#------------------------------------------------------------------------------ #$Date: 2024-11-22 01:06:07 +0200 (Fri, 22 Nov 2024) $ #$Revision: 296050 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573251.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_1573251 loop_ _publ_author_name 'Navaneetha, N.' 'Maurya, Sundaram' 'Behera, Prativa' 'Jadhav, Sandip B.' 'Magham, Lakshmi Revati' 'Nanubolu, Jagadeesh Babu' 'Roy, Lisa' 'Chegondi, Rambabu' _publ_section_title ; BINAP-CuH-catalysed enantioselective allylation using alkoxyallenes to access 1,2-syn-tert,sec-diols ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC07002J _journal_year 2024 _chemical_absolute_configuration syn _chemical_formula_moiety 'C25 H26 O3' _chemical_formula_sum 'C25 H26 O3' _chemical_formula_weight 374.46 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2019/3 _audit_update_record ; 2024-04-21 deposited with the CCDC. 2024-11-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 117.903(5) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.0727(18) _cell_length_b 17.381(3) _cell_length_c 8.2903(16) _cell_measurement_reflns_used 9920 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.516 _cell_measurement_theta_min 2.345 _cell_volume 1028.0(4) _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction 'Bruker SAINT' _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON III C7 HPAD' _diffrn_measurement_method '\w and \f' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_unetI/netI 0.0457 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 14285 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.496 _diffrn_reflns_theta_min 2.907 _diffrn_source microfocus _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6369 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_density_diffrn 1.210 _exptl_crystal_description BLOCK _exptl_crystal_F_000 400 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DCM/hexane (1:9)' _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.220 _refine_diff_density_max 0.214 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.037 _refine_ls_abs_structure_details ; Flack x determined using 1921 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.0(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 259 _refine_ls_number_reflns 4670 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0351 _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^)+(0.0399P)^2^+0.1090P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.0845 _reflns_Friedel_coverage 0.932 _reflns_Friedel_fraction_full 0.987 _reflns_Friedel_fraction_max 0.989 _reflns_number_gt 4304 _reflns_number_total 4670 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc07002j2.cif _cod_data_source_block KB741_0m _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 1573251 _shelx_shelxl_version_number 2019/3 _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_min 0.978 _shelx_estimated_absorpt_t_max 0.983 _shelx_res_file ; TITL KB741_0m_a.res in P2(1) KB741_0m.res created by SHELXL-2019/3 at 14:55:11 on 20-Apr-2024 CELL 0.71073 8.0727 17.3814 8.2903 90.000 117.903 90.000 ZERR 2.00 0.0018 0.0032 0.0016 0.000 0.005 0.000 LATT -1 SYMM -x, y+1/2, -z SFAC C H O UNIT 50 52 6 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.150 ACTA L.S. 40 FMAP 2 PLAN 5 OMIT -3 55 OMIT 0 -2 0 OMIT -2 -2 1 OMIT 0 0 3 OMIT -3 -9 3 OMIT 3 9 0 HTAB BOND $H CONF SIZE 0.29 0.25 0.22 WGHT 0.039900 0.109000 FVAR 1.76771 O1 3 0.622324 0.516206 0.611378 11.00000 0.01689 0.01849 = 0.01430 0.00073 0.00701 -0.00223 O2 3 0.518184 0.401765 0.758506 11.00000 0.03223 0.02647 = 0.01417 0.00103 0.01218 -0.00309 H2O 2 0.609332 0.436053 0.793933 11.00000 0.03691 O3 3 0.322784 0.385167 0.184549 11.00000 0.02478 0.02990 = 0.01387 -0.00185 0.00781 -0.00120 C1 1 0.660194 0.588408 0.551638 11.00000 0.01721 0.01616 = 0.01534 0.00046 0.00847 -0.00052 AFIX 13 H1 2 0.554264 0.624471 0.526243 11.00000 -1.20000 AFIX 0 C2 1 0.837189 0.620302 0.708038 11.00000 0.01845 0.01958 = 0.01116 0.00105 0.00845 -0.00186 C3 1 0.836931 0.693291 0.777231 11.00000 0.02039 0.01997 = 0.01827 0.00037 0.01020 0.00031 AFIX 43 H3 2 0.725922 0.723464 0.724748 11.00000 -1.20000 AFIX 0 C4 1 0.998169 0.722240 0.922639 11.00000 0.02762 0.02171 = 0.02083 -0.00584 0.01050 -0.00271 AFIX 43 H4 2 0.997472 0.772383 0.967911 11.00000 -1.20000 AFIX 0 C5 1 1.159206 0.678377 1.001417 11.00000 0.02182 0.03129 = 0.01636 -0.00519 0.00594 -0.00544 AFIX 43 H5 2 1.268337 0.697975 1.102368 11.00000 -1.20000 AFIX 0 C6 1 1.162160 0.605643 0.933494 11.00000 0.01868 0.03035 = 0.01939 -0.00053 0.00620 0.00310 AFIX 43 H6 2 1.273267 0.575550 0.987094 11.00000 -1.20000 AFIX 0 C7 1 1.001198 0.577094 0.786295 11.00000 0.02219 0.02089 = 0.01643 -0.00318 0.00875 0.00001 AFIX 43 H7 2 1.003468 0.527580 0.738845 11.00000 -1.20000 AFIX 0 C8 1 0.679725 0.579396 0.379133 11.00000 0.01534 0.02304 = 0.01192 -0.00072 0.00480 -0.00470 C9 