#------------------------------------------------------------------------------ #$Date: 2020-03-26 08:04:52 +0200 (Thu, 26 Mar 2020) $ #$Revision: 249730 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/76/1557661.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_1557661 loop_ _publ_author_name 'Shi, Peng' 'Xu, Shijie' 'Ma, Yiming' 'Tang, Weiwei' 'Zhang, Feng' 'Wang, Jingkang' 'Gong, Junbo' _publ_section_title ; Probing the structural pathway of conformational polymorph nucleation by comparing a series of \a,\w-alkanedicarboxylic acids ; _journal_issue 3 _journal_name_full IUCrJ _journal_page_first ; ; _journal_paper_doi 10.1107/S205225252000233X _journal_volume 7 _journal_year 2020 _chemical_formula_moiety 'C15 H28 O4' _chemical_formula_sum 'C15 H28 O4' _chemical_formula_weight 272.37 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2019-12-09 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 94.449(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.4671(3) _cell_length_b 9.2806(5) _cell_length_c 29.8270(14) _cell_measurement_reflns_used 5268 _cell_measurement_temperature 128.15 _cell_measurement_theta_max 31.1710 _cell_measurement_theta_min 2.6190 _cell_volume 1508.80(14) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection CrystalClear(Rigaku,2008) _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 128.15 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -120.00 60.00 1.00 1.00 -- -30.00 45.00 0.00 180 2 \w -120.00 60.00 1.00 1.00 -- -30.00 45.00 90.00 180 3 \w -120.00 60.00 1.00 1.00 -- -30.00 45.00 180.00 180 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'Rigaku Saturn 70' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.1094453000 _diffrn_orient_matrix_UB_12 -0.0363795000 _diffrn_orient_matrix_UB_13 -0.0045414000 _diffrn_orient_matrix_UB_21 0.0387545000 _diffrn_orient_matrix_UB_22 0.0009286000 _diffrn_orient_matrix_UB_23 0.0232535000 _diffrn_orient_matrix_UB_31 -0.0586423000 _diffrn_orient_matrix_UB_32 -0.0672348000 _diffrn_orient_matrix_UB_33 0.0027842000 _diffrn_radiation_monochromator confocal _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_unetI/netI 0.0417 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 14484 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.877 _diffrn_reflns_theta_min 2.299 _diffrn_source 'rotating anode' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.78661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.199 _exptl_crystal_description plate _exptl_crystal_F_000 600 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.267 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.046 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 180 _refine_ls_number_reflns 3599 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0479 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.3020P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1140 _refine_ls_wR_factor_ref 0.1302 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2690 _reflns_number_total 3599 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lq5027.cif _cod_data_source_block DA15 _cod_database_code 1557661 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C15H28O4 _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. ; _reflns_odcompleteness_completeness 99.91 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C4(H4A,H4B), C2(H2A,H2B), C13(H13A,H13B), C12(H12A,H12B), C5(H5A, H5B), C11(H11A,H11B), C6(H6A,H6B), C10(H10A,H10B), C9(H9A,H9B), C8(H8A,H8B), C14(H14A,H14B), C7(H7A,H7B) ; _shelx_res_file ; TITL r20181009g_a.res in P2(1)/c r20181009g.res created by SHELXL-2018/3 at 10:52:37 on 09-Dec-2019 REM Old TITL r20181009g in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.174, Rweak 0.129, Alpha 0.019, Orientation as input REM Formula found by SHELXT: C15 O4 CELL 0.71073 5.4671 9.2806 29.827 90 94.449 90 ZERR 4 0.0003 0.0005 0.0014 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H O UNIT 60 112 16 L.S. 10 PLAN 20 TEMP -145 BOND $H conf htab fmap 2 acta SHEL 99 0.76 OMIT 0 1 2 REM REM REM WGHT 0.053000 0.302000 FVAR 0.57795 O4 3 -0.754113 0.403675 0.497642 11.00000 0.02450 0.03778 = 0.02202 -0.00555 -0.00874 0.00644 O2 3 1.864767 0.325602 0.989168 11.00000 0.02486 0.02471 = 0.03434 0.00194 -0.01721 -0.00047 O3 3 -0.868252 0.517050 0.557973 11.00000 0.02693 0.04472 = 0.02138 -0.00316 -0.00705 0.01374 O1 3 1.759662 0.545569 0.966039 11.00000 0.02647 0.02419 = 0.03566 0.00205 -0.01596 -0.00162 C1 1 1.724483 0.416908 0.965337 11.00000 0.01783 0.02563 = 0.01696 0.00135 -0.00250 0.00057 C15 1 -0.726187 0.429361 0.537830 11.00000 0.01855 0.02176 = 0.02342 -0.00094 -0.00605 -0.00214 C3 1 1.350729 0.445074 0.910134 11.00000 0.01753 0.02758 = 0.01955 -0.00015 -0.00556 -0.00188 AFIX 23 H3A 2 1.448233 0.507755 0.891425 11.00000 -1.20000 