#------------------------------------------------------------------------------ #$Date: 2022-12-01 01:43:26 +0000 (Thu, 01 Dec 2022) $ #$Revision: 279663 $ #$URL: svn://www.crystallography.net/cod/cif/3/00/04/3000415.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_3000415 loop_ _publ_author_name 'Phansuang Udomputtimekakul' _journal_name_full 'Personal communication to COD' _journal_year 2022 _chemical_absolute_configuration unk _chemical_formula_moiety 'C19 H20 O6' _chemical_formula_sum 'C19 H20 O6' _chemical_formula_weight 344.35 _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 _audit_creation_date 2022-07-19 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.40000(10) _cell_length_b 9.9684(2) _cell_length_c 25.9394(6) _cell_measurement_reflns_used 6568 _cell_measurement_temperature 296.15 _cell_measurement_theta_max 24.813 _cell_measurement_theta_min 2.577 _cell_volume 1654.88(6) _computing_cell_refinement 'SAINT V8.40A (Bruker, 2019)' _computing_data_reduction 'SAINT V8.40A (Bruker, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 296.15 _diffrn_detector 'Bruker PHOTON 200 area detector' _diffrn_detector_area_resol_mean 7.39 _diffrn_detector_type 'PHOTON II area detector' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device 'four-circle KAPPA diffractometer' _diffrn_measurement_device_type 'BRUKER D8 QUEST CMOS PHOTON II' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_collimation '0.5 mm' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_reflns_av_R_equivalents 0.0881 _diffrn_reflns_av_unetI/netI 0.0326 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 46671 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.409 _diffrn_reflns_theta_min 3.119 _diffrn_source 'sealed x-ray tube' _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.103 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6609 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0814 before and 0.0760 after correction. The Ratio of minimum to maximum transmission is 0.8866. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.382 _exptl_crystal_description plate _exptl_crystal_F_000 728 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.139 _refine_diff_density_min -0.124 _refine_diff_density_rms 0.034 _refine_ls_abs_structure_details ; Flack x determined using 962 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.2(6) _refine_ls_extinction_coef 0.0074(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 234 _refine_ls_number_reflns 3376 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.041 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0393 _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^)+(0.0366P)^2^+0.2803P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.0896 _reflns_Friedel_coverage 0.711 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.998 _reflns_number_gt 2693 _reflns_number_total 3376 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file KCWP3242_0m_a.cif _cod_data_source_block kcwp3242_0m_a _cod_depositor_comments ;Releasing structure 3000415 into public domain as personal communication to COD. ; _cod_database_code 3000415 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.996 _shelx_estimated_absorpt_t_min 0.968 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances O5-H5 0.82 with sigma of 0.02 3.a Ternary CH refined with riding coordinates: C8(H8), C9(H9), C16(H16) 3.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B) 3.c Aromatic/amide H refined with riding coordinates: C2(H2), C5(H5A), C11(H11), C13(H13), C14(H14) 3.d Idealised Me refined as rotating group: C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C) ; _shelx_res_file ; TITL KCWP3242_0m_a.res in P2(1)2(1)2(1) kcwp3242_0m_a.res created by SHELXL-2018/3 at 13:28:16 on 19-Jul-2022 REM Old TITL KCWP3242_0m in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.130, Rweak 0.039, Alpha 0.001, Orientation as input REM Flack x = -0.111 ( 0.553 ) from Parsons' quotients REM Formula found by SHELXT: C19 O6 CELL 0.71073 6.4 9.9684 25.9394 90 90 90 ZERR 4 0.0001 0.0002 0.0006 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 76 80 24 DFIX 0.82 O5 H5 L.S. 10 PLAN 8 SIZE 0.32 0.28 0.04 TEMP 23 CONF HTAB C5 O5 BOND $H LIST 4 MORE -1 fmap 2 acta REM REM REM WGHT 0.036600 0.280300 EXTI 0.007437 FVAR 0.57610 O1 3 0.609132 0.812738 0.245194 11.00000 0.03673 0.06769 = 0.03652 -0.00149 -0.00031 -0.01827 O2 3 0.293150 0.754492 0.358677 11.00000 0.05017 0.06174 = 0.03298 -0.00548 0.00470 -0.02183 O3 3 0.513229 0.728320 0.065088 11.00000 0.05063 0.06115 = 0.03578 -0.00069 0.01140 -0.00503 O4 3 0.155281 0.613086 0.081564 11.00000 0.05121 0.06113 = 0.03474 -0.00757 -0.00318 -0.01192 O5 3 -0.126788 0.574454 0.256838 11.00000 0.03768 0.06175 = 0.04394 -0.00097 -0.00442 -0.01582 H5 2 -0.191396 0.649886 0.259079 11.00000 0.07443 O6 3 -0.099158 0.586324 0.500338 11.00000 0.06606 0.07379 = 0.03667 0.00064 0.01130 -0.01170 C1 1 0.451968 0.721959 0.115572 11.00000 0.03892 0.04168 = 0.03429 0.00280 0.00486 0.00477 C2 1 0.562683 0.771469 0.156748 11.00000 0.03137 0.04632 = 0.04061 0.00250 0.00454 -0.00338 AFIX 43 H2 2 0.692925 0.810513 0.151488 11.00000 -1.20000 AFIX 0 C3 1 0.480442 0.763358 0.206344 11.00000 0.03294 0.03995 = 0.03618 0.00131 -0.00388 -0.00340 C4 1 0.286596 0.707121 0.215965 11.00000 0.03192 0.03533 = 0.03142 0.00208 -0.00041 -0.00045 C5 1 0.178382 0.654201 0.173697 11.00000 0.03263 0.03918 = 0.03679 0.00173 0.00066 -0.00109 AFIX 43 H5A 2 0.049488 0.613499 