1 0.651928 0.643481 0.266362 11.00000 0.02026 0.02412 = 0.01602 0.00215 0.00587 -0.00139 AFIX 43 H9 2 0.617927 0.691617 0.296585 11.00000 -1.20000 AFIX 0 C10 1 0.674092 0.636630 0.110324 11.00000 0.02552 0.03429 = 0.01619 0.00658 0.00707 -0.00559 AFIX 43 H10 2 0.655705 0.680232 0.034683 11.00000 -1.20000 AFIX 0 C11 1 0.722687 0.566786 0.064749 11.00000 0.02965 0.04012 = 0.01319 -0.00304 0.01036 -0.01115 AFIX 43 H11 2 0.736224 0.562297 -0.042691 11.00000 -1.20000 AFIX 0 C12 1 0.751717 0.503162 0.176154 11.00000 0.02879 0.02847 = 0.02080 -0.00601 0.01476 -0.00720 AFIX 43 H12 2 0.785261 0.455157 0.144878 11.00000 -1.20000 AFIX 0 C13 1 0.731771 0.509568 0.333587 11.00000 0.02288 0.02293 = 0.01606 -0.00101 0.00995 -0.00505 AFIX 43 H13 2 0.753778 0.466075 0.410380 11.00000 -1.20000 AFIX 0 C14 1 0.428408 0.491673 0.509903 11.00000 0.01574 0.02103 = 0.01244 -0.00077 0.00638 -0.00301 AFIX 13 H14 2 0.386116 0.496022 0.375992 11.00000 -1.20000 AFIX 0 C15 1 0.306823 0.540734 0.559838 11.00000 0.02006 0.02239 = 0.02307 -0.00460 0.01270 -0.00401 AFIX 43 H15 2 0.329220 0.540428 0.683001 11.00000 -1.20000 AFIX 0 C16 1 0.170362 0.584310 0.441733 11.00000 0.02256 0.02529 = 0.03691 0.00004 0.01640 -0.00031 AFIX 93 H16A 2 0.145039 0.585662 0.317729 11.00000 -1.20000 H16B 2 0.097303 0.614374 0.480591 11.00000 -1.20000 AFIX 0 C17 1 0.431348 0.405833 0.562368 11.00000 0.02466 0.02032 = 0.01344 -0.00011 0.01103 -0.00196 C18 1 0.233962 0.374310 0.496448 11.00000 0.02577 0.02289 = 0.02666 -0.00265 0.01542 -0.00601 AFIX 137 H18A 2 0.163202 0.379197 0.363402 11.00000 -1.50000 H18B 2 0.170761 0.403489 0.552930 11.00000 -1.50000 H18C 2 0.241004 0.319974 0.530626 11.00000 -1.50000 AFIX 0 C19 1 0.544660 0.358697 0.490945 11.00000 0.02286 0.01512 = 0.01860 -0.00100 0.01173 -0.00374 C20 1 0.712242 0.323990 0.613188 11.00000 0.02864 0.01950 = 0.02027 -0.00003 0.01007 -0.00009 AFIX 43 H20 2 0.751489 0.327954 0.740258 11.00000 -1.20000 AFIX 0 C21 1 0.824185 0.283754 0.556028 11.00000 0.02873 0.02427 = 0.03157 0.00017 0.01075 0.00359 AFIX 43 H21 2 0.937652 0.260506 0.642678 11.00000 -1.20000 AFIX 0 C22 1 0.768040 0.278023 0.371037 11.00000 0.03365 0.02375 = 0.03551 -0.00757 0.02179 -0.00170 AFIX 43 H22 2 0.844241 0.251148 0.330551 11.00000 -1.20000 AFIX 0 C23 1 0.601862 0.311128 0.244763 11.00000 0.03169 0.02255 = 0.02270 -0.00583 0.01607 -0.00657 AFIX 43 H23 2 0.564282 0.306726 0.118092 11.00000 -1.20000 AFIX 0 C24 1 0.489213 0.350961 0.302682 11.00000 0.02331 0.01771 = 0.01873 -0.00192 0.01061 -0.00439 C25 1 0.271103 0.384301 -0.006108 11.00000 0.03944 0.03422 = 0.01611 -0.00078 0.01239 -0.00258 AFIX 137 H25A 2 0.260534 0.330950 -0.048065 11.00000 -1.50000 H25B 2 0.367105 0.410996 -0.025733 11.00000 -1.50000 H25C 2 0.150341 0.410365 -0.074851 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM KB741_0m_a.res in P2(1) REM wR2 = 0.0845, GooF = S = 1.053, Restrained GooF = 1.052 for all data REM R1 = 0.0351 for 4304 Fo > 4sig(Fo) and 0.0395 for all 4670 data REM 259 parameters refined using 1 restraints END WGHT 0.0399 0.1095 REM Instructions for potential hydrogen bonds HTAB O2 O1 HTAB C14 O3 HTAB C18 O3 EQIV $1 x, y, z-1 HTAB C25 O2_$1 REM Highest difference peak 0.214, deepest hole -0.195, 1-sigma level 0.037 Q1 1 0.5183 0.3058 0.2771 11.00000 0.05 0.21 Q2 1 0.5837 0.3583 0.2754 11.00000 0.05 0.21 Q3 1 0.3283 0.5021 0.5204 11.00000 0.05 0.21 Q4 1 0.4161 0.4506 0.5389 11.00000 0.05 0.20 Q5 1 0.4633 0.3718 0.5273 11.00000 0.05 0.20 ; _shelx_res_checksum 40093 _shelx_hkl_file ; 3 0 0 420.86 21.85 3 0 0 380.99 22.58 3 0 0 387.96 21.63 -3 0 0 382.82 22.01 -3 0 0 398.48 22.70 4 0 0 387.57 20.71 4 0 0 349.27 21.76 4 0 0 346.15 20.40 -4 0 0 342.01 21.00 -4 0 0 379.64 22.08 5 0 0 8.96 4.13 -5 0 0 2.61 4.13 -5 0 0 11.17 4.78 5 0 0 4.34 3.01 6 0 0 1763.76 91.42 -6 0 0 1669.85 92.83 7 0 0 493.40 30.85 -7 0 0 541.93 33.03 -8 0 0 15.05 8.17 8 0 0 83.86 18.40 9 0 0 123.77 26.03 10 0 0 114.68 24.58 0 -1 0 -0.09 0.13 0 -1 0 -0.23 0.16 0 -1 0 -0.10 0.20 0 1 0 -0.10 0.16 0 1 0 -0.25 0.09 0 1 0 -0.15 0.10 0 1 0 -0.45 0.22 -1 -1 0 2450.43 126.00 1 1 0 2430.09 126.00 -2 -1 0 5765.34 324.61 2 -1 0 5746.83 328.74 2 1 0 5772.66 326.48 3 -1 0 258.92 15.86 3 -1 0 257.34 14.79 -3 -1 0 244.68 15.97 3 -1 0 288.14 15.44 -3 -1 0 284.63 15.45 3 1 0 265.52 16.04 3 1 0 229.10 15.01 -3 1 0 262.78 15.64 -3 1 0 274.64 16.12 3 1 0 285.12 15.12 3 1 0 243.66 13.92 4 -1 0 1923.99 102.96 -4 -1 0 2050.13 104.59 4 -1 0 1886.69 104.20 -4 -1 0 1955.71 103.46 4 -1 0 2051.82 103.26 4 1 0 2062.65 103.04 4 1 0 1955.62 103.32 -4 1 0 1941.98 103.65 4 1 0 1966.48 101.77 4 1 0 1978.06 104.57 -4 1 0 1959.47 104.42 -5 -1 0 177.50 13.88 -5 -1 0 192.74 14.44 5 -1 0 191.53 12.29 5 -1 0 211.76 13.52 -5 1 0 199.42 14.48 5 1 0 208.72 13.27 -5 1 0 186.89 14.20 5 1 0 191.04 12.68 6 -1 0 58.37 9.75 6 1 0 60.73 9.26 6 1 0 40.87 6.08 -6 1 0 49.09 8.78 7 -1 0 67.59 10.98 -7 -1 0 70.31 10.85 -7 1 0 88.37 12.67 7 1 0 