H3B 2 1.263380 0.507545 0.930550 11.00000 -1.20000 AFIX 0 C4 1 1.164718 0.361181 0.879948 11.00000 0.01742 0.02812 = 0.01985 -0.00013 -0.00561 -0.00166 AFIX 23 H4A 2 1.253888 0.298483 0.859871 11.00000 -1.20000 H4B 2 1.069664 0.298023 0.898937 11.00000 -1.20000 AFIX 0 C2 1 1.521308 0.344646 0.937730 11.00000 0.01770 0.02457 = 0.02129 0.00039 -0.00625 -0.00241 AFIX 23 H2A 2 1.423013 0.288178 0.958019 11.00000 -1.20000 H2B 2 1.593620 0.275897 0.917091 11.00000 -1.20000 AFIX 0 C13 1 -0.413077 0.449791 0.605787 11.00000 0.01995 0.02539 = 0.01909 -0.00162 -0.00729 0.00179 AFIX 23 H13A 2 -0.541241 0.486726 0.624484 11.00000 -1.20000 H13B 2 -0.331267 0.533533 0.592835 11.00000 -1.20000 AFIX 0 C12 1 -0.225849 0.363985 0.635127 11.00000 0.02105 0.02665 = 0.02343 0.00155 -0.00989 0.00011 AFIX 23 H12A 2 -0.312900 0.289848 0.651680 11.00000 -1.20000 H12B 2 -0.115357 0.313489 0.615553 11.00000 -1.20000 AFIX 0 C5 1 0.987420 0.455156 0.851361 11.00000 0.01775 0.03072 = 0.02191 0.00051 -0.00732 -0.00054 AFIX 23 H5A 2 1.082024 0.521453 0.833283 11.00000 -1.20000 H5B 2 0.891734 0.514429 0.871349 11.00000 -1.20000 AFIX 0 C11 1 -0.072372 0.455548 0.668695 11.00000 0.01868 0.03067 = 0.02152 -0.00062 -0.00752 0.00134 AFIX 23 H11A 2 -0.182629 0.506492 0.688210 11.00000 -1.20000 H11B 2 0.015914 0.529242 0.652185 11.00000 -1.20000 AFIX 0 C6 1 0.811573 0.368773 0.820014 11.00000 0.01863 0.03202 = 0.02056 0.00070 -0.00762 -0.00027 AFIX 23 H6A 2 0.716590 0.303184 0.838256 11.00000 -1.20000 H6B 2 0.908143 0.308459 0.800457 11.00000 -1.20000 AFIX 0 C10 1 0.112715 0.368546 0.697984 11.00000 0.01897 0.03292 = 0.02274 0.00220 -0.00914 0.00036 AFIX 23 H10A 2 0.023253 0.299105 0.715884 11.00000 -1.20000 H10B 2 0.215222 0.312451 0.678319 11.00000 -1.20000 AFIX 0 C9 1 0.279172 0.459061 0.729736 11.00000 0.01832 0.03293 = 0.02044 0.00035 -0.00729 0.00033 AFIX 23 H9A 2 0.176929 0.515985 0.749232 11.00000 -1.20000 H9B 2 0.370564 0.527659 0.711874 11.00000 -1.20000 AFIX 0 C8 1 0.461232 0.370598 0.759182 11.00000 0.01884 0.03383 = 0.02026 0.00218 -0.00672 -0.00033 AFIX 23 H8A 2 0.560372 0.311908 0.739617 11.00000 -1.20000 H8B 2 0.369332 0.303491 0.777463 11.00000 -1.20000 AFIX 0 C14 1 -0.531682 0.358106 0.568093 11.00000 0.02563 0.02601 = 0.02715 -0.00194 -0.01357 0.00449 AFIX 23 H14A 2 -0.401359 0.323750 0.549447 11.00000 -1.20000 H14B 2 -0.604380 0.272229 0.581592 11.00000 -1.20000 AFIX 0 C7 1 0.633274 0.459846 0.790481 11.00000 0.01956 0.03403 = 0.02031 -0.00016 -0.00859 0.00150 AFIX 23 H7A 2 0.534702 0.519378 0.809914 11.00000 -1.20000 H7B 2 0.727522 0.525974 0.772284 11.00000 -1.20000 AFIX 0 H3 2 -0.989950 0.551808 0.535615 11.00000 0.06710 H2 2 1.996088 0.374280 1.004795 11.00000 0.07086 HKLF 4 REM r20181009g_a.res in P2(1)/c REM wR2 = 0.1302, GooF = S = 1.040, Restrained GooF = 1.040 for all data REM R1 = 0.0479 for 2690 Fo > 4sig(Fo) and 0.0688 for all 3599 data REM 180 parameters refined using 0 restraints END WGHT 0.0519 0.2477 REM Instructions for potential hydrogen bonds EQIV $1 x+2, -y+1/2, z+1/2 HTAB C2 O4_$1 EQIV $2 -x+1, y-1/2, -z+3/2 HTAB C14 O1_$2 EQIV $3 -x-2, -y+1, -z+1 HTAB O3 O4_$3 EQIV $4 -x+4, -y+1, -z+2 HTAB O2 O1_$4 REM Highest difference peak 0.267, deepest hole -0.202, 1-sigma level 0.046 Q1 1 -0.6282 0.3983 0.5579 11.00000 0.05 0.27 Q2 1 1.2427 0.4095 0.8975 11.00000 0.05 0.26 Q3 1 -0.1569 0.4212 0.6507 11.00000 0.05 0.26 Q4 1 0.0428 0.4105 0.6842 11.00000 0.05 0.25 Q5 1 1.6181 0.3745 0.9493 11.00000 0.05 0.25 Q6 1 -0.2981 0.4137 0.6179 11.00000 0.05 0.25 Q7 1 -0.4758 0.4020 0.5869 11.00000 0.05 0.24 Q8 1 0.3814 0.4232 0.7467 11.00000 0.05 0.22 Q9 1 0.1714 0.4166 0.7167 11.00000 0.05 0.22 Q10 1 0.7188 0.4006 0.8033 11.00000 0.05 0.22 Q11 1 -0.4731 0.2625 0.5612 11.00000 0.05 0.17 Q12 1 1.4624 0.4042 0.9240 11.00000 0.05 0.17 Q13 1 0.5724 0.4083 0.7721 11.00000 0.05 0.17 Q14 1 1.0852 0.4126 0.8667 11.00000 0.05 0.17 Q15 1 1.8710 0.5207 0.9391 11.00000 0.05 0.16 Q16 1 -0.7577 0.5573 0.5397 11.00000 0.05 0.16 Q17 1 -0.2543 0.2667 0.6385 11.00000 0.05 0.16 Q18 1 -0.4000 0.5719 0.6062 11.00000 0.05 0.15 Q19 1 0.8678 0.4349 0.8362 11.00000 0.05 0.15 Q20 1 -0.7049 0.2996 0.6018 11.00000 0.05 0.14 ; _shelx_res_checksum 21543 _shelx_hkl_file ; 0 0 3 0.27 0.18 0 0 3 -0.05 0.10 0 0 -4 681.84 8.22 0 0 4 627.96 7.46 0 0 -5 0.11 0.21 0 0 5 -0.19 0.26 0 0 5 0.10 0.29 0 0 6 100.70 3.68 0 0 -6 92.93 3.71 0 0 6 97.19 4.13 0 0 7 -0.07 0.36 0 0 -7 -0.02 0.23 0 0 7 -0.80 0.46 0 0 -8 3.77 0.89 0 0 8 2.47 0.82 0 0 8 4.20 0.90 0 0 -9 0.04 0.34 0 0 9 -0.33 0.51 0 0 9 -1.16 0.75 0 0 -10 44.89 3.31 0 0 10 39.39 2.97 0 0 10 41.40 3.45 0 0 11 0.17 0.33 0 0 -11 0.10 0.40 0 0 11 -0.04 0.29 0 0 12 20.04 2.71 0 0 -12 26.64 2.81 0 0 12 25.73 2.67 0 0 13 0.11 0.41 0 0 -13 0.81 0.76 0 0 13 -0.13 0.38 0 0 14 2.90 0.98 0 0 14 2.46 1.03 0 0 -14 2.79 1.15 0 0 15 -0.62 1.15 0 0 -15 0.31 0.61 0 0 15 -0.15 0.54 0 0 -16 137.35 7.36 0 0 16 149.56 7.41 0 0 16 141.98 8.15 0 0 17 1.69 0.66 0 0 17 0.06 0.77 0 0 -17 0.25 0.51 0 0 18 103.80 7.53 0 0 -18 96.45 6.53 0 0 18 98.89 6.38 0 0 19 0.89 1.01 0 0 19 0.14 0.65 0 0 -19 0.02 0.73 0 0 20 55.28 5.79 0 0 20 53.71 4.98 0 0 -20 57.27 5.30 0 0 -21 0.17 0.73 0 0 21 -0.18 1.17 0 0 21 1.60 1.09 0 0 -22 21.63 3.43 0 0 22 19.88 3.78 0 0 22 20.93 3.40 0 0 23 0.03 0.42 0 0 -23 -1.12 1.00 0 0 24 7.63 2.59 0 0 -24 7.52 2.22 0 0 24 5.41 1.74 0 0 25 -0.70 0.52 0 0 25 -0.66 0.69 0 0 -25 0.17 0.59 0 0 26 18.13 3.47 0 0 26 17.23 4.05 0 0 -26 19.87 3.60 0 0 27 -1.18 1.08 0 0 27 -0.35 1.07 0 0 28 92.91 8.23 0 0 28 100.43 9.31 0 0 29 -1.48 1.63 0 0 29 0.94 1.44 0 0 30 212.01 12.96 0 0 30 219.67 14.43 0 0 31 0.53 1.16 0 0 31 -2.21 2.01 0 0 32 34.28 5.92 0 0 32 31.99 5.38 0 0 33 0.69 0.85 0 0 33 2.00 2.41 0 0 34 156.08 13.23 0 0 35 5.08 2.81 0 0 36 6.35 3.13 0 0 37 3.92 3.04 0 0 38 36.74 7.01 0 0 39 1.12 2.28 0 0 40 40.91 7.57 0 0 41 -0.11 1.51 0 0 42 30.11 7.14 0 -1 0 0.24 0.20 0 -1 0 0.27 0.24 0 1 0 -0.05 0.15 0 -1 1 -0.02 0.07 0 -1 1 0.02 0.11 0 -1 -1 0.04 0.07 0 -1 -1 0.02 0.12 0 -1 2 9.72 1.06 0 -1 2 8.58 1.08 0 1 3 1.39 0.38 0 -1 3 1.19 0.49 0 -1 3 1.26 0.43 0 -1 -3 1.24 0.54 0 1 3 1.26 0.43 0 1 4 47.25 2.68 0 -1 4 51.26 2.66 0 -1 -4 45.52 3.07 0 -1 4 52.80 2.79 0 1 4 50.05 1.97 0 -1 5 11.60 1.38 0 1 5 10.15 1.26 0 -1 5 11.56 1.34 0 -1 -5 10.78 1.58 0 1 5 10.25 0.98 0 -1 -6 27.29 2.58 0 -1 6 25.40 2.09 0 1 6 21.54 2.12 0 -1 6 24.67 2.19 0 1 6 26.33 1.75 0 1 7 35.04 2.88 0 -1 7 39.33 2.76 0 1 -7 38.34 1.63 0 -1 7 40.96 2.96 0 1 7 38.60 2.28 0 -1 -7 40.72 3.34 0 -1 8 19.24 2.10 0 1 8 17.24 1.68 0 -1 -8 15.30 2.20 0 -1 8 18.87 2.08 0 1 -8 17.07 1.25 0 1 8 19.19 2.17 0 1 -9 9.90 1.05 0 -1 -9 8.18 1.62 0 -1 9 10.87 1.72 0 1 9 10.03 1.40 0 1 9 6.77 1.40 0 -1 9 9.01 1.53 0 -1 -10 23.84 2.89 0 1 -10 20.84 1.70 0 -1 10 25.13 2.60 0 1 10 22.57 2.67 0 1 10 27.63 2.37 0 -1 10 24.62 2.53 0 1 -11 16.97 1.65 0 1 11 17.70 2.54 0 -1 11 16.06 2.18 0 1 11 15.50 1.84 0 -1 11 16.65 2.21 0 -1 -11 14.52 2.35 0 -1 -12 61.65 5.03 0 -1 12 58.53 4.37 0 1 12 66.07 5.05 0 1 -12 60.90 3.36 0 -1 12 65.05 4.59 0 1 12 62.31 3.83 0 -1 -13 121.22 7.28 0 1 -13 111.83 4.91 0 1 13 120.19 5.60 0 -1 13 118.62 6.43 0 1 13 110.53 6.71 0 -1 13 116.55 6.41 0 -1 -14 123.73 7.57 0 1 14 119.35 7.18 0 1 -14 119.43 5.22 0 -1 14 118.47 6.68 0 -1 14 129.67 7.10 0 1 14 130.61 5.98 0 1 15 247.03 8.57 0 -1 15 234.08 9.69 0 1 -15 218.41 7.38 0 1 15 223.59 10.23 0 -1 15 228.86 9.69 0 -1 -15 229.17 10.58 0 -1 16 2.83 1.49 0 1 16 0.88 0.66 0 1 -16 0.27 0.57 0 -1 -16 0.53 0.89 0 -1 16 0.28 0.62 0 1 16 3.09 1.23 0 -1 17 848.52 19.57 0 1 -17 840.95 15.62 0 1 17 818.71 21.07 0 -1 -17 818.55 20.96 0 1 17 850.09 17.19 0 -1 17 806.65 19.50 0 -1 -18 124.30 8.40 0 1 18 115.90 6.64 0 -1 18 121.56 7.68 0 1 -18 123.56 6.25 0 1 18 105.14 7.81 0 -1 18 119.21 7.74 0 1 19 244.09 12.21 0 1 19 233.91 9.67 0 -1 19 266.70 11.96 0 1 -19 240.54 9.18 0 -1 19 242.04 11.12 0 -1 -19 226.34 11.53 0 -1 20 61.48 5.93 0 -1 -20 60.10 6.12 0 1 20 54.26 5.79 0 1 -20 62.97 4.77 0 1 20 63.22 5.11 0 -1 20 63.79 5.89 0 1 21 43.93 5.57 0 1 21 50.96 4.82 0 -1 -21 45.97 5.41 0 -1 21 38.48 4.68 0 1 -21 42.10 3.92 0 -1 21 38.67 4.86 0 -1 -22 48.09 5.65 0 -1 22 49.18 5.50 0 -1 22 48.00 5.52 0 1 22 50.13 6.03 0 1 -22 47.82 4.30 0 1 22 48.75 4.71 0 1 -23 0.39 0.70 0 1 23 0.95 0.75 0 -1 23 0.14 1.18 0 -1 23 -0.44 1.20 0 1 23 0.66 0.87 0 -1 -23 1.95 1.40 0 -1 24 37.17 4.90 0 -1 24 46.85 5.68 0 1 24 36.24 5.68 0 1 24 39.51 4.46 0 -1 -24 40.56 5.39 0 1 25 14.43 2.87 0 -1 -25 15.89 3.70 0 1 25 10.72 3.35 0 -1 25 12.46 2.93 0 -1 25 7.80 2.51 0 1 26 27.42 5.03 0 -1 26 28.81 4.74 0 -1 26 30.10 4.55 0 1 26 32.72 4.40 0 -1 -26 38.10 5.35 0 1 27 3.76 2.28 0 -1 -27 5.77 2.28 0 -1 27 3.22 1.74 0 1 27 2.46 1.23 0 -1 27 2.73 1.61 0 -1 28 21.14 4.26 0 1 28 19.27 3.57 0 -1 -28 21.86 4.28 0 -1 28 20.10 4.04 0 1 28 18.78 4.16 0 -1 29 14.44 3.65 0 1 29 10.64 2.81 0 -1 -29 11.49 2.83 0 1 29 6.32 2.11 0 -1 29 6.82 2.58 0 1 30 0.54 1.19 0 -1 30 2.05 2.35 0 -1 30 1.98 1.85 0 1 30 1.31 1.44 0 -1 31 97.36 9.71 0 1 31 84.88 9.33 0 -1 31 107.34 9.82 0 -1 32 98.24 10.06 0 -1 32 95.78 9.64 0 1 32 86.67 9.72 0 1 33 329.45 18.91 0 -1 33 280.28 16.75 0 -1 33 286.35 17.62 0 -1 34 103.50 10.42 0 -1 34 91.98 10.46 0 1 34 98.02 10.54 0 1 35 26.56 5.70 0 -1 35 38.50 6.61 0 -1 35 34.87 6.27 0 -1 36 14.74 4.14 0 -1 36 22.49 5.07 0 1 36 16.86 4.46 0 1 37 26.36 5.94 0 -1 37 31.85 6.34 0 -1 38 0.66 1.19 0 1 38 6.39 3.47 0 1 39 18.28 5.34 0 -1 39 12.62 4.11 0 1 40 4.01 3.10 0 -1 40 5.59 3.26 0 -1 41 2.05 2.77 0 1 41 1.27 2.11 0 -1 42 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5 6 51.27 4.71 0 5 -6 56.30 6.05 0 5 6 46.83 5.52 0 -5 6 55.22 6.00 