0.179118 11.00000 -1.20000 AFIX 0 C6 1 0.256970 0.660581 0.124349 11.00000 0.03854 0.03867 = 0.03519 -0.00185 -0.00214 0.00071 C7 1 0.506482 0.841730 0.293075 11.00000 0.04417 0.06155 = 0.03677 -0.00524 0.00100 -0.02011 AFIX 23 H7A 2 0.422347 0.922127 0.289486 11.00000 -1.20000 H7B 2 0.609870 0.857586 0.319731 11.00000 -1.20000 AFIX 0 C8 1 0.368992 0.725100 0.308213 11.00000 0.03721 0.04713 = 0.03034 -0.00061 0.00063 -0.00638 AFIX 13 H8 2 0.452529 0.642748 0.309195 11.00000 -1.20000 AFIX 0 C9 1 0.192347 0.708697 0.269858 11.00000 0.03091 0.03478 = 0.03179 0.00019 -0.00086 0.00168 AFIX 13 H9 2 0.101879 0.787708 0.272540 11.00000 -1.20000 AFIX 0 C10 1 0.137429 0.669956 0.375707 11.00000 0.03559 0.03838 = 0.03590 0.00279 0.00177 -0.00334 C11 1 0.100932 0.672108 0.428668 11.00000 0.04339 0.04392 = 0.03633 -0.00251 -0.00120 -0.00207 AFIX 43 H11 2 0.179888 0.727140 0.450085 11.00000 -1.20000 AFIX 0 C12 1 -0.053520 0.591696 0.448837 11.00000 0.04893 0.04589 = 0.03604 0.00100 0.00737 0.00169 C13 1 -0.171120 0.510636 0.416916 11.00000 0.06119 0.05180 = 0.04591 0.00011 0.01324 -0.01915 AFIX 43 H13 2 -0.275749 0.456517 0.430571 11.00000 -1.20000 AFIX 0 C14 1 -0.132299 0.510495 0.364608 11.00000 0.05027 0.04910 = 0.04149 -0.00304 0.00477 -0.01346 AFIX 43 H14 2 -0.213069 0.456144 0.343347 11.00000 -1.20000 AFIX 0 C15 1 0.024003 0.589142 0.342591 11.00000 0.03532 0.03333 = 0.03764 0.00142 0.00332 -0.00287 C16 1 0.064268 0.586475 0.284874 11.00000 0.02911 0.03721 = 0.03605 -0.00057 -0.00076 -0.00213 AFIX 13 H16 2 0.148568 0.506744 0.277396 11.00000 -1.20000 AFIX 0 C17 1 0.689232 0.811593 0.052648 11.00000 0.05462 0.07614 = 0.04967 0.00930 0.01480 -0.00644 AFIX 137 H17A 2 0.711944 0.810336 0.016069 11.00000 -1.50000 H17B 2 0.811311 0.778232 0.069913 11.00000 -1.50000 H17C 2 0.662105 0.901882 0.063646 11.00000 -1.50000 AFIX 0 C18 1 -0.014827 0.522992 0.090536 11.00000 0.05621 0.06463 = 0.05051 -0.01183 -0.00514 -0.01827 AFIX 137 H18A 2 -0.070705 0.493492 0.058115 11.00000 -1.50000 H18B 2 -0.121897 0.568172 0.109781 11.00000 -1.50000 H18C 2 0.033951 0.446845 0.109733 11.00000 -1.50000 AFIX 0 C19 1 0.055495 0.633783 0.534653 11.00000 0.06532 0.09983 = 0.03697 0.00204 0.00298 0.01085 AFIX 137 H19A 2 0.188560 0.596526 0.525336 11.00000 -1.50000 H19B 2 0.020797 0.607208 0.569180 11.00000 -1.50000 H19C 2 0.062221 0.729865 0.532763 11.00000 -1.50000 AFIX 0 HKLF 4 REM KCWP3242_0m_a.res in P2(1)2(1)2(1) REM wR2 = 0.0896, GooF = S = 1.040, Restrained GooF = 1.041 for all data REM R1 = 0.0393 for 2693 Fo > 4sig(Fo) and 0.0571 for all 3376 data REM 234 parameters refined using 1 restraints END WGHT 0.0367 0.2779 REM Highest difference peak 0.139, deepest hole -0.124, 1-sigma level 0.034 Q1 1 0.6983 0.8591 0.0179 11.00000 0.05 0.14 Q2 1 0.0504 0.5997 0.3172 11.00000 0.05 0.14 Q3 1 -0.0085 0.6540 0.4364 11.00000 0.05 0.13 Q4 1 -0.1084 0.6121 0.3445 11.00000 0.05 0.13 Q5 1 0.5504 0.8327 -0.0048 11.00000 0.05 0.13 Q6 1 0.3917 0.7248 0.2114 11.00000 0.05 0.12 Q7 1 -0.0257 0.5449 0.2135 11.00000 0.05 0.12 Q8 1 0.1186 0.5938 0.3658 11.00000 0.05 0.12 ; _shelx_res_checksum 25229 _shelx_hkl_file ; -1 0 0 0.90 1.60 -1 0 0 0.20 0.90 -1 0 0 0.20 0.90 1 0 0 -1.20 1.00 1 0 0 0.20 0.80 1 0 0 0.60 1.10 1 0 0 -0.50 0.80 1 0 0 0.10 0.80 -1 0 0 0.10 0.90 -1 0 0 -0.40 1.70 -2 0 0 836.12 20.50 2 0 0 827.52 24.00 2 0 0 852.41 24.60 -2 0 0 773.22 20.20 -2 0 0 792.02 24.00 2 0 0 805.82 20.30 -2 0 0 815.82 20.90 2 0 0 821.22 20.50 -2 0 0 787.42 23.80 3 0 0 2.20 1.60 3 0 0 1.50 1.10 3 0 0 1.00 2.80 -3 0 0 3.60 1.90 -3 0 0 3.60 2.70 3 0 0 2.20 2.40 -3 0 0 1.90 1.60 -3 0 0 4.10 1.90 -3 0 0 2.80 2.50 -4 0 0 36.70 6.50 4 0 0 33.60 6.10 4 0 0 35.30 3.60 4 0 0 36.10 3.90 4 0 0 43.10 7.80 -4 0 0 42.60 4.30 -4 0 0 37.90 7.70 5 0 0 0.40 3.50 5 0 0 -2.20 3.20 -5 0 0 4.60 2.50 -6 0 0 50.79 7.50 6 0 0 31.10 7.30 -7 0 0 -2.60 3.30 7 0 0 -2.50 5.70 8 0 0 1.70 8.80 -1 -1 0 150.28 6.30 1 1 0 145.09 5.50 -1 -1 0 154.98 5.70 -1 1 0 156.18 7.10 -1 1 0 148.79 6.90 -1 -1 0 154.98 5.70 1 -1 0 151.88 6.90 1 -1 0 155.28 6.70 -1 1 0 160.68 5.70 -1 1 0 146.69 7.80 -1 1 0 166.58 8.00 1 -1 0 147.69 6.90 1 -1 0 156.88 5.60 -1 -1 0 148.89 5.60 1 1 0 129.89 5.30 1 1 0 149.29 6.40 1 1 0 150.38 5.80 1 -1 0 156.28 7.80 -2 1 0 836.72 26.90 2 -1 0 873.01 27.10 -2 1 0 822.72 25.70 -2 -1 0 876.81 21.30 -2 -1 0 866.21 21.20 2 1 0 842.42 21.20 -2 1 0 914.01 24.20 2 -1 0 906.81 24.20 2 -1 0 912.01 24.20 -2 1 0 879.91 23.90 -2 -1 0 846.42 24.40 -2 1 0 912.01 22.60 2 -1 0 930.61 26.40 -2 -1 0 903.51 23.10 2 1 0 858.91 24.50 2 1 0 857.11 21.30 2 1 0 846.12 24.70 3 -1 0 33.70 4.70 -3 -1 0 33.00 5.50 3 -1 0 38.60 6.90 3 1 0 29.40 5.00 3 1 0 39.60 6.10 -3 1 0 37.40 3.80 -3 1 0 45.70 7.50 -3 1 0 34.50 4.50 -3 1 0 38.20 5.00 3 -1 0 32.90 5.70 -3 -1 0 39.80 5.10 3 -1 0 29.10 4.20 -3 1 0 29.20 5.30 -4 -1 0 7.70 3.50 4 -1 0 8.30 4.90 -4 1 0 7.50 2.90 -4 1 0 14.80 5.30 4 1 0 10.50 4.40 4 1 0 3.80 3.10 4 -1 0 19.40 5.60 4 -1 0 10.90 3.10 -4 1 0 9.40 2.50 -4 -1 0 15.50 3.80 4 -1 0 5.90 2.40 -4 1 0 10.90 3.00 -5 1 0 29.90 4.60 -5 1 0 21.50 4.30 5 -1 0 21.80 6.50 5 -1 0 26.90 4.50 5 -1 0 23.50 4.60 5 -1 0 32.30 7.90 -5 -1 0 28.60 5.60 -5 1 0 29.10 5.10 5 1 0 32.70 7.60 5 1 0 31.60 7.00 -5 1 0 25.90 6.90 -6 1 0 5.60 3.40 -6 1 0 -1.70 4.60 6 1 0 3.80 4.50 6 -1 0 -0.40 2.90 6 -1 0 3.90 5.00 -6 -1 0 10.70 3.90 6 1 0 0.80 4.00 6 -1 0 4.70 4.10 6 -1 0 6.10 3.30 7 1 0 22.30 10.60 7 1 0 5.50 5.50 7 -1 0 -0.70 6.20 7 1 0 5.30 6.40 -7 1 0 6.10 3.60 0 2 0 4775.92 106.79 0 -2 0 4815.32 102.09 0 2 0 4617.74 