72.83 16.04 7 1 0 73.58 10.87 -8 -1 0 159.90 15.86 8 -1 0 146.69 15.60 8 1 0 154.70 23.44 8 1 0 127.64 15.21 -8 1 0 140.05 16.16 9 -1 0 231.08 31.34 9 -1 0 154.09 18.69 -9 1 0 180.63 19.36 9 1 0 197.36 29.02 9 1 0 147.85 18.62 10 -1 0 210.53 31.16 10 -1 0 136.97 20.15 10 1 0 167.77 29.34 0 -2 0 -0.44 0.39 2 2 0 2566.31 134.84 3 -2 0 3122.23 153.92 -3 -2 0 3145.51 154.14 3 -2 0 2914.48 154.84 -3 -2 0 2578.75 154.81 3 2 0 2777.18 157.17 -3 2 0 3212.58 155.13 3 2 0 3147.61 155.31 3 2 0 2970.01 153.32 -3 2 0 2906.26 153.95 4 -2 0 2845.95 145.49 -4 -2 0 2847.43 147.09 4 -2 0 2735.97 146.79 -4 -2 0 2752.28 145.86 4 2 0 2974.55 145.56 4 2 0 2782.99 147.10 -4 2 0 2739.51 146.32 -4 2 0 2836.63 147.00 4 2 0 2746.83 144.66 4 2 0 2790.20 146.02 5 -2 0 321.57 18.65 5 -2 0 340.84 19.79 -5 -2 0 303.89 19.87 -5 -2 0 322.89 20.79 5 2 0 299.45 19.25 5 2 0 321.71 17.23 5 2 0 358.24 19.48 5 2 0 294.32 25.44 -5 2 0 333.26 21.21 -6 -2 0 1631.64 87.72 6 -2 0 1677.03 86.37 -6 2 0 1619.17 87.63 6 2 0 1490.07 92.52 6 2 0 1536.37 85.88 6 2 0 1722.82 86.00 -7 -2 0 149.97 14.69 7 -2 0 105.53 12.80 -7 2 0 100.91 13.75 7 2 0 97.21 12.21 8 -2 0 25.21 8.44 -8 2 0 31.21 9.22 8 2 0 58.54 16.65 8 2 0 28.57 9.10 9 -2 0 18.05 10.00 -9 2 0 17.14 8.94 9 2 0 78.74 20.99 10 -2 0 134.04 27.62 10 -2 0 67.15 13.43 10 2 0 95.68 23.88 0 -3 0 0.18 2.13 0 3 0 2.16 1.94 0 3 0 0.21 1.05 0 3 0 2.21 1.29 -2 -3 0 5005.23 255.76 2 3 0 4866.79 256.65 -3 -3 0 2211.57 115.44 3 -3 0 2192.43 115.20 -3 -3 0 2112.85 115.31 3 -3 0 2249.70 114.71 -3 -3 0 2236.88 114.33 3 -3 0 2252.97 114.13 -3 3 0 2275.45 113.59 3 3 0 1970.99 117.47 -3 3 0 2215.91 115.41 -3 3 0 1983.28 115.37 3 3 0 2346.63 114.13 -3 3 0 2173.83 114.98 3 3 0 2403.67 115.84 4 -3 0 819.25 41.69 -4 -3 0 777.15 42.55 -4 -3 0 775.55 41.36 4 -3 0 761.96 42.27 4 -3 0 753.58 40.72 4 3 0 736.29 40.19 -4 3 0 820.35 41.03 4 3 0 689.64 45.34 4 3 0 765.48 43.39 -4 3 0 699.58 41.88 4 3 0 829.73 41.01 -4 3 0 758.40 42.49 -5 -3 0 105.15 10.27 5 -3 0 100.77 7.29 5 -3 0 98.31 9.43 -5 -3 0 93.37 9.21 -5 3 0 99.05 10.40 5 3 0 117.57 8.83 5 3 0 91.56 6.44 5 3 0 100.75 14.42 5 3 0 93.08 8.63 -6 -3 0 86.99 11.07 6 -3 0 94.04 10.86 6 3 0 60.95 8.15 6 3 0 71.55 14.44 -6 3 0 84.65 11.49 6 3 0 87.17 9.47 7 -3 0 369.04 25.21 7 3 0 384.81 24.79 7 3 0 410.02 34.60 -7 3 0 394.09 26.56 8 -3 0 27.73 8.79 -8 3 0 16.25 7.64 8 3 0 50.74 15.97 8 3 0 32.03 8.68 9 -3 0 106.12 16.86 -9 3 0 131.34 16.87 9 3 0 121.53 23.48 10 -3 0 119.93 19.25 10 3 0 179.61 29.20 -10 3 0 144.61 18.88 -1 -4 0 2221.92 118.84 1 4 0 2309.05 118.99 2 -4 0 2273.08 117.66 -2 -4 0 2156.53 117.32 -2 -4 0 2361.23 120.56 -2 -4 0 2248.77 118.83 2 -4 0 2182.06 118.56 -2 4 0 2151.46 118.20 2 4 0 2450.74 120.82 2 4 0 2377.99 118.63 -2 4 0 2027.65 118.21 2 4 0 2541.70 117.58 -3 -4 0 1856.57 103.18 3 -4 0 1942.94 102.38 -3 -4 0 1887.02 101.77 3 -4 0 1965.48 101.71 -3 4 0 1831.00 102.66 3 4 0 1951.27 103.26 -3 4 0 1945.46 101.87 -3 4 0 1983.39 101.37 3 4 0 2203.52 101.66 3 4 0 1986.76 101.61 3 4 0 2045.39 106.05 -3 4 0 1944.64 102.97 -4 -4 0 228.19 15.53 4 -4 0 217.61 12.61 4 -4 0 211.81 14.27 -4 -4 0 214.36 13.47 4 -4 0 223.71 14.27 -4 4 0 221.87 12.99 -4 4 0 215.88 14.67 -4 4 0 189.10 14.43 -4 4 0 233.98 11.94 4 4 0 239.16 13.11 4 4 0 202.07 12.34 4 4 0 222.42 19.49 5 -4 0 1052.98 55.11 5 -4 0 1100.34 56.31 -5 -4 0 996.02 55.92 5 4 0 984.90 54.61 -5 4 0 1076.03 57.60 5 4 0 1098.05 55.50 5 4 0 956.43 56.40 5 4 0 1072.94 62.41 6 -4 0 1411.73 76.19 6 4 0 1464.58 83.77 6 4 0 1387.92 75.54 -6 4 0 1413.93 77.56 7 -4 0 24.77 7.89 7 4 0 23.39 11.86 7 4 0 33.57 7.53 -7 4 0 31.35 8.47 8 -4 0 138.05 15.84 -8 4 0 168.30 17.05 8 4 0 158.77 18.61 9 -4 0 20.93 10.14 -9 4 0 24.08 9.79 9 4 0 31.57 17.13 10 -4 0 115.60 16.56 -10 4 0 103.03 15.58 10 4 0 168.40 29.21 0 -5 0 3.65 3.12 0 -5 0 9.20 2.00 0 5 0 6.72 1.99 0 5 0 6.19 2.93 2 -5 0 563.25 27.90 2 -5 0 532.61 28.19 2 -5 0 487.36 27.63 -2 -5 0 506.53 29.31 2 -5 0 518.15 28.60 -2 -5 0 436.08 30.35 -2 5 0 548.39 28.36 2 5 0 589.44 27.63 2 5 0 539.56 28.70 -2 5 0 566.75 27.51 2 5 0 475.24 30.91 -2 5 0 432.14 27.77 -2 5 0 520.71 28.45 -3 -5 0 1162.73 62.31 3 -5 0 1186.84 61.20 3 -5 0 1180.58 60.44 -3 -5 0 1107.16 60.28 3 -5 0 1083.61 61.72 -3 5 0 1242.29 60.20 -3 5 0 1109.66 61.56 -3 5 0 1111.64 61.53 3 5 0 1029.45 64.34 -3 5 0 1155.66 60.55 3 5 0 1278.00 60.42 3 5 0 1225.59 60.20 3 5 0 1119.72 61.98 -4 -5 0 286.69 17.26 4 -5 0 325.69 18.36 4 -5 0 321.70 16.75 -4 -5 0 293.43 19.92 -4 5 0 294.30 18.73 4 5 0 285.74 22.68 -4 5 0 311.16 16.28 -4 5 0 305.12 17.03 4 5 0 264.45 16.50 -4 5 0 258.83 18.44 4 5 0 315.69 16.97 5 -5 0 244.57 15.75 5 -5 0 228.11 13.49 -5 -5 0 222.10 15.00 5 5 0 247.47 14.58 -5 5 0 238.98 16.50 -5 5 0 231.77 14.00 5 5 0 204.18 13.31 5 5 0 204.45 20.94 6 -5 0 241.27 16.90 6 5 0 198.36 22.41 6 5 0 222.84 15.37 -6 5 0 198.13 17.07 7 -5 0 310.50 21.99 -7 5 0 303.05 22.49 7 5 0 308.87 29.18 7 5 0 302.04 20.89 8 -5 0 272.62 21.80 8 5 0 288.14 