#------------------------------------------------------------------------------ #$Date: 2020-03-26 08:04:52 +0200 (Thu, 26 Mar 2020) $ #$Revision: 249730 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/76/1557660.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_1557660 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_coeditor_code LQ5027 _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 'C13 H24 O4' _chemical_formula_sum 'C13 H24 O4' _chemical_formula_weight 244.32 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-11-28 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; ???? ; _cell_angle_alpha 90 _cell_angle_beta 90.84(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.5195(11) _cell_length_b 9.4058(19) _cell_length_c 26.283(5) _cell_measurement_reflns_used 3205 _cell_measurement_temperature 113(2) _cell_measurement_theta_max 27.8784 _cell_measurement_theta_min 2.6632 _cell_volume 1364.3(5) _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _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 113.15 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Rigaku Saturn 70 CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_unetI/netI 0.0415 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.988 _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 34 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 12368 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.867 _diffrn_reflns_theta_min 1.550 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7635 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details CrystalClear(Rigaku,2008) _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.189 _exptl_crystal_description prism _exptl_crystal_F_000 536 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.473 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.154 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 156 _refine_ls_number_reflns 3215 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0573 _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^)+(0.1658P)^2^+0.1380P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1826 _refine_ls_wR_factor_ref 0.2351 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2511 _reflns_number_total 3215 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lq5027.cif _cod_data_source_block DA13 _cod_database_code 1557660 _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 0.987 _shelx_estimated_absorpt_t_min 0.983 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All O(H) groups 2. Rigid bond restraints O4, C13 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 3.a Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6B,H6A), C7(H7B,H7A), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B) 3.b Idealised tetrahedral OH refined as rotating group: O2(H2), O3(H3) ; _shelx_res_file ; TITL R20181010E1 in P2(1)/n r20181010e1.res created by SHELXL-2018/3 at 15:42:17 on 28-Nov-2019 CELL 0.71073 5.5195 9.4058 26.2825 90 90.842 90 ZERR 4 0.0011 0.0019 0.0053 0 0.03 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O UNIT 52 96 16 EQIV $1 -2-X,1-Y,-Z EQIV $2 3-X,1-Y,1-Z EQIV $3 1.5+X,0.5-Y,0.5+Z DELU 0.001 0.001 O4 C13 L.S. 4 PLAN 20 SIZE 0.2 0.18 0.15 TEMP -160 HTAB C12 O1_$3 HTAB O3 O4_$2 HTAB O2 O1_$1 BOND $h HTAB fmap 2 acta REM REM REM WGHT 0.165800 0.138000 FVAR 0.87549 O1 3 -0.754038 0.403210 -0.002969 11.00000 0.02649 0.04133 = 0.02236 -0.00636 -0.00928 0.00808 O2 3 -0.885295 0.517349 0.065903 11.00000 0.02880 0.04926 = 0.02277 -0.00372 -0.00891 0.01572 AFIX 147 H2 2 -0.991731 0.545969 0.045153 11.00000 -1.50000 AFIX 0 O3 3 1.370000 0.326623 0.487535 11.00000 0.02890 0.02862 = 0.03590 0.00327 -0.01830 -0.00215 AFIX 147 H3 2 1.482105 0.370864 0.502601 11.00000 -1.50000 AFIX 0 O4 3 1.271305 0.545640 0.461267 11.00000 0.03082 0.02600 = 0.03583 0.00163 -0.01737 -0.00163 C1 1 -0.737996 0.428930 0.042789 11.00000 0.01886 0.02579 = 0.02170 -0.00183 -0.00702 -0.00141 C2 1 -0.552894 0.358290 0.076871 11.00000 0.02877 0.02835 = 0.02699 -0.00277 -0.01393 0.00532 AFIX 23 H2A 2 -0.417595 0.325409 0.055535 11.00000 -1.20000 H2B 2 -0.628122 0.272900 0.091985 11.00000 -1.20000 AFIX 0 C3 1 -0.447041 0.449108 0.120146 11.00000 0.02330 0.02910 = 0.02073 -0.00190 -0.00781 0.00252 AFIX 23 H3A 2 -0.580141 0.484559 0.141570 11.00000 -1.20000 H3B 2 -0.362722 0.532376 0.105663 11.00000 -1.20000 AFIX 0 C4 1 -0.268346 0.363220 0.153152 11.00000 0.02303 0.03282 = 0.02265 0.00130 -0.00888 0.00028 AFIX 23 H4A 2 -0.359114 0.289610 0.171888 11.00000 -1.20000 H4B 2 -0.152816 0.313995 0.130705 11.00000 -1.20000 AFIX 0 C5 1 -0.125808 0.454212 0.191391 11.00000 0.02078 0.03622 = 0.02191 -0.00068 -0.00876 0.00177 AFIX 23 H5A 2 -0.241032 0.504656 0.213565 11.00000 -1.20000 H5B 2 -0.032320 0.526722 0.172703 11.00000 -1.20000 AFIX 0 C6 1 0.049059 0.366221 0.224712 11.00000 0.02274 0.03545 = 0.02206 0.00240 -0.01042 -0.00051 AFIX 23 H6B 2 -0.046043 0.297876 0.244957 11.00000 -1.20000 H6A 2 0.156545 0.310728 0.202350 11.00000 -1.20000 AFIX 0 C7 1 0.205973 0.456222 0.261045 11.00000 0.02126 0.03442 = 0.02274 0.00084 -0.00935 0.00031 AFIX 23 H7B 2 0.303351 0.523648 0.240888 11.00000 -1.20000 H7A 2 0.099036 0.512546 0.283261 11.00000 -1.20000 AFIX 0 C8 1 0.376672 0.365965 0.294347 11.00000 0.02102 0.03475 = 0.02240 0.00070 -0.00889 -0.00140 AFIX 23 H8A 2 0.278403 0.300046 0.314937 11.00000 -1.20000 H8B 2 0.480025 0.307783 0.271988 11.00000 -1.20000 AFIX 0 C9 1 0.540077 0.453275 0.330178 11.00000 0.02023 0.03583 = 0.02271 0.00098 -0.00929 -0.00037 AFIX 23 H9A 2 0.639609 0.518871 0.309726 11.00000 -1.20000 H9B 2 0.437443 0.511539 0.352656 11.00000 -1.20000 AFIX 0 C10 1 0.707981 0.360150 0.363053 11.00000 0.01923 0.03246 = 0.02101 -0.00022 -0.00781 -0.00324 AFIX 23 H10A 2 0.607518 0.297945 0.384612 11.00000 -1.20000 H10B 2 0.803509 0.298157 0.340451 11.00000 -1.20000 AFIX 0 C11 1 0.882672 0.444184 0.397367 11.00000 0.01964 0.03009 = 0.02108 0.00132 -0.00765 -0.00205 AFIX 23 H11A 2 0.984986 0.506223 0.376134 11.00000 -1.20000 H11B 2 0.788803 0.505667 0.420448 11.00000 -1.20000 AFIX 0 C12 1 1.044805 0.344760 0.428932 11.00000 0.01940 0.02793 = 0.02180 0.00069 -0.00777 -0.00209 AFIX 23 H12A 2 0.941027 0.288683 0.451876 11.00000 -1.20000 H12B 2 1.124149 0.277187 0.405588 11.00000 -1.20000 AFIX 0 C13 1 1.237290 0.417058 0.460426 11.00000 0.01819 0.02993 = 0.01713 0.00079 -0.00376 -0.00030 HKLF 4 REM R20181010E1 in P2(1)/n REM wR2 = 0.2351, GooF = S = 1.024, Restrained GooF = 1.026 for all data REM R1 = 0.0573 for 2511 Fo > 4sig(Fo) and 0.0808 for all 3215 data REM 156 parameters refined using 1 restraints END WGHT 0.1532 0.1271 REM Instructions for potential hydrogen bonds HTAB O2 O1_$1 HTAB O3 O4_$2 HTAB C12 O1_$3 REM Highest difference peak 0.473, deepest hole -0.502, 1-sigma level 0.154 Q1 1 0.3256 0.4171 0.2706 11.00000 0.05 0.47 Q2 1 -0.0020 0.4066 0.2043 11.00000 0.05 0.47 Q3 1 0.4338 0.2417 0.2749 11.00000 0.05 0.40 Q4 1 0.6424 0.4121 0.3423 11.00000 0.05 0.40 Q5 1 -0.3834 0.4548 0.2290 11.00000 0.05 0.39 Q6 1 0.1556 0.4364 0.2387 11.00000 0.05 0.39 Q7 1 0.4631 0.4319 0.3157 11.00000 0.05 0.38 Q8 1 -0.2401 0.4200 0.1816 11.00000 0.05 0.38 Q9 1 0.1206 0.2433 0.2064 11.00000 0.05 0.37 Q10 1 0.1004 0.4227 0.2472 11.00000 0.05 0.36 Q11 1 0.8238 0.5281 0.2733 11.00000 0.05 0.35 Q12 1 0.2038 0.5602 0.2610 11.00000 0.05 0.35 Q13 1 0.3875 0.1817 0.2351 11.00000 0.05 0.34 Q14 1 -0.0487 0.2425 0.1981 11.00000 0.05 0.34 Q15 1 0.0976 0.6136 0.2938 11.00000 0.05 0.33 Q16 1 0.3784 0.3046 0.2309 11.00000 0.05 0.33 Q17 1 0.0078 0.5259 0.2854 11.00000 0.05 0.33 Q18 1 -0.0768 0.3867 0.2677 11.00000 0.05 0.32 Q19 1 0.2505 0.2463 0.2643 11.00000 0.05 0.32 Q20 1 0.8138 0.5994 0.3099 11.00000 0.05 0.32 ; _shelx_res_checksum 36743 _shelx_hkl_file ; 0 0 2 -0.15 0.14 0 0 -3 -0.36 0.92 0 0 3 -1.14 0.98 0 0 3 -0.25 0.30 0 0 -4 1146.11 26.17 0 0 4 1076.35 24.53 0 0 4 1241.23 27.54 0 0 -5 1.40 1.75 0 0 5 0.73 1.99 0 0 5 0.65 0.47 0 0 -6 38.59 3.33 0 0 6 36.29 3.20 0 0 6 35.77 2.41 0 0 -7 0.16 2.52 0 0 7 0.82 3.00 0 0 7 -0.09 0.62 0 0 -8 68.20 5.05 0 0 8 68.11 5.18 0 0 8 65.77 4.18 0 0 -9 -0.55 2.21 0 0 9 3.89 3.03 0 0 9 0.47 0.52 0 0 -10 101.25 6.96 0 0 10 89.14 6.50 0 0 10 89.10 5.62 0 0 -11 -0.56 1.91 0 0 11 9.69 3.86 0 0 11 0.82 0.69 0 0 -12 1.33 0.89 0 0 12 3.89 3.77 0 0 12 1.17 0.88 0 0 -13 -2.87 2.08 0 0 13 3.92 4.20 0 0 13 0.74 1.11 0 0 -14 342.02 11.33 0 0 14 317.90 10.65 0 0 -15 0.17 1.79 0 0 15 -0.92 3.77 0 0 -15 0.51 1.16 0 0 -16 220.14 15.23 0 0 16 241.25 11.02 0 0 -16 246.02 9.37 0 0 -17 -0.07 2.46 0 0 17 1.43 3.49 0 0 -17 -0.51 1.29 0 0 -18 104.99 10.55 0 0 18 102.49 13.23 0 0 -18 114.24 26.84 0 0 -19 2.12 2.23 0 0 19 -3.55 4.00 0 0 -19 1.03 0.56 0 0 -20 28.91 12.23 0 0 20 27.73 15.14 0 0 -20 33.70 2.37 0 0 -21 2.33 2.91 0 0 21 -1.31 3.77 0 0 -21 2.16 1.23 0 0 -22 28.94 5.35 0 0 22 22.65 4.50 0 0 -23 2.59 2.85 0 0 23 0.82 3.96 0 0 -24 91.65 6.90 0 0 24 96.60 15.64 0 0 25 -5.15 4.64 0 0 26 469.60 28.21 0 0 26 475.90 29.62 0 0 27 1.74 2.34 0 0 27 7.28 4.50 0 0 28 202.30 19.43 0 0 28 191.07 19.02 0 0 29 -2.02 3.44 0 0 29 2.32 5.26 0 0 30 225.41 23.33 0 0 30 199.64 21.50 0 0 31 -3.32 3.69 0 0 31 1.29 3.75 0 0 32 2.33 6.25 0 0 32 11.37 7.19 0 0 33 0.88 2.21 0 0 33 2.74 3.43 0 0 34 68.07 7.76 0 -1 0 -0.05 0.29 0 -1 0 -0.65 0.51 0 -1 0 0.21 0.24 0 -1 -1 -0.27 0.51 0 -1 -1 -0.26 