.99 3 -8 0 93.59 5.70 -3 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14.50 -1 -9 0 340.87 15.00 1 -9 0 334.77 13.80 -1 -9 0 358.96 14.50 1 -9 0 340.67 14.60 -1 -9 0 337.87 14.60 -1 -9 0 324.17 14.90 -1 -9 0 328.47 13.20 1 -9 0 329.67 13.80 1 9 0 328.97 14.70 -1 9 0 326.47 15.00 1 9 0 356.26 15.40 2 -9 0 6.30 2.00 -2 -9 0 5.40 3.10 -2 -9 0 7.30 2.10 -2 -9 0 5.50 2.50 -2 -9 0 9.00 2.10 -2 9 0 10.10 4.40 -2 9 0 9.90 3.80 -3 -9 0 358.96 15.20 3 -9 0 344.37 15.10 3 -9 0 360.36 15.20 -3 -9 0 356.36 16.00 -3 -9 0 381.26 15.50 -3 -9 0 370.36 16.20 -3 -9 0 372.46 15.50 -3 9 0 357.56 16.00 -3 9 0 382.06 16.60 -4 -9 0 150.28 7.30 -4 -9 0 148.19 7.50 -4 -9 0 142.49 6.70 -4 -9 0 147.49 7.70 -4 -9 0 139.89 7.90 4 -9 0 130.69 6.80 -4 9 0 145.09 7.50 -4 9 0 132.09 7.70 -4 9 0 139.69 7.60 -5 -9 0 160.48 6.90 -5 -9 0 154.78 7.70 -5 9 0 155.48 6.70 -6 -9 0 89.19 4.70 6 -9 0 89.09 4.80 -6 -9 0 88.59 5.30 -6 -9 0 94.19 5.50 -6 -9 0 88.69 4.60 -6 -9 0 92.49 5.00 -6 9 0 93.09 4.90 7 -9 0 3.80 1.10 -7 -9 0 3.80 1.20 -7 -9 0 2.40 1.30 -7 -9 0 2.00 0.80 -7 -9 0 2.20 0.80 -7 9 0 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3.30 -5 -2 -24 58.29 4.10 -5 2 -24 59.09 11.00 5 2 24 64.49 4.20 5 2 24 60.99 3.10 -5 -3 24 11.50 1.70 5 -3 -24 9.00 1.30 -4 -3 24 79.69 5.80 4 -3 -24 80.59 4.20 -4 -3 24 88.69 4.50 4 3 -24 80.29 4.70 4 3 -24 78.69 4.80 3 -3 -24 70.79 4.00 -3 -3 24 71.89 4.10 3 3 -24 68.79 3.70 -3 3 24 64.19 3.60 3 3 -24 66.79 5.00 2 -3 -24 154.58 8.30 2 -3 -24 180.48 7.80 -2 -3 24 185.28 8.20 2 3 -24 168.58 8.30 2 3 -24 166.28 8.60 -2 3 24 172.28 8.20 2 3 -24 144.89 8.00 1 -3 -24 162.98 7.80 -1 -3 24 176.78 7.70 1 3 -24 164.18 8.30 1 3 -24 169.48 8.80 -1 3 24 171.98 7.80 1 3 -24 158.58 8.10 0 -3 -24 27.50 4.60 0 -3 -24 28.00 2.60 0 -3 -24 27.80 3.40 0 -3 24 27.90 2.20 0 3 -24 27.10 3.00 0 3 -24 26.20 2.80 0 3 -24 22.30 3.30 0 3 24 26.80 2.70 -1 -3 -24 160.98 8.70 -1 -3 -24 153.58 8.50 -1 -3 -24 165.68 7.40 -1 3 -24 142.09 8.80 1 3 24 165.28 7.00 -1 3 -24 163.18 8.50 1 3 24 162.18 7.60 -1 3 -24 157.28 7.80 -2 -3 -24 138.89 9.20 -2 -3 -24 161.78 8.40 -2 -3 -24 154.18 7.10 2 -3 24 183.08 9.10 -2 -3 -24 146.39 7.70 -2 3 -24 172.98 10.70 2 3 24 164.18 7.50 -2 3 -24 147.39 7.80 -2 3 -24 159.18 7.70 2 3 24 154.58 6.90 -3 -3 -24 57.09 4.20 3 -3 24 53.49 3.40 -3 -3 -24 57.89 3.10 -3 -3 -24 54.59 4.10 3 -3 24 62.19 3.40 -3 -3 -24 62.39 3.80 3 3 24 52.29 3.60 -3 3 -24 54.79 4.10 4 -3 24 73.89 4.30 4 -3 24 73.69 3.90 -4 -3 -24 74.39 4.50 -4 -3 -24 68.59 4.40 -4 -3 -24 73.69 4.80 4 3 24 70.69 3.80 4 3 24 74.99 3.60 -5 -3 -24 8.70 1.40 5 3 24 6.20 1.20 -5 3 -24 9.50 8.70 5 3 24 8.00 1.10 4 -4 -24 236.08 9.10 -4 -4 24 195.88 9.30 -4 -4 24 209.48 8.80 4 4 -24 197.48 9.10 4 4 -24 195.58 8.40 -3 -4 24 17.60 1.90 3 -4 -24 17.30 1.90 -3 4 24 17.90 1.80 3 4 -24 17.30 2.40 3 4 -24 19.30 2.80 2 -4 -24 41.90 3.50 2 -4 -24 35.50 3.30 2 -4 -24 