106.39 0 -2 0 4768.62 106.79 0 -2 0 4749.92 106.59 0 2 0 4956.30 104.59 0 2 0 4762.52 106.49 -1 2 0 9323.37 212.78 -1 2 0 9759.32 211.68 -1 -2 0 9472.45 209.68 -1 -2 0 9843.92 209.68 -1 -2 0 9631.04 209.48 1 2 0 9903.31 209.68 1 2 0 9916.31 208.98 1 2 0 9999.00 205.88 1 -2 0 9625.54 213.08 1 2 0 9657.53 209.58 1 -2 0 9796.42 211.78 1 -2 0 9743.92 211.58 1 2 0 9770.42 209.98 -1 -2 0 9837.02 205.88 -1 2 0 9795.32 208.48 1 -2 0 9721.03 209.68 -2 2 0 69.19 7.70 -2 2 0 71.39 6.40 2 2 0 65.09 5.50 2 -2 0 66.09 6.40 2 2 0 76.59 5.30 2 -2 0 69.29 7.60 2 -2 0 54.19 6.10 -2 2 0 76.39 6.80 2 2 0 69.09 4.90 2 2 0 73.99 4.90 -2 2 0 78.09 5.20 -2 -2 0 65.09 5.20 -2 2 0 73.09 6.90 -2 -2 0 69.69 4.90 -2 -2 0 66.29 4.80 2 -2 0 79.49 6.70 3 2 0 338.77 15.30 -3 2 0 345.37 14.90 3 -2 0 347.27 15.10 -3 2 0 364.66 13.30 -3 -2 0 355.06 14.70 -3 -2 0 357.16 11.60 -3 2 0 365.06 15.40 3 2 0 341.57 11.50 3 -2 0 355.46 16.80 3 -2 0 337.47 17.60 3 2 0 365.66 12.00 -3 2 0 364.26 18.60 3 2 0 368.56 14.80 3 2 0 347.57 15.10 -3 -2 0 359.66 11.70 3 -2 0 346.97 15.00 -3 2 0 372.86 17.20 -4 2 0 140.69 9.50 -4 -2 0 144.59 10.40 4 -2 0 149.99 10.20 4 -2 0 133.59 9.30 4 2 0 165.08 11.00 4 -2 0 148.79 12.60 -4 2 0 146.69 9.90 4 2 0 153.88 10.70 4 2 0 153.98 10.80 -4 2 0 140.79 12.50 4 -2 0 163.68 12.30 -4 2 0 145.99 8.30 5 2 0 12.60 4.70 5 -2 0 5.00 3.40 -5 2 0 17.50 4.20 -5 2 0 9.90 3.70 5 2 0 1.30 3.60 -5 2 0 15.00 6.50 -5 2 0 9.10 3.40 5 -2 0 3.30 3.70 5 2 0 4.20 4.00 5 -2 0 14.10 5.40 5 -2 0 4.40 4.60 -6 2 0 2.70 2.90 6 2 0 -3.70 4.30 6 -2 0 0.50 5.40 6 2 0 4.80 4.30 6 -2 0 5.40 3.60 -6 2 0 -0.10 2.90 -6 2 0 2.20 3.70 6 2 0 6.40 4.20 6 -2 0 -0.10 5.80 -6 2 0 0.10 5.00 7 -2 0 0.40 6.50 7 2 0 7.10 5.30 7 -2 0 -0.60 4.00 -7 2 0 -1.50 6.40 7 2 0 8.40 8.80 7 2 0 10.10 7.00 -7 2 0 0.70 3.50 0 -3 0 1.30 1.70 0 -3 0 -0.90 1.40 0 -3 0 -0.10 2.80 0 3 0 -0.60 2.30 0 3 0 -1.90 2.70 0 3 0 1.30 2.80 0 3 0 0.10 2.70 0 -3 0 -0.90 2.30 0 -3 0 -0.50 2.30 1 3 0 6680.33 147.19 1 -3 0 6652.83 150.48 -1 3 0 6524.65 148.99 -1 3 0 6258.67 148.29 1 -3 0 6578.34 149.09 -1 -3 0 6577.14 147.09 1 3 0 6574.24 145.19 1 3 0 6646.23 147.09 -1 3 0 6816.92 145.09 1 3 0 6514.95 146.89 -1 -3 0 6657.73 147.19 -1 3 0 6561.74 150.58 1 -3 0 6662.93 144.99 1 -3 0 6559.94 148.89 2 -3 0 41.20 5.40 -2 -3 0 53.49 5.40 2 3 0 69.79 6.20 2 -3 0 44.20 6.20 -2 -3 0 64.29 4.60 2 3 0 61.29 6.00 -2 3 0 51.89 5.10 2 3 0 60.99 5.60 -2 3 0 39.50 7.00 -2 -3 0 64.79 5.90 -2 -3 0 68.09 5.90 -2 3 0 61.19 8.30 2 -3 0 71.19 9.90 2 -3 0 59.09 8.10 2 3 0 61.59 5.70 2 3 0 63.79 4.60 -3 -3 0 201.88 9.50 3 -3 0 215.48 14.90 3 -3 0 212.88 12.60 3 -3 0 214.98 13.10 -3 -3 0 206.98 10.30 3 3 0 219.48 10.50 -3 3 0 209.68 10.30 -3 3 0 227.98 12.90 -3 3 0 213.98 12.80 3 3 0 212.68 9.80 3 3 0 205.58 11.60 3 -3 0 220.98 13.00 3 3 0 201.58 9.80 -3 -3 0 208.78 9.70 -3 3 0 210.88 14.70 4 3 0 55.09 5.00 4 -3 0 57.09 7.90 -4 3 0 52.49 6.90 -4 3 0 38.40 8.00 -4 3 0 55.49 7.70 4 3 0 53.79 4.60 4 3 0 51.39 8.20 4 -3 0 31.60 5.90 -4 3 0 48.80 8.20 4 -3 0 55.99 9.40 4 3 0 54.29 6.40 -4 -3 0 45.80 4.40 4 3 0 55.59 6.80 4 -3 0 39.50 6.80 5 3 0 35.80 7.00 5 3 0 39.20 8.30 5 3 0 13.70 5.00 -5 3 0 20.40 4.80 -5 3 0 23.50 5.70 -5 3 0 23.90 7.70 5 -3 0 26.70 8.50 5 -3 0 21.90 5.80 -5 3 0 37.60 6.70 5 -3 0 30.50 8.10 5 -3 0 15.50 5.60 6 3 0 40.20 8.80 6 3 0 36.70 7.90 -6 3 0 41.20 7.00 -6 3 0 33.10 10.00 -6 3 0 46.20 7.60 6 -3 0 45.40 10.90 6 3 0 51.59 9.90 6 -3 0 48.30 9.00 6 -3 0 39.50 8.90 -6 3 0 46.10 7.90 6 -3 0 31.80 6.30 -7 3 0 0.10 3.40 7 -3 0 0.30 4.30 7 3 0 5.60 5.70 -7 3 0 -5.10 3.70 -7 3 0 -0.40 3.20 7 3 0 1.30 4.70 7 3 0 -1.80 7.00 7 -3 0 3.20 7.60 -7 3 0 1.40 6.30 0 -4 0 127.39 5.90 0 -4 0 143.39 10.20 0 -4 0 141.69 10.20 0 4 0 130.09 10.20 0 4 0 110.39 9.50 0 -4 0 137.39 6.00 0 -4 0 136.49 10.10 0 4 0 141.09 10.70 0 4 0 128.79 8.30 -1 -4 0 225.88 12.70 1 -4 0 234.88 13.80 1 4 0 240.48 13.00 -1 4 0 230.88 13.70 -1 4 0 262.37 11.80 1 -4 0 228.78 14.20 1 -4 0 239.98 10.90 -1 4 0 263.87 14.30 -1 4 0 244.18 14.70 1 4 0 245.88 13.20 1 4 0 225.28 11.50 1 4 0 238.28 12.90 -1 -4 0 241.78 13.00 1 -4 0 244.08 13.90 2 4 0 3.00 2.70 2 -4 0 0.40 2.90 2 -4 0 -1.80 2.40 2 -4 0 4.00 3.70 -2 -4 0 6.10 3.00 -2 4 0 4.00 3.60 -2 -4 0 4.40 2.60 2 -4 0 2.80 3.40 -2 4 0 -1.10 2.20 2 4 0 2.10 2.50 2 4 0 1.40 1.50 -2 4 0 0.90 3.30 2 4 0 2.60 2.70 -2 4 0 2.20 2.70 -2 -4 0 4.70 2.90 2 4 0 5.10 3.00 3 -4 0 97.99 9.40 3 4 0 85.79 7.50 3 4 0 74.79 7.80 -3 -4 0 98.19 8.50 3 -4 0 92.69 11.10 -3 4 0 88.89 7.20 -3 4 0 116.59 11.60 3 4 0 97.29 6.50 3 -4 0 86.99 9.00 -3 4 0 84.29 9.30 3 -4 0 100.79 9.20 -3 -4 0 105.69 6.70 -3 -4 0 90.19 7.40 3 4 0 103.89 8.10 3 4 0 96.69 7.60 -3 -4 0 95.79 7.50 -4 4 0 65.89 9.30 4 4 0 78.49 6.70 -4 4 0 74.39 7.00 4 4 0 63.29 8.20 4 -4 0 61.29 11.50 4 -4 0 81.79 9.30 4 -4 0 61.19 9.90 -4 -4 0 71.99 6.40 4 4 0 70.19 9.60 -4 4 0 65.49 11.40 -4 -4 0 73.29 6.40 4 -4 0 72.49 10.20 -4 4 0 65.59 9.40 4 4 0 63.59 6.20 4 4 0 65.09 6.60 5 -4 0 3.00 5.90 5 -4 0 -2.60 3.60 -5 4 0 3.10 3.80 5 -4 0 -0.10 4.90 5 4 0 -2.80 2.60 -5 4 0 2.60 4.70 5 4 0 1.00 3.30 -5 4 0 -4.50 3.40 5 4 0 2.40 3.50 5 -4 0 -1.40 4.30 -5 4 0 -0.40 2.80 6 -4 0 9.50 6.90 -6 4 0 8.20 5.10 -6 4 0 8.50 6.10 6 -4 0 13.30 5.30 6 4 0 2.60 3.60 6 4 0 18.90 6.20 6 4 0 15.10 5.70 -6 4 0 10.30 4.80 6 4 0 12.10 4.20 -6 4 0 10.40 4.90 7 4 0 5.50 6.00 7 -4 0 -8.70 4.30 -7 4 0 -2.40 3.10 7 4 0 -0.60 6.30 -7 4 0 4.80 4.80 -7 4 0 4.80 6.80 -7 4 0 4.20 4.70 7 4 0 2.20 4.10 7 4 0 -5.90 4.30 0 -5 0 1.70 1.80 0 -5 0 -0.50 2.90 0 -5 0 0.20 1.40 0 -5 0 2.10 2.60 0 5 0 -3.10 2.20 0 5 0 0.00 2.80 0 -5 0 0.60 3.00 0 5 0 -0.70 3.20 0 5 0 -0.20 2.50 -1 5 0 436.26 22.20 1 -5 0 466.65 22.60 1 -5 0 459.55 16.60 1 5 0 469.55 20.90 -1 5 0 462.25 21.80 1 5 0 481.95 21.00 -1 5 0 436.26 21.40 1 -5 0 468.25 21.90 1 5 0 465.75 18.80 1 5 0 459.75 20.60 1 -5 0 463.05 21.70 -1 -5 0 461.35 20.40 -1 -5 0 443.16 20.20 -1 -5 0 503.85 21.40 -1 5 0 451.65 18.30 -2 5 0 1016.10 38.80 2 -5 0 1037.70 38.60 -2 -5 0 1047.30 34.00 -2 -5 0 1009.00 33.70 2 -5 0 1021.70 32.20 -2 -5 0 1030.80 33.70 2 -5 0 1020.70 36.60 -2 5 0 1008.40 36.30 -2 5 0 996.40 31.50 -2 5 0 1013.50 36.30 2 5 0 1034.10 34.20 2 5 0 1012.30 33.80 2 5 0 1020.00 32.20 2 5 0 1012.60 33.60 2 -5 0 976.10 35.80 3 5 0 39.70 4.70 3 5 0 32.40 6.90 -3 -5 0 34.70 6.90 -3 5 0 16.70 6.40 -3 5 0 26.80 5.40 3 5 0 23.30 5.40 3 -5 0 20.20 5.80 3 5 0 29.60 6.10 3 -5 0 38.70 7.10 3 -5 0 37.30 7.20 -3 -5 0 27.50 5.10 3 5 0 48.00 7.80 -3 5 0 35.10 7.50 3 -5 0 23.70 7.80 -3 5 0 27.00 6.20 -3 -5 0 30.80 6.20 4 -5 0 17.50 6.10 4 5 0 17.70 4.20 -4 5 0 23.90 6.40 -4 5 0 21.10 7.00 4 -5 0 13.70 6.60 -4 -5 0 22.00 4.80 4 -5 0 15.80 7.10 4 -5 0 28.50 8.50 -4 5 0 19.00 6.30 4 5 0 15.70 4.80 4 5 0 13.10 4.40 -4 -5 0 21.20 4.60 -4 5 0 18.30 5.40 4 5 0 14.70 4.50 4 5 0 18.70 5.40 5 5 0 -1.60 3.60 5 5 0 3.40 3.40 -5 -5 0 -2.60 1.80 5 5 0 5.70 3.40 5 5 0 3.00 3.20 -5 5 0 -6.90 3.70 -5 5 0 9.40 4.10 5 5 0 2.20 2.80 5 -5 0 2.10 4.50 5 5 0 2.30 3.60 5 -5 0 1.70 6.20 -5 5 0 1.70 5.50 5 -5 0 5.20 6.50 -5 -5 0 5.00 2.90 5 -5 0 1.10 4.50 -5 5 0 -1.80 5.00 -6 5 0 4.60 5.20 6 5 0 2.10 4.30 -6 5 0 -0.70 4.80 6 5 0 5.40 4.30 6 -5 0 -0.90 4.70 6 -5 0 -6.30 7.80 6 5 0 -0.50 3.80 -6 5 0 0.10 6.30 6 5 0 10.60 4.50 -6 5 0 2.20 3.70 7 5 0 -2.20 5.40 -7 5 0 4.10 4.30 7 5 0 14.80 6.10 7 5 0 17.60 8.00 7 -5 0 23.70 6.50 -7 5 0 11.50 9.60 -7 5 0 6.60 7.30 7 5 0 13.70 6.40 -7 5 0 16.90 6.70 0 6 0 110.89 11.40 0 -6 0 116.19 11.30 0 -6 0 116.89 6.30 0 6 0 140.09 12.10 0 -6 0 114.89 6.20 0 -6 0 102.39 10.70 0 -6 0 137.39 12.30 0 6 0 120.49 11.00 0 6 0 126.39 9.90 -1 6 0 30.00 7.10 1 6 0 46.30 9.00 1 6 0 17.70 6.10 1 -6 0 29.80 5.40 -1 6 0 34.90 6.40 -1 -6 0 31.80 7.10 1 -6 0 34.50 6.80 1 -6 0 39.80 9.10 -1 -6 0 23.20 5.90 -1 6 0 36.30 6.70 1 -6 0 33.80 6.70 1 6 0 22.50 5.50 -1 -6 0 29.30 7.00 1 -6 0 45.70 5.70 1 6 0 39.10 8.00 -2 6 0 264.87 17.50 2 -6 0 258.17 14.00 2 -6 0 247.48 18.60 -2 6 0 264.17 14.40 -2 6 0 238.08 18.50 -2 -6 0 240.38 15.10 -2 -6 0 243.48 15.80 2 6 0 252.97 15.70 2 6 0 248.18 14.50 2 -6 0 243.98 17.20 2 -6 0 249.58 17.20 2 6 0 264.67 16.00 2 6 0 233.78 15.60 -2 -6 0 254.67 15.80 -2 6 0 265.87 17.60 3 -6 0 9.60 3.90 3 6 0 12.60 5.30 3 -6 0 10.50 5.50 3 6 0 16.50 5.30 -3 6 0 13.50 6.00 -3 6 0 1.70 4.60 -3 -6 0 10.60 4.00 -3 6 0 9.00 4.10 3 6 0 12.40 4.90 3 -6 0 7.20 3.40 -3 -6 0 7.70 4.20 -3 6 0 8.90 4.90 3 -6 0 8.30 5.40 -3 -6 0 7.30 3.90 3 6 0 8.40 4.20 -4 -6 0 29.30 6.30 4 -6 0 21.10 7.20 -4 6 0 14.40 7.70 4 6 0 17.60 5.30 4 6 0 33.50 6.80 4 6 0 23.10 4.30 4 -6 0 40.40 11.40 4 6 0 34.50 6.90 4 6 0 25.00 6.80 4 -6 0 29.60 8.00 4 -6 0 37.00 8.90 -4 6 0 24.10 8.10 -4 -6 0 31.30 6.70 -4 6 0 29.90 6.60 5 -6 0 7.10 6.80 5 -6 0 5.60 5.10 5 -6 0 12.50 7.50 -5 6 0 6.40 5.10 -5 -6 0 1.60 3.10 -5 -6 0 5.10 3.00 -5 6 0 -0.70 4.70 5 6 0 4.90 3.80 5 6 0 5.00 3.90 5 6 0 10.20 4.60 -5 6 0 1.20 3.40 5 6 0 11.90 4.00 -5 6 0 3.70 5.40 5 -6 0 10.90 6.50 5 6 0 1.20 4.60 -6 6 0 -4.10 7.00 6 6 0 9.30 3.90 6 6 0 -0.60 4.70 6 6 0 5.00 4.80 -6 6 0 3.30 3.60 -6 6 0 -0.40 5.30 6 6 0 5.90 4.70 -6 6 0 -6.80 5.50 6 -6 0 -1.90 5.30 -7 6 0 7.80 5.20 7 6 0 -3.50 5.40 7 6 0 1.80 4.80 7 6 0 4.70 7.20 -7 6 0 -4.00 6.10 7 -6 0 -3.90 6.60 7 6 0 1.90 5.00 7 6 0 6.30 5.40 -7 6 0 7.30 6.80 -7 6 0 -11.20 8.50 0 7 0 5.70 4.50 0 -7 0 -0.20 1.60 0 -7 0 -1.30 3.20 0 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0.20 4.00 -4 7 0 1.60 5.70 -4 -7 0 -0.40 4.10 4 7 0 11.10 6.10 -4 -7 0 7.60 4.40 -4 7 0 3.10 4.70 4 7 0 3.70 4.50 4 -7 0 -10.30 5.00 4 -7 0 9.80 6.40 -4 -7 0 4.40 3.50 -4 7 0 7.90 6.30 5 -7 0 -0.20 5.10 -5 7 0 3.90 5.60 -5 -7 0 0.60 4.10 5 -7 0 1.40 7.40 -5 -7 0 0.10 3.80 5 7 0 0.70 2.60 -5 7 0 0.80 6.30 5 7 0 1.60 3.30 -5 7 0 6.10 5.50 5 7 0 -3.70 3.90 -5 7 0 -3.70 3.20 5 7 0 2.10 4.70 5 7 0 -1.60 2.80 6 7 0 2.20 3.80 -6 7 0 -4.80 7.30 6 -7 0 1.50 6.30 6 7 0 13.30 4.70 -6 7 0 17.60 11.00 6 7 0 7.60 5.90 -6 7 0 -1.20 4.30 6 7 0 2.90 4.70 6 7 0 4.20 5.40 -6 7 0 8.30 7.30 6 7 0 11.60 5.90 0 8 0 -0.60 4.90 0 8 0 1.70 4.40 0 8 0 -0.90 4.60 0 -8 0 -0.20 2.40 0 -8 0 0.30 4.20 0 8 0 -1.80 3.10 0 -8 0 0.30 2.00 0 -8 0 4.20 5.70 0 -8 0 0.50 1.70 -1 8 0 6.80 5.50 -1 -8 0 -2.70 2.80 1 -8 0 0.00 3.30 1 -8 0 0.10 1.80 -1 -8 0 2.30 4.50 1 8 0 -5.40 3.20 -1 8 0 2.00 4.70 1 -8 0 -4.60 3.50 1 8 0 2.10 4.10 1 8 0 4.70 4.80 1 -8 0 -0.60 3.60 -1 8 0 -1.00 4.80 1 8 0 3.70 4.10 -1 -8 0 -0.80 4.20 -1 8 0 4.90 4.70 1 -8 0 1.30 3.00 -2 8 0 10.10 6.90 2 -8 0 7.70 5.40 2 8 0 4.80 4.40 -2 8 0 6.00 4.10 -2 -8 0 9.70 5.70 2 -8 0 14.30 4.50 -2 -8 0 12.70 6.70 -2 8 0 3.60 5.80 2 8 0 8.40 5.70 2 -8 0 3.10 3.40 2 -8 0 8.10 5.80 2 -8 0 12.10 7.20 2 8 0 6.30 4.50 -2 8 0 13.30 6.50 2 8 0 9.20 6.40 -3 8 0 8.80 4.80 -3 -8 0 8.80 5.70 3 -8 0 9.70 4.40 3 8 0 0.40 4.20 -3 8 0 -6.00 4.70 3 8 0 2.40 4.30 3 8 0 1.50 3.80 3 -8 0 10.90 7.40 -3 -8 0 3.50 4.40 -3 8 0 10.10 6.80 -3 -8 0 10.50 4.60 3 -8 0 0.40 5.20 3 -8 0 12.20 5.60 3 -8 0 12.40 5.20 3 8 0 2.80 4.80 -3 8 0 2.50 6.30 4 -8 0 21.90 14.40 -4 -8 0 13.30 5.40 -4 -8 0 13.00 4.90 -4 8 0 16.90 8.70 4 8 0 11.90 6.60 -4 8 0 32.30 8.40 4 -8 0 20.60 7.60 4 -8 0 29.00 8.70 4 8 0 19.20 5.70 4 -8 0 9.20 5.90 -4 -8 0 17.30 6.70 -4 8 0 24.80 8.00 -4 8 0 18.70 7.60 4 8 0 13.70 6.30 4 -8 0 -0.90 6.50 5 -8 0 0.40 6.40 5 8 0 2.60 4.90 5 8 0 4.60 5.90 -5 8 0 -6.10 5.50 -5 8 0 -4.20 7.30 5 -8 0 -3.70 5.50 5 8 0 3.90 4.80 -5 -8 0 5.90 5.20 -5 8 0 0.80 3.20 -5 -8 0 8.30 4.00 -5 8 0 3.60 8.50 6 8 0 13.60 7.00 6 8 0 28.50 8.60 -6 8 0 34.70 9.50 6 8 0 6.70 6.80 6 -8 0 18.50 9.50 -6 -8 0 11.10 5.40 6 8 0 27.50 7.30 -6 8 0 29.80 7.80 -6 8 0 23.00 9.70 -6 -8 0 24.10 6.10 6 -8 0 13.10 7.70 -6 8 0 4.80 7.70 0 9 0 3.50 5.70 0 -9 0 0.70 3.90 0 -9 0 4.30 5.90 0 9 0 -2.80 2.50 0 9 0 -1.60 5.40 0 9 0 3.20 5.80 0 -9 0 -2.30 5.00 1 -9 0 5.00 2.90 1 -9 0 9.80 5.90 -1 -9 0 4.30 4.60 -1 -9 0 7.70 6.40 1 -9 0 5.50 3.20 1 9 0 -2.00 5.90 1 9 0 0.20 3.90 1 -9 0 6.60 5.80 1 9 0 0.20 3.30 -1 9 0 1.30 4.70 1 -9 0 3.00 5.40 1 9 0 3.40 5.00 -1 9 0 5.30 5.70 -1 9 0 8.10 4.80 -1 -9 0 0.50 5.00 -1 9 0 1.60 6.80 2 -9 0 9.20 7.00 2 -9 0 12.90 7.80 -2 9 0 13.40 7.00 2 9 0 11.40 7.20 -2 -9 0 10.60 5.60 -2 9 0 23.10 8.10 2 -9 0 9.50 6.30 -2 9 0 10.20 7.00 2 9 0 19.60 7.90 -2 -9 0 7.50 5.00 2 9 0 14.10 8.70 -2 -9 0 11.30 6.80 -2 9 0 7.90 6.40 2 9 0 10.60 5.50 2 -9 0 12.30 4.80 2 -9 0 9.50 4.90 3 -9 0 1.50 3.80 -3 9 0 3.60 6.70 -3 -9 0 -4.70 4.80 3 -9 0 3.70 7.80 3 9 0 1.50 4.20 3 9 0 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6.90 -2 4 -29 -2.50 8.20 2 -4 -29 4.00 7.40 2 -4 -29 1.80 8.80 -2 4 -29 -6.10 5.10 2 4 29 -5.40 8.00 0 -5 29 -1.30 7.70 0 5 -29 -7.50 7.40 0 -5 -29 1.40 7.30 0 -5 29 1.60 10.70 0 5 29 10.30 15.80 0 -5 -29 -14.00 6.70 0 -5 -29 16.50 17.70 0 5 29 7.50 9.20 0 5 29 -3.70 4.10 0 -5 -29 -3.10 6.30 0 -5 -29 2.90 6.60 0 5 -29 -1.70 8.40 0 5 -29 -3.80 4.90 -1 -5 -29 15.20 8.30 1 5 -29 17.20 9.60 -1 5 29 -0.80 13.30 1 -5 29 1.10 10.40 1 5 -29 1.00 6.30 -1 -5 -29 -1.40 4.20 -1 5 29 10.20 9.00 -1 -5 -29 14.90 9.60 1 5 -29 4.00 5.00 -1 5 29 -4.80 3.60 1 -5 29 6.60 8.00 -1 -5 -29 -4.60 12.20 -1 -5 -29 1.50 6.10 -1 5 -29 1.90 4.60 1 5 29 -1.60 8.90 1 -5 -29 -2.20 7.70 1 -5 -29 14.70 8.30 -1 5 -29 -5.30 7.70 -1 5 -29 3.00 7.90 1 -5 -29 -3.90 8.10 -1 -5 29 8.20 6.80 1 5 29 3.60 4.70 1 5 29 -30.00 15.90 -1 -5 29 -18.10 8.50 0 0 -30 7.70 5.70 0 0 30 8.80 5.90 0 0 -30 14.10 10.00 0 0 -30 0.70 6.50 0 0 -30 21.00 8.10 0 0 -30 -0.10 9.40 0 0 30 -2.10 6.70 0 0 30 11.10 10.50 1 0 -30 5.70 7.60 -1 0 30 8.30 7.20 -1 0 -30 12.30 10.20 -1 0 -30 2.50 7.60 -1 0 -30 12.90 8.20 -1 0 -30 28.00 8.60 -1 0 -30 22.90 10.20 1 0 30 16.30 6.80 -1 0 30 8.90 6.50 1 0 -30 15.90 7.40 -1 0 30 7.10 11.50 1 0 30 29.20 12.60 1 0 30 14.70 7.50 1 0 -30 6.60 7.00 -2 0 -30 -19.80 9.60 -2 0 -30 5.90 5.60 2 0 -30 4.10 5.60 -2 0 -30 12.20 9.20 -2 0 -30 5.80 8.80 2 0 30 5.20 11.60 2 0 -30 3.60 8.90 -2 0 -30 8.10 6.80 2 0 30 13.30 11.10 2 0 -30 7.10 7.10 2 0 30 2.40 4.20 -2 0 30 3.60 7.00 -2 0 30 0.20 3.80 3 0 -30 26.80 9.50 -3 0 -30 26.30 10.20 3 0 -30 18.60 8.50 -3 0 -30 9.70 13.20 -3 0 -30 12.30 6.90 -3 0 -30 -1.50 8.20 3 0 30 9.40 4.90 -3 0 30 7.10 10.20 3 0 30 26.90 14.00 -3 0 30 9.50 7.90 3 0 30 3.60 14.50 -3 0 -30 32.60 9.40 3 0 -30 20.60 10.00 -3 0 30 12.80 8.00 0 -1 -30 -6.20 6.40 0 -1 -30 4.70 7.10 0 1 30 -2.80 4.30 0 1 -30 3.00 7.20 0 -1 30 -4.80 9.10 0 1 30 9.70 6.10 0 -1 -30 -3.40 6.00 0 1 -30 10.50 7.90 0 1 -30 6.70 5.80 0 -1 30 -0.80 4.60 0 -1 30 0.90 6.80 0 -1 -30 2.70 9.00 0 -1 -30 -5.90 8.10 0 1 30 9.00 9.90 -1 -1 -30 14.80 12.20 -1 -1 -30 3.00 6.80 1 -1 30 -2.40 7.20 1 -1 30 -2.10 5.00 1 1 -30 2.20 8.70 -1 1 30 9.60 9.80 -1 -1 -30 5.60 8.00 1 -1 30 8.60 10.20 -1 1 30 2.30 5.10 1 1 -30 -0.70 6.60 -1 -1 -30 7.00 7.40 1 1 -30 8.00 6.60 -1 1 30 4.70 6.90 -1 -1 -30 19.70 7.90 1 1 30 18.60 8.90 -1 -1 30 1.50 7.00 1 1 30 17.70 6.10 1 -1 -30 11.30 7.00 1 1 30 -2.50 9.60 1 -1 -30 9.90 6.80 -1 -1 30 8.20 6.20 1 -1 -30 12.70 7.00 -1 1 -30 22.10 12.70 -1 1 -30 8.30 7.50 -1 -1 30 1.40 8.80 -1 1 -30 -3.30 3.90 -1 1 -30 -5.40 6.00 -2 1 30 10.30 6.50 2 -1 30 6.60 4.80 2 -1 30 -4.20 11.60 2 -1 30 3.60 9.10 -2 -1 -30 -7.90 10.90 -2 1 30 -4.80 8.30 -2 -1 -30 13.40 9.70 -2 -1 -30 -4.70 5.00 -2 -1 -30 -0.80 6.80 -2 -1 -30 -8.90 5.60 2 1 -30 -3.80 5.40 -2 1 30 5.20 6.00 2 1 -30 -6.30 7.80 2 1 -30 -1.10 8.20 -2 -1 30 7.60 10.30 -2 1 -30 -7.00 4.80 2 1 30 -6.70 3.60 -2 1 -30 -4.50 6.80 -2 1 -30 -5.70 13.40 -2 -1 30 1.30 4.50 2 -1 -30 -3.20 5.70 2 1 30 -2.20 6.70 -2 1 -30 -1.50 4.20 2 -1 -30 -0.20 6.80 2 -1 -30 -7.60 6.80 2 1 30 -2.30 10.50 -2 -1 30 -2.10 5.10 0 -2 -30 11.70 9.10 0 2 -30 12.80 5.70 0 2 30 6.10 10.00 0 -2 -30 -0.50 5.50 0 2 30 0.20 4.00 0 2 30 14.60 10.00 0 -2 -30 -13.80 7.10 0 -2 30 -9.70 10.00 0 -2 30 -10.20 5.90 0 -2 -30 -13.10 5.60 0 2 -30 -12.00 6.70 0 -2 -30 -7.60 4.70 0 2 -30 3.50 7.40 0 -2 30 2.90 5.20 -1 -2 -30 -8.50 7.90 -1 -2 -30 16.70 11.70 -1 2 30 3.20 8.40 1 -2 30 -23.80 8.70 1 2 -30 -0.10 7.80 1 2 -30 -8.20 5.20 -1 -2 -30 1.60 6.00 -1 -2 -30 2.70 7.20 -1 2 30 0.40 3.40 1 -2 30 3.00 6.10 -1 2 30 3.00 9.80 1 -2 30 -15.40 5.80 1 2 -30 9.90 6.80 -1 2 -30 7.80 11.80 -1 -2 30 -9.70 9.00 1 2 30 1.40 7.10 1 2 30 7.40 8.90 1 -2 -30 -2.10 5.70 -1 2 -30 9.10 6.60 1 2 30 3.70 4.20 -1 -2 30 4.30 5.20 1 -2 -30 2.20 6.40 -1 2 -30 2.70 7.00 -1 2 -30 24.00 8.90 -1 -2 30 3.60 6.40 1 -2 -30 2.00 6.00 -2 2 30 22.50 11.20 2 -2 30 20.90 9.30 -2 -2 -30 -4.70 12.30 2 -2 30 3.70 12.50 2 2 -30 17.00 10.70 -2 -2 -30 0.20 6.40 2 2 -30 14.00 8.10 -2 -2 -30 17.70 7.90 -2 2 30 8.20 5.90 2 2 -30 -2.70 6.20 -2 -2 -30 16.10 9.60 -2 2 30 6.70 6.80 -2 -2 -30 3.60 6.30 2 2 30 24.70 14.50 -2 2 -30 6.40 9.10 -2 2 -30 28.70 10.60 2 2 30 4.90 5.00 -2 -2 30 13.10 8.90 2 2 30 25.60 11.00 -2 -2 30 8.40 7.70 2 -2 -30 3.30 7.70 -2 2 -30 25.40 9.70 -2 2 -30 10.70 9.10 2 -2 -30 9.00 8.80 -2 -2 30 20.00 9.20 2 -2 -30 17.40 7.30 0 3 -30 28.40 11.20 0 3 30 40.80 13.60 0 -3 -30 21.30 9.30 0 -3 -30 32.70 10.60 0 3 30 41.30 15.10 0 -3 -30 40.20 17.20 0 3 -30 15.00 6.70 0 3 -30 14.10 9.10 0 3 30 35.30 8.00 0 -3 -30 27.80 9.50 0 -3 -30 38.60 10.50 0 -3 30 5.60 7.70 0 -3 30 16.40 5.30 0 -3 30 9.60 9.00 1 -3 30 -8.90 8.30 -1 -3 -30 14.90 7.50 1 3 -30 21.60 9.20 -1 3 30 4.70 11.00 -1 -3 -30 -14.30 11.20 -1 -3 -30 3.20 7.90 -1 -3 -30 -6.50 7.10 1 3 -30 7.10 8.50 1 -3 30 4.60 7.70 -1 3 30 0.20 4.80 1 3 -30 7.40 7.00 -1 -3 -30 6.90 6.90 -1 3 30 8.50 6.60 -1 -3 30 9.70 5.90 -1 3 -30 11.00 8.40 1 -3 -30 -5.50 5.70 -1 3 -30 12.60 8.80 -1 -3 30 5.20 11.10 1 3 30 0.90 11.70 1 3 30 7.40 5.80 1 3 30 14.50 9.00 1 -3 -30 6.80 9.10 1 -3 -30 1.70 7.40 -1 3 -30 -7.30 10.00 -1 3 -30 2.70 5.20 -1 -3 30 13.10 6.60 2 3 -30 -8.60 6.70 -2 -3 -30 18.10 6.90 2 3 -30 15.10 9.20 -2 -3 -30 6.30 7.30 -2 -3 -30 11.50 7.30 2 -3 30 -0.30 13.40 2 3 -30 6.10 7.20 2 -3 30 12.70 8.80 -2 -3 -30 -1.00 11.80 -2 3 30 19.20 9.70 -2 -3 -30 29.00 9.50 -2 3 30 19.00 7.50 -2 3 30 -5.30 11.40 -2 3 -30 22.50 9.50 2 -3 -30 -3.40 7.20 -2 -3 30 19.60 8.00 -2 -3 30 5.10 10.30 -2 -3 30 3.00 5.50 -2 3 -30 6.70 5.50 -2 3 -30 10.70 13.20 2 -3 -30 14.40 9.70 2 -3 -30 9.60 7.90 2 3 30 11.60 5.60 -2 3 -30 13.00 9.50 2 3 30 0.10 11.40 2 3 30 -1.50 9.60 0 -4 -30 -3.90 7.40 0 -4 30 -6.80 6.90 0 -4 -30 5.30 7.50 0 4 30 13.90 12.60 0 4 30 7.20 6.20 0 4 -30 8.00 6.10 0 -4 30 4.60 9.40 0 4 -30 3.20 8.80 0 4 30 1.40 8.40 0 -4 -30 -6.50 8.60 0 4 -30 -0.80 6.80 0 -4 -30 3.60 7.60 1 4 -30 3.50 7.40 -1 -4 -30 6.20 10.00 1 4 -30 9.50 5.90 -1 4 30 0.40 11.90 -1 -4 -30 3.60 6.60 -1 -4 -30 -3.90 8.20 1 4 -30 5.50 8.40 1 -4 30 -16.70 10.10 -1 -4 -30 8.80 12.40 1 -4 30 18.80 8.90 -1 -4 -30 16.70 8.80 -1 4 30 9.10 8.50 -1 4 30 6.50 5.10 1 -4 -30 -2.60 6.70 -1 -4 30 5.00 7.10 1 4 30 14.80 14.60 1 -4 -30 24.80 11.70 1 -4 -30 3.40 8.20 -1 4 -30 5.50 6.70 -1 4 -30 11.30 6.20 1 4 30 4.00 5.00 -1 -4 30 -1.60 8.60 1 4 30 0.70 7.90 -1 -4 30 9.20 6.70 -1 4 -30 1.70 9.40 0 0 31 7.70 10.10 0 0 -31 -3.40 4.60 0 0 -31 3.80 6.90 0 0 -31 1.30 6.30 0 0 31 -1.20 3.50 0 0 31 1.80 6.20 -1 0 31 -2.80 6.20 -1 0 -31 8.20 12.40 1 0 -31 13.70 7.80 1 0 31 0.50 4.40 1 0 -31 -3.70 7.70 -1 0 -31 3.00 9.10 1 0 -31 8.20 7.10 -1 0 -31 13.70 7.90 1 0 31 13.70 10.20 -1 0 -31 18.40 7.40 -1 0 31 -13.60 9.50 -1 0 -31 2.30 6.50 -1 0 31 20.20 7.40 1 0 31 12.80 11.40 -2 0 -31 21.50 14.80 2 0 -31 28.80 10.50 -2 0 -31 43.60 11.70 2 0 -31 11.80 8.30 2 0 31 31.00 9.50 -2 0 -31 3.20 6.50 -2 0 -31 19.40 8.10 -2 0 31 9.80 6.40 2 0 -31 17.40 10.60 2 0 31 11.80 5.50 2 0 31 2.50 12.30 -2 0 31 24.40 8.10 -2 0 -31 26.60 11.40 0 -1 -31 50.99 11.10 0 1 -31 19.90 7.50 0 -1 31 34.50 7.50 0 -1 -31 25.90 11.60 0 -1 -31 38.90 10.50 0 1 31 51.89 15.40 0 1 31 15.00 8.60 0 -1 31 44.70 11.50 0 1 -31 14.90 7.70 0 1 -31 24.00 11.00 0 1 31 25.00 6.60 0 -1 31 58.19 14.20 0 -1 -31 42.60 11.70 -1 -1 -31 7.40 8.10 1 -1 31 14.00 5.80 1 1 -31 -1.50 7.20 1 1 -31 9.40 7.30 -1 -1 -31 6.50 9.90 -1 -1 -31 -1.30 5.20 -1 1 31 -3.70 4.40 -1 1 31 1.80 9.80 1 -1 31 1.60 11.00 1 -1 31 19.50 10.20 1 1 -31 -2.20 5.80 -1 1 31 -2.40 7.20 -1 -1 -31 11.10 7.70 -1 -1 -31 -4.40 8.30 1 -1 -31 0.00 6.10 -1 1 -31 -7.70 12.40 -1 1 -31 6.10 7.80 1 1 31 7.10 5.20 1 1 31 7.80 13.10 1 1 31 10.40 9.70 -1 -1 31 -1.30 6.30 -1 1 -31 1.20 5.10 -1 1 -31 4.40 7.60 1 -1 -31 -4.10 6.00 1 -1 -31 8.70 8.00 -1 -1 31 -12.70 10.50 -1 -1 31 8.50 5.40 -2 -1 -31 3.50 12.20 2 1 -31 8.50 8.50 2 1 -31 9.90 8.40 -2 1 31 -7.80 9.50 -2 -1 -31 -8.10 6.60 2 -1 31 -4.60 13.70 -2 -1 -31 -0.60 6.40 -2 1 31 -4.10 4.80 -2 1 31 4.10 6.80 -2 -1 -31 3.70 5.30 -2 -1 -31 -21.10 8.20 2 -1 31 -2.20 9.20 2 1 -31 -4.30 6.80 2 -1 31 2.10 4.90 2 -1 -31 -4.90 6.80 -2 -1 31 4.60 5.60 2 1 31 1.50 4.30 -2 1 -31 -9.20 7.30 -2 1 -31 4.70 5.10 -2 1 -31 -5.10 13.00 2 1 31 -6.50 8.00 2 -1 -31 -1.10 4.70 -2 -1 31 -3.20 6.70 -2 -1 31 -4.00 10.20 -2 1 -31 -4.40 6.70 2 -1 -31 -3.40 7.10 2 1 31 0.60 12.20 0 -2 -31 4.90 7.20 0 2 31 9.80 6.70 0 2 -31 2.40 8.70 0 -2 31 7.60 7.40 0 2 -31 9.20 8.40 0 2 -31 31.80 10.90 0 -2 -31 10.50 7.90 0 -2 31 12.80 7.00 0 2 31 0.30 12.20 0 2 31 13.70 9.00 0 -2 -31 -17.10 7.90 0 -2 31 3.50 11.40 1 2 -31 37.20 11.20 1 -2 31 33.20 7.60 -1 -2 -31 27.30 9.30 -1 -2 -31 63.69 15.90 1 -2 31 19.60 12.60 -1 2 31 31.40 14.70 -1 -2 -31 21.60 10.30 1 2 -31 46.70 11.70 1 -2 31 9.00 9.00 1 2 -31 26.10 9.80 -1 2 31 24.30 9.80 -1 -2 -31 29.10 9.20 -1 2 31 25.00 8.30 -1 2 -31 11.70 8.50 1 2 31 54.69 15.40 1 2 31 50.99 11.20 -1 2 -31 53.79 13.20 1 -2 -31 28.40 10.70 1 2 31 58.89 14.90 -1 -2 31 33.00 10.80 -1 2 -31 50.69 11.20 -1 -2 31 7.30 11.10 1 -2 -31 37.70 10.60 -1 -2 31 58.69 11.70 0 3 -31 7.90 8.50 0 -3 31 -9.70 8.80 0 -3 31 -3.10 4.40 0 -3 -31 4.10 7.10 0 -3 -31 4.70 6.60 0 3 -31 2.10 8.00 0 -3 31 -3.90 6.70 0 -3 -31 -0.20 6.30 0 3 31 -7.10 7.00 0 3 31 4.20 5.70 0 3 -31 -4.40 5.40 0 -3 -31 2.50 9.90 0 3 31 -3.20 12.30 -1 -3 -31 -6.80 7.20 1 3 -31 26.60 10.80 1 -3 31 6.60 10.20 1 -3 31 7.70 7.30 -1 -3 -31 11.60 7.50 -1 -3 -31 9.20 11.10 -1 3 31 7.70 7.60 -1 3 31 0.00 3.90 1 3 -31 19.30 8.50 -1 3 31 7.00 13.60 -1 -3 -31 6.20 13.80 1 3 -31 -4.20 7.60 -1 -3 -31 0.80 7.00 1 3 31 11.50 5.60 1 3 31 4.20 9.60 -1 -3 31 15.60 8.10 -1 3 -31 10.50 7.80 -1 -3 31 24.10 9.40 -1 3 -31 25.00 9.70 1 -3 -31 16.30 9.10 1 -3 -31 11.10 9.70 1 -3 -31 16.50 9.10 -1 -3 31 6.70 10.30 1 3 31 22.00 14.00 -1 3 -31 8.90 6.40 0 0 32 41.10 15.10 0 0 -32 34.00 10.00 0 0 -32 10.00 9.10 0 0 32 29.70 8.40 0 0 32 14.40 8.50 -1 0 32 14.70 7.20 1 0 -32 15.90 10.40 -1 0 -32 29.90 9.60 1 0 32 12.60 7.10 -1 0 32 13.20 7.90 -1 0 -32 3.20 10.20 1 0 -32 2.60 7.60 -1 0 32 15.70 14.20 1 0 32 18.70 10.70 1 0 -32 17.70 9.70 1 0 32 28.20 15.10 -1 0 -32 21.90 9.20 -1 0 -32 23.30 9.60 0 -1 32 4.30 8.60 0 1 -32 15.00 9.70 0 1 32 2.70 5.30 0 -1 32 -18.40 11.20 0 -1 -32 1.70 7.20 0 -1 -32 12.90 8.20 0 -1 -32 7.80 8.60 0 -1 32 3.00 5.10 0 1 -32 -6.40 5.20 0 1 -32 -1.00 7.80 0 1 32 -6.90 7.20 0 1 32 -10.50 11.40 -1 1 32 -6.60 11.30 1 1 -32 19.20 10.80 -1 -1 -32 5.50 8.50 -1 -1 -32 -14.40 9.30 -1 -1 -32 -2.00 7.20 -1 -1 -32 23.30 20.90 -1 -1 -32 -4.50 7.90 1 1 -32 -5.40 8.40 1 -1 32 8.00 6.80 1 -1 32 5.60 12.40 1 -1 32 9.00 9.80 1 1 -32 7.00 6.50 -1 1 32 5.80 7.70 -1 1 32 5.00 5.60 1 1 32 8.30 5.90 -1 1 -32 -9.30 7.50 1 -1 -32 6.80 7.40 1 -1 -32 1.20 7.80 1 -1 -32 9.40 7.10 -1 -1 32 -3.00 6.90 -1 1 -32 1.40 5.60 -1 1 -32 15.00 9.20 -1 -1 32 5.40 13.10 -1 -1 32 11.90 6.50 1 1 32 14.70 14.90 1 1 32 -10.00 7.60 0 2 32 7.50 7.20 0 2 32 -2.20 12.50 0 2 -32 -3.30 7.20 0 2 -32 -8.40 7.60 0 2 -32 -2.40 6.10 0 -2 -32 6.00 6.60 0 -2 32 -9.80 13.80 0 -2 32 -15.70 7.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 45107 _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 0.6091(3) 0.8127(2) 0.24519(7) 0.0470(5) Uani 1 1 d . . . . . O2 O 0.2931(3) 0.7545(2) 0.35868(7) 0.0483(6) Uani 1 1 d . . . . . O3 O 0.5132(3) 0.7283(2) 0.06509(7) 0.0492(5) Uani 1 1 d . . . . . O4 O 0.1553(3) 0.6131(2) 0.08156(7) 0.0490(6) Uani 1 1 d . . . . . O5 O -0.1268(3) 0.5745(2) 0.25684(8) 0.0478(6) Uani 1 1 d D . . . . H5 H -0.191(5) 0.650(3) 0.2591(14) 0.074(13) Uiso 1 1 d D . . . . O6 O -0.0992(4) 0.5863(2) 0.50034(7) 0.0588(6) Uani 1 1 d . . . . . C1 C 0.4520(5) 0.7220(3) 0.11557(10) 0.0383(6) Uani 1 1 d . . . . . C2 C 0.5627(4) 0.7715(3) 0.15675(10) 0.0394(7) Uani 1 1 d . . . . . H2 H 0.692925 0.810513 0.151488 0.047 Uiso 1 1 calc R U . . . C3 C 0.4804(4) 0.7634(3) 0.20634(10) 0.0364(6) Uani 1 1 d . . . . . C4 C 0.2866(4) 0.7071(3) 0.21597(10) 0.0329(6) Uani 1 1 d . . . . . C5 C 0.1784(4) 0.6542(3) 0.17370(10) 0.0362(6) Uani 1 1 d . . . . . H5A H 0.049488 0.613499 0.179118 0.043 Uiso 1 1 calc R U . . . C6 C 0.2570(4) 0.6606(3) 0.12435(10) 0.0375(7) Uani 1 1 d . . . . . C7 C 0.5065(5) 0.8417(3) 0.29307(11) 0.0475(8) Uani 1 1 d . . . . . H7A H 0.422347 0.922127 0.289486 0.057 Uiso 1 1 calc R U . . . H7B H 0.609870 0.857586 0.319731 0.057 Uiso 1 1 calc R U . . . C8 C 0.3690(4) 0.7251(3) 0.30821(9) 0.0382(7) Uani 1 1 d . . . . . H8 H 0.452529 0.642748 0.309195 0.046 Uiso 1 1 calc R U . . . C9 C 0.1923(4) 0.7087(3) 0.26986(9) 0.0325(6) Uani 1 1 d . . . . . H9 H 0.101879 0.787708 0.272540 0.039 Uiso 1 1 calc R U . . . C10 C 0.1374(4) 0.6700(3) 0.37571(10) 0.0366(6) Uani 1 1 d . . . . . C11 C 0.1009(5) 0.6721(3) 0.42867(11) 0.0412(7) Uani 1 1 d . . . . . H11 H 0.179888 0.727140 0.450085 0.049 Uiso 1 1 calc R U . . . C12 C -0.0535(5) 0.5917(3) 0.44884(11) 0.0436(7) Uani 1 1 d . . . . . C13 C -0.1711(5) 0.5106(3) 0.41692(11) 0.0530(9) Uani 1 1 d . . . . . H13 H -0.275749 0.456517 0.430571 0.064 Uiso 1 1 calc R U . . . C14 C -0.1323(5) 0.5105(3) 0.36461(11) 0.0470(8) Uani 1 1 d . . . . . H14 H -0.213069 0.456144 0.343347 0.056 Uiso 1 1 calc R U . . . C15 C 0.0240(4) 0.5891(3) 0.34259(10) 0.0354(6) Uani 1 1 d . . . . . C16 C 0.0643(4) 0.5865(3) 0.28487(10) 0.0341(6) Uani 1 1 d . . . . . H16 H 0.148568 0.506744 0.277396 0.041 Uiso 1 1 calc R U . . . C17 C 0.6892(5) 0.8116(4) 0.05265(12) 0.0601(9) Uani 1 1 d . . . . . H17A H 0.711944 0.810336 0.016069 0.090 Uiso 1 1 calc R U . . . H17B H 0.811311 0.778232 0.069913 0.090 Uiso 1 1 calc R U . . . H17C H 0.662105 0.901882 0.063646 0.090 Uiso 1 1 calc R U . . . C18 C -0.0148(5) 0.5230(4) 0.09054(12) 0.0571(9) Uani 1 1 d . . . . . H18A H -0.070705 0.493492 0.058115 0.086 Uiso 1 1 calc R U . . . H18B H -0.121897 0.568172 0.109781 0.086 Uiso 1 1 calc R U . . . H18C H 0.033951 0.446845 0.109733 0.086 Uiso 1 1 calc R U . . . C19 C 0.0555(6) 0.6338(4) 0.53465(12) 0.0674(11) Uani 1 1 d . . . . . H19A H 0.188560 0.596526 0.525336 0.101 Uiso 1 1 calc R U . . . H19B H 0.020797 0.607208 0.569180 0.101 Uiso 1 1 calc R U . . . H19C H 0.062221 0.729865 0.532763 0.101 Uiso 1 1 calc R U . . . 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 0.0367(11) 0.0677(14) 0.0365(11) -0.0015(9) -0.0003(9) -0.0183(10) O2 0.0502(12) 0.0617(14) 0.0330(10) -0.0055(9) 0.0047(9) -0.0218(11) O3 0.0506(13) 0.0612(13) 0.0358(11) -0.0007(10) 0.0114(10) -0.0050(11) O4 0.0512(13) 0.0611(14) 0.0347(11) -0.0076(9) -0.0032(9) -0.0119(11) O5 0.0377(12) 0.0617(15) 0.0439(12) -0.0010(11) -0.0044(10) -0.0158(11) O6 0.0661(15) 0.0738(15) 0.0367(12) 0.0006(11) 0.0113(11) -0.0117(13) C1 0.0389(15) 0.0417(16) 0.0343(14) 0.0028(12) 0.0049(13) 0.0048(13) C2 0.0314(14) 0.0463(16) 0.0406(15) 0.0025(13) 0.0045(13) -0.0034(13) C3 0.0329(15) 0.0400(15) 0.0362(14) 0.0013(12) -0.0039(12) -0.0034(13) C4 0.0319(14) 0.0353(15) 0.0314(14) 0.0021(11) -0.0004(11) -0.0004(12) C5 0.0326(15) 0.0392(15) 0.0368(15) 0.0017(12) 0.0007(12) -0.0011(12) C6 0.0385(16) 0.0387(16) 0.0352(15) -0.0019(12) -0.0021(12) 0.0007(13) C7 0.0442(18) 0.0616(19) 0.0368(15) -0.0052(14) 0.0010(14) -0.0201(16) C8 0.0372(15) 0.0471(17) 0.0303(14) -0.0006(12) 0.0006(12) -0.0064(13) C9 0.0309(13) 0.0348(15) 0.0318(14) 0.0002(11) -0.0009(11) 0.0017(12) C10 0.0356(15) 0.0384(15) 0.0359(14) 0.0028(12) 0.0018(12) -0.0033(13) C11 0.0434(17) 0.0439(17) 0.0363(14) -0.0025(12) -0.0012(13) -0.0021(14) C12 0.0489(17) 0.0459(17) 0.0360(15) 0.0010(13) 0.0074(13) 0.0017(15) C13 0.061(2) 0.0518(19) 0.0459(18) 0.0001(15) 0.0132(17) -0.0192(17) C14 0.0503(19) 0.0491(18) 0.0415(17) -0.0030(14) 0.0048(15) -0.0135(15) C15 0.0353(15) 0.0333(14) 0.0376(15) 0.0014(12) 0.0033(12) -0.0029(12) C16 0.0291(14) 0.0372(15) 0.0361(14) -0.0006(12) -0.0008(11) -0.0021(12) C17 0.055(2) 0.076(2) 0.0497(19) 0.0093(17) 0.0148(16) -0.0064(19) C18 0.056(2) 0.065(2) 0.0505(19) -0.0118(16) -0.0051(16) -0.0183(18) C19 0.065(2) 0.100(3) 0.0370(18) 0.0020(18) 0.0030(17) 0.011(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0106 0.0060 '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 C3 O1 C7 115.3(2) . . C10 O2 C8 114.5(2) . . C1 O3 C17 117.8(2) . . C6 O4 C18 116.5(2) . . C16 O5 H5 108(3) . . C12 O6 C19 116.9(3) . . O3 C1 C2 125.4(3) . . O3 C1 C6 115.4(2) . . C2 C1 C6 119.2(2) . . C1 C2 H2 119.9 . . C1 C2 C3 120.2(3) . . C3 C2 H2 119.9 . . O1 C3 C2 115.1(2) . . C4 C3 O1 122.9(2) . . C4 C3 C2 121.9(2) . . C3 C4 C5 117.1(2) . . C3 C4 C9 121.1(2) . . C5 C4 C9 121.8(2) . . C4 C5 H5A 119.0 . . C6 C5 C4 122.0(3) . . C6 C5 H5A 119.0 . . O4 C6 C1 116.1(2) . . O4 C6 C5 124.3(2) . . C5 C6 C1 119.6(3) . . O1 C7 H7A 109.7 . . O1 C7 H7B 109.7 . . O1 C7 C8 109.7(2) . . H7A C7 H7B 108.2 . . C8 C7 H7A 109.7 . . C8 C7 H7B 109.7 . . O2 C8 C7 106.2(2) . . O2 C8 H8 109.5 . . O2 C8 C9 111.8(2) . . C7 C8 H8 109.5 . . C7 C8 C9 110.3(2) . . C9 C8 H8 109.5 . . C4 C9 H9 107.9 . . C8 C9 C4 108.0(2) . . C8 C9 H9 107.9 . . C8 C9 C16 108.7(2) . . C16 C9 C4 116.2(2) . . C16 C9 H9 107.9 . . O2 C10 C11 115.3(2) . . O2 C10 C15 122.5(2) . . C15 C10 C11 122.2(3) . . C10 C11 H11 120.5 . . C12 C11 C10 119.1(3) . . C12 C11 H11 120.5 . . O6 C12 C11 123.2(3) . . O6 C12 C13 116.5(3) . . C11 C12 C13 120.3(3) . . C12 C13 H13 120.2 . . C14 C13 C12 119.5(3) . . C14 C13 H13 120.2 . . C13 C14 H14 118.9 . . C13 C14 C15 122.1(3) . . C15 C14 H14 118.9 . . C10 C15 C14 116.7(2) . . C10 C15 C16 122.2(2) . . C14 C15 C16 121.1(2) . . O5 C16 C9 113.5(2) . . O5 C16 C15 111.0(2) . . O5 C16 H16 107.6 . . C9 C16 C15 109.3(2) . . C9 C16 H16 107.6 . . C15 C16 H16 107.6 . . O3 C17 H17A 109.5 . . O3 C17 H17B 109.5 . . O3 C17 H17C 109.5 . . H17A C17 H17B 109.5 . . H17A C17 H17C 109.5 . . H17B C17 H17C 109.5 . . O4 C18 H18A 109.5 . . O4 C18 H18B 109.5 . . O4 C18 H18C 109.5 . . H18A C18 H18B 109.5 . . H18A C18 H18C 109.5 . . H18B C18 H18C 109.5 . . O6 C19 H19A 109.5 . . O6 C19 H19B 109.5 . . O6 C19 H19C 109.5 . . H19A C19 H19B 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O1 C3 1.391(3) . O1 C7 1.434(3) . O2 C8 1.427(3) . O2 C10 1.378(3) . O3 C1 1.368(3) . O3 C17 1.436(4) . O4 C6 1.371(3) . O4 C18 1.430(4) . O5 H5 0.86(2) . O5 C16 1.428(3) . O6 C12 1.368(3) . O6 C19 1.413(4) . C1 C2 1.373(4) . C1 C6 1.408(4) . C2 H2 0.9300 . C2 C3 1.392(4) . C3 C4 1.384(4) . C4 C5 1.400(4) . C4 C9 1.523(3) . C5 H5A 0.9300 . C5 C6 1.377(4) . C7 H7A 0.9700 . C7 H7B 0.9700 . C7 C8 1.510(4) . C8 H8 0.9800 . C8 C9 1.515(4) . C9 H9 0.9800 . C9 C16 1.519(4) . C10 C11 1.394(4) . C10 C15 1.383(4) . C11 H11 0.9300 . C11 C12 1.376(4) . C12 C13 1.380(4) . C13 H13 0.9300 . C13 C14 1.379(4) . C14 H14 0.9300 . C14 C15 1.393(4) . C15 C16 1.519(4) . C16 H16 0.9800 . C17 H17A 0.9600 . C17 H17B 0.9600 . C17 H17C 0.9600 . C18 H18A 0.9600 . C18 H18B 0.9600 . C18 H18C 0.9600 . C19 H19A 0.9600 . C19 H19B 0.9600 . C19 H19C 0.9600 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C5 H5A O5 0.93 2.34 3.016(3) 129.0 . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O1 C3 C4 C5 -176.4(2) . . . . O1 C3 C4 C9 6.2(4) . . . . O1 C7 C8 O2 173.2(2) . . . . O1 C7 C8 C9 -65.5(3) . . . . O2 C8 C9 C4 168.3(2) . . . . O2 C8 C9 C16 -64.9(3) . . . . O2 C10 C11 C12 179.3(3) . . . . O2 C10 C15 C14 -178.6(3) . . . . O2 C10 C15 C16 0.6(4) . . . . O3 C1 C2 C3 177.6(3) . . . . O3 C1 C6 O4 1.1(4) . . . . O3 C1 C6 C5 -177.5(3) . . . . O6 C12 C13 C14 -179.6(3) . . . . C1 C2 C3 O1 178.0(3) . . . . C1 C2 C3 C4 -0.5(4) . . . . C2 C1 C6 O4 -179.8(3) . . . . C2 C1 C6 C5 1.6(4) . . . . C2 C3 C4 C5 2.1(4) . . . . C2 C3 C4 C9 -175.3(3) . . . . C3 O1 C7 C8 47.7(3) . . . . C3 C4 C5 C6 -1.8(4) . . . . C3 C4 C9 C8 -22.3(3) . . . . C3 C4 C9 C16 -144.7(3) . . . . C4 C5 C6 O4 -178.5(3) . . . . C4 C5 C6 C1 0.0(4) . . . . C4 C9 C16 O5 -68.2(3) . . . . C4 C9 C16 C15 167.3(2) . . . . C5 C4 C9 C8 160.4(2) . . . . C5 C4 C9 C16 38.1(3) . . . . C6 C1 C2 C3 -1.3(4) . . . . C7 O1 C3 C2 162.3(3) . . . . C7 O1 C3 C4 -19.1(4) . . . . C7 C8 C9 C4 50.4(3) . . . . C7 C8 C9 C16 177.2(2) . . . . C8 O2 C10 C11 163.2(2) . . . . C8 O2 C10 C15 -17.2(4) . . . . C8 C9 C16 O5 169.8(2) . . . . C8 C9 C16 C15 45.3(3) . . . . C9 C4 C5 C6 175.6(3) . . . . C10 O2 C8 C7 169.8(2) . . . . C10 O2 C8 C9 49.5(3) . . . . C10 C11 C12 O6 179.4(3) . . . . C10 C11 C12 C13 -0.3(4) . . . . C10 C15 C16 O5 -142.1(3) . . . . C10 C15 C16 C9 -16.2(4) . . . . C11 C10 C15 C14 0.9(4) . . . . C11 C10 C15 C16 -179.8(3) . . . . C11 C12 C13 C14 0.2(5) . . . . C12 C13 C14 C15 0.5(5) . . . . C13 C14 C15 C10 -1.1(4) . . . . C13 C14 C15 C16 179.7(3) . . . . C14 C15 C16 O5 37.1(4) . . . . C14 C15 C16 C9 163.0(3) . . . . C15 C10 C11 C12 -0.3(4) . . . . C17 O3 C1 C2 -10.7(4) . . . . C17 O3 C1 C6 168.3(3) . . . . C18 O4 C6 C1 165.2(3) . . . . C18 O4 C6 C5 -16.3(4) . . . . C19 O6 C12 C11 -18.8(4) . . . . C19 O6 C12 C13 160.9(3) . . . .