0.29 0 -1 1 -1.21 0.78 0 -1 1 -1.09 0.44 0 -1 -1 -0.08 0.31 0 -1 2 13.41 1.25 0 -1 -3 0.63 1.53 0 1 -3 0.82 0.50 0 -1 3 2.15 2.10 0 1 3 0.61 0.46 0 -1 3 0.14 0.43 0 -1 -4 99.23 6.47 0 1 -4 96.25 5.89 0 -1 4 101.56 6.52 0 1 4 106.47 6.50 0 -1 4 108.53 6.64 0 1 -5 59.93 3.94 0 -1 -5 51.02 4.04 0 -1 5 60.09 8.14 0 1 5 55.15 3.69 0 -1 5 61.48 4.07 0 1 -6 53.26 4.56 0 -1 -6 46.47 4.02 0 -1 6 47.89 4.04 0 1 6 50.13 3.58 0 -1 6 45.97 3.08 0 -1 -7 68.93 5.31 0 1 -7 72.30 5.21 0 -1 7 72.86 5.23 0 1 7 69.39 5.04 0 -1 7 73.87 4.71 0 -1 -7 65.04 3.87 0 -1 -9 1.72 1.73 0 1 -9 4.87 1.29 0 -1 9 5.01 2.94 0 1 9 4.49 2.51 0 -1 9 4.72 1.07 0 -1 -9 2.56 0.61 0 1 -10 120.44 7.91 0 -1 -10 129.71 5.00 0 -1 10 114.87 7.93 0 1 10 105.02 7.18 0 -1 10 117.09 7.40 0 -1 -10 112.33 6.69 0 1 -11 216.77 6.83 0 -1 -11 219.04 7.87 0 -1 11 201.01 9.18 0 1 11 205.20 6.92 0 -1 11 223.31 6.30 0 -1 -11 194.92 5.16 0 -1 -12 294.53 10.92 0 1 -12 305.25 9.46 0 -1 12 265.57 8.84 0 1 12 281.77 9.61 0 -1 12 260.19 7.41 0 -1 -12 271.39 12.13 0 1 -13 579.17 15.99 0 -1 -13 535.00 15.65 0 -1 13 526.78 15.48 0 1 13 538.58 15.66 0 -1 13 502.87 13.24 0 -1 -13 520.92 13.31 0 1 -14 8.47 3.00 0 -1 -14 9.83 4.16 0 -1 14 12.90 13.64 0 1 14 8.63 3.84 0 -1 14 9.51 2.41 0 -1 -14 0.07 9.14 0 1 -15 1777.51 63.98 0 -1 -15 2069.31 75.05 0 -1 15 1868.14 67.92 0 1 15 1784.66 65.01 0 -1 15 1698.64 60.63 0 -1 -15 1827.20 64.58 0 -1 -16 239.63 10.73 0 1 -16 243.57 10.45 0 -1 16 267.73 14.31 0 1 16 243.38 12.04 0 -1 16 236.41 9.50 0 -1 -16 220.27 8.85 0 1 -17 482.49 14.51 0 -1 -17 457.24 14.49 0 -1 17 432.42 14.42 0 1 17 469.69 16.07 0 -1 17 429.33 12.72 0 -1 -17 443.35 11.52 0 -1 -18 136.69 6.56 0 1 -18 152.31 7.15 0 -1 18 134.66 7.45 0 1 18 141.55 8.83 0 -1 18 124.33 4.86 0 -1 -18 135.35 4.50 0 1 -19 36.75 3.83 0 -1 -19 38.25 9.89 0 -1 19 31.48 5.03 0 1 19 39.05 6.27 0 -1 -19 42.03 1.67 0 -1 -20 116.58 15.10 0 1 -20 105.86 6.60 0 -1 20 113.91 7.00 0 1 20 107.03 7.45 0 1 -20 105.13 4.01 0 1 -21 14.79 3.75 0 -1 -21 7.66 3.22 0 -1 21 20.40 6.61 0 1 21 8.67 5.14 0 1 -21 12.77 2.30 0 1 -22 96.84 6.83 0 -1 -22 81.04 6.59 0 -1 22 78.13 6.53 0 1 22 79.11 6.59 0 1 -22 88.10 5.00 0 -1 -23 31.43 4.87 0 -1 23 23.25 4.87 0 1 23 38.85 17.48 0 1 -23 25.67 7.40 0 -1 -24 58.73 4.94 0 -1 24 62.92 3.93 0 1 24 71.52 6.32 0 -1 24 69.13 7.31 0 -1 -25 4.85 3.78 0 -1 25 7.50 3.27 0 -1 25 6.34 5.35 0 1 25 4.40 4.99 0 -1 26 12.96 3.06 0 1 26 13.55 4.80 0 -1 26 8.51 5.81 0 1 27 186.61 12.41 0 -1 27 199.27 12.60 0 1 27 226.77 15.96 0 -1 27 218.60 29.37 0 1 28 162.11 15.96 0 -1 28 161.74 15.71 0 -1 28 173.25 17.47 0 1 28 161.51 17.14 0 -1 29 443.11 17.16 0 1 29 445.40 17.89 0 -1 29 445.26 20.27 0 1 29 424.16 19.18 0 1 30 164.84 17.45 0 -1 30 154.37 17.61 0 1 30 170.72 19.47 0 1 31 82.34 7.30 0 -1 31 79.72 13.41 0 1 31 70.10 7.72 0 1 32 11.28 11.34 0 -1 32 10.10 12.36 0 1 32 35.47 5.87 0 1 33 26.39 14.27 0 -1 33 59.47 7.44 0 1 33 79.93 8.09 0 1 34 3.69 5.05 0 1 34 2.20 7.08 0 -1 34 4.96 5.00 0 -2 -2 150.59 4.98 0 2 -2 139.58 1.25 0 -2 -2 138.69 3.29 0 -2 2 133.64 2.77 0 -2 -2 144.16 8.88 0 -2 2 131.75 2.56 0 -2 -3 1114.65 26.05 0 -2 3 1030.03 23.70 0 2 3 1064.47 23.96 0 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8.01 0 -2 16 73.82 6.58 0 -2 -16 75.44 5.98 0 -2 -17 19.93 5.43 0 -2 17 6.73 4.43 0 -2 17 1.91 0.96 0 -2 -18 62.21 17.33 0 2 -18 68.12 4.76 0 -2 18 94.34 9.31 0 2 18 67.36 6.48 0 -2 18 66.76 4.31 0 -2 -19 4.25 2.37 0 2 -19 3.99 2.21 0 -2 19 2.31 3.53 0 2 19 4.84 4.10 0 -2 19 1.05 1.73 0 -2 -20 34.61 9.71 0 -2 20 36.59 13.39 0 2 20 27.43 5.28 0 -2 20 26.43 8.83 0 -2 -21 7.42 3.74 0 -2 21 5.02 2.30 0 -2 21 3.77 4.55 0 2 21 -1.16 3.77 0 -2 21 2.99 1.73 0 -2 -22 16.28 5.13 0 -2 22 13.38 4.20 0 -2 22 12.53 2.80 0 2 22 13.47 3.78 0 -2 22 10.87 3.43 0 -2 -23 17.62 4.46 0 -2 23 15.19 3.37 0 -2 23 4.94 2.49 0 2 23 12.09 4.10 0 2 -23 16.22 2.45 0 -2 -24 43.02 7.87 0 -2 24 30.71 4.39 0 -2 24 23.06 6.36 0 2 24 17.68 5.60 0 2 -24 24.99 8.77 0 -2 -25 17.64 5.34 0 -2 25 9.79 6.58 0 -2 25 21.23 4.91 0 2 25 23.00 9.58 0 2 -25 11.19 2.07 0 -2 26 91.89 9.52 0 2 26 95.09 8.29 0 2 27 31.29 4.42 0 -2 27 22.83 7.75 0 2 27 23.73 7.03 0 2 28 17.95 6.46 0 -2 28 29.37 5.25 0 2 28 28.44 8.67 0 2 29 22.55 5.33 0 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2 -8 156.98 12.34 -2 -2 8 169.53 4.55 -2 2 8 177.52 4.87 -2 -2 8 174.81 4.60 -2 2 8 160.09 11.74 2 -2 -7 481.85 15.87 2 2 -7 488.96 14.11 -2 -2 7 493.21 13.46 -2 2 7 516.67 14.30 -2 -2 7 479.06 14.52 -2 2 7 506.16 12.92 2 -2 -6 7.64 3.66 2 2 -6 11.63 3.89 -2 -2 6 7.08 2.84 -2 2 6 8.22 4.01 -2 -2 6 9.43 1.86 -2 2 6 8.87 2.62 2 -2 -5 17.01 4.05 2 2 -5 19.29 2.72 2 -2 -5 26.00 4.11 -2 -2 5 15.38 4.40 -2 -2 