31.69 -8 5 0 301.41 22.83 9 -5 0 5.74 9.22 -9 5 0 4.06 8.36 9 5 0 48.65 19.88 0 -6 0 3741.61 193.80 -1 -6 0 2532.74 140.34 1 -6 0 2771.66 139.04 1 -6 0 2687.76 138.33 1 6 0 2654.07 138.05 -1 6 0 2701.81 138.35 1 6 0 2671.66 140.23 2 -6 0 242.91 13.69 2 -6 0 246.94 14.05 2 -6 0 214.80 13.19 2 -6 0 221.80 14.12 -2 -6 0 182.74 16.67 -2 -6 0 191.82 15.41 -2 6 0 231.63 13.17 -2 6 0 238.02 12.98 -2 6 0 227.67 14.21 2 6 0 222.41 17.43 2 6 0 268.22 13.23 -3 -6 0 540.52 30.43 3 -6 0 517.11 28.11 3 -6 0 517.86 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473.60 33.27 4 3 4 440.49 26.39 4 3 4 428.90 26.62 4 3 4 447.66 27.29 -5 -3 -4 29.86 9.25 5 -3 4 22.51 7.87 5 3 4 25.65 7.03 5 3 4 31.03 13.38 -5 3 -4 39.81 10.48 -6 -3 -4 0.90 9.16 6 -3 4 6.42 7.93 6 3 4 2.03 6.45 -6 3 -4 18.02 9.75 6 3 4 18.07 13.99 7 -3 4 42.54 10.69 -7 -3 -4 68.23 14.67 -7 3 -4 94.36 16.24 7 3 4 78.47 20.41 11 -4 -4 209.09 25.90 11 -4 -4 198.74 32.43 11 4 -4 158.17 28.96 10 -4 -4 360.49 31.29 10 -4 -4 448.46 41.46 10 4 -4 335.91 37.90 9 -4 -4 69.33 12.90 -9 4 4 50.02 10.37 8 -4 -4 878.10 53.42 8 4 -4 953.30 53.86 -8 4 4 867.03 50.59 8 4 -4 853.44 57.84 -7 -4 4 432.48 24.27 7 -4 -4 395.07 28.89 7 4 -4 411.79 32.85 -7 4 4 405.60 26.16 7 4 -4 410.80 28.62 -7 4 4 442.68 25.01 6 -4 -4 118.45 14.99 -6 -4 4 125.71 10.02 -6 4 4 123.48 11.75 6 4 -4 120.83 14.55 -6 4 4 115.81 10.68 6 4 -4 116.25 10.64 6 4 -4 113.74 16.48 5 -4 -4 409.05 27.60 -5 -4 4 427.23 25.30 -5 -4 4 441.87 25.16 5 -4 -4 443.76 23.51 -5 4 4 431.80 25.74 5 4 -4 411.82 29.41 5 4 -4 424.67 25.85 -5 4 4 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16.91 6 -15 -9 -7.31 12.01 -6 -15 9 2.47 7.97 -6 15 9 27.25 13.31 -6 15 9 5.60 9.33 -5 -15 9 9.72 8.41 5 -15 -9 3.22 12.59 -5 15 9 22.18 11.00 -5 15 9 28.81 12.53 -4 -15 9 1.63 7.26 4 -15 -9 6.09 14.54 -4 15 9 25.06 12.26 -4 15 9 9.09 9.05 -3 -15 9 -9.35 6.23 3 -15 -9 -12.42 14.60 -3 -15 9 36.04 13.19 -3 15 9 13.25 12.20 -3 15 9 4.64 9.14 2 -15 -9 85.80 20.65 -2 -15 9 67.80 11.24 -2 15 9 67.21 15.47 -2 15 9 92.95 13.65 4 -16 -9 9.99 16.42 -4 -16 9 -4.60 6.73 -4 16 9 5.82 9.10 -4 16 9 -11.93 9.70 -10 0 10 13.76 12.12 -9 0 10 210.63 22.36 -9 0 10 179.56 21.20 -8 0 10 11.03 9.95 -8 0 10 5.35 9.28 -7 0 10 90.80 14.18 -7 0 10 78.23 13.37 -6 0 10 -2.16 8.52 -6 0 10 2.05 8.40 -5 0 10 1.22 8.45 -5 0 10 3.26 8.16 -4 0 10 49.29 10.18 -4 0 10 48.17 11.46 -3 0 10 -8.16 7.72 -2 0 10 64.43 12.73 -1 0 10 3.64 8.89 0 0 10 50.85 11.34 -9 -1 10 374.83 28.28 -9 -1 10 286.20 27.87 -9 1 10 300.60 26.96 -9 1 10 362.48 28.79 8 -1 -10 44.36 8.03 -8 -1 10 55.87 12.01 -8 -1 10 61.50 12.80 -8 1 10 42.68 11.90 -8 1 10 57.11 12.46 -7 -1 10 24.46 9.96 -7 -1 10 40.76 10.75 -7 1 10 31.77 10.62 -7 1 10 43.79 11.53 -6 -1 10 14.87 9.86 -6 -1 10 8.58 8.32 -6 1 10 13.90 8.82 -6 1 10 10.94 9.20 -5 -1 10 10.72 8.35 -5 -1 10 13.22 8.88 -5 1 10 4.02 7.69 -5 1 10 -0.42 9.05 -4 -1 10 240.92 23.24 -4 -1 10 192.56 18.09 -4 1 10 185.34 21.32 -4 1 10 211.02 18.62 -3 -1 10 77.76 13.87 -3 1 10 67.23 13.21 -3 1 10 82.27 11.53 -2 -1 10 54.18 11.69 -2 1 10 67.16 13.62 -1 -1 10 49.74 12.05 -1 1 10 39.63 11.82 1 1 -10 48.97 16.84 0 -1 10 64.65 13.42 0 1 -10 115.00 16.72 0 1 10 86.35 14.81 -9 -2 10 51.16 11.31 9 -2 -10 71.60 9.86 -9 -2 10 17.20 12.73 -9 2 10 92.78 14.34 8 -2 -10 27.06 7.04 -8 -2 10 28.84 10.20 -8 -2 10 15.52 10.40 -8 2 10 36.68 10.80 -8 2 10 28.25 10.84 -7 -2 10 67.01 12.62 -7 -2 10 63.93 13.03 -7 2 10 58.90 13.28 -7 2 10 61.75 12.31 -6 -2 10 98.92 14.62 -6 -2 10 121.07 16.17 -6 2 10 118.58 15.31 -6 2 10 107.84 15.77 -5 -2 10 438.91 32.76 -5 -2 10 361.58 28.36 -5 2 10 464.17 30.42 -5 2 10 473.56 34.18 -4 -2 10 41.76 9.49 -4 -2 10 37.35 10.45 -4 2 10 25.29 8.45 -4 2 10 41.15 11.33 -3 -2 10 130.76 17.36 -3 2 10 130.47 14.72 -3 2 10 128.13 18.28 -2 -2 10 39.21 11.11 -2 2 10 40.45 12.02 2 2 -10 52.49 15.24 -1 -2 10 308.90 27.62 1 2 -10 368.83 28.19 -1 2 10 352.30 30.24 0 -2 10 19.56 10.14 0 2 -10 50.01 13.38 0 2 10 20.36 11.15 9 -3 -10 80.03 10.70 -9 -3 10 66.63 12.82 -9 3 10 67.91 13.59 -9 3 10 73.30 13.85 8 -3 -10 30.60 7.58 -8 -3 10 11.37 12.21 -8 -3 10 30.76 9.92 -8 3 10 28.16 11.05 -8 3 10 25.29 10.58 7 -3 -10 114.99 12.90 -7 -3 10 118.56 17.06 -7 -3 10 129.75 16.51 -7 3 10 130.54 16.37 -7 3 10 98.56 16.26 -6 -3 10 95.50 14.01 -6 -3 10 84.61 13.35 -6 3 10 102.13 14.11 -6 3 10 108.56 15.91 -5 -3 10 12.46 8.25 -5 -3 10 21.57 9.48 -5 3 10 36.10 10.36 -5 3 10 30.08 10.25 -4 -3 10 88.70 12.32 -4 -3 10 69.67 12.73 -4 3 10 97.17 15.21 -4 3 10 89.32 12.86 -3 -3 10 426.06 32.10 -3 3 10 434.49 29.65 -3 3 10 483.22 35.06 -2 -3 10 37.29 10.32 2 3 -10 36.70 11.04 -2 3 10 34.06 11.00 -1 -3 10 -8.20 7.92 1 3 -10 5.10 10.14 -1 3 10 9.96 10.10 0 -3 10 51.19 13.98 0 -3 10 1.88 9.11 0 3 -10 17.04 11.82 0 3 10 14.41 10.50 -9 -4 10 35.78 10.58 -9 -4 10 0.89 11.16 9 -4 -10 15.35 7.68 -9 4 10 23.04 14.35 -9 4 10 15.49 11.45 -8 -4 10 -2.93 11.53 8 -4 -10 4.08 6.42 -8 -4 10 9.86 9.39 -8 4 10 6.18 10.58 -8 