47.20 3.80 -2 -4 24 43.50 2.80 -2 4 24 43.50 3.00 2 4 -24 43.30 5.50 1 -4 -24 56.39 5.20 1 -4 -24 54.79 3.40 1 -4 -24 53.69 4.30 1 4 -24 49.90 4.30 1 4 -24 50.99 4.80 -1 4 24 55.59 3.70 1 4 -24 59.39 5.50 0 -4 -24 325.57 13.10 0 -4 -24 316.37 16.10 0 -4 -24 318.47 14.60 0 4 -24 292.17 13.50 0 4 24 301.67 12.50 0 4 -24 309.77 14.40 0 4 24 319.17 13.30 0 4 -24 370.96 15.90 -1 -4 -24 51.09 4.20 -1 -4 -24 49.20 3.80 -1 -4 -24 51.39 3.40 -1 -4 -24 65.39 6.10 -1 4 -24 47.80 3.60 1 4 24 46.70 3.40 -1 4 -24 51.09 6.50 -2 -4 -24 39.80 2.50 2 -4 24 42.30 2.80 -2 -4 -24 40.00 3.60 -2 -4 -24 39.00 3.60 -2 -4 -24 36.50 3.10 2 -4 24 40.40 2.50 -2 4 -24 38.80 3.70 2 4 24 41.10 2.60 2 4 24 41.20 3.00 -3 -4 -24 16.00 2.40 3 -4 24 14.90 1.70 3 -4 24 16.10 1.60 -3 -4 -24 11.90 1.90 3 4 24 16.40 1.80 -3 4 -24 16.20 2.90 3 4 24 12.70 1.50 -4 -4 -24 161.68 7.90 4 -4 24 183.78 7.30 4 -4 24 142.19 7.10 -4 -4 -24 171.58 7.40 -4 -4 -24 180.08 8.50 4 4 24 181.08 7.10 4 4 24 167.58 7.10 -3 -5 24 259.07 11.10 -3 -5 24 272.07 12.00 3 -5 -24 292.77 11.20 3 -5 -24 311.57 13.60 -3 -5 24 280.57 11.00 3 5 -24 255.07 13.40 -3 5 24 283.47 11.00 3 5 -24 265.17 11.70 -2 -5 24 76.59 3.70 2 -5 -24 76.99 3.90 2 -5 -24 73.39 4.70 -2 -5 24 85.29 4.70 2 -5 -24 74.39 5.00 2 5 -24 73.49 4.40 2 5 -24 70.99 4.90 -2 5 24 71.79 3.90 1 -5 -24 265.67 10.50 1 -5 -24 254.77 11.50 1 -5 -24 239.98 12.80 1 5 -24 250.67 11.10 -1 5 24 261.27 10.60 1 5 -24 247.28 11.70 0 -5 -24 2.70 1.70 0 -5 -24 3.60 0.90 0 -5 24 3.00 1.10 0 -5 -24 4.40 1.60 0 -5 -24 3.10 1.50 0 5 -24 2.80 1.60 0 5 -24 3.20 1.40 0 5 24 3.10 0.70 0 5 24 2.80 1.10 1 -5 24 254.97 10.30 -1 -5 -24 250.67 13.20 -1 -5 -24 246.48 9.90 -1 -5 -24 254.87 11.30 -1 -5 -24 245.88 11.10 -1 5 -24 237.38 11.40 1 5 24 247.88 9.90 1 5 24 243.78 10.30 -1 5 -24 234.28 10.50 2 -5 24 72.69 3.60 -2 -5 -24 64.99 4.10 -2 -5 -24 67.89 4.30 -2 -5 -24 66.59 6.20 2 5 24 73.99 3.70 -2 5 -24 62.99 3.50 -2 5 -24 65.29 4.60 2 5 24 70.29 3.40 -3 -5 -24 296.27 13.40 -3 -5 -24 254.87 11.40 3 -5 24 251.87 10.30 3 5 24 242.98 10.20 -3 5 -24 248.48 13.40 3 5 24 259.87 10.50 -2 -6 24 411.66 16.50 -2 -6 24 383.66 15.20 2 -6 -24 385.66 16.40 2 -6 -24 403.96 15.90 2 6 -24 458.95 17.20 -2 6 24 377.26 15.60 1 -6 -24 99.69 6.90 -1 -6 24 109.19 4.70 1 -6 -24 101.39 5.90 1 -6 -24 111.59 6.00 1 -6 -24 93.29 5.20 -1 -6 24 104.79 5.30 1 6 -24 106.09 7.00 -1 6 24 100.39 4.80 1 6 -24 98.09 5.20 0 -6 -24 46.30 4.20 0 -6 -24 34.90 2.30 0 -6 -24 31.90 3.00 0 -6 24 36.70 2.20 0 -6 -24 34.90 3.10 0 -6 24 41.60 3.40 0 6 -24 31.60 2.90 0 6 24 33.60 2.30 0 6 -24 35.00 4.00 -1 -6 -24 83.09 5.10 1 -6 24 100.19 4.40 -1 -6 -24 87.89 5.90 -1 -6 -24 98.19 5.40 1 -6 24 106.99 4.80 1 6 24 92.19 4.10 -1 6 -24 92.29 4.60 -1 6 -24 96.29 6.30 1 6 24 83.39 4.90 -2 -6 -24 357.96 14.70 2 -6 24 373.16 14.10 -2 -6 -24 363.76 14.70 -2 -6 -24 359.26 15.20 2 6 24 360.26 13.90 2 6 24 