0 -5 -6 56.82 6.17 0 -5 6 51.16 4.18 0 5 7 235.38 12.01 0 5 7 248.04 9.80 0 -5 7 263.17 13.49 0 -5 -7 238.56 13.05 0 5 -7 252.90 12.69 0 -5 7 251.50 8.91 0 5 8 107.87 6.27 0 -5 8 108.19 5.70 0 5 8 107.72 8.16 0 -5 8 101.96 8.36 0 5 -8 100.29 8.16 0 -5 -8 129.14 9.68 0 -5 9 209.28 7.35 0 5 9 201.25 8.42 0 -5 9 209.78 12.14 0 5 -9 228.83 12.42 0 -5 -9 228.26 13.40 0 5 9 200.22 11.11 0 -5 10 180.61 11.35 0 5 10 158.29 10.14 0 -5 10 172.84 6.27 0 5 10 177.09 7.82 0 -5 -10 163.47 11.55 0 5 -10 172.66 11.09 0 5 11 122.52 6.40 0 5 11 125.87 8.88 0 -5 -11 99.32 9.17 0 -5 11 114.95 4.78 0 -5 11 119.35 9.38 0 -5 12 201.46 5.62 0 5 12 198.30 8.08 0 -5 12 191.73 11.99 0 5 12 210.54 11.88 0 -5 12 175.83 11.45 0 -5 -12 194.10 12.93 0 -5 13 44.61 5.89 0 5 13 42.76 5.28 0 5 13 53.71 4.17 0 -5 13 56.01 6.59 0 -5 -13 58.88 7.29 0 5 14 108.29 5.85 0 -5 14 95.28 8.64 0 -5 -14 125.76 10.79 0 5 14 106.98 8.66 0 -5 14 110.45 9.36 0 5 15 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5.03 2.73 0 -5 28 5.64 3.02 0 -5 28 3.13 2.38 0 -5 29 13.82 4.56 0 5 29 10.91 4.13 0 -5 -29 14.76 4.47 0 -5 29 10.69 4.07 0 -5 -30 11.24 4.08 0 -5 30 12.39 3.95 0 5 30 15.92 4.72 0 -5 30 10.50 3.54 0 -5 31 6.02 3.36 0 -5 -31 5.64 3.07 0 -5 31 1.27 1.88 0 5 31 5.20 2.20 0 5 32 7.06 2.94 0 -5 32 8.65 3.66 0 -5 32 8.87 3.91 0 -5 -32 12.53 4.26 0 -5 33 15.43 4.86 0 -5 -33 14.91 4.94 0 -5 33 16.01 5.03 0 5 33 21.90 5.83 0 -5 34 2.58 2.23 0 5 34 -1.41 2.25 0 -5 -34 -0.56 0.99 0 5 35 -1.27 2.24 0 -5 35 3.77 3.27 0 -5 -35 1.47 1.27 0 5 36 6.25 3.83 0 -5 -36 1.74 2.04 0 -5 36 3.13 2.90 0 5 -37 2.53 3.10 0 -5 -37 -0.58 1.51 0 -5 37 1.21 2.26 0 5 37 4.00 3.63 0 5 38 7.69 3.74 0 5 -38 2.28 3.12 0 -5 38 8.50 4.43 0 -5 39 0.92 3.40 0 5 -39 1.23 3.56 0 6 0 94.85 7.42 0 -6 0 96.10 8.53 0 -6 0 103.14 7.90 0 -6 -1 1.65 1.67 0 6 -1 -0.44 0.88 0 -6 1 -0.04 0.92 0 -6 -1 1.23 1.13 0 -6 1 1.24 1.69 0 6 1 0.42 0.63 0 -6 -2 18.34 3.78 0 6 -2 18.04 3.49 0 -6 2 20.77 3.41 0 6 2 23.02 3.57 0 -6 2 18.00 3.88 0 -6 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0.82 0 6 12 1.11 0.88 0 -6 -12 0.48 1.10 0 -6 12 0.44 0.61 0 6 12 0.49 0.68 0 6 -13 83.73 8.90 0 -6 -13 100.97 10.33 0 6 13 86.63 5.82 0 6 13 87.40 8.28 0 -6 13 89.18 8.95 0 6 -14 118.58 10.62 0 -6 14 116.42 10.47 0 -6 -14 113.10 10.85 0 6 14 110.76 9.67 0 6 15 299.82 15.94 0 6 -15 312.83 17.37 0 -6 -15 291.84 18.17 0 -6 15 297.51 16.77 0 6 16 335.46 16.74 0 -6 -16 289.80 17.99 0 -6 16 282.35 16.59 0 6 -16 294.36 17.48 0 6 17 294.68 15.96 0 -6 -17 268.55 17.75 0 6 -17 285.46 17.40 0 -6 17 279.52 16.67 0 -6 18 41.79 6.49 0 -6 -18 33.04 5.83 0 6 18 37.40 5.62 0 -6 19 -0.73 0.91 0 -6 -19 -1.62 1.05 0 -6 -20 8.28 3.31 0 -6 20 4.72 2.57 0 6 20 3.74 1.56 0 6 21 8.09 2.94 0 -6 -21 5.05 2.97 0 -6 21 2.90 1.66 0 6 22 58.34 7.61 0 -6 -22 59.71 8.66 0 -6 22 58.05 8.01 0 -6 -23 11.37 3.79 0 6 23 11.11 4.00 0 -6 23 7.86 2.94 0 -6 24 110.74 11.70 0 6 24 93.56 10.01 0 -6 -24 101.85 11.99 0 -6 25 12.58 4.20 0 -6 -25 11.22 4.19 0 6 25 13.10 4.41 0 6 26 80.20 9.59 0 -6 -26 103.68 12.07 0 -6 26 85.94 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1.03 0 7 -2 0.99 1.12 0 -7 2 1.95 1.33 0 -7 -3 0.40 1.17 0 7 3 2.46 1.68 0 -7 -3 0.86 1.84 0 7 -3 0.90 1.13 0 -7 3 1.64 1.34 0 -7 3 1.41 2.54 0 -7 -4 4.43 2.12 0 -7 -4 2.57 1.98 0 7 4 2.13 1.50 0 -7 4 2.90 0.87 0 -7 4 6.59 2.41 0 7 -4 2.30 1.72 0 -7 5 7.02 2.08 0 7 -5 10.59 2.68 0 7 5 11.28 2.82 0 -7 -5 13.62 3.44 0 -7 5 12.83 3.33 0 -7 -6 0.52 1.34 0 7 6 -0.12 1.02 0 -7 6 1.38 1.50 0 -7 6 0.11 0.36 0 7 -6 1.03 1.30 0 7 6 1.35 1.70 0 -7 7 41.23 6.22 0 7 7 33.94 5.61 0 -7 -7 36.51 5.82 0 7 -7 36.73 5.57 0 7 7 39.69 4.83 0 -7 7 41.09 4.53 0 7 8 6.79 2.51 0 -7 8 13.01 3.63 0 -7 8 9.87 2.21 0 -7 -8 5.61 2.54 0 7 -8 7.60 2.26 0 7 8 10.85 2.33 0 7 9 46.65 5.28 0 -7 9 44.68 4.55 0 7 -9 47.61 6.66 0 -7 9 43.67 6.41 0 7 9 44.80 6.22 0 -7 -9 48.46 7.11 0 -7 -10 24.52 5.11 0 7 -10 28.27 5.38 0 7 10 27.59 5.24 0 7 10 24.69 3.73 0 -7 10 26.39 5.19 0 -7 11 22.58 4.85 0 7 -11 20.72 4.56 0 7 11 21.02 4.27 0 -7 -11 15.33 4.18 0 7 12 38.08 5.87 0 -7 12 38.14 6.33 0 -7 -12 50.00 7.50 0 7 -12 39.40 6.52 0 7 13 3.10 2.31 0 -7 -13 1.14 1.40 0 7 -13 -0.95 0.68 0 -7 13 -0.89 1.70 0 7 -14 27.75 5.39 0 7 14 41.08 6.18 0 -7 14 28.04 5.47 0 -7 -14 24.92 5.43 0 -7 15 45.83 7.17 0 7 -15 46.24 7.00 0 -7 -15 44.70 7.48 0 7 15 49.93 7.32 0 -7 -16 338.89 20.84 0 -7 16 361.01 20.09 0 7 -16 334.20 19.80 0 7 16 330.71 18.05 0 7 17 230.32 15.11 0 -7 -17 261.41 18.45 0 -7 17 202.60 15.26 0 7 -17 275.65 18.19 0 7 18 15.48 4.00 0 -7 -18 10.81 3.97 0 7 -18 12.21 4.19 0 -7 18 7.69 3.06 0 -7 -19 6.99 3.96 0 -7 19 8.67 3.30 0 7 -19 9.59 3.80 0 7 19 2.82 2.02 0 -7 20 72.75 9.43 0 7 20 61.38 8.09 0 -7 -20 63.11 9.37 0 7 -20 68.29 9.54 0 -7 -21 2.21 1.37 0 7 21 1.10 0.76 0 -7 21 0.67 0.92 0 7 -21 -0.52 2.06 0 -7 22 76.89 