4 10 7.22 9.69 -7 -4 10 30.11 10.33 7 -4 -10 53.30 9.39 -7 4 10 44.75 12.79 -7 4 10 48.46 12.28 -6 -4 10 25.33 10.30 -6 -4 10 25.47 10.51 -6 4 10 23.88 11.06 -6 4 10 30.32 10.21 -5 -4 10 253.78 21.80 -5 -4 10 276.85 23.83 -5 4 10 277.37 22.84 -5 4 10 253.18 24.64 -4 -4 10 314.31 24.70 -4 -4 10 351.86 28.44 -4 4 10 381.79 26.52 -4 4 10 354.89 30.28 -3 -4 10 28.95 9.91 -3 4 10 49.48 12.62 -3 4 10 48.25 10.28 3 4 -10 49.51 11.21 -2 -4 10 337.63 28.14 2 4 -10 378.95 27.78 -2 4 10 343.59 29.47 -1 -4 10 -15.82 7.64 1 4 -10 4.55 10.08 -1 4 10 -0.83 9.80 0 -4 10 41.93 11.29 0 4 -10 69.23 14.80 0 4 10 44.15 12.23 -9 -5 10 236.85 23.23 9 -5 -10 257.52 21.24 -9 5 10 277.28 24.49 -8 -5 10 298.31 24.90 8 -5 -10 217.53 20.69 -8 5 10 292.61 25.86 -8 5 10 282.72 24.46 -7 -5 10 -1.25 11.04 7 -5 -10 18.60 7.66 -7 -5 10 7.04 9.49 -7 5 10 29.14 10.54 -7 5 10 -2.34 9.93 -6 -5 10 -8.31 9.54 -6 -5 10 6.67 8.53 -6 5 10 6.19 8.77 -6 5 10 23.37 10.74 -5 -5 10 31.64 10.57 -5 5 10 39.68 12.10 -5 5 10 41.52 11.35 -4 -5 10 680.30 43.69 -4 5 10 682.18 42.48 -4 5 10 661.67 46.08 -3 -5 10 94.69 14.29 -3 5 10 118.12 17.48 3 5 -10 139.78 17.28 -3 5 10 147.67 15.94 -2 -5 10 -5.04 7.20 -2 5 10 7.88 9.43 2 5 -10 16.13 10.50 -1 -5 10 148.59 17.86 1 5 -10 164.48 20.60 -1 5 10 175.17 22.73 0 -5 10 213.89 25.51 0 -5 10 152.56 19.02 0 5 10 122.36 17.93 0 5 -10 197.58 23.63 9 -6 -10 0.07 7.68 -9 -6 10 -8.47 7.37 -9 -6 10 -8.38 11.60 -9 6 10 14.05 10.93 -8 -6 10 179.62 18.91 8 -6 -10 161.81 17.37 -8 6 10 190.49 23.02 -8 6 10 173.13 19.70 7 -6 -10 20.79 8.04 -7 -6 10 22.19 9.25 -7 -6 10 -1.14 10.29 -7 6 10 22.99 11.32 -7 6 10 16.30 10.38 6 -6 -10 105.34 13.54 -6 -6 10 81.68 13.31 -6 6 10 114.82 15.31 -6 6 10 106.57 16.14 -5 -6 10 55.74 11.55 -5 6 10 60.83 14.16 -5 6 10 98.54 14.37 -4 -6 10 158.72 19.96 -4 6 10 186.08 18.64 -4 6 10 151.76 20.94 -3 -6 10 10.04 9.24 -3 6 10 18.60 9.17 -3 6 10 14.82 10.19 3 6 -10 19.76 9.95 -2 -6 10 44.37 11.10 2 6 -10 61.96 13.35 -2 6 10 52.50 12.93 -1 -6 10 369.84 29.06 1 6 -10 414.70 31.68 -1 6 10 347.28 32.31 0 -6 10 414.04 34.32 0 6 10 323.51 31.21 0 6 -10 365.71 31.43 9 -7 -10 3.43 8.11 -9 -7 10 -5.07 7.72 -9 7 10 14.98 11.00 -8 -7 10 35.36 10.58 8 -7 -10 41.60 10.33 -8 7 10 44.01 12.94 -8 7 10 46.42 12.16 -7 -7 10 289.97 24.34 7 -7 -10 282.78 22.27 -7 7 10 300.74 27.73 -7 7 10 316.73 26.38 -6 -7 10 27.34 10.41 -6 -7 10 -4.90 9.89 6 -7 -10 17.03 8.27 -6 7 10 13.62 10.47 -6 7 10 32.86 11.54 -5 -7 10 87.06 13.67 -5 7 10 93.98 14.00 -5 7 10 72.55 14.52 -4 -7 10 -7.41 7.42 -4 7 10 4.47 8.98 -4 7 10 -10.57 8.47 -3 -7 10 295.20 24.30 -3 7 10 253.93 26.39 -3 7 10 298.12 23.91 -2 -7 10 59.86 12.20 -2 7 10 74.55 15.44 -2 7 10 59.03 11.75 2 7 -10 88.12 15.47 -1 -7 10 10.15 8.28 1 7 -10 47.05 13.23 -1 7 10 24.24 11.80 0 -7 10 423.21 35.22 0 7 -10 414.47 32.86 0 7 10 315.78 32.11 -8 -8 10 50.52 11.80 8 -8 -10 68.34 11.49 -8 8 10 47.79 12.34 -8 8 10 44.84 13.27 -7 -8 10 102.71 14.56 7 -8 -10 115.62 13.58 -7 8 10 107.60 16.45 -7 8 10 103.99 15.62 -6 -8 10 54.20 11.36 6 -8 -10 38.71 10.20 -6 8 10 55.52 12.50 -6 8 10 68.37 14.99 -5 -8 10 142.05 17.60 -5 8 10 163.87 19.26 -5 8 10 160.42 21.47 -4 -8 10 263.47 23.30 -4 8 10 285.97 23.39 -4 8 10 274.05 28.33 -3 -8 10 62.03 12.52 -3 8 10 86.43 13.08 -3 8 10 83.23 16.03 -2 -8 10 25.18 9.41 -2 8 10 29.28 11.61 2 8 -10 36.17 12.55 -2 8 10 38.16 10.63 -1 -8 10 312.93 29.26 -1 -8 10 244.23 23.79 -1 8 10 258.78 26.85 1 8 -10 284.85 25.83 -8 -9 10 12.39 9.13 8 -9 -10 22.89 9.69 -8 9 10 26.09 12.14 -8 9 10 22.55 10.67 7 -9 -10 60.49 11.55 -7 -9 10 77.82 12.98 -7 9 10 89.90 14.72 -7 9 10 59.80 14.61 6 -9 -10 119.15 15.30 -6 -9 10 115.38 16.63 -6 9 10 133.07 17.26 -6 9 10 120.58 17.85 -5 -9 10 13.34 9.04 -5 9 10 40.15 11.54 -5 9 10 33.46 13.22 -4 -9 10 148.50 19.24 -4 9 10 132.47 18.81 -4 9 10 167.66 19.31 -3 -9 10 96.23 13.84 -3 9 10 131.61 16.16 -3 9 10 91.89 16.40 -2 -9 10 202.86 21.85 -2 9 10 264.59 20.96 -2 9 10 181.30 25.64 2 9 -10 235.29 24.54 -1 -9 10 70.02 12.15 1 9 -10 95.98 16.83 -1 9 10 100.52 17.49 -8 -10 10 45.84 10.48 8 -10 -10 49.82 10.95 -8 10 10 43.77 12.82 -8 10 10 74.75 15.41 7 -10 -10 94.27 14.63 -7 -10 10 98.94 14.00 -7 10 10 141.12 18.76 -7 10 10 115.70 17.21 -6 -10 10 120.92 15.62 6 -10 -10 111.23 15.25 -6 10 10 135.52 19.21 -6 10 10 171.17 19.98 5 -10 -10 -12.99 10.85 -5 -10 10 -9.91 8.32 -5 10 10 10.80 10.13 -5 10 10 -7.37 9.34 -4 -10 10 97.06 13.99 -4 10 10 132.71 16.94 -4 10 10 123.33 19.08 -3 -10 10 38.09 10.22 -3 10 10 52.58 14.45 -3 10 10 49.68 11.19 -2 -10 10 -4.63 7.68 -2 10 10 1.19 9.98 2 10 -10 11.44 11.60 -2 10 10 3.12 9.07 -1 -10 10 118.89 15.45 1 10 -10 169.47 21.30 -1 10 10 115.36 18.11 -7 -11 10 34.45 9.65 7 -11 -10 36.58 12.40 -7 11 10 47.44 13.46 -7 11 10 67.26 14.27 6 -11 -10 6.86 10.54 -6 -11 10 13.23 9.20 -6 11 10 39.29 11.52 -6 11 10 14.60 11.10 -5 -11 10 7.11 8.03 5 -11 -10 10.71 12.17 -5 11 10 16.48 11.60 -5 11 10 31.05 11.71 -4 -11 10 17.01 9.80 -4 11 10 25.97 