362.66 14.20 -5 0 25 5.70 1.20 4 0 -25 133.09 7.60 3 0 -25 291.57 12.30 -2 0 25 38.10 2.90 2 0 -25 40.80 3.00 1 0 -25 7.50 2.20 1 0 -25 7.60 1.60 0 0 -25 0.50 1.20 0 0 -25 0.60 1.10 0 0 -25 -0.20 2.00 0 0 25 3.10 1.20 -1 0 -25 8.30 1.70 -1 0 -25 7.70 1.60 1 0 25 7.50 1.60 2 0 25 44.00 3.10 -2 0 -25 33.80 3.00 -2 0 -25 41.80 3.10 3 0 25 269.47 11.40 3 0 25 319.27 13.80 4 0 25 124.29 5.10 -4 0 -25 97.39 6.10 -4 0 -25 111.59 12.30 4 0 25 107.89 5.30 5 0 25 4.70 1.00 -4 -1 25 36.30 2.70 4 -1 -25 33.00 2.30 3 -1 -25 14.50 2.00 3 1 -25 16.70 2.50 2 -1 -25 73.69 4.80 -2 1 25 57.09 3.40 2 1 -25 55.79 3.70 1 -1 -25 12.00 1.70 -1 -1 25 14.70 1.80 1 -1 -25 13.90 2.00 1 1 -25 17.80 2.80 1 1 -25 13.90 2.80 -1 1 25 15.40 2.20 0 -1 25 1.10 1.30 0 -1 -25 0.00 0.90 0 1 25 0.70 1.10 0 1 -25 1.00 1.10 0 1 -25 1.00 1.00 1 -1 25 16.60 2.20 -1 -1 -25 14.90 2.20 -1 -1 -25 14.00 2.40 1 1 25 14.90 2.20 -1 1 -25 16.90 2.20 2 -1 25 52.69 3.50 -2 -1 -25 53.89 4.10 -2 -1 -25 54.39 3.60 -2 1 -25 56.09 3.80 2 1 25 60.19 2.90 2 1 25 59.69 3.70 -3 -1 -25 11.00 1.80 -3 -1 -25 11.20 1.60 3 -1 25 15.00 2.10 3 1 25 11.10 1.30 3 1 25 15.50 2.30 -3 1 -25 10.00 1.70 -4 -1 -25 25.00 2.40 4 -1 25 35.90 2.40 4 1 25 31.00 2.40 4 1 25 31.20 1.90 -4 -2 25 125.49 6.70 4 -2 -25 126.89 5.80 -4 -2 25 123.89 5.80 3 -2 -25 158.98 7.30 -3 -2 25 159.08 7.30 3 2 -25 169.58 9.00 2 -2 -25 223.98 9.70 -2 -2 25 224.18 9.50 2 2 -25 218.88 9.80 2 2 -25 213.98 10.10 -2 2 25 218.18 9.30 -1 -2 25 20.50 2.00 1 -2 -25 18.20 2.30 1 2 -25 14.30 3.00 1 2 -25 21.30 2.30 1 2 -25 21.20 3.00 -1 2 25 18.80 3.20 0 -2 25 47.40 3.00 0 -2 -25 44.80 4.80 0 -2 -25 54.19 3.40 0 2 -25 49.20 4.00 0 2 -25 37.80 4.40 0 2 -25 49.00 3.50 0 2 25 50.09 3.40 -1 -2 -25 18.00 2.10 -1 -2 -25 19.80 3.10 1 -2 25 21.80 2.40 1 2 25 16.10 1.50 -1 2 -25 14.50 2.60 -1 2 -25 14.60 2.70 1 2 25 21.30 2.30 2 -2 25 214.28 9.10 -2 -2 -25 198.88 9.70 2 2 25 201.48 8.40 2 2 25 208.58 10.40 -3 -2 -25 133.99 6.90 -3 -2 -25 135.29 6.10 3 -2 25 134.79 6.30 3 -2 25 141.29 6.10 3 2 25 139.59 5.90 3 2 25 142.69 6.50 4 -2 25 105.19 5.00 -4 -2 -25 112.89 6.60 4 2 25 103.09 4.60 4 2 25 105.69 5.00 -4 -3 25 124.19 5.40 4 -3 -25 122.59 5.40 -4 -3 25 100.39 5.90 4 3 -25 123.29 6.90 3 -3 -25 139.49 6.20 -3 -3 25 141.49 6.30 3 -3 -25 135.49 7.50 3 3 -25 114.49 7.70 -3 3 25 133.59 6.30 3 3 -25 138.89 6.60 2 -3 -25 141.19 8.70 -2 -3 25 147.79 7.10 2 -3 -25 143.89 6.60 2 3 -25 153.68 7.40 2 3 -25 136.89 6.90 2 3 -25 128.99 6.60 -2 3 25 140.69 6.40 1 -3 -25 49.30 3.90 1 -3 -25 41.40 3.30 1 3 -25 45.50 3.40 -1 3 25 44.40 3.10 1 3 -25 40.00 3.70 1 3 -25 46.10 3.20 0 -3 -25 91.69 5.70 0 -3 -25 91.39 5.20 0 -3 -25 102.79 6.30 0 3 -25 95.49 5.70 0 3 -25 85.19 5.00 0 3 -25 90.49 5.00 -1 -3 -25 36.50 3.40 -1 -3 -25 46.30 3.20 -1 -3 -25 47.70 3.40 1 -3 25 43.40 2.80 -1 3 -25 42.60 3.00 -1 3 -25 41.70 3.70 1 3 25 41.40 2.40 -1 3 -25 45.20 3.20 2 -3 25 139.69 6.10 -2 -3 -25 128.09 5.90 -2 -3 -25 124.19 6.90 -2 -3 -25 135.39 6.70 2 -3 25 132.99 5.90 2 3 25 131.29 5.70 2 3 25 136.39 6.30 3 -3 25 127.69 5.50 -3 -3 -25 116.69 5.50 -3 -3 -25 114.99 6.20 3 -3 25 128.59 5.60 3 3 25 119.19 5.30 3 3 25 130.79 5.80 -4 -3 -25 106.59 5.40 4 -3 25 106.19 4.80 4 3 25 122.49 5.40 4 3 25 104.29 4.90 -3 -4 25 43.80 3.90 -3 -4 25 40.70 2.30 3 -4 -25 36.70 2.70 3 -4 -25 39.90 2.80 3 4 -25 36.80 2.80 2 -4 -25 3.60 1.50 -2 -4 25 7.60 1.60 2 -4 -25 5.80 1.10 -2 4 25 6.60 1.10 2 4 -25 5.20 1.40 2 4 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-25 1.90 1.20 -1 -5 -25 44.90 2.10 1 -5 25 46.30 2.60 1 -5 25 51.79 3.50 -1 -5 -25 50.99 5.10 -1 -5 -25 40.20 3.00 -1 5 -25 40.10 2.70 1 5 25 38.80 2.10 1 5 25 43.40 2.60 -1 5 -25 39.10 4.10 2 -5 25 36.00 2.10 -2 -5 -25 37.40 2.80 -2 -5 -25 39.20 2.50 2 5 25 35.40 2.20 2 5 25 38.30 2.00 -4 0 26 692.23 26.50 3 0 -26 21.10 1.90 2 0 -26 9.90 1.90 2 0 -26 8.00 1.70 1 0 -26 94.99 5.00 1 0 -26 92.09 5.20 1 0 -26 95.99 5.30 -1 0 26 102.19 4.60 0 0 -26 110.09 6.80 0 0 26 116.19 5.40 0 0 -26 104.69 5.60 -1 0 -26 89.69 4.90 1 0 26 96.39 4.80 -1 0 -26 88.99 5.60 2 0 26 7.50 1.30 -2 0 -26 10.00 1.60 -2 0 -26 8.50 1.40 -3 0 -26 20.30 1.90 3 0 26 25.00 2.20 4 0 26 621.54 24.70 -4 -1 26 135.99 5.90 4 1 -26 126.29 5.90 3 -1 -26 54.79 3.10 -3 -1 26 52.79 3.50 3 -1 -26 52.49 2.90 3 1 -26 53.79 3.30 3 1 -26 51.69 3.30 2 -1 -26 21.00 2.40 -2 -1 26 19.30 1.90 2 -1 -26 20.90 2.10 2 1 -26 20.90 3.00 2 1 -26 24.00 2.30 -2 1 26 22.20 2.30 1 -1 -26 240.98 11.10 1 -1 -26 253.77 10.80 -1 -1 26 288.27 11.60 1 1 -26 246.58 10.80 1 1 -26 243.38 10.50 -1 1 26 243.98 10.40 0 -1 -26 8.30 1.40 0 -1 -26 13.00 2.00 0 -1 26 12.00 1.70 0 1 26 11.20 1.80 0 1 -26 11.30 1.70 -1 -1 -26 231.78 10.50 1 -1 26 245.58 10.00 -1 -1 -26 234.48 10.10 1 1 26 235.78 10.10 -1 1 -26 233.98 10.30 2 -1 26 19.50 2.10 -2 -1 -26 20.50 2.00 -2 -1 -26 24.20 3.70 -2 1 -26 21.10 2.20 2 1 26 21.10 2.10 -3 -1 -26 41.10 2.80 -3 -1 -26 46.70 2.70 3 -1 26 49.20 2.80 3 1 26 48.20 2.90 4 -1 26 116.89 5.10 4 1 26 109.79 5.10 -3 -2 26 247.88 10.30 3 -2 -26 258.07 10.50 3 2 -26 256.37 10.90 -2 -2 26 2.00 0.90 2 -2 -26 1.50 0.90 2 2 -26 0.70 0.90 2 2 -26 1.50 1.10 -2 2 26 1.00 0.70 1 -2 -26 24.60 2.20 1 2 -26 21.40 2.10 -1 2 26 27.00 2.20 1 2 -26 24.20 2.30 0 -2 -26 31.30 2.50 0 -2 -26 28.20 2.80 0 2 -26 31.50 3.30 0 2 26 30.10 2.40 0 2 -26 27.60 2.50 -1 -2 -26 22.70 2.10 -1 -2 -26 20.40 2.50 1 -2 26 27.20 2.70 1 2 26 23.10 2.20 -1 2 -26 22.70 2.30 -2 -2 -26 -0.40 1.10 2 -2 26 0.40 0.70 -2 -2 -26 1.00 0.80 2 -2 26 0.90 0.80 -2 2 -26 0.70 0.80 2 2 26 0.90 0.90 3 -2 26 246.28 9.60 -3 -2 -26 206.48 9.40 3 2 26 228.08 9.20 3 2 26 202.78 8.70 -3 -3 26 4.70 1.00 -3 -3 26 3.10 0.90 3 -3 -26 2.60 0.80 3 3 -26 2.60 1.00 2 -3 -26 3.20 1.00 2 3 -26 1.70 1.10 -2 3 26 4.20 0.80 1 -3 -26 23.40 2.00 1 -3 -26 24.80 2.50 