9.97 0 -7 -22 89.92 11.63 0 7 -22 77.01 10.50 0 7 22 76.24 9.09 0 7 23 0.77 1.42 0 7 -23 2.74 2.98 0 -7 -23 -1.27 2.79 0 -7 23 3.55 2.24 0 7 -24 45.95 8.34 0 -7 -24 42.21 8.01 0 -7 24 41.44 7.34 0 7 24 51.05 8.06 0 7 25 4.72 2.75 0 -7 25 7.60 3.11 0 -7 -25 4.68 2.24 0 7 -25 7.42 4.27 0 -7 26 8.96 3.89 0 7 -26 11.99 4.46 0 -7 -26 15.85 5.17 0 7 26 14.99 4.49 0 7 27 8.73 3.37 0 7 -27 5.58 3.37 0 -7 -27 4.89 3.55 0 -7 27 11.53 4.28 0 7 28 -0.41 1.78 0 -7 -28 1.06 2.73 0 7 -28 1.06 1.50 0 -7 28 1.38 1.90 0 -7 29 -0.94 1.51 0 7 -29 0.19 2.28 0 7 29 -0.64 1.41 0 -7 -29 2.63 2.85 0 -7 30 11.26 4.53 0 7 -30 7.01 3.76 0 7 30 8.11 4.34 0 -7 -30 13.94 5.01 0 -7 -31 41.79 8.62 0 7 -31 26.77 7.26 0 7 31 29.45 6.57 0 -7 31 28.22 7.00 0 -7 -32 27.91 7.16 0 7 -32 36.76 8.82 0 7 32 36.24 7.25 0 -7 32 39.95 8.26 0 7 -33 4.22 3.90 0 -7 33 5.86 3.97 0 7 33 2.61 2.16 0 -7 -33 7.52 3.63 0 7 -34 4.51 3.55 0 7 34 10.58 4.80 0 -7 -34 7.23 3.92 0 -7 34 3.11 3.96 0 -7 -35 12.00 5.30 0 -7 35 9.90 5.32 0 7 -35 7.35 4.98 0 -7 36 7.92 4.76 0 -7 -36 -0.30 1.83 0 -8 0 24.35 4.47 0 -8 0 26.23 5.13 0 8 0 31.18 5.02 0 -8 1 134.52 10.32 0 8 -1 116.14 9.90 0 8 1 145.86 10.99 0 -8 -1 132.86 10.70 0 -8 -1 134.99 11.84 0 -8 1 106.31 10.46 0 8 2 95.06 8.80 0 8 -2 115.93 9.93 0 -8 2 108.40 9.14 0 -8 2 104.19 10.32 0 -8 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6.60 0 8 -14 33.55 6.40 0 -8 14 31.94 6.39 0 -8 -15 21.59 5.58 0 8 -15 9.20 3.70 0 -8 15 22.02 5.45 0 8 15 18.51 4.27 0 8 -16 348.16 21.20 0 -8 16 419.34 23.12 0 -8 -16 427.69 24.41 0 8 16 416.26 21.52 0 8 17 36.64 6.42 0 -8 -17 26.94 6.48 0 -8 17 33.05 6.71 0 8 -17 34.24 6.81 0 8 -18 0.01 2.82 0 8 18 2.50 2.08 0 -8 -18 2.69 2.84 0 -8 18 3.85 3.17 0 -8 19 105.89 12.53 0 8 19 102.48 10.88 0 8 -19 112.59 12.88 0 -8 -19 91.65 11.81 0 -8 -20 1.60 1.63 0 8 -20 8.11 3.77 0 -8 20 7.40 4.35 0 8 20 6.11 3.28 0 8 -21 52.87 9.04 0 -8 21 57.13 9.10 0 8 21 56.30 8.33 0 -8 -21 62.87 9.77 0 8 22 5.26 2.54 0 -8 22 3.27 2.49 0 -8 -22 1.59 1.15 0 8 -22 0.52 1.14 0 8 -23 29.16 6.78 0 -8 -23 23.08 6.32 0 -8 23 20.83 5.91 0 8 23 22.63 5.94 0 -8 24 4.35 2.84 0 8 24 1.05 1.39 0 -8 25 10.38 4.34 0 8 25 12.67 4.01 0 -8 -25 9.63 4.84 0 8 -25 16.60 6.28 0 -8 -26 18.42 6.13 0 -8 26 12.58 4.88 0 8 26 15.27 4.69 0 8 -26 13.66 5.17 0 8 27 -0.81 1.43 0 -8 27 2.71 3.07 0 -8 -27 0.81 2.40 0 8 -27 4.73 2.62 0 8 28 13.06 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1.43 2 0 -15 0.19 0.93 -2 0 15 -1.27 0.98 -2 0 14 246.84 11.92 -2 0 14 220.56 8.56 2 0 -14 230.89 10.44 -2 0 13 0.62 0.86 2 0 -13 0.72 0.90 -2 0 13 0.00 0.36 -2 0 12 766.85 14.45 -2 0 12 749.17 19.59 2 0 -12 761.48 18.20 2 0 -11 -0.15 0.32 -2 0 11 -0.86 1.03 -2 0 11 -0.30 0.35 -2 0 10 274.49 11.21 -2 0 10 289.76 7.83 2 0 -10 290.28 10.84 -2 0 9 -0.70 1.07 2 0 -9 1.00 0.94 -2 0 9 0.34 0.23 -2 0 8 368.58 7.60 2 0 -8 385.79 12.31 2 0 -7 0.97 0.78 -2 0 7 0.75 0.60 -2 0 7 -0.20 0.39 -2 0 6 238.77 5.20 -2 0 6 212.76 9.22 2 0 -6 228.03 9.26 2 0 -5 0.37 0.66 -2 0 5 0.17 0.54 -2 0 5 -0.24 0.28 -2 0 4 159.92 7.63 -2 0 4 165.99 3.90 2 0 -4 166.48 7.76 -2 0 3 0.67 0.59 2 0 -3 -0.03 0.28 2 0 -3 0.02 0.30 -2 0 2 330.77 10.65 2 0 -2 328.98 6.36 2 0 -2 306.58 10.45 -2 0 1 0.44 0.47 2 0 -1 0.35 0.39 2 0 -1 -0.19 0.10 2 0 0 750.49 16.05 -2 0 0 754.08 15.57 2 0 1 0.71 1.01 -2 0 -1 1.30 1.15 2 0 1 -0.14 0.23 -2 0 -2 1364.12 21.10 2 0 2 1424.37 21.98 2 0 3 0.25 0.43 -2 0 -3 -0.42 0.25 2 0 3 -0.36 0.50 -2 0 -4 2187.13 26.78 2 0 4 2196.69 21.98 2 0 5 -0.06 0.34 -2 0 -5 -0.46 0.87 2 0 5 0.21 0.68 2 0 6 1508.34 23.46 2 0 6 1527.10 19.79 -2 0 -7 0.33 0.49 2 0 7 -0.38 0.53 2 0 7 -0.25 0.44 -2 0 -8 306.22 10.53 2 0 8 299.45 10.68 2 0 8 310.68 9.88 -2 0 -9 -0.01 0.70 2 0 9 0.60 0.37 2 0 9 0.86 0.87 -2 0 -10 11.47 2.06 2 0 10 12.63 2.20 2 0 10 8.18 1.89 -2 0 -11 0.94 1.10 2 0 11 0.24 0.30 2 0 11 -0.09 0.60 2 0 12 19.51 2.82 2 0 12 24.08 3.13 -2 0 -12 24.51 3.23 2 0 13 -0.18 0.45 2 0 13 -0.53 0.50 2 0 14 49.79 4.82 2 0 14 49.16 4.92 -2 0 -14 45.40 4.39 -2 0 -15 0.66 0.66 2 0 15 0.34 0.68 2 0 15 0.63 0.94 2 0 16 28.39 3.81 -2 0 -16 36.85 4.11 2 0 16 39.79 4.66 -2 0 -17 0.05 0.33 2 0 17 0.89 1.05 2 0 17 1.44 1.19 2 0 18 21.06 3.62 2 0 18 28.58 3.85 -2 0 -18 24.06 3.50 2 0 19 0.38 1.21 -2 0 -19 1.37 1.16 2 0 19 0.43 0.65 2 0 20 120.26 8.14 -2 0 -20 120.19 8.18 2 0 20 103.64 8.47 2 0 21 0.23 1.25 2 0 21 2.33 1.42 -2 0 -21 -1.48 1.01 -2 0 -22 2378.80 38.41 2 0 22 2440.90 38.06 2 0 22 2414.72 42.53 -2 0 -23 -0.09 0.72 2 0 23 1.33 1.31 2 0 23 1.02 1.76 2 0 24 511.36 20.52 -2 0 -24 478.03 17.99 2 0 24 513.24 18.13 -2 0 -25 0.80 1.27 2 0 25 -1.44 1.20 2 0 25 -0.29 1.08 2 0 26 175.27 10.87 2 0 26 174.68 12.68 2 0 27 -1.67 0.98 2 0 27 0.34 1.96 2 0 28 69.80 7.13 2 0 28 79.16 8.89 2 0 29 -0.52 1.32 2 0 30 28.01 5.38 2 0 31 0.83 1.48 2 0 32 13.19 4.08 2 0 33 0.44 1.84 2 0 34 8.46 3.79 2 0 35 -0.71 1.02 2 0 36 -0.98 1.75 2 0 37 -0.64 1.05 2 0 38 43.28 8.17 2 0 39 2.51 2.26 -2 1 42 2.35 2.47 -2 -1 42 -0.61 1.35 -2 1 41 8.51 3.58 -2 -1 41 9.12 3.68 -2 -1 40 3.10 2.41 -2 1 40 2.76 2.33 -2 -1 40 1.90 1.82 -2 -1 39 0.89 1.30 -2 -1 39 -0.90 1.24 -2 1 39 1.04 1.23 -2 1 38 2.74 2.58 -2 1 38 1.42 1.95 -2 -1 38 5.13 2.83 -2 -1 38 1.60 1.62 -2 -1 37 5.57 2.75 -2 -1 37 3.77 1.94 -2 1 37 3.54 2.27 -2 1 37 2.36 2.53 -2 1 36 -1.66 1.92 -2 -1 36 0.03 1.18 -2 1 36 0.81 1.47 -2 -1 36 1.15 2.08 -2 -1 35 7.88 3.08 -2 1 35 4.16 2.50 -2 1 35 9.04 3.62 -2 -1 35 5.11 2.51 -2 1 34 2.72 2.29 -2 -1 34 -1.16 1.26 -2 -1 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-1 22 6.59 2.35 -2 1 22 6.81 2.03 -2 -1 22 5.91 1.68 2 1 -21 -0.12 0.32 2 -1 -21 1.33 1.49 -2 1 21 2.84 1.53 -2 1 21 0.97 1.30 -2 -1 21 -0.12 0.93 -2 -1 21 0.83 0.84 -2 1 20 6.65 2.64 2 1 -20 15.34 2.76 -2 1 20 10.43 2.45 -2 -1 20 11.28 2.19 2 -1 -20 14.56 3.34 -2 -1 20 12.55 2.90 2 1 -19 24.83 3.38 -2 1 19 19.61 3.74 -2 -1 19 28.00 4.43 2 -1 -19 30.42 4.41 -2 1 19 28.80 3.95 -2 -1 19 22.69 3.14 2 1 -18 12.64 2.34 2 -1 -18 8.47 2.51 -2 1 18 6.84 2.26 -2 -1 18 16.03 3.29 -2 1 18 10.27 2.06 -2 -1 18 10.71 2.11 2 -1 -17 177.78 10.66 -2 1 17 177.53 10.70 -2 -1 17 188.45 10.95 -2 1 17 176.43 9.00 -2 -1 17 186.19 8.32 2 1 -17 189.67 8.98 -2 1 16 5.47 1.41 -2 1 16 4.72 1.93 -2 -1 16 5.92 1.91 2 1 -16 5.87 1.54 -2 -1 16 5.48 1.38 2 -1 -16 4.67 1.74 2 1 -15 618.41 15.78 -2 -1 15 576.88 18.50 -2 1 15 629.43 16.00 -2 -1 15 599.51 13.64 -2 1 15 618.42 18.97 2 -1 -15 601.05 18.75 -2 1 14 11.51 2.77 -2 -1 14 7.23 1.65 2 1 -14 10.02 1.91 -2 1 14 7.89 1.60 2 -1 -14 10.35 2.51 -2 -1 14 8.34 1.59 2 1 -13 2078.07 27.53 -2 -1 13 2051.67 34.12 2 -1 -13 2007.11 33.37 -2 1 13 1997.69 26.21 -2 -1 13 2014.35 22.57 -2 1 13 1986.87 32.65 -2 1 12 851.97 20.90 -2 -1 12 902.33 21.76 -2 1 12 860.83 16.32 -2 -1 12 841.05 13.77 2 -1 -12 815.32 20.73 2 1 -12 784.83 16.86 2 -1 -11 247.48 11.19 -2 1 11 243.95 8.44 -2 -1 11 239.05 6.80 -2 1 11 252.27 11.12 2 1 -11 252.50 9.44 -2 -1 11 243.94 10.95 -2 1 10 104.91 7.07 -2 1 10 116.64 5.58 -2 -1 10 107.53 4.21 2 1 -10 116.49 6.33 2 -1 -10 116.23 7.58 -2 -1 10 105.05 7.06 -2 1 9 496.12 15.03 -2 -1 9 498.28 14.97 -2 1 9 543.00 11.79 -2 -1 9 501.48 8.12 2 1 -9 525.66 13.37 2 -1 -9 505.64 15.44 -2 1 8 0.29 0.63 -2 -1 8 0.49 0.22 2 -1 -8 0.08 0.33 -2 1 8 0.63 0.65 -2 -1 8 -0.01 0.45 2 1 -8 -0.14 0.34 2 1 -7 140.76 6.78 -2 1 7 128.27 5.36 -2 -1 7 143.20 7.66 -2 -1 7 133.15 3.23 2 -1 -7 153.49 8.40 -2 1 7 138.33 7.80 -2 -1 6 44.55 4.13 -2 1 6 47.06 3.22 2 1 -6 46.44 3.88 -2 1 6 42.86 4.22 2 -1 -6 44.43 4.37 2 -1 -5 4.63 1.41 -2 -1 5 3.59 1.27 -2 1 5 4.30 1.47 2 1 -5 4.49 1.34 2 -1 -4 83.95 4.52 2 1 -4 76.34 4.90 2 -1 -4 94.20 6.23 -2 1 4 89.39 6.02 -2 -1 4 88.11 5.45 2 1 -3 62.14 4.40 2 -1 -3 61.89 5.01 2 -1 -3 62.97 3.94 -2 -1 3 57.05 4.25 -2 1 3 49.76 4.55 2 -1 -2 114.36 5.34 -2 -1 2 97.33 5.42 2 1 -2 99.54 5.58 2 -1 -2 111.17 6.67 -2 1 2 94.25 6.17 2 -1 -1 36.28 3.05 -2 -1 1 36.35 3.21 -2 1 1 29.13 3.47 2 1 -1 38.50 3.44 2 -1 -1 34.01 3.65 2 -1 0 99.14 5.19 2 1 0 107.25 5.90 2 -1 0 107.86 6.49 2 1 0 105.66 2.85 -2 -1 0 105.65 5.43 -2 1 0 100.72 6.44 -2 1 -1 -0.87 0.98 2 -1 1 0.18 0.42 -2 -1 -1 0.56 0.32 2 -1 1 0.49 0.48 2 1 1 0.59 0.33 2 1 1 0.22 0.35 -2 -1 -2 109.92 5.22 2 -1 2 111.38 6.53 2 1 2 116.00 6.20 2 1 2 105.00 3.81 -2 1 -2 110.51 6.81 2 -1 2 103.86 5.50 2 1 3 13.40 2.15 2 -1 3 16.23 2.40 2 1 3 15.49 1.62 2 -1 3 14.18 2.05 -2 -1 -3 17.07 1.98 -2 1 -3 12.84 2.39 2 1 4 256.95 9.55 2 -1 4 261.92 9.86 -2 1 -4 287.88 11.18 2 1 4 273.23 7.35 2 -1 4 267.96 9.03 -2 -1 -4 268.33 7.87 2 1 5 319.27 10.82 2 -1 5 313.42 10.90 2 1 5 323.71 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-7 4 12 11.67 4.22 7 -4 -12 11.27 5.11 -7 4 11 0.04 1.88 7 -4 -11 3.98 3.69 -7 4 10 6.49 3.91 7 -4 -10 0.45 1.96 7 4 -9 14.82 5.09 -7 4 9 13.40 5.19 7 -4 -9 13.01 5.16 7 4 -8 8.10 3.92 -7 4 8 -0.16 1.56 7 -4 -8 3.16 2.97 7 4 -7 5.93 3.60 -7 4 7 0.78 2.03 7 -4 -7 3.87 3.55 7 4 -6 9.99 4.01 -7 4 6 12.45 4.71 7 -4 -6 10.01 4.78 7 4 -5 15.31 5.00 -7 4 5 10.97 4.58 7 -4 -5 19.09 6.11 7 4 -4 11.35 4.11 -7 4 4 25.10 7.45 7 -4 -4 18.21 5.97 7 4 -3 8.37 4.02 -7 4 3 11.73 4.96 7 -4 -3 4.88 3.24 7 4 -2 1.51 2.54 -7 4 2 0.25 1.68 7 -4 -2 0.46 1.45 7 4 -1 1.60 2.63 -7 4 1 2.82 3.54 7 -4 -1 -0.48 1.85 7 4 0 3.10 2.52 -7 4 0 4.01 3.98 7 -4 0 1.17 1.38 7 4 1 5.69 3.57 -7 4 -1 4.13 3.86 7 -4 1 1.23 2.59 -7 4 -2 8.21 4.52 7 -4 2 7.48 4.69 7 4 2 3.29 3.23 -7 4 -3 3.48 2.92 7 -4 3 2.41 3.27 7 4 3 -1.63 1.06 -7 4 -4 2.28 1.98 7 -4 4 2.67 3.26 7 4 4 2.09 2.26 -7 4 -5 -0.02 1.61 7 -4 5 2.67 3.33 7 4 5 -0.31 1.42 -7 4 -6 2.10 1.52 7 -4 6 3.35 2.85 7 4 6 -0.34 1.77 -7 4 -7 9.23 3.66 7 -4 7 14.22 5.57 7 4 7 16.65 5.82 -7 4 -8 1.59 1.91 7 -4 8 3.34 3.51 7 4 8 -0.91 2.82 7 -4 9 52.29 10.52 -7 4 -9 54.52 9.48 7 -4 10 67.94 11.78 -7 4 -10 69.62 10.72 -7 4 -11 4.11 2.88 -7 5 8 0.93 1.44 -7 5 7 2.09 2.63 7 5 -6 3.97 2.48 -7 5 6 4.53 2.95 7 -5 -6 4.05 2.99 7 5 -5 5.93 3.20 -7 5 5 1.09 1.39 7 -5 -5 9.41 4.15 7 5 -4 -2.51 2.48 -7 5 4 1.41 2.22 7 5 -3 1.47 2.05 -7 5 3 2.99 3.18 7 -5 -3 4.11 2.44 7 5 -2 13.78 5.26 -7 5 2 8.43 4.11 7 -5 -2 7.69 4.57 7 5 -1 0.19 1.53 -7 5 1 8.32 4.91 7 -5 -1 3.63 3.15 -7 5 0 5.71 3.59 7 -5 0 4.94 3.13 7 5 0 0.11 1.77 -7 5 -1 9.11 4.79 7 -5 1 6.95 3.73 7 5 1 3.84 3.27 -7 5 -2 0.02 1.34 7 -5 2 -1.46 1.84 7 5 2 1.90 2.49 -7 5 -3 2.79 1.80 7 -5 3 1.44 2.04 -7 5 -4 1.94 2.07 7 -5 4 2.64 2.76 7 5 4 3.51 2.90 -7 5 -5 2.98 3.11 7 -5 5 1.22 2.41 7 5 5 0.88 1.76 -7 5 -6 0.66 1.48 -7 5 -7 14.59 5.53 -7 5 -8 188.41 18.41 -7 5 -9 8.46 3.68 7 6 -3 1.25 1.09 7 6 -2 0.97 2.61 7 6 -1 -0.04 1.74 7 6 0 -2.65 3.06 7 6 1 2.88 2.71 -8 1 5 0.11 1.24 0 0 0 0.00 0.00 TITL r20181009g in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 5.467093 9.280594 29.827017 90.0000 94.4487 90.0000 ZERR 4.00 0.000286 0.000496 0.001372 0.0000 0.0045 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H O UNIT 60.00 112.00 16.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 10058 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.245 _oxdiff_exptl_absorpt_empirical_full_min 0.750 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 O4 O -0.75411(17) 0.40367(12) 0.49764(3) 0.0287(3) Uani 1 1 d . . . . . O2 O 1.86477(18) 0.32560(11) 0.98917(3) 0.0290(3) Uani 1 1 d . . . . . O3 O -0.86825(19) 0.51705(12) 0.55797(3) 0.0315(3) Uani 1 1 d . . . . . O1 O 1.75966(18) 0.54557(11) 0.96604(3) 0.0297(3) Uani 1 1 d . . . . . C1 C 1.7245(2) 0.41691(15) 0.96534(4) 0.0203(3) Uani 1 1 d . . . . . C15 C -0.7262(2) 0.42936(15) 0.53783(4) 0.0216(3) Uani 1 1 d . . . . . C3 C 1.3507(2) 0.44507(15) 0.91013(4) 0.0219(3) Uani 1 1 d . . . . . H3A H 1.448233 0.507755 0.891425 0.026 Uiso 1 1 calc R . . . . H3B H 1.263380 0.507545 0.930550 0.026 Uiso 1 1 calc R . . . . C4 C 1.1647(2) 0.36118(15) 0.87995(4) 0.0222(3) Uani 1 1 d . . . . . H4A H 1.253888 0.298483 0.859871 0.027 Uiso 1 1 calc R . . . . H4B H 1.069664 0.298023 0.898937 0.027 Uiso 1 1 calc R . . . . C2 C 1.5213(2) 0.34465(15) 0.93773(4) 0.0216(3) Uani 1 1 d . . . . . H2A H 1.423013 0.288178 0.958019 0.026 Uiso 1 1 calc R . . . . H2B H 1.593620 0.275897 0.917091 0.026 Uiso 1 1 calc R . . . . C13 C -0.4131(2) 0.44979(15) 0.60579(4) 0.0219(3) Uani 1 1 d . . . . . H13A H -0.541241 0.486726 0.624484 0.026 Uiso 1 1 calc R . . . . H13B H -0.331267 0.533533 0.592835 0.026 Uiso 1 1 calc R . . . . C12 C -0.2258(2) 0.36398(16) 0.63513(4) 0.0243(3) Uani 1 1 d . . . . . H12A H -0.312900 0.289848 0.651680 0.029 Uiso 1 1 calc R . . . . H12B H -0.115357 0.313489 0.615553 0.029 Uiso 1 1 calc R . . . . C5 C 0.9874(2) 0.45516(16) 0.85136(4) 0.0239(3) Uani 1 1 d . . . . . H5A H 1.082024 0.521453 0.833283 0.029 Uiso 1 1 calc R . . . . H5B H 0.891734 0.514429 0.871349 0.029 Uiso 1 1 calc R . . . . C11 C -0.0724(2) 0.45555(16) 0.66870(4) 0.0241(3) Uani 1 1 d . . . . . H11A H -0.182629 0.506492 0.688210 0.029 Uiso 1 1 calc R . . . . H11B H 0.015914 0.529242 0.652185 0.029 Uiso 1 1 calc R . . . . C6 C 0.8116(2) 0.36877(16) 0.82001(4) 0.0242(3) Uani 1 1 d . . . . . H6A H 0.716590 0.303184 0.838256 0.029 Uiso 1 1 calc R . . . . H6B H 0.908143 0.308459 0.800457 0.029 Uiso 1 1 calc R . . . . C10 C 0.1127(2) 0.36855(16) 0.69798(4) 0.0254(3) Uani 1 1 d . . . . . H10A H 0.023253 0.299105 0.715884 0.031 Uiso 1 1 calc R . . . . H10B H 0.215222 0.312451 0.678319 0.031 Uiso 1 1 calc R . . . . C9 C 0.2792(2) 0.45906(16) 0.72974(4) 0.0244(3) Uani 1 1 d . . . . . H9A H 0.176929 0.515985 0.749232 0.029 Uiso 1 1 calc R . . . . H9B H 0.370564 0.527659 0.711874 0.029 Uiso 1 1 calc R . . . . C8 C 0.4612(2) 0.37060(16) 0.75918(4) 0.0247(3) Uani 1 1 d . . . . . H8A H 0.560372 0.311908 0.739617 0.030 Uiso 1 1 calc R . . . . H8B H 0.369332 0.303491 0.777463 0.030 Uiso 1 1 calc R . . . . C14 C -0.5317(3) 0.35811(16) 0.56809(5) 0.0271(3) Uani 1 1 d . . . . . H14A H -0.401359 0.323750 0.549447 0.032 Uiso 1 1 calc R . . . . H14B H -0.604380 0.272229 0.581592 0.032 Uiso 1 1 calc R . . . . C7 C 0.6333(2) 0.45985(16) 0.79048(4) 0.0252(3) Uani 1 1 d . . . . . H7A H 0.534702 0.519378 0.809914 0.030 Uiso 1 1 calc R . . . . H7B H 0.727522 0.525974 0.772284 0.030 Uiso 1 1 calc R . . . . H3 H -0.990(4) 0.552(2) 0.5356(7) 0.067(6) Uiso 1 1 d . . . . . H2 H 1.996(4) 0.374(2) 1.0048(7) 0.071(7) Uiso 1 1 d . . . . . 