11.81 -4 11 10 26.46 10.65 -3 -11 10 92.67 14.02 -3 11 10 115.37 17.87 -3 11 10 108.88 15.14 -2 -11 10 58.21 12.23 2 11 -10 102.44 17.46 -2 11 10 77.97 14.06 -2 11 10 93.18 17.26 -6 -12 10 8.54 8.18 6 -12 -10 4.28 11.18 -6 12 10 22.87 10.78 -6 12 10 21.26 12.04 5 -12 -10 -13.58 11.81 -5 -12 10 -10.53 7.05 -5 12 10 -1.88 11.10 -5 12 10 7.25 10.76 -4 -12 10 39.62 11.02 -4 12 10 83.10 14.09 -4 12 10 66.55 15.29 -3 -12 10 74.42 12.22 -3 12 10 86.21 16.70 -3 12 10 114.58 15.58 5 -13 -10 -7.18 13.46 -5 -13 10 -8.43 7.06 -5 13 10 -3.22 11.91 -5 13 10 -4.44 9.92 -4 -13 10 41.46 10.37 -4 13 10 60.74 13.19 -4 13 10 54.10 14.96 -8 0 11 181.04 21.96 -8 0 11 196.83 20.86 -7 0 11 201.65 22.31 -7 0 11 225.69 23.42 -6 0 11 68.75 12.78 -5 0 11 24.98 11.05 -5 0 11 20.22 9.97 -4 0 11 80.98 15.31 -3 0 11 157.05 22.48 -2 0 11 283.67 27.97 -8 -1 11 414.61 32.89 -8 -1 11 342.80 29.74 -8 1 11 379.60 30.53 -8 1 11 443.92 32.55 -7 -1 11 198.54 20.69 -7 -1 11 190.50 22.44 -7 1 11 230.53 23.79 -7 1 11 226.23 22.81 -6 -1 11 493.07 36.53 -6 -1 11 479.30 34.60 -6 1 11 533.77 38.63 -6 1 11 482.06 34.69 -5 -1 11 151.54 17.66 -5 -1 11 141.70 19.86 -5 1 11 128.58 17.33 -5 1 11 144.88 20.28 -4 -1 11 26.12 11.72 -4 1 11 26.85 12.02 -3 -1 11 387.99 31.43 -3 1 11 396.84 33.56 -2 -1 11 452.72 34.67 -2 1 11 416.11 35.15 -8 -2 11 61.43 13.62 -8 -2 11 48.98 12.82 -8 2 11 55.33 13.25 -7 -2 11 160.21 19.35 -7 -2 11 173.75 22.53 -7 2 11 176.87 20.86 -7 2 11 158.06 21.48 -6 -2 11 15.78 10.34 -6 -2 11 15.85 10.37 -6 2 11 24.07 10.95 -5 -2 11 6.64 8.64 -5 -2 11 7.98 9.66 -5 2 11 19.61 10.65 -5 2 11 6.20 8.84 -4 -2 11 95.99 15.28 -4 2 11 86.34 16.25 -4 2 11 108.49 17.07 -3 -2 11 56.70 12.73 -3 2 11 52.06 14.08 -2 -2 11 232.51 23.22 -2 2 11 198.00 25.56 -8 -3 11 181.95 22.78 -8 3 11 187.02 24.48 -8 3 11 170.67 20.62 -7 -3 11 67.25 13.73 -7 -3 11 38.66 12.63 -7 3 11 54.38 13.21 -7 3 11 48.52 12.36 -6 -3 11 36.64 11.41 -6 -3 11 31.45 11.12 -6 3 11 31.80 11.98 -6 3 11 46.64 13.24 -5 -3 11 95.33 15.19 -5 3 11 126.70 15.83 -5 3 11 113.51 17.26 -4 -3 11 243.26 24.03 -4 3 11 276.28 28.00 -4 3 11 237.01 22.00 -3 -3 11 55.11 12.41 -3 3 11 61.31 14.72 -2 -3 11 305.60 26.83 -2 3 11 300.66 30.22 -8 -4 11 -1.55 10.75 -8 -4 11 14.22 11.11 -8 4 11 20.39 12.28 -8 4 11 33.49 12.63 -7 -4 11 178.91 22.76 -7 4 11 202.61 25.37 -7 4 11 185.89 20.58 -6 -4 11 30.38 11.22 -6 4 11 31.98 11.49 -6 4 11 25.88 11.99 -5 -4 11 53.81 12.76 -5 4 11 26.12 11.58 -5 4 11 37.76 10.84 -4 -4 11 713.71 47.08 -4 4 11 723.80 49.79 -4 4 11 722.74 45.22 -3 -4 11 249.03 25.49 -3 4 11 250.08 26.30 -2 -4 11 51.18 12.86 -2 4 11 70.36 15.27 -8 -5 11 -5.21 12.09 -8 -5 11 -0.59 9.66 -8 5 11 27.94 11.44 -8 5 11 -0.41 10.69 -7 -5 11 24.69 11.33 -7 -5 11 -4.83 9.91 -7 5 11 30.22 13.01 -7 5 11 29.61 11.34 -6 -5 11 93.28 15.66 -6 5 11 114.21 17.30 -6 5 11 107.82 15.42 -5 -5 11 378.31 30.38 -5 5 11 317.01 26.48 -5 5 11 347.84 30.76 -4 -5 11 13.01 10.15 -4 5 11 1.02 10.27 -4 5 11 5.25 9.67 -3 -5 11 25.59 11.52 -3 5 11 38.10 12.78 -2 -5 11 155.98 21.06 -2 5 11 167.39 22.86 -7 -6 11 21.86 10.40 -7 6 11 31.01 12.19 -7 6 11 41.03 12.91 -6 -6 11 12.11 10.55 -6 -6 11 -11.29 9.50 -6 6 11 5.83 9.25 -6 6 11 9.83 11.84 -5 -6 11 -1.95 8.90 -5 6 11 0.89 8.91 -5 6 11 8.70 11.75 -4 -6 11 101.40 16.38 -4 6 11 120.92 17.94 -4 6 11 148.74 18.48 -3 -6 11 69.21 13.24 -3 6 11 63.51 15.19 -7 -7 11 42.48 11.41 -7 7 11 61.85 13.33 -7 7 11 47.88 14.60 -6 -7 11 51.11 12.59 -6 7 11 96.52 15.49 -6 7 11 73.31 15.43 -5 -7 11 14.84 9.83 -5 7 11 40.12 12.13 -5 7 11 21.86 12.03 -4 -7 11 -15.63 7.89 -4 7 11 -0.03 9.41 -4 7 11 -2.20 11.16 -3 -7 11 21.61 10.03 3 7 -11 26.76 13.93 -3 7 11 18.16 12.15 -6 -8 11 60.64 12.88 -6 8 11 78.06 16.53 -6 8 11 97.43 15.56 -5 -8 11 66.25 13.00 -5 8 11 91.54 14.91 -5 8 11 89.60 17.16 -4 -8 11 -3.84 8.51 -4 8 11 4.91 11.02 -4 8 11 7.42 9.79 -5 -9 11 30.94 11.93 -5 9 11 27.04 12.91 -5 9 11 45.70 12.87 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6369 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71070 8.080 17.397 8.285 90.059 117.949 89.907 ) _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 15419 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 0.62232(18) 0.51621(7) 0.61138(17) 0.0167(3) Uani 1 1 d . . . . . O2 O 0.5182(2) 0.40177(9) 0.75851(18) 0.0238(3) Uani 1 1 d . . . . . H2O H 0.609(4) 0.4361(17) 0.794(4) 0.037(7) Uiso 1 1 d . . . . . O3 O 0.3228(2) 0.38517(8) 0.18455(17) 0.0233(3) Uani 1 1 d . . . . . C1 C 0.6602(3) 0.58841(10) 0.5516(2) 0.0159(4) Uani 1 1 d . . . . . H1 H 0.554264 0.624471 0.526243 0.019 Uiso 1 1 calc R U . . . C2 C 0.8372(3) 0.62030(11) 0.7080(2) 0.0158(4) Uani 1 1 d . . . . . C3 C 0.8369(3) 0.69329(11) 0.7772(3) 0.0191(4) Uani 1 1 d . . . . . H3 H 0.725922 0.723464 0.724748 0.023 Uiso 1 1 calc R U . . . C4 C 0.9982(3) 0.72224(12) 0.9226(3) 0.0237(4) Uani 1 1 d . . . . . H4 H 0.997472 0.772383 0.967911 0.028 Uiso 1 1 calc R U . . . C5 C 1.1592(3) 0.67838(13) 1.0014(3) 0.0244(4) Uani 1 1 d . . . . . H5 H 1.268337 0.697975 1.102368 0.029 Uiso 1 1 calc R U . . . C6 C 1.1622(3) 0.60564(12) 0.9335(3) 0.0239(4) Uani 1 1 d . . . . . H6 H 1.273267 0.575550 0.987094 0.029 Uiso 1 1 calc R U . . . C7 C 1.0012(3) 0.57709(12) 0.7863(3) 0.0200(4) Uani 1 1 d . . . . . H7 H 1.003468 0.527580 0.738845 0.024 Uiso 1 1 calc R U . . . C8 C 0.6797(3) 0.57940(11) 0.3791(2) 0.0174(4) Uani 1 1 d . . . . . C9 C 0.6519(3) 0.64348(12) 0.2664(3) 0.0212(4) Uani 1 1 d . . . . . H9 H 0.617927 0.691617 0.296585 0.025 Uiso 1 1 calc R U . . . C10 C 0.6741(3) 0.63663(13) 0.1103(3) 0.0264(5) Uani 1 1 d . . . . . H10 H 0.655705 0.680232 0.034683 0.032 Uiso 1 1 calc R U . . . C11 C 0.7227(3) 0.56679(14) 0.0647(3) 0.0275(5) Uani 1 1 d . . . . . H11 H 0.736224 0.562297 -0.042691 0.033 Uiso 1 1 calc R U . . . C12 C 0.7517(3) 0.50316(13) 0.1762(3) 0.0248(4) Uani 1 1 d . . . . . H12 H 0.785261 0.455157 0.144878 0.030 Uiso 1 1 calc R U . . . C13 C 0.7318(3) 0.50957(12) 0.3336(3) 0.0203(4) Uani 1 1 d . . . . . H13 H 0.753778 0.466075 0.410380 0.024 Uiso 1 1 calc R U . . . C14 C 0.4284(3) 0.49167(11) 0.5099(2) 0.0165(4) Uani 1 1 d . . . . . H14 H 0.386116 0.496022 0.375992 0.020 Uiso 1 1 calc R U . . . C15 C 0.3068(3) 0.54073(11) 0.5598(3) 0.0208(4) Uani 1 1 d . . . . . H15 H 0.329220 0.540428 0.683001 0.025 Uiso 1 1 calc R U . . . C16 C 0.1704(3) 0.58431(13) 0.4417(3) 0.0273(5) Uani 1 1 d . . . . . H16A H 0.145039 0.585662 0.317729 0.033 Uiso 1 1 calc R U . . . H16B H 0.097303 0.614374 0.480591 0.033 Uiso 1 1 calc R U . . . C17 C 0.4313(3) 0.40583(11) 0.5624(2) 0.0186(4) Uani 1 1 d . . . . . C18 C 0.2340(3) 0.37431(12) 0.4964(3) 0.0238(4) Uani 1 1 d . . . . . H18A H 0.163202 0.379197 0.363402 0.036 Uiso 1 1 calc R U . . . H18B H 0.170761 0.403489 0.552930 0.036 Uiso 1 1 calc R U . . . H18C H 0.241004 0.319974 0.530626 0.036 Uiso 1 1 calc R U . . . C19 C 0.5447(3) 0.35870(11) 0.4909(3) 0.0181(4) Uani 1 1 d . . . . . C20 C 0.7122(3) 0.32399(11) 0.6132(3) 0.0234(4) Uani 1 1 d . . . . . H20 H 0.751489 0.327954 0.740258 0.028 Uiso 1 1 calc R U . . . C21 C 0.8242(3) 0.28375(13) 0.5560(3) 0.0295(5) Uani 1 1 d . . . . . H21 H 0.937652 0.260506 0.642678 0.035 Uiso 1 1 calc R U . . . C22 C 0.7680(3) 0.27802(12) 0.3710(3) 0.0287(5) Uani 1 1 d . . . . . H22 H 0.844241 0.251148 0.330551 0.034 Uiso 1 1 calc R U . . . C23 C 0.6019(3) 0.31113(12) 0.2448(3) 0.0243(4) Uani 1 1 d . . . . . H23 H 0.564282 0.306726 0.118092 0.029 Uiso 1 1 calc R U . . . C24 C 0.4892(3) 0.35096(11) 0.3027(3) 0.0196(4) Uani 1 1 d . . . . . C25 C 0.2711(3) 0.38430(14) -0.0061(3) 0.0302(5) Uani 1 1 d . . . . . H25A H 0.260534 0.330950 -0.048065 0.045 Uiso 1 1 calc R U . . . H25B H 0.367105 0.410996 -0.025733 0.045 Uiso 1 1 calc R U . . . H25C H 0.150341 0.410365 -0.074851 0.045 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 0.0169(6) 0.0185(7) 0.0143(6) 0.0007(5) 0.0070(5) -0.0022(5) O2 0.0322(9) 0.0265(7) 0.0142(6) 0.0010(5) 0.0122(6) -0.0031(7) O3 0.0248(8) 0.0299(8) 0.0139(6) -0.0018(5) 0.0078(6) -0.0012(6) C1 0.0172(9) 0.0162(9) 0.0153(8) 0.0005(7) 0.0085(7) -0.0005(7) C2 0.0184(9) 0.0196(9) 0.0112(8) 0.0010(7) 0.0084(7) -0.0019(7) C3 0.0204(10) 0.0200(10) 0.0183(9) 0.0004(7) 0.0102(8) 0.0003(8) C4 0.0276(11) 0.0217(10) 0.0208(10) -0.0058(8) 0.0105(9) -0.0027(8) C5 0.0218(10) 0.0313(11) 0.0164(9) -0.0052(8) 0.0059(8) -0.0054(9) C6 0.0187(10) 0.0303(11) 0.0194(10) -0.0005(8) 0.0062(8) 0.0031(8) C7 0.0222(10) 0.0209(9) 0.0164(9) -0.0032(7) 0.0087(8) 0.0000(8) C8 0.0153(9) 0.0230(9) 0.0119(8) -0.0007(7) 0.0048(7) -0.0047(7) C9 0.0203(10) 0.0241(10) 0.0160(9) 0.0021(8) 0.0059(8) -0.0014(8) C10 0.0255(11) 0.0343(12) 0.0162(9) 0.0066(8) 0.0071(8) -0.0056(9) C11 0.0297(12) 0.0401(13) 0.0132(9) -0.0030(8) 0.0104(8) -0.0111(9) C12 0.0288(11) 0.0285(11) 0.0208(10) -0.0060(8) 0.0148(9) -0.0072(9) C13 0.0229(10) 0.0229(10) 0.0161(9) -0.0010(7) 0.0099(8) -0.0050(8) C14 0.0157(9) 0.0210(9) 0.0124(8) -0.0008(7) 0.0064(7) -0.0030(7) C15 0.0201(10) 0.0224(10) 0.0231(10) -0.0046(7) 0.0127(8) -0.0040(8) C16 0.0226(11) 0.0253(11) 0.0369(12) 0.0000(9) 0.0164(9) -0.0003(8) C17 0.0247(10) 0.0203(9) 0.0134(8) -0.0001(7) 0.0110(8) -0.0020(8) C18 0.0258(11) 0.0229(10) 0.0267(10) -0.0027(8) 0.0154(9) -0.0060(8) C19 0.0229(10) 0.0151(8) 0.0186(9) -0.0010(7) 0.0117(8) -0.0037(7) C20 0.0286(12) 0.0195(10) 0.0203(9) 0.0000(7) 0.0101(8) -0.0001(8) C21 0.0287(12) 0.0243(11) 0.0316(12) 0.0002(8) 0.0108(10) 0.0036(9) C22 0.0336(13) 0.0238(11) 0.0355(12) -0.0076(9) 0.0218(10) -0.0017(9) C23 0.0317(11) 0.0226(10) 0.0227(10) -0.0058(8) 0.0161(9) -0.0066(9) C24 0.0233(11) 0.0177(9) 0.0187(9) -0.0019(7) 0.0106(8) -0.0044(8) C25 0.0394(13) 0.0342(12) 0.0161(10) -0.0008(9) 0.0124(9) -0.0026(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 _geom_angle_publ_flag C1 O1 C14 113.79(13) . . ? C17 O2 H2O 103.4(18) . . ? C24 O3 C25 117.68(16) . . ? O1 C1 C2 107.02(14) . . ? O1 C1 C8 111.59(14) . . ? C2 C1 