1 3 -26 22.60 2.20 -1 3 26 21.60 1.90 1 3 -26 22.60 2.00 0 -3 -26 -1.10 1.20 0 -3 -26 -0.70 0.90 0 -3 -26 1.10 0.80 0 3 26 0.80 0.90 0 3 -26 0.70 1.00 -1 -3 -26 19.90 2.40 -1 -3 -26 21.80 1.80 1 3 26 22.00 2.00 2 -3 26 3.10 1.10 -2 -3 -26 3.80 1.60 2 -3 26 3.00 0.90 2 3 26 2.20 0.90 -3 -3 -26 3.10 1.00 3 -3 26 2.10 1.00 3 3 26 2.70 0.90 2 -4 -26 155.98 7.20 -2 -4 26 183.08 8.40 -2 4 26 173.48 7.60 -1 -4 26 16.30 1.50 1 -4 -26 17.50 1.60 1 -4 -26 11.50 2.50 -1 4 26 21.20 2.20 1 4 -26 17.60 1.90 0 -4 26 43.10 2.50 0 -4 -26 42.30 2.40 0 -4 -26 47.20 3.60 0 4 -26 38.20 2.50 0 4 26 40.70 2.50 1 -4 26 15.20 1.60 -1 -4 -26 16.80 1.30 -1 -4 -26 11.00 1.80 1 4 26 18.90 1.70 -2 -4 -26 141.19 7.40 2 4 26 150.18 6.40 2 0 -27 2.40 0.90 -2 0 27 0.70 0.70 1 0 -27 3.00 1.00 0 0 -27 0.50 0.80 0 0 27 0.30 0.80 1 0 27 2.00 1.10 -1 0 -27 1.60 0.80 -2 0 -27 1.70 0.80 2 0 27 1.10 1.30 2 -1 -27 211.28 8.90 2 1 -27 212.18 9.40 1 -1 -27 53.69 4.40 1 -1 -27 66.69 3.50 1 1 -27 69.49 3.80 -1 1 27 61.29 3.30 0 -1 -27 176.88 7.70 0 -1 -27 176.48 7.60 0 1 27 156.58 7.60 0 1 -27 182.08 7.70 -1 -1 -27 68.89 4.50 -1 -1 -27 64.09 3.50 1 -1 27 63.39 3.20 1 1 27 69.99 3.50 -1 1 -27 66.39 3.70 2 -1 27 200.48 8.10 -2 -1 -27 198.18 8.40 2 1 27 205.18 8.70 -2 1 -27 189.28 8.40 2 -2 -27 70.79 3.60 2 2 -27 70.49 3.80 1 -2 -27 149.29 6.40 1 -2 -27 143.69 6.70 -1 2 27 144.79 6.00 1 2 -27 141.19 6.40 0 -2 -27 58.49 3.20 0 -2 -27 55.69 3.50 0 2 -27 59.39 3.40 0 2 27 67.89 3.70 -1 -2 -27 140.09 6.50 -1 -2 -27 144.39 6.10 1 2 27 143.49 6.30 -1 2 -27 125.99 7.60 -2 -2 -27 64.39 3.20 2 2 27 76.99 4.20 0 -3 -27 171.08 7.20 0 -3 -27 148.99 7.10 0 -3 27 153.78 6.60 0 3 27 155.78 6.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 58202 _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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.76615(18) 0.70512(14) 0.25464(6) 0.0381(3) Uani 1 1 d . . . . . H1 H 0.769433 0.785950 0.249019 0.057 Uiso 1 1 calc GR . . . . O2 O 0.50978(19) 0.6198(2) 0.25591(7) 0.0519(4) Uani 1 1 d . . . . . H2 H 0.590235 0.649285 0.245340 0.078 Uiso 1 1 calc GR . . . . O3 O 0.38027(14) 0.60666(15) 0.33711(6) 0.0360(3) Uani 1 1 d . . . . . O4 O 0.50050(17) 0.63903(16) 0.59253(6) 0.0429(4) Uani 1 1 d . . . . . O5 O 0.71128(15) 0.53469(13) 0.59619(5) 0.0316(3) Uani 1 1 d . . . . . C1 C 0.70743(17) 0.43171(14) 0.41575(7) 0.0191(3) Uani 1 1 d . . . . . H1A H 0.621489 0.467875 0.394660 0.023 Uiso 1 1 calc R . . . . C2 C 0.69118(17) 0.46517(15) 0.48039(7) 0.0203(3) Uani 1 1 d . . . . . H2A H 0.759499 0.428450 0.506915 0.024 Uiso 1 1 calc R . . . . C3 C 0.58924(17) 0.54195(15) 0.50392(7) 0.0208(3) Uani 1 1 d . . . . . C4 C 0.46177(18) 0.59785(17) 0.47065(8) 0.0245(3) Uani 1 1 d . . . . . H4A H 0.378537 0.602073 0.498031 0.029 Uiso 1 1 calc R . . . . H4B H 0.435990 0.537022 0.438323 0.029 Uiso 1 1 calc R . . . . C5 C 0.4851(2) 0.73498(17) 