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 O4 0.0245(5) 0.0378(6) 0.0220(5) -0.0056(4) -0.0087(4) 0.0064(5) O2 0.0249(6) 0.0247(6) 0.0343(6) 0.0019(4) -0.0172(4) -0.0005(4) O3 0.0269(6) 0.0447(7) 0.0214(5) -0.0032(5) -0.0071(4) 0.0137(5) O1 0.0265(6) 0.0242(6) 0.0357(6) 0.0021(4) -0.0160(4) -0.0016(4) C1 0.0178(6) 0.0256(7) 0.0170(6) 0.0013(5) -0.0025(5) 0.0006(5) C15 0.0185(7) 0.0218(7) 0.0234(7) -0.0009(5) -0.0061(5) -0.0021(5) C3 0.0175(7) 0.0276(8) 0.0196(6) -0.0001(5) -0.0056(5) -0.0019(5) C4 0.0174(7) 0.0281(8) 0.0199(6) -0.0001(5) -0.0056(5) -0.0017(6) C2 0.0177(7) 0.0246(7) 0.0213(7) 0.0004(5) -0.0063(5) -0.0024(5) C13 0.0200(7) 0.0254(7) 0.0191(6) -0.0016(5) -0.0073(5) 0.0018(6) C12 0.0211(7) 0.0267(8) 0.0234(7) 0.0016(6) -0.0099(5) 0.0001(6) C5 0.0178(7) 0.0307(8) 0.0219(7) 0.0005(6) -0.0073(5) -0.0005(6) C11 0.0187(7) 0.0307(8) 0.0215(7) -0.0006(6) -0.0075(5) 0.0013(6) C6 0.0186(7) 0.0320(8) 0.0206(7) 0.0007(6) -0.0076(5) -0.0003(6) C10 0.0190(7) 0.0329(8) 0.0227(7) 0.0022(6) -0.0091(5) 0.0004(6) C9 0.0183(7) 0.0329(8) 0.0204(7) 0.0004(6) -0.0073(5) 0.0003(6) C8 0.0188(7) 0.0338(8) 0.0203(7) 0.0022(6) -0.0067(5) -0.0003(6) C14 0.0256(8) 0.0260(8) 0.0271(7) -0.0019(6) -0.0136(6) 0.0045(6) C7 0.0196(7) 0.0340(8) 0.0203(7) -0.0002(6) -0.0086(5) 0.0015(6) 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 O2 H2 110.4(13) . . ? C15 O3 H3 107.2(12) . . ? O2 C1 C2 112.80(12) . . ? O1 C1 O2 122.82(12) . . ? O1 C1 C2 124.38(12) . . ? O4 C15 O3 122.77(12) . . ? O4 C15 C14 122.40(13) . . ? O3 C15 C14 114.79(12) . . ? H3A C3 H3B 108.0 . . ? C4 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C2 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? C2 C3 C4 111.23(12) . . ? C3 C4 H4A 108.7 . . ? C3 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C5 C4 C3 114.06(12) . . ? C5 C4 H4A 108.7 . . ? C5 C4 H4B 108.7 . . ? C1 C2 C3 115.11(12) . . ? C1 C2 H2A 108.5 . . ? C1 C2 H2B 108.5 . . ? C3 C2 H2A 108.5 . . ? C3 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? H13A C13 H13B 108.0 . . ? C12 C13 H13A 109.4 . . ? C12 C13 H13B 109.4 . . ? C14 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? C14 C13 C12 111.31(11) . . ? C13 C12 H12A 108.8 . . ? C13 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C11 C12 C13 113.59(12) . . ? C11 C12 H12A 108.8 . . ? C11 C12 H12B 108.8 . . ? C4 C5 H5A 109.0 . . ? C4 C5 H5B 109.0 . . ? C4 C5 C6 112.92(12) . . ? H5A C5 H5B 107.8 . . ? C6 C5 H5A 109.0 . . ? C6 C5 H5B 109.0 . . ? C12 C11 H11A 109.0 . . ? C12 C11 H11B 109.0 . . ? C12 C11 C10 113.09(12) . . ? H11A C11 H11B 107.8 . . ? C10 C11 H11A 109.0 . . ? C10 C11 H11B 109.0 . . ? C5 C6 H6A 108.7 . . ? C5 C6 H6B 108.7 . . ? C5 C6 C7 114.26(12) . . ? H6A C6 H6B 107.6 . . ? C7 C6 H6A 108.7 . . ? C7 C6 H6B 108.7 . . ? C11 C10 H10A 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C9 C10 C11 113.96(12) . . ? C9 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? C10 C9 H9A 108.9 . . ? C10 C9 H9B 108.9 . . ? C10 C9 C8 113.40(12) . . ? H9A C9 H9B 107.7 . . ? C8 C9 H9A 108.9 . . ? C8 C9 H9B 108.9 . . ? C9 C8 H8A 108.7 . . ? C9 C8 H8B 108.7 . . ? C9 C8 C7 114.09(12) . . ? H8A C8 H8B 107.6 . . ? C7 C8 H8A 108.7 . . ? C7 C8 H8B 108.7 . . ? C15 C14 C13 116.31(12) . . ? C15 C14 H14A 108.2 . . ? C15 C14 H14B 108.2 . . ? C13 C14 H14A 108.2 . . ? C13 C14 H14B 108.2 . . ? H14A C14 H14B 107.4 . . ? C6 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? C8 C7 C6 113.08(12) . . ? C8 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? 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 O4 C15 1.2201(15) . ? O2 C1 1.3141(16) . ? O2 H2 0.94(2) . ? O3 C15 1.3034(17) . ? O3 H3 0.96(2) . ? O1 C1 1.2094(17) . ? C1 C2 1.4899(17) . ? C15 C14 1.4946(18) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.5195(17) . ? C3 C2 1.5155(18) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.5162(18) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C12 1.5195(17) . ? C13 C14 1.5151(18) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C11 1.5160(18) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.5171(18) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C10 1.5172(18) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C7 1.5190(18) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C9 1.5156(18) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C8 1.5167(18) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C7 1.5185(18) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? 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 O4 C15 C14 C13 144.35(14) . . . . ? O2 C1 C2 C3 178.98(11) . . . . ? O3 C15 C14 C13 -37.86(18) . . . . ? O1 C1 C2 C3 -1.2(2) . . . . ? C3 C4 C5 C6 177.33(11) . . . . ? C4 C3 C2 C1 174.72(11) . . . . ? C4 C5 C6 C7 -179.32(11) . . . . ? C2 C3 C4 C5 179.90(11) . . . . ? C13 C12 C11 C10 179.63(12) . . . . ? C12 C13 C14 C15 177.90(12) . . . . ? C12 C11 C10 C9 176.28(12) . . . . ? C5 C6 C7 C8 179.47(11) . . . . ? C11 C10 C9 C8 179.33(12) . . . . ? C10 C9 C8 C7 178.71(12) . . . . ? C9 C8 C7 C6 179.27(12) . . . . ? C14 C13 C12 C11 170.70(12) . . . . ?