5 16.54 2.17 -2 2 5 15.99 1.71 2 -2 -4 4.03 3.36 2 2 -4 -1.05 2.28 2 -2 -4 2.33 2.00 -2 -2 4 0.04 0.56 -2 -2 4 2.25 1.85 -2 2 4 1.26 1.46 2 -2 -3 7.21 3.13 2 2 -3 -0.14 2.35 2 -2 -3 5.08 2.93 -2 -2 3 1.84 0.98 -2 -2 3 2.19 1.75 -2 2 3 2.23 1.36 2 -2 -2 41.49 14.77 2 2 -2 42.63 3.71 2 -2 -2 59.91 5.47 -2 -2 2 45.65 3.46 -2 -2 2 50.66 3.96 -2 2 2 45.36 4.65 2 -2 -1 0.41 2.44 2 2 -1 1.67 2.23 2 -2 -1 0.57 1.76 -2 -2 1 1.01 0.80 -2 -2 1 1.21 1.67 -2 2 1 -0.06 1.74 2 -2 0 502.12 16.64 2 2 0 533.29 14.07 2 -2 0 520.90 14.09 -2 -2 0 548.26 12.66 -2 -2 0 547.44 14.91 -2 2 0 579.12 13.99 2 -2 1 22.01 2.92 2 2 1 18.34 3.00 2 -2 1 24.82 6.30 -2 -2 -1 22.30 1.59 -2 -2 -1 25.20 2.26 -2 2 -1 21.29 2.22 2 -2 2 1994.59 46.05 2 2 2 1715.73 40.07 2 2 2 1914.31 42.69 2 -2 2 1943.54 45.36 -2 -2 -2 1858.97 42.09 -2 2 -2 1917.30 43.43 2 -2 3 43.40 4.77 2 2 3 42.44 12.45 2 2 3 38.98 4.16 2 -2 3 34.27 3.79 -2 -2 -3 32.78 2.76 -2 2 -3 37.40 3.23 2 -2 5 2299.81 56.73 2 2 5 2428.33 58.33 -2 -2 -5 2329.32 56.12 -2 2 -5 2324.97 61.84 2 -2 6 1811.05 44.66 2 2 6 1788.29 44.70 2 2 6 1953.19 47.11 2 -2 6 1861.16 46.60 -2 -2 -6 1874.24 45.35 -2 2 -6 1871.73 45.58 2 -2 7 1.79 1.83 2 2 7 1.28 1.59 2 -2 7 0.64 2.97 2 2 7 1.08 0.68 -2 -2 -7 1.73 1.12 -2 2 -7 -0.04 2.57 2 -2 8 467.84 13.09 2 2 8 462.26 13.75 2 -2 8 473.50 14.36 2 2 8 432.52 11.63 -2 -2 -8 409.32 10.82 -2 2 -8 403.87 11.14 2 -2 9 43.65 7.38 2 2 9 49.43 5.04 2 -2 9 36.63 4.46 2 2 9 49.40 6.07 -2 -2 -9 42.86 4.73 -2 2 -9 43.03 6.04 2 -2 10 488.35 21.73 2 2 10 508.58 20.12 2 -2 10 475.49 19.08 2 2 10 516.19 20.75 -2 -2 -10 472.81 17.40 -2 2 -10 449.62 17.54 2 -2 11 31.22 6.92 2 2 11 33.13 5.81 2 -2 11 38.90 10.71 2 2 11 38.94 3.61 -2 -2 -11 39.61 3.90 -2 2 -11 34.55 5.14 2 -2 12 493.36 19.25 2 2 12 500.70 19.93 2 -2 12 477.50 19.43 2 2 12 515.96 19.61 -2 -2 -12 497.95 18.39 -2 2 -12 459.81 17.33 2 -2 13 15.33 4.63 2 2 13 7.04 3.88 2 -2 13 12.67 4.24 2 2 13 9.93 4.11 -2 -2 -13 10.19 3.75 -2 2 -13 11.53 4.10 2 -2 14 288.37 9.60 2 2 14 266.19 9.58 2 -2 14 283.48 10.91 2 2 14 299.96 9.72 -2 -2 -14 278.21 8.16 -2 2 -14 272.93 8.66 2 -2 15 4.57 2.24 2 2 15 9.34 2.57 2 -2 15 4.01 4.28 2 2 15 4.76 2.69 -2 -2 -15 1.63 1.21 -2 2 -15 2.85 2.78 2 -2 16 81.29 5.46 2 2 16 67.15 5.39 2 -2 16 72.62 6.18 2 2 16 81.51 5.54 -2 -2 -16 76.01 4.24 -2 2 -16 74.95 4.84 2 -2 17 34.64 9.00 2 2 17 33.93 9.39 2 -2 17 35.71 11.54 2 2 17 34.14 3.71 -2 -2 -17 34.81 2.58 -2 2 -17 37.17 3.25 2 -2 18 83.44 6.12 2 2 18 75.63 14.62 2 -2 18 69.54 9.15 2 2 18 70.15 9.52 -2 -2 -18 44.76 12.38 -2 2 -18 66.16 19.05 2 -2 19 1818.65 76.44 2 2 19 1871.92 79.20 2 -2 19 1859.12 78.77 2 2 19 1949.46 81.79 -2 -2 -19 1960.09 81.09 -2 2 -19 1831.10 76.37 2 -2 20 265.64 8.39 2 2 20 273.54 16.93 2 -2 20 272.18 9.85 2 2 20 219.10 9.60 2 -2 21 34.20 12.63 2 2 21 44.45 4.89 2 -2 21 33.28 17.97 2 2 21 30.93 17.66 -2 2 -21 42.41 3.02 2 -2 22 34.83 6.17 2 2 22 24.81 4.93 2 -2 22 19.81 11.13 2 2 22 19.00 7.25 -2 2 -22 23.76 6.89 2 -2 23 42.32 10.08 2 2 23 45.88 5.54 2 -2 23 39.93 20.23 2 2 23 55.02 5.79 -2 2 -23 37.87 2.71 2 -2 24 2.75 2.81 2 2 24 9.51 5.14 2 -2 24 -2.73 4.10 2 2 24 2.95 3.29 -2 2 -24 2.70 2.30 2 2 25 44.14 5.49 2 -2 25 31.88 15.36 2 2 25 48.55 5.19 -2 2 -25 31.31 9.64 2 2 26 3.83 4.15 2 -2 26 0.98 3.17 2 2 26 0.62 3.04 -2 2 -26 2.59 2.30 2 2 27 28.65 9.70 2 -2 27 18.61 12.10 2 2 27 27.67 7.26 2 2 28 -2.55 3.64 2 -2 28 1.90 2.71 2 2 28 3.05 2.43 2 2 29 13.96 5.99 2 -2 29 7.96 6.11 2 2 29 11.85 6.31 2 2 30 6.51 4.78 2 -2 30 -0.15 4.54 2 2 30 8.91 3.80 2 2 31 0.15 3.13 2 -2 31 5.14 5.36 2 2 31 1.36 3.58 2 2 32 1.82 2.70 2 -2 32 0.08 5.36 2 2 32 -0.23 3.39 2 -3 -32 -1.23 4.22 -2 -3 32 3.04 4.78 -2 3 32 0.62 4.86 2 -3 -31 6.15 5.93 -2 -3 31 6.69 5.28 -2 3 31 11.29 5.00 2 -3 -30 13.94 8.47 -2 -3 30 20.15 11.79 -2 3 30 14.37 5.43 2 -3 -29 3.76 4.37 -2 -3 29 4.61 5.40 -2 3 29 -3.69 4.72 2 -3 -28 9.83 6.41 -2 -3 28 4.71 4.80 -2 3 28 9.99 5.24 2 -3 -27 9.12 5.86 -2 -3 27 10.93 7.23 -2 3 27 16.50 7.84 2 -3 -26 0.81 5.65 -2 -3 26 5.69 5.47 -2 3 26 -3.24 4.72 2 -3 -25 242.28 24.83 -2 -3 25 214.20 21.23 -2 3 25 221.73 21.45 -2 -3 25 243.34 22.25 2 -3 -24 17.91 7.82 -2 -3 24 19.57 10.17 -2 3 24 39.52 14.22 -2 -3 24 -1.15 1.95 2 -3 -23 258.68 18.92 -2 -3 23 235.58 17.09 -2 3 23 239.70 16.24 -2 -3 23 246.58 16.63 2 -3 -22 2.36 5.38 -2 -3 22 -0.71 4.96 -2 3 22 3.05 2.43 -2 -3 22 2.31 1.71 2 -3 -21 108.94 10.90 2 3 -21 104.33 9.13 -2 -3 21 111.51 8.66 -2 3 21 104.22 7.89 -2 -3 21 103.32 12.01 2 -3 -20 51.76 9.82 2 3 -20 52.46 4.79 -2 -3 20 53.58 20.55 -2 3 20 51.54 5.11 -2 -3 20 52.16 2.99 2 -3 -19 280.72 13.15 2 3 -19 275.18 10.32 -2 -3 19 258.91 9.77 -2 3 19 273.79 8.89 -2 -3 19 289.00 7.90 2 -3 -18 131.67 12.76 2 3 -18 100.65 7.03 -2 -3 18 90.17 6.97 -2 3 18 121.05 17.33 -2 -3 18 107.45 6.01 2 -3 -17 179.89 13.12 2 3 -17 185.04 10.47 -2 -3 17 177.47 10.49 -2 3 17 184.09 9.85 -2 -3 17 176.00 9.03 2 -3 -16 60.87 8.79 2 3 -16 71.39 10.44 -2 -3 16 69.47 5.59 -2 3 16 53.95 4.55 -2 -3 16 61.99 5.39 2 -3 -15 30.68 6.64 2 3 -15 46.90 5.11 -2 -3 15 39.14 4.94 -2 3 15 40.34 3.75 -2 -3 15 38.88 4.19 2 -3 -14 8.03 6.64 2 3 -14 -0.06 2.85 -2 -3 14 0.69 4.25 -2 3 14 2.34 2.12 -2 -3 14 3.85 2.01 2 -3 -13 7.97 6.21 2 3 -13 2.60 2.44 -2 -3 13 -0.98 3.64 -2 3 13 3.19 2.76 -2 -3 13 0.45 1.38 -2 3 13 1.49 0.76 2 -3 -12 40.79 6.57 2 3 -12 32.64 4.48 -2 -3 12 45.15 6.15 -2 3 12 37.97 14.44 -2 -3 12 43.74 4.25 -2 3 12 41.26 3.53 2 -3 -11 2.78 5.06 2 3 -11 6.49 3.88 -2 -3 11 8.66 5.06 -2 3 11 4.22 1.66 -2 -3 11 3.25 2.19 -2 3 11 5.76 1.88 2 -3 -10 1531.75 58.18 2 3 -10 1420.00 51.78 -2 -3 10 1417.17 51.75 -2 3 10 1380.01 50.27 -2 -3 10 1447.30 52.10 -2 3 10 1377.82 49.01 2 3 -9 53.07 5.75 -2 -3 9 52.39 7.18 -2 3 9 65.30 5.93 -2 -3 9 62.04 9.72 -2 3 9 66.63 5.24 2 -3 -8 1567.58 59.34 2 3 -8 1638.73 59.30 -2 -3 8 1730.33 62.34 -2 3 8 1640.05 59.21 -2 -3 8 1565.25 56.75 -2 3 8 1657.06 59.06 2 -3 -7 49.54 17.16 2 3 -7 49.28 13.24 -2 3 7 44.25 4.33 -2 -3 7 48.16 4.39 -2 3 7 45.53 3.85 2 -3 -6 277.78 10.82 2 3 -6 268.88 9.09 -2 -3 6 260.63 7.80 -2 3 6 261.17 7.21 2 -3 -5 327.80 12.68 2 3 -5 330.06 10.32 2 -3 -5 316.26 11.21 -2 -3 5 297.50 8.59 -2 -3 5 306.32 9.00 -2 3 5 311.18 8.44 2 -3 -4 69.52 6.59 2 3 -4 65.35 5.94 2 -3 -4 65.17 6.88 -2 -3 4 61.16 4.99 -2 -3 4 65.31 5.44 -2 3 4 53.28 4.33 2 -3 -3 506.36 15.65 2 3 -3 434.27 12.63 2 -3 -3 429.15 13.31 -2 -3 3 483.57 12.58 -2 -3 3 476.39 12.87 -2 3 3 467.86 12.37 2 -3 -2 5.61 2.50 2 3 -2 3.82 1.98 2 -3 -2 1.13 0.80 -2 -3 2 -1.60 1.40 -2 -3 2 1.02 2.06 2 -3 -1 285.12 9.41 2 3 -1 328.85 14.88 2 -3 -1 309.70 10.54 -2 -3 1 310.17 8.10 -2 -3 1 314.42 10.05 -2 3 1 322.07 8.94 2 -3 0 11.84 2.32 2 3 0 13.70 2.39 2 -3 0 15.80 4.30 -2 -3 0 6.71 0.84 -2 -3 0 14.34 4.08 -2 3 0 14.86 4.20 2 -3 1 104.46 8.58 2 3 1 119.24 9.74 2 -3 1 90.92 8.87 -2 -3 -1 90.83 6.59 -2 -3 -1 105.65 8.25 -2 3 -1 100.56 7.77 2 -3 2 2.96 2.54 2 3 2 3.88 2.80 2 -3 2 2.79 1.40 -2 -3 -2 3.83 2.33 -2 3 -2 5.72 3.44 2 -3 3 85.04 6.94 2 3 3 88.19 7.50 2 -3 3 103.31 8.76 -2 -3 -3 88.68 7.02 -2 3 -3 94.99 7.48 2 -3 4 38.35 3.65 2 3 4 39.36 4.71 2 -3 4 40.87 4.43 -2 -3 -4 39.09 5.79 -2 3 -4 33.97 3.41 2 -3 5 411.24 11.76 2 3 5 395.98 12.02 2 3 5 396.09 9.76 2 -3 5 378.93 12.09 -2 -3 -5 400.74 10.87 -2 3 -5 384.50 10.71 2 -3 6 8.40 2.25 2 3 6 5.47 3.75 2 3 6 4.69 1.81 2 -3 6 4.21 4.16 -2 -3 -6 6.55 1.98 -2 3 -6 4.85 1.51 2 -3 7 26.19 9.26 2 3 7 24.57 6.95 2 -3 7 23.12 5.37 2 3 7 24.67 3.00 -2 -3 -7 26.31 2.45 -2 3 -7 25.55 7.11 2 -3 8 11.25 3.15 2 3 8 14.43 4.22 2 -3 8 7.27 2.25 2 3 8 6.40 2.94 -2 -3 -8 8.25 2.55 -2 3 -8 7.36 2.12 2 -3 9 21.17 6.62 2 3 9 23.31 7.62 2 -3 9 25.42 5.33 2 3 9 21.49 2.17 -2 -3 -9 21.52 2.32 -2 3 -9 15.44 2.43 2 -3 10 9.98 3.39 2 3 10 13.68 2.97 2 3 10 14.09 2.21 -2 -3 -10 13.64 4.22 -2 3 -10 11.68 2.19 2 -3 11 9.30 2.75 2 3 11 9.09 3.48 2 -3 11 7.77 4.07 2 3 11 3.55 1.46 -2 -3 -11 4.22 2.82 -2 3 -11 8.06 2.91 2 -3 12 6.56 3.49 2 3 12 5.62 4.20 2 -3 12 5.22 3.76 2 3 12 3.72 1.50 -2 -3 -12 6.25 1.21 -2 3 -12 5.26 3.01 2 -3 13 16.44 6.30 2 3 13 20.85 5.63 2 -3 13 26.51 6.33 2 3 13 17.58 5.55 -2 -3 -13 16.60 1.48 -2 3 -13 16.65 2.85 2 -3 14 1.30 1.73 2 3 14 -0.38 4.33 2 -3 14 -0.26 3.76 2 3 14 2.08 1.68 -2 -3 -14 0.85 1.13 -2 3 -14 0.92 2.61 2 -3 15 74.20 3.99 2 3 15 79.10 6.68 2 -3 15 65.46 4.77 2 3 15 73.22 3.72 -2 -3 -15 65.26 2.40 -2 3 -15 72.30 3.83 2 -3 16 29.83 9.30 2 3 16 35.59 5.33 2 -3 16 28.31 8.47 2 3 16 34.23 3.01 -2 -3 -16 30.66 2.50 -2 3 -16 31.07 3.26 2 -3 17 128.17 7.08 2 3 17 145.47 9.10 2 -3 17 152.14 9.26 2 3 17 128.95 6.89 -2 -3 -17 133.52 6.34 -2 3 -17 147.23 7.73 2 -3 18 375.86 17.24 2 3 18 419.33 20.13 2 -3 18 408.59 20.03 2 3 18 385.63 17.56 -2 3 -18 380.89 17.27 2 -3 19 160.41 6.14 2 3 19 150.27 10.38 2 -3 19 165.89 7.89 2 3 19 141.66 5.60 -2 3 -19 163.92 5.94 2 -3 20 89.97 6.05 2 3 20 105.80 8.07 2 -3 20 86.45 7.60 2 3 20 101.49 6.84 -2 3 -20 99.26 6.94 2 3 21 99.35 8.90 2 -3 21 111.65 9.76 2 3 21 96.28 7.37 -2 3 -21 97.29 7.20 2 3 22 65.09 21.63 2 -3 22 67.11 5.99 2 3 22 66.56 9.26 -2 3 -22 64.72 7.70 2 3 23 8.07 4.95 2 -3 23 6.59 3.13 2 3 23 11.53 5.02 -2 3 -23 14.16 3.67 2 3 24 53.96 6.23 2 -3 24 58.40 20.14 2 3 24 61.20 5.49 -2 3 -24 46.40 3.96 2 3 25 13.79 5.13 2 -3 25 2.35 4.25 2 3 25 2.51 3.01 -2 3 -25 4.22 2.83 2 3 26 11.93 5.20 2 -3 26 4.89 4.87 2 3 26 4.33 3.57 -2 3 -26 7.70 2.43 2 3 27 6.94 4.80 2 -3 27 0.93 3.82 -2 3 -27 9.15 3.92 2 3 28 5.74 4.41 2 -3 28 2.32 5.23 -2 3 -28 2.37 1.87 2 3 29 2.36 3.67 2 -3 29 -3.36 4.19 2 3 30 12.37 9.48 2 -3 30 6.35 4.25 2 3 31 0.92 5.33 2 -3 31 4.05 4.00 2 -4 -31 5.99 4.23 -2 -4 31 11.95 8.85 -2 4 31 16.27 6.96 2 -4 -30 1.43 7.21 -2 -4 30 7.04 4.06 -2 4 30 12.52 5.89 2 -4 -29 15.53 11.71 -2 -4 29 13.68 9.41 -2 4 29 10.86 5.53 2 -4 -28 4.22 3.08 -2 -4 28 1.40 3.71 -2 4 28 -3.48 5.06 2 -4 -27 10.20 9.94 -2 -4 27 14.71 5.25 -2 4 27 6.53 5.22 2 -4 -26 66.42 10.16 -2 -4 26 40.12 6.59 -2 4 26 71.03 10.47 -2 -4 26 63.00 7.31 2 -4 -25 45.89 24.15 -2 -4 25 45.08 8.63 -2 4 25 39.42 16.63 -2 -4 25 41.92 9.42 2 -4 -24 12.19 6.47 -2 -4 24 4.24 5.40 -2 4 24 -1.01 4.41 -2 -4 24 2.00 1.71 2 -4 -23 -7.62 5.81 -2 -4 23 5.09 4.90 -2 4 23 3.65 4.06 -2 -4 23 -0.57 2.36 2 -4 -22 -1.02 6.28 -2 -4 22 1.12 4.66 -2 4 22 -2.73 4.17 -2 -4 22 1.99 2.54 2 -4 -21 78.29 11.40 -2 -4 21 59.01 8.42 -2 4 21 50.63 17.47 -2 -4 21 61.03 7.56 2 -4 -20 161.09 14.14 -2 -4 20 146.47 11.30 -2 4 20 160.27 12.13 -2 -4 20 173.67 11.94 2 -4 -19 18.49 7.22 -2 -4 19 35.82 12.53 -2 4 19 35.48 12.80 -2 -4 19 26.51 8.97 2 -4 -18 99.27 8.05 -2 -4 18 130.94 6.93 -2 4 18 130.71 11.69 -2 -4 18 135.26 5.52 2 -4 -17 24.68 6.26 -2 -4 17 13.29 3.22 -2 4 17 16.10 3.88 -2 -4 17 10.74 2.19 2 -4 -16 19.80 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2.39 -2 -4 7 13.73 4.62 -2 4 7 11.29 2.67 -2 -4 7 15.57 2.40 -2 4 7 18.38 5.34 2 -4 -6 577.56 23.78 2 4 -6 550.11 20.98 2 -4 -6 568.32 22.44 -2 -4 6 566.77 21.16 -2 -4 6 568.94 21.54 -2 4 6 570.60 21.23 2 -4 -5 80.65 9.03 2 4 -5 80.55 6.86 2 -4 -5 78.39 7.37 -2 -4 5 85.72 7.02 -2 -4 5 80.81 9.20 -2 4 5 91.91 7.21 2 -4 -4 452.54 18.97 2 4 -4 464.82 18.19 2 -4 -4 461.37 18.94 -2 -4 4 456.38 16.98 -2 -4 4 459.88 17.45 -2 4 4 480.87 17.79 2 -4 -3 204.46 9.96 2 4 -3 209.33 9.06 2 -4 -3 206.74 10.27 -2 -4 3 221.11 8.56 -2 -4 3 197.42 8.29 -2 4 3 210.03 8.36 2 -4 -2 321.13 13.92 2 4 -2 321.08 13.12 2 -4 -2 353.67 15.55 -2 -4 2 317.02 11.70 -2 -4 2 308.24 13.72 -2 4 2 340.31 13.07 2 -4 -1 231.91 10.35 2 4 -1 213.77 9.43 2 -4 -1 249.41 11.77 -2 -4 1 243.92 8.95 -2 -4 1 230.62 10.13 -2 4 1 254.07 10.12 2 -4 0 92.80 7.93 2 4 0 86.83 7.71 2 -4 0 105.72 9.07 -2 -4 0 103.31 8.20 -2 4 0 96.08 7.82 2 -4 1 109.96 4.19 2 4 1 118.66 7.11 2 -4 1 107.17 9.15 -2 -4 -1 105.98 9.65 -2 4 -1 114.08 5.23 2 -4 2 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17.12 5.08 -6 6 5 10.03 5.83 -6 -6 5 16.56 8.72 6 -6 -4 14.10 6.09 6 6 -4 7.11 4.43 -6 -6 4 6.89 4.24 -6 6 4 2.62 1.92 6 -6 -3 0.09 4.89 6 6 -3 16.59 5.47 -6 -6 3 4.41 3.18 -6 6 3 4.48 3.31 6 -6 -2 13.41 6.99 6 6 -2 11.58 7.87 -6 -6 2 3.00 2.57 -6 6 2 3.32 3.30 6 -6 -1 4.33 5.29 6 6 -1 -3.03 4.13 -6 -6 1 1.71 1.85 -6 6 1 2.93 1.18 6 -6 0 16.92 5.54 6 6 0 22.44 9.19 -6 -6 0 24.74 13.98 -6 6 0 16.14 3.77 6 -6 1 16.37 5.24 6 6 1 16.19 6.17 -6 -6 -1 5.65 3.88 -6 6 -1 3.40 6.14 6 -6 2 165.82 13.64 6 6 2 110.59 9.31 -6 -6 -2 122.22 8.08 -6 6 -2 111.18 7.16 6 -6 3 27.56 7.22 6 6 3 8.23 5.44 -6 -6 -3 9.97 4.91 -6 6 -3 19.79 4.43 6 6 4 79.56 8.20 -6 -6 -4 94.87 6.81 -6 6 -4 97.63 7.55 6 6 5 22.84 8.69 -6 -6 -5 22.95 4.84 -6 6 -5 6.12 3.80 6 6 6 26.57 5.75 6 -6 6 24.48 13.15 -6 -6 -6 29.47 3.89 -6 6 -6 19.51 13.50 6 6 7 3.86 6.18 -6 -6 -7 4.34 3.62 -6 6 -7 5.00 3.18 6 6 8 10.24 6.32 6 -6 8 7.84 5.69 -6 -6 -8 -0.54 2.74 -6 6 -8 3.70 3.97 6 6 9 11.82 7.88 6 -6 9 6.71 5.92 -6 -6 -9 0.84 1.63 -6 6 -9 0.08 3.07 7 0 -9 64.96 8.46 -7 0 9 58.24 5.97 7 0 -8 5.22 6.33 -7 0 8 3.94 4.46 7 0 -7 217.55 17.10 -7 0 7 223.27 14.47 7 0 -6 1.28 6.92 -7 0 6 5.37 4.20 7 0 -5 3.65 7.12 -7 0 5 3.07 2.75 7 0 -4 8.87 7.89 -7 0 4 10.98 3.79 7 0 -3 17.43 12.23 -7 0 3 9.87 5.06 7 0 -2 1.47 7.18 -7 0 2 -0.79 3.42 7 0 -1 58.91 9.09 -7 0 1 41.74 4.77 7 0 0 7.97 4.10 -7 0 0 0.74 2.16 7 0 1 38.03 16.99 -7 0 -1 25.06 13.10 7 0 2 3.21 5.98 -7 0 -2 -1.89 2.93 7 0 3 22.94 7.23 -7 0 -3 17.53 4.36 7 0 4 2.19 6.76 -7 0 -4 2.75 3.32 7 0 5 31.48 6.96 -7 0 -5 46.82 9.21 7 0 6 12.37 6.70 -7 0 -6 -2.54 3.05 7 0 7 41.69 11.71 -7 0 -7 52.24 5.38 7 0 8 2.78 5.40 -7 0 -8 3.18 2.92 7 -1 -9 6.51 7.38 7 1 -9 0.29 6.37 -7 1 9 3.82 2.06 -7 1 9 1.70 2.82 -7 -1 9 -3.12 2.85 7 1 -8 7.64 6.57 7 -1 -8 17.37 8.71 -7 1 8 11.63 4.63 -7 -1 8 10.88 4.62 -7 1 8 6.56 4.01 7 1 -7 12.92 7.39 7 -1 -7 3.15 7.18 -7 1 7 6.06 3.83 -7 -1 7 3.44 3.92 -7 1 7 4.59 3.83 7 1 -6 60.88 20.30 7 -1 -6 44.12 9.08 -7 1 6 80.81 14.29 -7 -1 6 66.60 15.32 -7 1 6 65.33 6.13 7 -1 -5 124.17 13.72 7 1 -5 130.33 15.38 -7 1 5 128.73 8.51 -7 -1 5 115.82 15.87 -7 1 5 121.08 8.43 7 -1 -4 291.06 18.55 7 1 -4 303.27 18.55 -7 1 4 410.44 20.11 -7 -1 4 381.57 19.36 -7 1 4 363.20 19.01 7 -1 -3 52.18 18.11 7 1 -3 91.55 11.69 -7 1 3 59.78 5.33 -7 -1 3 79.96 6.91 -7 1 3 46.36 15.21 7 -1 -2 6.57 5.79 7 1 -2 22.03 12.95 -7 1 2 12.31 3.57 -7 -1 2 7.59 4.81 7 -1 -1 9.96 6.67 7 1 -1 3.62 5.40 -7 1 1 3.26 3.06 -7 -1 1 2.53 1.78 7 1 0 15.36 18.45 7 -1 0 25.29 9.56 -7 -1 0 27.75 3.85 -7 1 0 27.89 4.04 7 -1 1 7.73 6.11 7 1 1 0.66 6.45 -7 -1 -1 1.91 1.56 -7 1 -1 2.08 3.03 7 -1 2 7.74 5.81 7 1 2 19.32 7.24 -7 -1 -2 9.19 3.34 -7 1 -2 5.58 3.52 7 -1 3 7.80 5.22 7 1 3 5.04 6.07 -7 -1 -3 -0.13 3.40 -7 1 -3 -1.26 2.64 7 -1 4 -0.13 5.38 7 1 4 -0.04 5.35 -7 -1 -4 0.07 1.31 -7 1 -4 -1.88 2.91 7 -1 5 17.95 7.59 7 1 5 6.35 5.75 -7 -1 -5 7.85 5.69 -7 1 -5 5.80 4.33 7 1 6 12.25 6.73 7 -1 6 24.51 8.52 -7 -1 -6 14.23 7.72 -7 1 -6 5.66 6.17 7 1 7 3.67 3.79 7 -1 7 5.77 5.67 -7 -1 -7 2.13 3.43 -7 1 -7 4.56 3.09 7 1 8 101.02 11.31 7 -1 8 114.62 11.60 -7 -1 -8 106.81 8.82 -7 1 -8 108.55 9.15 7 2 -7 20.43 19.49 7 -2 -7 46.78 10.34 -7 2 7 32.34 20.67 -7 -2 7 46.11 7.18 -7 2 7 31.52 4.25 7 -2 -6 234.26 18.29 7 2 -6 207.50 19.58 -7 2 6 245.82 17.37 -7 -2 6 242.99 16.32 -7 2 6 203.31 13.49 7 -2 -5 19.51 9.40 -7 2 5 9.84 4.85 -7 -2 5 8.36 4.64 -7 2 5 7.41 3.52 7 -2 -4 37.29 8.13 7 2 -4 45.13 8.28 -7 -2 4 52.15 6.08 -7 2 4 48.10 5.32 7 -2 -3 53.47 37.45 7 2 -3 59.88 29.68 -7 -2 3 93.03 7.77 -7 2 3 94.13 8.59 7 -2 -2 78.38 10.27 7 2 -2 70.19 30.72 -7 2 2 71.43 6.64 -7 -2 2 88.55 7.57 -7 2 2 65.16 7.26 7 -2 -1 10.61 7.29 7 2 -1 13.35 6.62 -7 2 1 3.08 3.03 -7 -2 1 6.92 3.05 -7 2 1 0.70 2.92 7 -2 0 17.67 7.53 7 2 0 -0.62 4.90 -7 2 0 3.10 3.01 -7 -2 0 5.21 4.75 -7 2 0 4.76 3.33 7 -2 1 5.04 4.57 7 2 1 1.53 5.12 -7 -2 -1 6.50 4.33 -7 2 -1 1.18 2.32 7 -2 2 2.97 4.41 7 2 2 -2.77 5.53 -7 -2 -2 2.86 1.85 -7 2 -2 3.25 2.80 7 -2 3 22.09 8.15 7 2 3 12.12 10.24 -7 -2 -3 3.05 3.05 -7 2 -3 12.20 7.29 7 -2 4 11.77 6.09 7 2 4 16.77 7.73 -7 -2 -4 5.60 4.28 -7 2 -4 4.57 2.92 7 -2 5 10.96 6.24 7 2 5 12.02 13.98 -7 -2 -5 10.70 4.60 -7 2 -5 18.18 5.83 7 -2 6 8.18 5.32 7 2 6 12.60 7.33 -7 -2 -6 2.85 2.98 -7 2 -6 8.83 4.41 7 -3 -3 106.43 11.48 7 3 -3 107.13 10.96 -7 3 3 113.57 9.72 -7 -3 3 126.88 9.91 -7 3 3 107.96 8.53 7 -3 -2 7.32 5.50 7 3 -2 -1.30 6.23 -7 3 2 1.59 2.59 -7 -3 2 2.28 3.51 -7 3 2 5.09 3.42 7 -3 -1 20.79 8.15 7 3 -1 17.05 11.76 -7 3 1 15.23 5.76 -7 -3 1 7.43 3.88 -7 3 1 8.14 7.62 7 -3 0 14.02 8.45 7 3 0 15.16 7.30 -7 -3 0 11.85 4.79 -7 3 0 22.10 6.98 7 -3 1 2.41 5.69 7 3 1 12.78 8.83 -7 -3 -1 3.59 2.77 -7 3 -1 9.90 4.23 7 -3 2 56.77 7.89 7 3 2 69.42 8.52 -7 -3 -2 63.58 6.16 -7 3 -2 71.97 6.35 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 54037 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 O1 O -0.7540(2) 0.40321(16) -0.00297(5) 0.0302(4) Uani 1 1 d . . . . . O2 O -0.8853(2) 0.51735(17) 0.06590(5) 0.0337(4) Uani 1 1 d . . . . . H2 H -0.991731 0.545969 0.045153 0.051 Uiso 1 1 calc GR . . . . O3 O 1.3700(2) 0.32662(15) 0.48754(5) 0.0313(4) Uani 1 1 d . . . . . H3 H 1.482105 0.370864 0.502601 0.047 Uiso 1 1 calc GR . . . . O4 O 1.2713(2) 0.54564(15) 0.46127(5) 0.0311(4) Uani 1 1 d . U . . . C1 C -0.7380(3) 0.4289(2) 0.04279(6) 0.0222(4) Uani 1 1 d . . . . . C2 C -0.5529(3) 0.3583(2) 0.07687(7) 0.0282(5) Uani 1 1 d . . . . . H2A H -0.417595 0.325409 0.055535 0.034 Uiso 1 1 calc R . . . . H2B H -0.628122 0.272900 0.091985 0.034 Uiso 1 1 calc R . . . . C3 C -0.4470(3) 0.4491(2) 0.12015(7) 0.0245(4) Uani 1 1 d . . . . . H3A H -0.580141 0.484559 0.141570 0.029 Uiso 1 1 calc R . . . . H3B H -0.362722 0.532376 0.105663 0.029 Uiso 1 1 calc R . . . . C4 C -0.2683(3) 0.3632(2) 0.15315(7) 0.0263(4) Uani 1 1 d . . . . . H4A H -0.359114 0.289610 0.171888 0.032 Uiso 1 1 calc R . . . . H4B H -0.152816 0.313995 0.130705 0.032 Uiso 1 1 calc R . . . . C5 C -0.1258(3) 0.4542(2) 0.19139(7) 0.0264(4) Uani 1 1 d . . . . . H5A H -0.241032 0.504656 0.213565 0.032 Uiso 1 1 calc R . . . . H5B H -0.032320 0.526722 0.172703 0.032 Uiso 1 1 calc R . . . . C6 C 0.0491(3) 0.3662(2) 0.22471(7) 0.0269(5) Uani 1 1 d . . . . . H6B H -0.046043 0.297876 0.244957 0.032 Uiso 1 1 calc R . . . . H6A H 0.156545 0.310728 0.202350 0.032 Uiso 1 1 calc R . . . . C7 C 0.2060(3) 0.4562(2) 0.26104(7) 0.0262(4) Uani 1 1 d . . . . . H7B H 0.303351 0.523648 0.240888 0.031 Uiso 1 1 calc R . . . . H7A H 0.099036 0.512546 0.283261 0.031 Uiso 1 1 calc R . . . . C8 C 0.3767(3) 0.3660(2) 0.29435(7) 0.0261(4) Uani 1 1 d . . . . . H8A H 0.278403 0.300046 0.314937 0.031 Uiso 1 1 calc R . . . . H8B H 0.480025 0.307783 0.271988 0.031 Uiso 1 1 calc R . . . . C9 C 0.5401(3) 0.4533(2) 0.33018(7) 0.0263(5) Uani 1 1 d . . . . . H9A H 0.639609 0.518871 0.309726 0.032 Uiso 1 1 calc R . . . . H9B H 0.437443 0.511539 0.352656 0.032 Uiso 1 1 calc R . . . . C10 C 0.7080(3) 0.3602(2) 0.36305(7) 0.0243(4) Uani 1 1 d . . . . . H10A H 0.607518 0.297945 0.384612 0.029 Uiso 1 1 calc R . . . . H10B H 0.803509 0.298157 0.340451 0.029 Uiso 1 1 calc R . . . . C11 C 0.8827(3) 0.4442(2) 0.39737(7) 0.0237(4) Uani 1 1 d . . . . . H11A H 0.984986 0.506223 0.376134 0.028 Uiso 1 1 calc R . . . . H11B H 0.788803 0.505667 0.420448 0.028 Uiso 1 1 calc R . . . . C12 C 1.0448(3) 0.3448(2) 0.42893(7) 0.0231(4) Uani 1 1 d . . . . . H12A H 0.941027 0.288683 0.451876 0.028 Uiso 1 1 calc R . . . . H12B H 1.124149 0.277187 0.405588 0.028 Uiso 1 1 calc R . . . . C13 C 1.2373(3) 0.4171(2) 0.46043(6) 0.0218(4) Uani 1 1 d . 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 0.0265(7) 0.0413(9) 0.0224(7) -0.0064(6) -0.0093(5) 0.0081(6) O2 0.0288(7) 0.0493(10) 0.0228(7) -0.0037(6) -0.0089(5) 0.0157(6) O3 0.0289(7) 0.0286(8) 0.0359(8) 0.0033(6) -0.0183(6) -0.0021(5) O4 0.0308(7) 0.0260(7) 0.0358(8) 0.0016(6) -0.0174(6) -0.0016(5) C1 0.0189(8) 0.0258(9) 0.0217(9) -0.0018(7) -0.0070(6) -0.0014(6) C2 0.0288(9) 0.0284(10) 0.0270(10) -0.0028(8) -0.0139(7) 0.0053(7) C3 0.0233(8) 0.0291(10) 0.0207(9) -0.0019(7) -0.0078(7) 0.0025(7) C4 0.0230(8) 0.0328(10) 0.0227(9) 0.0013(7) -0.0089(7) 0.0003(7) C5 0.0208(9) 0.0362(11) 0.0219(9) -0.0007(7) -0.0088(7) 0.0018(7) C6 0.0227(9) 0.0354(11) 0.0221(9) 0.0024(7) -0.0104(7) -0.0005(7) C7 0.0213(9) 0.0344(11) 0.0227(9) 0.0008(7) -0.0094(7) 0.0003(7) C8 0.0210(8) 0.0347(11) 0.0224(9) 0.0007(8) -0.0089(7) -0.0014(7) C9 0.0202(9) 0.0358(11) 0.0227(9) 0.0010(8) -0.0093(7) -0.0004(7) C10 0.0192(8) 0.0325(10) 0.0210(9) -0.0002(7) -0.0078(6) -0.0032(7) C11 0.0196(8) 0.0301(10) 0.0211(9) 0.0013(7) -0.0076(6) -0.0021(7) C12 0.0194(8) 0.0279(10) 0.0218(9) 0.0007(7) -0.0078(6) -0.0021(7) C13 0.0182(7) 0.0299(8) 0.0171(8) 0.0008(7) -0.0038(6) -0.0003(7) 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 109.5 . . ? C13 O3 H3 109.5 . . ? O1 C1 O2 122.65(15) . . ? O1 C1 C2 122.32(16) . . ? O2 C1 C2 115.01(15) . . ? C1 C2 H2A 108.2 . . ? C1 C2 H2B 108.2 . . ? C1 C2 C3 116.39(16) . . ? H2A C2 H2B 107.3 . . ? C3 C2 H2A 108.2 . . ? C3 C2 H2B 108.2 . . ? C2 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? C2 C3 C4 111.19(15) . . ? H3A C3 H3B 108.0 . . ? C4 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C3 C4 H4A 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C5 C4 C3 113.41(16) . . ? C5 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? C4 C5 H5A 109.0 . . ? C4 C5 H5B 109.0 . . ? C4 C5 C6 112.71(16) . . ? H5A C5 H5B 107.8 . . ? C6 C5 H5A 109.0 . . ? C6 C5 H5B 109.0 . . ? C5 C6 H6B 108.8 . . ? C5 C6 H6A 108.8 . . ? H6B C6 H6A 107.7 . . ? C7 C6 C5 113.69(16) . . ? C7 C6 H6B 108.8 . . ? C7 C6 H6A 108.8 . . ? C6 C7 H7B 109.0 . . ? C6 C7 H7A 109.0 . . ? H7B C7 H7A 107.8 . . ? C8 C7 C6 112.73(17) . . ? C8 C7 H7B 109.0 . . ? C8 C7 H7A 109.0 . . ? C7 C8 H8A 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C9 C8 C7 113.90(16) . . ? C9 C8 H8A 108.8 . . ? C9 C8 H8B 108.8 . . ? C8 C9 H9A 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C10 C9 C8 112.68(16) . . ? C10 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? C9 C10 H10A 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C11 C10 C9 114.05(15) . . ? C11 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? C10 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C12 C11 C10 111.24(15) . . ? C12 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C11 C12 H12A 108.5 . . ? C11 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C13 C12 C11 115.21(15) . . ? C13 C12 H12A 108.5 . . ? C13 C12 H12B 108.5 . . ? O3 C13 C12 112.80(16) . . ? O4 C13 O3 122.80(15) . . ? O4 C13 C12 124.40(15) . . ? 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 1.229(2) . ? O2 H2 0.8400 . ? O2 C1 1.318(2) . ? O3 H3 0.8400 . ? O3 C13 1.324(2) . ? O4 C13 1.224(2) . ? C1 C2 1.504(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.531(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.534(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.529(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.536(2) . ? C6 H6B 0.9900 . ? C6 H6A 0.9900 . ? C6 C7 1.534(2) . ? C7 H7B 0.9900 . ? C7 H7A 0.9900 . ? C7 C8 1.533(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.533(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.533(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.530(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.530(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.500(2) . ? 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 O2 H2 O1 0.84 1.84 2.6759(18) 174.3 3_365 yes O3 H3 O4 0.84 1.83 2.6637(18) 175.3 3_866 yes C12 H12A O1 0.99 2.42 3.384(2) 164.0 4_766 yes