0.44357(8) 0.0292(4) Uani 1 1 d . . . . . H5A H 0.396605 0.761699 0.422275 0.035 Uiso 1 1 calc R . . . . H5B H 0.501899 0.798327 0.475892 0.035 Uiso 1 1 calc R . . . . C6 C 0.6107(2) 0.73873(15) 0.40143(8) 0.0270(4) Uani 1 1 d . . . . . H6 H 0.695308 0.779634 0.416165 0.032 Uiso 1 1 calc R . . . . C7 C 0.6202(2) 0.69249(16) 0.34600(8) 0.0260(4) Uani 1 1 d . . . . . C8 C 0.7683(2) 0.67869(17) 0.31752(7) 0.0287(4) Uani 1 1 d . . . . . H8 H 0.835932 0.741318 0.336990 0.034 Uiso 1 1 calc R . . . . C9 C 0.8273(2) 0.54018(18) 0.32561(7) 0.0273(4) Uani 1 1 d . . . . . H9A H 0.922489 0.533172 0.306063 0.033 Uiso 1 1 calc R . . . . H9B H 0.761233 0.477259 0.306412 0.033 Uiso 1 1 calc R . . . . C10 C 0.84281(17) 0.50557(16) 0.39199(7) 0.0220(3) Uani 1 1 d . . . . . H10 H 0.847105 0.590143 0.413891 0.026 Uiso 1 1 calc R . . . . C11 C 0.98253(19) 0.43484(17) 0.40533(8) 0.0263(4) Uani 1 1 d . . . . . C12 C 0.98366(19) 0.29077(19) 0.39297(9) 0.0328(4) Uani 1 1 d . . . . . H12A H 1.074696 0.252509 0.407853 0.039 Uiso 1 1 calc R . . . . H12B H 0.979265 0.276046 0.349688 0.039 Uiso 1 1 calc R . . . . C13 C 0.85582(19) 0.22338(17) 0.42271(9) 0.0282(4) Uani 1 1 d . . . . . H13A H 0.864327 0.232084 0.466233 0.034 Uiso 1 1 calc R . . . . H13B H 0.857025 0.129412 0.412866 0.034 Uiso 1 1 calc R . . . . C14 C 0.71317(18) 0.28339(15) 0.40215(7) 0.0217(3) Uani 1 1 d . . . . . H14 H 0.711441 0.274960 0.358041 0.026 Uiso 1 1 calc R . . . . C15 C 0.59355(19) 0.57709(15) 0.56804(7) 0.0235(3) Uani 1 1 d . . . . . C16 C 0.4935(2) 0.63677(18) 0.31363(8) 0.0303(4) Uani 1 1 d . . . . . C17 C 1.0959(2) 0.4972(2) 0.42634(10) 0.0378(4) Uani 1 1 d . . . . . H17A H 1.182552 0.451020 0.434244 0.045 Uiso 1 1 calc R . . . . H17B H 1.090861 0.588233 0.433554 0.045 Uiso 1 1 calc R . . . . C18 C 0.57878(19) 0.21157(16) 0.42510(8) 0.0252(3) Uani 1 1 d . . . . . H18 H 0.569862 0.229105 0.468499 0.030 Uiso 1 1 calc R . . . . C19 C 0.5870(2) 0.06403(18) 0.41621(11) 0.0375(4) Uani 1 1 d . . . . . H19A H 0.598325 0.044722 0.373964 0.056 Uiso 1 1 calc GR . . . . H19B H 0.498254 0.023559 0.430886 0.056 Uiso 1 1 calc GR . . . . H19C H 0.669795 0.029290 0.438081 0.056 Uiso 1 1 calc GR . . . . C20 C 0.4418(2) 0.25979(18) 0.39490(10) 0.0343(4) Uani 1 1 d . . . . . H20A H 0.428069 0.352478 0.403636 0.051 Uiso 1 1 calc GR . . . . H20B H 0.358885 0.210280 0.409655 0.051 Uiso 1 1 calc GR . . . . H20C H 0.450319 0.247612 0.352005 0.051 Uiso 1 1 calc GR . . . . C21 C 0.7233(3) 0.5672(2) 0.65814(8) 0.0406(5) Uani 1 1 d . . . . . H21A H 0.699902 0.659458 0.663809 0.061 Uiso 1 1 calc GR . . . . H21B H 0.822037 0.550684 0.671617 0.061 Uiso 1 1 calc GR . . . . H21C H 0.656042 0.513544 0.681067 0.061 Uiso 1 1 calc GR . . . . O6 O 0.18963(18) 0.45810(15) 0.26799(6) 0.0395(3) Uani 1 1 d D . . . . C22 C 0.1612(3) 0.5455(3) 0.22154(10) 0.0480(5) Uani 1 1 d . . . . . H22A H 0.119864 0.497961 0.187950 0.072 Uiso 1 1 calc GR . . . . H22B H 0.251159 0.587616 0.209242 0.072 Uiso 1 1 calc GR . . . . H22C H 0.092698 0.611856 0.235033 0.072 Uiso 1 1 calc GR . . . . H6A H 0.236(4) 0.502(3) 0.2914(13) 0.072 Uiso 1 1 d DR . . . . 