C8 111.82(15) . . ? O1 C1 H1 108.8 . . ? C2 C1 H1 108.8 . . ? C8 C1 H1 108.8 . . ? C7 C2 C3 118.97(17) . . ? C7 C2 C1 120.81(17) . . ? C3 C2 C1 120.21(17) . . ? C4 C3 C2 120.38(18) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 120.20(19) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.15(18) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 119.58(19) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C2 C7 C6 120.70(18) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C13 C8 C9 119.05(17) . . ? C13 C8 C1 121.50(16) . . ? C9 C8 C1 119.40(17) . . ? C10 C9 C8 120.10(19) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.39(19) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 119.93(18) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C13 120.1(2) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C8 120.37(18) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? O1 C14 C15 109.94(15) . . ? O1 C14 C17 104.43(14) . . ? C15 C14 C17 113.34(16) . . ? O1 C14 H14 109.7 . . ? C15 C14 H14 109.7 . . ? C17 C14 H14 109.7 . . ? C16 C15 C14 123.38(19) . . ? C16 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? C15 C16 H16A 120.0 . . ? C15 C16 H16B 120.0 . . ? H16A C16 H16B 120.0 . . ? O2 C17 C18 105.19(15) . . ? O2 C17 C19 110.22(15) . . ? C18 C17 C19 112.38(16) . . ? O2 C17 C14 107.42(15) . . ? C18 C17 C14 111.65(16) . . ? C19 C17 C14 109.77(15) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 117.39(17) . . ? C20 C19 C17 120.07(16) . . ? C24 C19 C17 122.50(17) . . ? C21 C20 C19 122.37(19) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C22 C21 C20 119.1(2) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C23 C22 C21 120.5(2) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.25(19) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? O3 C24 C23 123.18(17) . . ? O3 C24 C19 116.39(16) . . ? C23 C24 C19 120.43(18) . . ? O3 C25 H25A 109.5 . . ? O3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 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 C1 1.434(2) . ? O1 C14 1.452(2) . ? O2 C17 1.440(2) . ? O2 H2O 0.88(3) . ? O3 C24 1.373(2) . ? O3 C25 1.434(2) . ? C1 C2 1.515(3) . ? C1 C8 1.518(2) . ? C1 H1 1.0000 . ? C2 C7 1.391(3) . ? C2 C3 1.393(3) . ? C3 C4 1.390(3) . ? C3 H3 0.9500 . ? C4 C5 1.380(3) . ? C4 H4 0.9500 . ? C5 C6 1.389(3) . ? C5 H5 0.9500 . ? C6 C7 1.393(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.393(3) . ? C8 C9 1.403(3) . ? C9 C10 1.391(3) . ? C9 H9 0.9500 . ? C10 C11 1.382(3) . ? C10 H10 0.9500 . ? C11 C12 1.389(3) . ? C11 H11 0.9500 . ? C12 C13 1.392(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.497(3) . ? C14 C17 1.551(3) . ? C14 H14 1.0000 . ? C15 C16 1.318(3) . ? C15 H15 0.9500 . ? C16 H16A 0.9500 . ? C16 H16B 0.9500 . ? C17 C18 1.524(3) . ? C17 C19 1.538(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.392(3) . ? C19 C24 1.414(3) . ? C20 C21 1.390(3) . ? C20 H20 0.9500 . ? C21 C22 1.384(3) . ? C21 H21 0.9500 . ? C22 C23 1.383(3) . ? C22 H22 0.9500 . ? C23 C24 1.395(3) . ? C23 H23 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 O1 C1 C2 158.58(14) . . . . ? C14 O1 C1 C8 -78.79(18) . . . . ? O1 C1 C2 C7 54.8(2) . . . . ? C8 C1 C2 C7 -67.7(2) . . . . ? O1 C1 C2 C3 -124.34(18) . . . . ? C8 C1 C2 C3 113.17(19) . . . . ? C7 C2 C3 C4 -0.2(3) . . . . ? C1 C2 C3 C4 178.94(18) . . . . ? C2 C3 C4 C5 -1.0(3) . . . . ? C3 C4 C5 C6 1.3(3) . . . . ? C4 C5 C6 C7 -0.5(3) . . . . ? C3 C2 C7 C6 1.0(3) . . . . ? C1 C2 C7 C6 -178.11(18) . . . . ? C5 C6 C7 C2 -0.7(3) . . . . ? O1 C1 C8 C13 -24.5(2) . . . . ? C2 C1 C8 C13 95.3(2) . . . . ? O1 C1 C8 C9 157.98(16) . . . . ? C2 C1 C8 C9 -82.2(2) . . . . ? C13 C8 C9 C10 0.8(3) . . . . ? C1 C8 C9 C10 178.33(18) . . . . ? C8 C9 C10 C11 0.3(3) . . . . ? C9 C10 C11 C12 -0.7(3) . . . . ? C10 C11 C12 C13 0.1(3) . . . . ? C11 C12 C13 C8 1.0(3) . . . . ? C9 C8 C13 C12 -1.4(3) . . . . ? C1 C8 C13 C12 -178.93(18) . . . . ? C1 O1 C14 C15 -71.90(18) . . . . ? C1 O1 C14 C17 166.19(13) . . . . ? O1 C14 C15 C16 118.4(2) . . . . ? C17 C14 C15 C16 -125.1(2) . . . . ? O1 C14 C17 O2 54.42(17) . . . . ? C15 C14 C17 O2 -65.2(2) . . . . ? O1 C14 C17 C18 169.26(14) . . . . ? C15 C14 C17 C18 49.6(2) . . . . ? O1 C14 C17 C19 -65.42(17) . . . . ? C15 C14 C17 C19 174.93(16) . . . . ? O2 C17 C19 C20 -3.9(2) . . . . ? C18 C17 C19 C20 -120.92(19) . . . . ? C14 C17 C19 C20 114.18(19) . . . . ? O2 C17 C19 C24 178.46(17) . . . . ? C18 C17 C19 C24 61.5(2) . . . . ? C14 C17 C19 C24 -63.4(2) . . . . ? C24 C19 C20 C21 0.7(3) . . . . ? C17 C19 C20 C21 -177.01(19) . . . . ? C19 C20 C21 C22 0.2(3) . . . . ? C20 C21 C22 C23 -0.7(3) . . . . ? C21 C22 C23 C24 0.2(3) . . . . ? C25 O3 C24 C23 -4.7(3) . . . . ? C25 O3 C24 C19 174.51(17) . . . . ? C22 C23 C24 O3 179.97(19) . . . . ? C22 C23 C24 C19 0.7(3) . . . . ? C20 C19 C24 O3 179.53(17) . . . . ? C17 C19 C24 O3 -2.8(3) . . . . ? C20 C19 C24 C23 -1.2(3) . . . . ? C17 C19 C24 C23 176.47(17) . . . . ?