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 0.0521(9) 0.0391(7) 0.0230(6) 0.0081(5) -0.0007(6) -0.0108(7) O2 0.0487(9) 0.0815(12) 0.0254(7) -0.0059(7) -0.0045(6) -0.0208(9) O3 0.0318(7) 0.0443(8) 0.0319(7) -0.0040(6) -0.0059(5) -0.0027(6) O4 0.0445(8) 0.0534(8) 0.0307(7) -0.0117(6) 0.0041(6) 0.0179(7) O5 0.0349(7) 0.0378(7) 0.0219(6) -0.0025(5) -0.0019(5) 0.0053(6) C1 0.0185(7) 0.0182(7) 0.0207(7) -0.0004(5) 0.0007(6) 0.0004(6) C2 0.0216(7) 0.0172(7) 0.0221(7) 0.0018(6) -0.0003(6) -0.0011(6) C3 0.0218(7) 0.0167(6) 0.0239(8) 0.0003(6) 0.0012(6) -0.0024(6) C4 0.0218(8) 0.0241(7) 0.0277(8) -0.0042(6) -0.0010(6) 0.0032(6) C5 0.0384(10) 0.0218(8) 0.0273(8) -0.0033(6) -0.0036(7) 0.0098(7) C6 0.0357(9) 0.0154(7) 0.0298(8) 0.0017(6) -0.0072(7) 0.0011(6) C7 0.0337(9) 0.0184(7) 0.0260(8) 0.0028(6) -0.0043(7) -0.0009(6) C8 0.0365(10) 0.0270(8) 0.0225(8) 0.0041(6) -0.0016(7) -0.0090(7) C9 0.0294(9) 0.0303(8) 0.0223(8) -0.0002(7) 0.0043(7) -0.0040(7) C10 0.0216(7) 0.0224(7) 0.0222(8) -0.0016(6) 0.0016(6) -0.0019(6) C11 0.0213(8) 0.0307(9) 0.0271(8) -0.0028(7) 0.0043(6) 0.0005(7) C12 0.0223(8) 0.0330(9) 0.0432(10) -0.0081(8) 0.0008(8) 0.0056(8) C13 0.0253(8) 0.0226(8) 0.0367(9) -0.0030(7) -0.0022(7) 0.0045(7) C14 0.0228(8) 0.0187(7) 0.0236(7) -0.0022(6) 0.0004(6) 0.0017(6) C15 0.0258(8) 0.0193(7) 0.0254(8) 0.0009(6) 0.0038(6) -0.0025(6) C16 0.0362(10) 0.0288(8) 0.0258(8) 0.0018(7) -0.0059(7) -0.0004(8) C17 0.0246(9) 0.0431(10) 0.0456(11) -0.0086(9) 0.0001(8) -0.0013(8) C18 0.0272(8) 0.0207(7) 0.0277(8) -0.0010(6) 0.0031(7) -0.0020(7) C19 0.0361(10) 0.0207(8) 0.0556(12) 0.0029(8) 0.0061(9) -0.0017(7) C20 0.0237(8) 0.0242(8) 0.0549(12) -0.0023(8) -0.0025(8) -0.0040(7) C21 0.0475(12) 0.0526(12) 0.0215(9) -0.0019(8) -0.0024(8) -0.0021(10) O6 0.0481(8) 0.0377(7) 0.0327(7) -0.0040(6) -0.0067(6) -0.0037(7) C22 0.0439(12) 0.0649(14) 0.0352(10) 0.0100(10) -0.0022(9) -0.0063(11) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 O1 H1 109.5 . . ? C16 O2 H2 109.5 . . ? C15 O5 C21 116.68(15) . . ? C2 C1 H1A 107.3 . . ? C2 C1 C10 107.61(12) . . ? C2 C1 C14 114.71(13) . . ? C10 C1 H1A 107.3 . . ? C14 C1 H1A 107.3 . . ? C14 C1 C10 112.34(13) . . ? C1 C2 H2A 117.0 . . ? C3 C2 C1 126.05(14) . . ? C3 C2 H2A 117.0 . . ? C2 C3 C4 125.23(15) . . ? C2 C3 C15 120.51(15) . . ? C15 C3 C4 114.25(14) . . ? C3 C4 H4A 108.4 . . ? C3 C4 H4B 108.4 . . ? C3 C4 C5 115.54(15) . . ? H4A C4 H4B 107.5 . . ? C5 C4 H4A 108.4 . . ? C5 C4 H4B 108.4 . . ? C4 C5 H5A 109.1 . . ? C4 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? C6 C5 C4 112.39(14) . . ? C6 C5 H5A 109.1 . . ? C6 C5 H5B 109.1 . . ? C5 C6 H6 115.4 . . ? C7 C6 C5 129.17(17) . . ? C7 C6 H6 115.4 . . ? C6 C7 C8 119.07(16) . . ? C6 C7 C16 122.64(17) . . ? C16 C7 C8 117.76(15) . . ? O1 C8 C7 112.63(15) . . ? O1 C8 H8 108.7 . . ? O1 C8 C9 107.21(15) . . ? C7 C8 H8 108.7 . . ? C7 C8 C9 110.93(14) . . ? C9 C8 H8 108.7 . . ? C8 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? C8 C9 C10 111.19(14) . . ? H9A C9 H9B 108.0 . . ? C10 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? C1 C10 H10 106.5 . . ? C9 C10 C1 111.67(13) . . ? C9 C10 H10 106.5 . . ? C11 C10 C1 112.73(13) . . ? C11 C10 C9 112.48(14) . . ? C11 C10 H10 106.5 . . ? C12 C11 C10 116.09(15) . . ? C17 C11 C10 121.37(16) . . ? C17 C11 C12 122.54(18) . . ? C11 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C11 C12 C13 110.97(15) . . ? H12A C12 H12B 108.0 . . ? C13 C12 H12A 109.4 . . ? C13 C12 H12B 109.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 C14 110.78(15) . . ? H13A C13 H13B 108.1 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? C1 C14 H14 106.3 . . ? C13 C14 C1 111.33(13) . . ? C13 C14 H14 106.3 . . ? C13 C14 C18 113.89(14) . . ? C18 C14 C1 112.04(13) . . ? C18 C14 H14 106.3 . . ? O4 C15 O5 122.56(16) . . ? O4 C15 C3 123.57(16) . . ? O5 C15 C3 113.87(14) . . ? O2 C16 C7 116.22(17) . . ? O3 C16 O2 119.61(17) . . ? O3 C16 C7 124.17(16) . . ? C11 C17 H17A 120.0 . . ? C11 C17 H17B 120.0 . . ? H17A C17 H17B 120.0 . . ? C14 C18 H18 108.1 . . ? C19 C18 C14 112.95(15) . . ? C19 C18 H18 108.1 . . ? C20 C18 C14 111.65(14) . . ? C20 C18 H18 108.1 . . ? C20 C18 C19 107.73(16) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 H21A 109.5 . . ? O5 C21 H21B 109.5 . . ? O5 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 O6 H6A 104(3) . . ? O6 C22 H22A 109.5 . . ? O6 C22 H22B 109.5 . . ? O6 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 H1 0.8400 . ? O1 C8 1.446(2) . ? O2 H2 0.8400 . ? O2 C16 1.324(2) . ? O3 C16 1.216(2) . ? O4 C15 1.206(2) . ? O5 C15 1.336(2) . ? O5 C21 1.442(2) . ? C1 H1A 1.0000 . ? C1 C2 1.507(2) . ? C1 C10 1.562(2) . ? C1 C14 1.554(2) . ? C2 H2A 0.9500 . ? C2 C3 1.341(2) . ? C3 C4 1.514(2) . ? C3 C15 1.493(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.550(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.505(3) . ? C6 H6 0.9500 . ? C6 C7 1.342(3) . ? C7 C8 1.524(3) . ? C7 C16 1.497(2) . ? C8 H8 1.0000 . ? C8 C9 1.534(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.547(2) . ? C10 H10 1.0000 . ? C10 C11 1.516(2) . ? C11 C12 1.505(2) . ? C11 C17 1.319(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.528(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.532(2) . ? C14 H14 1.0000 . ? C14 C18 1.538(2) . ? C17 H17A 0.9500 . ? C17 H17B 0.9500 . ? C18 H18 1.0000 . ? C18 C19 1.530(2) . ? C18 C20 1.525(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O6 C22 1.405(3) . ? O6 H6A 0.81(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ?