#------------------------------------------------------------------------------ #$Date: 2021-11-05 01:39:47 +0200 (Fri, 05 Nov 2021) $ #$Revision: 270310 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/38/7243838.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_7243838 loop_ _publ_author_name 'Haneda, Tsuyoshi' 'Matsuno, Shinya' 'Yamamoto, Hisanao' 'Ohtsu, Hiroyoshi' 'Kawano, Masaki' _publ_section_title ; Latency control of chemical reactions in polymerization of epoxy resins using a hydrogen bonding network ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D1CE01163D _journal_year 2021 _chemical_formula_moiety 'C16 H36 P, C6 H9 O4' _chemical_formula_sum 'C22 H45 O4 P' _chemical_formula_weight 404.55 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2021-06-23 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-06-28 deposited with the CCDC. 2021-10-14 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.560(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.3115(3) _cell_length_b 13.0344(4) _cell_length_c 19.6397(7) _cell_measurement_reflns_used 7896 _cell_measurement_temperature 123 _cell_measurement_theta_max 30.8450 _cell_measurement_theta_min 2.6620 _cell_volume 2382.78(14) _computing_cell_refinement 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 123 _diffrn_detector 'Rigaku HyPix-6000 area detector' _diffrn_detector_area_resol_mean 10.0 _diffrn_detector_type 'HPC area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.780 _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 -68.00 18.00 0.50 3.32 -- 4.43 -67.00 -7.00 172 2 \w -17.00 27.00 0.50 3.32 -- -6.23 -99.00 -30.00 88 3 \w -18.00 23.00 0.50 3.32 -- -6.23 -99.00-180.00 82 4 \w -7.00 68.00 0.50 3.32 -- 4.43 67.00 126.00 150 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-DW' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0701487000 _diffrn_orient_matrix_UB_12 -0.0210319000 _diffrn_orient_matrix_UB_13 -0.0029471000 _diffrn_orient_matrix_UB_21 0.0179957000 _diffrn_orient_matrix_UB_22 -0.0361563000 _diffrn_orient_matrix_UB_23 0.0258339000 _diffrn_orient_matrix_UB_31 -0.0236625000 _diffrn_orient_matrix_UB_32 0.0347953000 _diffrn_orient_matrix_UB_33 0.0251000000 _diffrn_radiation_monochromator 'multi-layer mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_unetI/netI 0.0196 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.780 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 10259 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.780 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.928 _diffrn_reflns_theta_min 2.689 _diffrn_source 'rotating anode X-ray generator' _diffrn_source_type PhotonJet-DW _exptl_absorpt_coefficient_mu 0.138 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.57851 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019) 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 1.128 _exptl_crystal_description block _exptl_crystal_F_000 896 _exptl_crystal_size_max 0.291 _exptl_crystal_size_mid 0.126 _exptl_crystal_size_min 0.089 _refine_diff_density_max 0.364 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.041 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 129 _refine_ls_number_reflns 2953 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.054 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0322 _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^)+(0.0400P)^2^+1.4477P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0841 _refine_ls_wR_factor_ref 0.0864 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2644 _reflns_number_total 2953 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ce01163d2.cif _cod_data_source_block haneda_ad_auto _cod_database_code 7243838 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'P C22 H44 O4' _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 99.92 _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 At 1.5 times of: All C(H,H,H) groups 2. Others Fixed Sof: H2(0.5) 3.a Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C5(H5A,H5B), C9(H9A,H9B), C2(H2A,H2B), C1(H1A,H1B), C10(H10A, H10B), C6(H6A,H6B), C7(H7A,H7B) 3.b Idealised Me refined as rotating group: C4(H4A,H4B,H4C), C8(H8A,H8B,H8C) ; _shelx_res_file ; TITL haneda_ad_auto_a.res in C2/c haneda_ad_auto.res created by SHELXL-2018/3 at 11:59:10 on 23-Jun-2021 REM Old TITL haneda_AD_auto in C2/c REM SHELXT solution in C2/c: R1 0.110, Rweak 0.005, Alpha 0.019 REM 0.540 for 110 systematic absences, Orientation as input REM Formula found by SHELXT: C22 O4 P CELL 0.71073 9.3115 13.0344 19.6397 90 91.56 90 ZERR 4 0.0003 0.0004 0.0007 0 0.003 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H O P UNIT 88 180 16 4 L.S. 64 PLAN 5 TEMP -150.15 CONF BOND list 4 fmap 2 ACTA MORE -1 BOND $H REM REM REM WGHT 0.040000 1.447700 FVAR 0.27209 P1 4 0.500000 0.455353 0.750000 10.50000 0.01567 0.01460 = 0.01523 0.00000 -0.00131 0.00000 O2 3 0.997533 0.269693 0.686816 11.00000 0.02193 0.02599 = 0.01321 0.00024 -0.00637 0.00157 O1 3 0.759498 0.241968 0.682806 11.00000 0.02404 0.02415 = 0.01472 0.00260 -0.00195 -0.00270 C11 1 0.874817 0.255619 0.655359 11.00000 0.02330 0.01291 = 0.01249 0.00080 -0.00469 0.00179 C3 1 0.876580 0.579625 0.674381 11.00000 0.02052 0.02073 = 0.01761 0.00151 -0.00173 -0.00425 AFIX 23 H3A 2 0.831249 0.630799 0.643367 11.00000 -1.20000 H3B 2 0.902331 0.614778 0.717698 11.00000 -1.20000 AFIX 0 C5 1 0.431568 0.373480 0.683195 11.00000 0.01878 0.01805 = 0.01686 -0.00130 -0.00209 -0.00211 AFIX 23 H5A 2 0.506487 0.322952 0.671686 11.00000 -1.20000 H5B 2 0.347967 0.335026 0.699997 11.00000 -1.20000 AFIX 0 C9 1 0.741919 0.252117 0.538594 11.00000 0.02225 0.02762 = 0.01132 0.00125 -0.00393 -0.00278 AFIX 23 H9A 2 0.685264 0.313666 0.550169 11.00000 -1.20000 H9B 2 0.687592 0.191065 0.553263 11.00000 -1.20000 AFIX 0 C2 1 0.768323 0.494661 0.688361 11.00000 0.01749 0.01678 = 0.01787 -0.00037 -0.00097 -0.00103 AFIX 23 H2A 2 0.740438 0.459740 0.645232 11.00000 -1.20000 H2B 2 0.812321 0.443206 0.719588 11.00000 -1.20000 AFIX 0 C1 1 0.635934 0.540919 0.720352 11.00000 0.01852 0.01501 = 0.02131 -0.00062 -0.00010 -0.00170 AFIX 23 H1A 2 0.590087 0.587586 0.686450 11.00000 -1.20000 H1B 2 0.668918 0.583659 0.759404 11.00000 -1.20000 AFIX 0 C10 1 0.884904 0.255618 0.577732 11.00000 0.02185 0.03028 = 0.01221 -0.00003 -0.00347 -0.00011 AFIX 23 H10A 2 0.937137 0.318089 0.563944 11.00000 -1.20000 H10B 2 0.942821 0.195666 0.564184 11.00000 -1.20000 AFIX 0 C6 1 0.385705 0.431929 0.618569 11.00000 0.02133 0.02576 = 0.01775 0.00176 -0.00315 -0.00181 AFIX 23 H6A 2 0.319578 0.488091 0.630733 11.00000 -1.20000 H6B 2 0.471463 0.463125 0.598220 11.00000 -1.20000 AFIX 0 C4 1 1.012672 0.539353 0.642668 11.00000 0.02123 0.03138 = 0.02844 0.00271 0.00303 -0.00457 AFIX 137 H4A 2 0.990126 0.514386 0.596539 11.00000 -1.50000 H4B 2 1.051974 0.483004 0.670459 11.00000 -1.50000 H4C 2 1.083624 0.594716 0.640570 11.00000 -1.50000 AFIX 0 C7 1 0.311575 0.362493 0.566398 11.00000 0.03362 0.03540 = 0.02018 -0.00331 -0.00686 -0.00311 AFIX 23 H7A 2 0.225617 0.331474 0.586678 11.00000 -1.20000 H7B 2 0.377576 0.306210 0.554320 11.00000 -1.20000 AFIX 0 C8 1 0.266558 0.420608 0.502201 11.00000 0.05601 0.05469 = 0.02092 -0.00147 -0.01395 0.00191 AFIX 137 H8A 2 0.214951 0.374197 0.470828 11.00000 -1.50000 H8B 2 0.352077 0.447359 0.480241 11.00000 -1.50000 H8C 2 0.203623 0.477737 0.514144 11.00000 -1.50000 AFIX 0 H2 2 0.992056 0.272165 0.726974 10.50000 0.03080 HKLF 4 REM haneda_ad_auto_a.res in C2/c REM wR2 = 0.0864, GooF = S = 1.054, Restrained GooF = 1.054 for all data REM R1 = 0.0322 for 2644 Fo > 4sig(Fo) and 0.0363 for all 2953 data REM 129 parameters refined using 0 restraints END WGHT 0.0406 1.4565 REM Highest difference peak 0.364, deepest hole -0.251, 1-sigma level 0.041 Q1 1 0.5725 0.4945 0.7315 11.00000 0.05 0.36 Q2 1 0.8801 0.2572 0.6160 11.00000 0.05 0.31 Q3 1 0.7500 0.2500 0.5000 10.50000 0.05 0.29 Q4 1 0.4573 0.4114 0.7166 11.00000 0.05 0.29 Q5 1 0.9416 0.5586 0.6582 11.00000 0.05 0.29 ; _shelx_res_checksum 48828 _shelx_hkl_file ; 0 0 -3 0.09 0.12 0 0 3 -0.08 0.12 0 0 -3 0.06 0.13 0 0 4 2.70 0.25 0 0 -4 2.47 0.24 0 0 -4 2.97 0.27 0 0 5 0.11 0.20 0 0 -5 0.11 0.19 0 0 -5 0.10 0.19 0 0 6 1022.61 18.18 0 0 -6 988.77 18.22 0 0 6 1030.34 18.25 0 0 -6 1016.67 18.19 0 0 7 0.16 0.22 0 0 -7 0.12 0.18 0 0 7 0.14 0.20 0 0 8 1006.43 18.33 0 0 8 1008.65 18.22 0 0 -8 1006.21 18.26 0 0 -9 0.86 0.27 0 0 9 0.61 0.30 0 0 9 0.31 0.23 0 0 10 1.14 0.33 0 0 -10 0.92 0.31 0 0 10 0.95 0.28 0 0 -11 0.09 0.29 0 0 11 -0.08 0.27 0 0 12 277.05 5.85 0 0 -12 288.27 6.00 0 0 -13 -0.05 0.32 0 0 13 0.14 0.30 0 0 14 185.77 4.29 0 0 -14 190.01 4.42 0 0 15 -0.05 0.34 0 0 -15 -0.06 0.39 0 0 -16 512.96 10.34 0 0 16 515.91 10.17 0 0 -17 -0.07 0.39 0 0 17 0.06 0.40 0 0 18 51.85 1.88 0 0 -18 52.11 2.01 0 0 19 0.07 0.41 0 0 -19 -0.08 0.46 0 0 -20 3.58 0.67 0 0 -21 -0.08 0.51 0 0 -22 23.32 1.43 0 0 -23 -0.18 0.56 0 0 -24 0.65 0.58 0 -2 0 0.70 0.10 0 -2 -1 183.62 3.42 0 -2 -2 539.73 9.92 0 -2 2 538.55 9.69 0 -2 -2 554.50 9.67 0 -2 -3 134.23 2.58 0 -2 3 131.29 2.59 0 -2 -3 129.16 2.78 0 -2 -4 143.94 2.82 0 -2 4 139.62 2.84 0 -2 -4 139.37 3.02 0 -2 -5 172.21 3.39 0 -2 5 166.36 3.42 0 -2 -5 166.16 3.61 0 -2 -6 108.37 2.35 0 -2 6 102.41 2.36 0 -2 -6 101.38 2.51 0 -2 -7 18.58 0.75 0 -2 -7 18.03 0.86 0 -2 7 17.32 0.77 0 -2 -8 2351.04 41.53 0 -2 -8 2362.38 41.80 0 2 8 2338.37 41.69 0 -2 8 2329.45 41.62 0 -2 -9 47.92 1.49 0 2 9 46.74 1.55 0 -2 9 47.89 1.53 0 -2 9 47.77 1.36 0 -2 -9 49.60 1.65 0 2 10 0.09 0.29 0 -2 10 0.16 0.23 0 -2 -10 0.05 0.28 0 -2 -10 0.13 0.26 0 -2 -11 7.45 0.68 0 -2 11 8.51 0.56 0 2 11 7.89 0.65 0 -2 -11 8.15 0.62 0 2 12 0.37 0.34 0 -2 12 0.30 0.26 0 -2 -12 0.60 0.34 0 -2 -12 0.40 0.30 0 -2 13 12.23 0.71 0 -2 -13 11.50 0.79 0 2 13 12.97 0.84 0 -2 -13 13.07 0.89 0 -2 14 18.11 0.89 0 -2 -14 16.19 0.96 0 2 14 15.83 0.99 0 -2 -14 17.66 1.07 0 -2 15 120.88 2.97 0 2 15 114.93 3.18 0 -2 -15 114.85 3.15 0 -2 -16 13.98 0.97 0 -2 16 15.33 0.88 0 -2 -17 96.60 2.90 0 -2 17 100.66 2.69 0 -2 18 4.44 0.59 0 -2 -18 4.66 0.68 0 -2 19 -0.11 0.41 0 -2 -19 0.08 0.44 0 -2 -20 28.68 1.51 0 -2 20 29.82 1.33 0 -2 -21 25.53 1.44 0 -2 -22 14.05 1.12 0 2 -22 15.16 1.18 0 -2 -23 6.86 0.88 0 2 -23 6.49 0.89 0 2 -24 13.75 1.18 0 -2 -24 14.16 1.18 0 4 0 2469.86 43.34 0 4 1 149.63 3.02 0 -4 -1 150.20 2.99 0 4 -1 148.47 2.98 0 -4 -2 503.64 8.88 0 4 -2 500.59 8.87 0 -4 -2 496.51 9.18 0 4 -3 4.48 0.24 0 -4 -3 5.30 0.26 0 -4 -3 5.00 0.37 0 -4 -3 4.81 0.46 0 4 -4 8.29 0.37 0 -4 -4 8.57 0.39 0 -4 -4 9.40 0.62 0 4 -5 90.42 1.96 0 -4 -5 87.15 1.96 0 -4 -5 90.37 2.37 0 4 -6 117.27 2.49 0 -4 -6 112.67 2.49 0 -4 -6 110.88 2.89 0 4 -7 545.54 10.05 0 -4 -7 538.36 10.06 0 -4 -7 539.70 10.57 0 4 -8 138.86 3.07 0 -4 -8 139.92 3.10 0 -4 -8 137.52 3.50 0 4 -9 180.18 3.80 0 -4 -9 173.29 3.80 0 -4 -9 167.01 4.20 0 -4 -10 4.78 0.47 0 4 -10 5.46 0.50 0 -4 -10 4.83 0.61 0 -4 -11 1.03 0.33 0 4 -11 0.71 0.32 0 -4 -11 0.76 0.38 0 -4 -12 6.84 0.72 0 -4 12 6.43 0.48 0 4 -12 6.69 0.59 0 -4 -12 5.74 0.56 0 -4 13 50.74 1.50 0 -4 -13 49.74 1.97 0 4 -13 48.79 1.69 0 -4 -13 46.26 1.68 0 -4 14 89.27 2.28 0 -4 -14 85.00 2.81 0 4 -14 85.45 2.52 0 -4 -14 88.95 2.53 0 -4 15 100.68 2.52 0 4 -15 100.90 2.82 0 -4 -15 97.36 2.79 0 -4 -15 95.68 3.09 0 -4 -16 0.09 0.45 0 4 -16 0.13 0.38 0 -4 -16 0.44 0.38 0 -4 16 0.69 0.32 0 -4 17 36.40 1.35 0 -4 -17 35.95 1.58 0 4 -17 38.27 1.61 0 -4 -17 35.22 1.76 0 -4 18 120.61 3.00 0 -4 -18 117.15 3.63 0 4 -18 126.35 3.43 0 -4 -18 115.72 3.33 0 -4 19 17.34 0.92 0 -4 -19 17.87 1.15 0 4 -19 16.76 1.14 0 -4 20 6.40 0.62 0 -4 -20 5.20 0.74 0 -4 21 58.64 1.85 0 4 -21 56.12 2.22 0 -4 -21 56.41 2.21 0 4 -22 7.04 0.87 0 -4 -22 8.28 0.91 0 4 -23 49.46 2.11 0 -4 -23 46.71 2.05 0 -4 -24 0.09 0.58 0 4 -24 1.02 0.54 0 6 0 1565.04 27.82 0 6 1 14.63 0.66 0 6 -1 12.42 0.61 0 -6 -1 13.90 0.61 0 6 2 19.32 0.80 0 -6 -2 21.78 0.80 0 6 -2 20.33 0.78 0 -6 -3 45.60 1.12 0 6 -3 49.14 1.16 0 -6 -3 44.79 1.33 0 6 -3 47.16 1.00 0 -6 -3 44.91 1.00 0 -6 -4 4.43 0.41 0 6 -4 4.15 0.26 0 -6 -4 4.47 0.26 0 -6 -5 42.43 1.34 0 6 -5 39.64 1.03 0 -6 -5 39.38 1.04 0 -6 -5 36.72 1.51 0 -6 -6 307.23 6.31 0 -6 -6 300.35 6.65 0 6 -6 314.18 5.88 0 -6 -6 310.45 5.89 0 -6 -7 139.00 3.62 0 -6 -7 134.94 2.92 0 6 -7 135.28 2.90 0 -6 -8 13.75 0.98 0 6 -8 14.52 0.67 0 -6 -8 13.90 0.67 0 -6 -9 85.85 2.76 0 -6 -9 86.71 2.16 0 6 -9 82.94 2.13 0 6 -10 1.31 0.31 0 -6 -10 1.16 0.30 0 -6 -10 1.43 0.50 0 -6 -11 4.53 0.49 0 6 -11 5.34 0.50 0 -6 -11 3.92 0.68 0 6 -12 58.66 1.85 0 -6 -12 62.95 1.89 0 -6 -12 63.39 2.40 0 -6 -13 106.88 2.81 0 6 -13 104.75 2.78 0 -6 -13 108.15 3.41 0 -6 -14 54.16 2.30 0 -6 -14 56.64 1.88 0 6 -14 55.50 1.87 0 -6 15 94.18 2.33 0 -6 -15 93.19 3.21 0 -6 -15 89.21 2.62 0 6 -15 92.85 2.66 0 -6 16 6.04 0.53 0 -6 -16 5.50 0.66 0 6 -16 5.49 0.68 0 -6 -16 6.09 0.87 0 -6 -17 39.41 1.98 0 -6 17 35.90 1.27 0 -6 -17 35.81 1.57 0 6 -17 36.31 1.58 0 -6 18 1.73 0.37 0 6 -18 2.09 0.55 0 -6 -18 1.73 0.51 0 -6 -18 1.86 0.65 0 -6 -19 62.62 2.64 0 -6 19 61.55 1.80 0 6 -19 65.49 2.29 0 -6 -19 63.06 2.24 0 -6 20 5.42 0.52 0 -6 -20 4.78 0.89 0 6 -20 4.64 0.72 0 -6 -20 7.16 0.85 0 -6 -21 42.60 1.90 0 -6 21 44.50 1.43 0 -6 -22 6.99 0.86 0 6 -22 9.10 0.99 0 -6 -23 63.48 2.42 0 6 -23 63.56 2.44 0 8 0 266.17 5.41 0 8 1 5.36 0.47 0 8 -1 6.17 0.47 0 8 2 1.04 0.31 0 8 -2 0.92 0.27 0 -8 -2 1.05 0.25 0 -8 -3 21.92 1.19 0 8 -3 23.52 0.95 0 -8 -3 22.80 0.94 0 -8 -4 49.46 1.54 0 -8 -4 49.66 1.06 0 8 -4 50.44 1.06 0 -8 -4 50.14 1.21 0 8 -4 48.15 1.21 0 -8 -5 51.91 1.18 0 8 -5 50.58 1.17 0 -8 -5 50.23 1.34 0 8 -5 50.70 1.38 0 -8 -5 50.42 1.61 0 8 -6 188.43 3.66 0 -8 -6 193.90 3.68 0 8 -6 188.96 4.00 0 -8 -6 188.84 4.22 0 -8 -7 7.71 0.44 0 8 -7 6.46 0.40 0 -8 -7 6.89 0.64 0 -8 -8 805.58 14.56 0 8 -8 801.48 14.53 0 -8 -8 788.85 15.15 0 -8 -8 799.95 15.75 0 -8 -9 2.26 0.68 0 -8 -9 1.77 0.47 0 8 -9 2.64 0.35 0 -8 -9 2.46 0.34 0 -8 -10 20.74 1.16 0 -8 -10 19.11 1.34 0 -8 -10 20.25 0.87 0 8 -10 20.53 0.88 0 -8 -11 79.03 2.57 0 8 -11 79.48 2.11 0 -8 -11 74.81 2.08 0 -8 -11 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0.92 0.51 2 -4 -18 7.21 0.96 2 4 -18 8.01 0.99 2 4 -18 9.62 0.90 2 -4 -18 10.62 0.98 2 -4 -18 7.91 0.83 2 4 -17 2.04 0.56 2 -4 -17 2.10 0.55 2 4 -17 1.00 0.56 2 -4 -17 1.78 0.59 2 -4 -17 1.33 0.54 2 4 -16 5.01 0.69 2 -4 -16 6.45 0.72 2 -4 -16 3.71 0.69 2 4 -16 4.63 0.72 2 -4 -16 4.68 0.78 2 -4 -15 8.52 0.85 2 4 -15 9.76 0.92 2 -4 -15 9.52 0.93 2 4 -15 9.06 0.81 2 -4 -15 8.94 0.81 2 -4 -14 32.25 1.53 2 -4 -14 28.69 1.55 2 4 -14 28.08 1.53 2 -4 -14 27.67 1.34 2 4 -14 32.27 1.43 2 -4 -13 12.82 0.96 2 4 -13 12.70 0.88 2 -4 -13 11.41 0.84 2 4 -13 10.68 0.91 2 -4 -13 11.68 0.94 2 -4 -12 94.89 2.70 2 4 -12 100.24 2.74 2 -4 -12 104.84 2.97 2 4 -12 94.03 2.96 2 -4 -12 95.21 3.00 2 4 -11 197.35 4.57 2 -4 -11 207.88 4.63 2 4 -11 195.65 4.88 2 -4 -11 195.07 4.87 2 -4 -11 209.12 4.83 2 4 -10 1.95 0.40 2 -4 -10 2.07 0.41 2 -4 -10 2.26 0.48 2 -4 -10 2.88 0.51 2 4 -10 2.58 0.51 2 -4 -9 521.15 10.41 2 4 -9 523.86 10.46 2 -4 -8 135.53 3.42 2 4 -8 134.94 3.47 2 -4 -7 265.35 5.67 2 4 -7 268.57 5.73 2 -4 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2 -6 -22 -0.34 0.66 2 -6 -21 6.01 0.82 2 6 -21 6.02 0.85 2 -6 -21 4.12 0.83 2 -6 -20 6.05 0.81 2 -6 -20 5.95 0.93 2 6 -20 8.50 0.92 2 -6 -19 0.44 0.58 2 6 -19 1.20 0.72 2 -6 -19 2.27 0.73 2 6 -19 1.38 0.58 2 -6 -19 1.30 0.56 2 -6 -18 31.73 1.80 2 6 -18 28.82 1.77 2 -6 -18 34.00 1.83 2 6 -18 31.78 1.56 2 -6 -18 32.58 1.58 2 -6 -17 16.21 1.30 2 6 -17 13.35 1.19 2 -6 -17 14.01 1.21 2 -6 -17 15.16 1.07 2 6 -17 16.73 1.11 2 6 -16 29.45 1.67 2 -6 -16 29.26 1.69 2 -6 -16 32.82 1.76 2 6 -16 29.89 1.44 2 -6 -16 29.72 1.44 2 -6 -15 107.76 3.49 2 6 -15 103.20 3.41 2 -6 -15 118.24 3.63 2 6 -15 114.50 3.14 2 -6 -15 110.44 3.12 2 -6 -14 15.26 1.15 2 6 -14 15.58 1.15 2 -6 -14 16.70 1.27 2 6 -14 18.62 1.06 2 -6 -14 16.31 1.02 2 6 -13 125.13 3.63 2 -6 -13 124.79 3.63 2 -6 -13 125.68 3.28 2 6 -13 122.87 3.25 2 -6 -13 128.22 3.77 2 -6 -12 0.35 0.43 2 -6 -12 -0.31 0.38 2 6 -12 0.78 0.49 2 -6 -12 0.27 0.37 2 6 -12 0.22 0.36 2 6 -11 209.38 4.62 2 -6 -11 196.98 4.58 2 -6 -11 203.84 5.06 2 -6 -11 217.19 5.23 2 -6 -11 201.44 4.93 2 6 -11 202.76 4.96 2 6 -10 42.66 1.72 2 -6 -10 44.53 1.72 2 -6 -10 40.44 1.76 2 6 -10 43.31 1.51 2 -6 -10 43.55 1.86 2 -6 -10 42.05 1.50 2 -6 -9 78.08 2.34 2 6 -9 75.13 2.36 2 -6 -9 70.65 2.10 2 6 -9 77.15 2.14 2 -6 -9 81.20 2.52 2 -6 -8 51.66 1.76 2 6 -8 56.28 1.85 2 -6 -8 49.45 1.59 2 6 -8 54.32 1.63 -2 -6 8 51.76 1.10 2 -6 -8 55.09 1.94 2 -6 -7 34.50 1.45 2 -6 -7 31.44 1.26 2 6 -7 33.24 1.30 -2 -6 7 33.75 0.87 2 6 -6 1.71 0.33 2 -6 -6 2.23 0.35 -2 -6 6 2.19 0.24 2 -6 -6 1.96 0.41 2 -6 -5 193.97 4.45 -2 -6 5 193.06 3.91 2 6 -5 199.78 4.19 2 -6 -5 196.70 4.14 2 -6 -4 0.85 0.22 2 6 -4 0.62 0.22 -2 -6 4 0.97 0.25 2 -6 -4 0.62 0.29 2 6 -3 170.62 3.67 2 -6 -3 172.35 3.62 -2 -6 3 181.21 3.76 -2 6 3 179.37 3.74 2 -6 -3 174.31 3.99 -2 6 3 182.68 4.08 -2 -6 3 177.90 3.74 -2 6 2 751.90 13.42 -2 -6 2 717.12 13.44 2 -6 -2 748.22 13.81 -2 -6 2 741.38 13.61 2 -6 -2 730.34 13.31 2 6 -2 732.33 13.34 -2 6 2 739.20 13.84 2 -6 -1 160.09 3.63 -2 -6 1 152.51 3.27 -2 6 1 160.72 3.29 2 -6 -1 160.22 3.22 2 6 -1 159.70 3.25 -2 -6 1 165.11 3.60 -2 6 1 157.74 3.67 2 6 -1 158.99 2.97 -2 6 0 7.35 0.57 -2 -6 0 7.50 0.57 2 6 0 7.95 0.32 -2 6 0 7.38 0.41 -2 -6 0 6.47 0.40 2 6 0 8.00 0.43 -2 -6 -1 78.33 2.24 -2 -6 -1 79.46 1.85 -2 6 -1 80.63 1.84 2 6 1 78.55 1.64 2 -6 1 81.25 1.66 -2 6 -1 81.66 2.19 -2 -6 -2 24.14 1.14 -2 6 -2 26.94 1.10 -2 -6 -2 24.81 0.65 -2 -6 -2 25.56 0.85 -2 6 -2 26.29 0.85 2 -6 2 26.17 0.72 2 6 2 25.70 0.71 -2 6 -3 66.47 1.96 -2 -6 -3 70.92 1.76 -2 6 -3 70.56 1.76 2 -6 3 71.32 1.59 2 6 3 69.81 1.59 -2 -6 -3 72.95 2.23 2 6 3 71.44 2.13 -2 -6 -3 70.18 1.56 -2 -6 -4 120.45 2.80 -2 6 -4 122.07 2.81 2 6 4 128.25 2.62 2 -6 4 124.99 2.61 2 6 4 120.33 3.19 -2 -6 -4 125.85 2.61 2 -6 5 240.84 4.78 2 6 5 245.46 4.79 -2 6 -5 247.78 4.67 -2 -6 -5 242.73 4.66 2 6 5 244.69 5.45 2 6 6 110.81 3.03 2 6 6 105.94 2.44 2 -6 6 106.60 2.44 -2 -6 -6 107.14 2.32 -2 6 -6 107.69 2.32 -2 -6 -7 28.16 0.94 -2 6 -7 30.30 0.97 2 -6 7 32.51 1.08 2 6 7 31.62 1.09 2 6 7 29.71 1.40 2 6 8 6.29 0.71 2 6 8 5.37 0.47 2 -6 8 5.67 0.48 -2 -6 -8 5.55 0.42 -2 6 -8 6.05 0.44 -2 -6 -8 5.36 0.72 2 6 9 132.64 3.70 -2 6 -9 137.28 3.05 -2 -6 -9 140.99 3.08 -2 -6 -9 133.74 3.87 2 -6 9 135.53 3.20 2 6 9 134.12 3.20 -2 6 -10 5.26 0.48 -2 -6 -10 6.96 0.53 2 -6 10 6.00 0.55 2 6 10 6.73 0.57 -2 -6 -10 6.83 0.83 2 6 10 6.77 0.76 2 -6 11 1.90 0.42 2 6 11 0.80 0.31 -2 6 -11 0.76 0.31 -2 -6 -11 0.96 0.31 -2 -6 -11 1.75 0.57 2 6 12 2.02 0.45 2 -6 12 1.91 0.42 -2 -6 -12 2.88 0.68 -2 6 -12 2.42 0.41 -2 -6 -12 2.22 0.39 -2 -6 -13 30.87 1.70 -2 6 -13 30.31 1.23 -2 -6 -13 30.12 1.22 2 -6 13 32.62 1.40 2 6 13 27.87 1.30 2 6 14 35.94 1.79 2 -6 14 38.75 1.60 2 6 14 40.30 1.62 -2 6 -14 39.01 1.45 -2 -6 -14 37.72 1.44 -2 -6 -14 33.43 1.85 2 6 15 73.78 2.44 2 6 15 76.44 2.78 2 -6 15 73.66 2.42 -2 -6 -15 78.00 2.28 -2 6 -15 73.04 2.23 2 6 16 2.84 0.61 2 -6 16 3.95 0.64 2 6 16 2.32 0.66 -2 6 -16 4.19 0.58 -2 -6 -16 3.70 0.54 -2 6 -17 89.61 2.63 -2 -6 -17 86.22 2.61 2 -6 17 90.35 2.89 2 6 17 92.06 2.91 2 -6 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3.13 2 -8 -16 74.51 2.43 2 8 -16 73.06 2.40 2 -8 -15 4.86 0.81 2 -8 -15 5.98 0.95 2 -8 -15 5.23 0.75 2 8 -15 4.28 0.74 2 8 -15 4.54 0.63 2 -8 -15 5.67 0.66 2 -8 -14 13.32 1.16 2 -8 -14 15.45 1.13 2 8 -14 14.06 1.08 2 -8 -14 15.49 1.33 2 8 -14 13.91 0.92 2 -8 -14 15.04 0.94 2 -8 -13 27.65 1.57 2 -8 -13 25.70 1.41 2 8 -13 28.97 1.52 2 -8 -13 29.95 1.77 2 8 -13 27.42 1.25 2 -8 -13 27.96 1.27 2 -8 -12 21.83 1.35 2 -8 -12 21.79 1.48 2 8 -12 23.43 1.10 2 -8 -12 21.29 1.08 2 8 -12 18.35 1.19 2 -8 -12 20.19 1.19 2 -8 -11 27.55 1.64 2 8 -11 26.77 1.16 2 -8 -11 26.52 1.16 2 8 -11 27.39 1.36 2 -8 -11 24.33 1.27 2 -8 -11 25.16 1.44 2 8 -10 238.29 4.94 2 -8 -10 233.30 4.94 2 -8 -10 239.60 5.84 2 -8 -10 222.22 5.17 2 8 -10 227.90 5.26 2 -8 -10 227.04 5.52 -2 -8 10 226.06 4.30 2 8 -9 87.16 2.29 2 -8 -9 87.61 2.31 2 8 -9 85.43 2.52 2 -8 -9 87.91 2.50 2 -8 -9 89.19 3.01 2 -8 -9 87.71 2.78 -2 -8 9 87.96 1.94 2 -8 -8 3.20 0.41 2 8 -8 2.59 0.37 -2 -8 8 2.74 0.30 2 -8 -8 3.26 0.56 2 8 -8 3.52 0.48 2 -8 -8 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3 -12 34.25 1.67 3 -3 -12 34.99 1.48 3 -3 -11 4.99 0.65 3 3 -11 4.60 0.66 3 3 -10 5.44 0.65 3 -3 -10 4.29 0.60 3 3 -9 36.38 1.58 3 -3 -9 35.84 1.55 3 -3 -8 38.26 1.57 3 -3 -8 40.39 1.58 3 3 -8 39.06 1.58 3 -3 -7 66.10 2.12 3 -3 -7 68.72 2.09 3 3 -7 64.29 2.08 3 3 -6 45.80 0.99 3 -3 -6 44.91 1.58 3 3 -6 48.66 1.65 -3 -3 6 46.32 1.68 -3 3 6 51.83 1.76 3 -3 -6 51.43 1.70 -3 -3 5 0.15 0.28 -3 3 5 0.31 0.31 3 -3 -5 -0.04 0.25 3 3 -5 0.69 0.28 3 3 -5 0.39 0.15 3 -3 -5 0.39 0.30 -3 -3 4 170.85 4.00 -3 3 4 181.38 4.05 3 3 -4 174.71 3.46 3 -3 -4 184.52 4.02 3 -3 -4 175.03 3.91 3 3 -4 176.73 3.94 3 -3 -3 2015.43 35.73 3 3 -3 1970.11 35.78 3 3 -3 2031.32 35.38 -3 -3 3 1961.61 35.82 -3 3 3 1986.65 35.81 3 3 -3 2012.13 35.31 -3 3 3 1994.67 35.85 3 -3 -3 2040.44 35.81 3 -3 -2 113.56 2.77 3 3 -2 119.96 2.56 3 3 -2 113.84 2.74 3 -3 -2 114.45 2.72 -3 3 2 116.46 2.78 -3 -3 2 114.43 2.79 -3 3 2 120.28 2.85 3 3 -2 115.56 2.33 3 -3 -1 151.53 3.32 3 3 -1 149.35 2.78 3 3 -1 139.59 3.23 3 -3 -1 145.45 3.22 -3 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3.49 4 10 -13 10.74 0.97 4 -10 -13 9.53 1.15 4 -10 -13 8.26 0.87 4 10 -13 8.31 0.76 4 -10 -13 8.30 0.78 4 -10 -13 7.55 0.98 4 -10 -12 -0.10 0.55 4 10 -12 -0.17 0.38 4 -10 -12 0.12 0.42 4 10 -12 0.30 0.42 4 -10 -12 -0.07 0.41 4 -10 -11 69.39 2.31 4 10 -11 69.10 2.33 4 -10 -11 68.55 2.64 4 10 -11 63.42 2.07 4 -10 -11 68.71 2.17 4 10 -10 69.72 2.28 4 -10 -10 64.42 2.19 4 -10 -10 64.94 2.56 4 -10 -10 70.99 2.15 4 10 -10 66.59 2.07 4 -10 -9 1.01 0.53 4 10 -9 1.09 0.41 4 -10 -9 1.88 0.44 4 10 -9 1.06 0.42 4 -10 -8 13.74 0.85 4 10 -8 13.97 0.89 4 -10 -8 11.85 1.05 4 -10 -7 5.92 0.77 4 -10 -7 5.53 0.57 4 10 -7 5.78 0.61 4 -10 -6 3.13 0.42 4 10 -6 3.53 0.50 4 -10 -6 3.81 0.66 4 10 -6 3.32 0.26 4 -10 -5 82.82 2.80 4 -10 -5 86.65 2.29 4 10 -5 84.26 2.32 4 -10 -4 69.72 2.45 4 10 -4 69.46 2.02 4 -10 -4 75.11 2.02 -4 10 4 70.93 2.55 -4 10 3 43.70 1.53 -4 -10 3 45.21 1.59 -4 10 3 40.87 1.86 4 -10 -3 44.13 1.43 4 10 -3 42.08 1.44 4 -10 -2 22.90 0.75 4 10 -2 23.20 0.76 -4 -10 2 24.56 1.08 -4 10 2 21.37 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1.65 4 -10 7 55.94 1.66 -4 -10 -7 51.67 1.81 -4 10 -7 57.17 1.88 -4 -10 -7 56.37 1.33 -4 -10 -7 54.54 2.42 -4 -10 -8 6.94 0.45 4 -10 8 7.62 0.62 4 10 8 6.51 0.55 -4 10 -8 6.33 0.65 -4 -10 -8 8.75 0.73 -4 -10 -8 4.86 0.91 -4 10 -8 7.48 0.85 4 -10 9 3.71 0.50 4 10 9 3.00 0.48 -4 -10 -9 3.14 0.40 -4 -10 -9 3.86 0.59 -4 10 -9 3.60 0.58 -4 -10 -9 2.41 0.74 -4 10 -10 40.55 1.68 -4 -10 -10 35.62 1.61 -4 -10 -10 38.56 1.34 4 -10 10 41.15 1.49 4 10 10 37.40 1.44 4 -10 11 0.93 0.43 4 10 11 1.33 0.43 -4 -10 -11 1.02 0.34 -4 10 -11 1.68 0.51 -4 -10 -11 0.91 0.44 -4 -10 -12 23.12 1.36 -4 10 -12 24.67 1.42 4 -10 12 24.65 1.21 4 10 12 21.71 1.14 -4 -10 -13 0.09 0.46 -4 10 -13 0.54 0.56 4 10 13 -0.18 0.43 4 -10 13 -0.06 0.44 -4 -10 -14 123.10 3.79 4 10 14 125.44 3.41 4 -10 14 130.09 3.45 4 -10 15 13.13 1.01 4 10 15 13.02 1.01 -4 -10 -15 14.22 0.85 -4 10 -15 13.25 0.84 4 10 16 29.15 1.51 4 -10 16 29.00 1.52 -4 10 -16 33.04 1.33 -4 -10 -16 30.71 1.29 -4 10 -17 2.05 0.49 -4 -10 -17 2.18 0.53 -4 10 -18 40.70 1.61 -4 -10 -18 41.99 1.61 -4 -10 -19 0.23 0.44 -4 10 -19 -0.06 0.45 -4 10 -20 4.75 0.67 -4 -10 -20 4.75 0.67 -4 -10 -21 2.25 0.60 4 12 -19 10.15 0.95 4 12 -18 24.06 1.34 4 12 -17 0.93 0.53 4 -12 -16 7.57 1.09 4 12 -16 5.85 0.71 4 -12 -15 4.62 0.93 4 -12 -15 4.22 1.05 4 12 -15 3.65 0.62 4 -12 -15 4.33 0.67 4 12 -15 4.02 0.77 4 -12 -14 0.11 0.61 4 12 -14 0.08 0.46 4 -12 -14 0.14 0.79 4 -12 -14 0.53 0.46 4 12 -14 0.29 0.43 4 12 -13 1.08 0.44 4 -12 -13 0.56 0.38 4 -12 -13 0.44 0.57 4 12 -13 0.36 0.46 4 -12 -13 0.13 0.69 4 12 -12 29.42 1.40 4 -12 -12 26.55 1.83 4 -12 -12 25.82 1.65 4 12 -12 27.85 1.21 4 -12 -12 27.10 1.22 4 12 -11 -0.12 0.37 4 -12 -11 -0.10 0.59 4 -12 -11 0.63 0.64 4 12 -11 0.19 0.35 4 -12 -11 -0.20 0.37 4 12 -10 76.61 2.34 4 -12 -10 73.78 2.24 4 -12 -10 77.93 2.18 4 12 -10 75.44 2.13 4 -12 -10 75.94 2.85 4 -12 -9 1.03 0.36 4 12 -9 0.66 0.34 4 12 -9 1.29 0.40 4 -12 -9 0.90 0.38 4 -12 -9 0.99 0.60 4 -12 -8 73.18 2.72 4 12 -8 70.41 1.70 4 12 -8 69.89 2.09 4 -12 -8 71.38 2.03 4 12 -8 71.91 1.94 4 -12 -8 70.26 1.96 4 -12 -7 2.72 0.40 4 12 -7 2.26 0.40 4 12 -7 2.06 0.24 4 12 -7 1.99 0.37 4 -12 -7 2.15 0.38 4 -12 -7 2.53 0.64 4 12 -6 66.49 1.74 4 -12 -6 65.19 1.78 4 -12 -6 62.02 2.43 4 -12 -6 66.61 1.84 4 12 -6 66.15 1.89 4 12 -5 14.15 0.75 4 -12 -5 12.99 0.68 4 12 -5 12.72 0.64 -4 -12 4 2.59 0.58 4 12 -4 2.24 0.25 4 -12 -4 2.64 0.27 -4 12 3 26.73 1.57 -4 -12 3 26.83 1.40 4 -12 -3 27.48 0.79 4 12 -3 28.39 0.79 -4 12 2 21.99 1.40 -4 -12 2 23.62 1.35 4 12 -2 24.10 0.70 4 -12 -2 22.76 0.71 -4 12 1 0.63 0.52 4 -12 -1 0.69 0.19 4 12 -1 0.70 0.18 -4 -12 1 0.41 0.52 4 -12 0 16.44 0.58 4 12 0 14.20 0.54 -4 -12 0 15.16 0.73 -4 12 0 15.62 1.18 -4 -12 0 16.55 1.22 4 12 1 0.16 0.20 4 -12 1 0.16 0.20 -4 12 -1 0.36 0.49 -4 -12 -1 -0.37 0.53 -4 12 -1 -0.09 0.23 -4 -12 -1 0.27 0.23 4 12 2 8.02 0.42 4 -12 2 7.23 0.44 -4 -12 -2 6.78 0.51 -4 12 -2 7.85 0.52 -4 12 -2 5.47 0.78 -4 -12 -2 7.91 0.98 -4 -12 -3 2.15 0.69 4 -12 3 2.39 0.32 -4 12 -3 3.32 0.67 4 12 3 2.44 0.29 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-7 57.27 2.69 -10 -4 -8 8.83 1.16 -10 4 -8 8.95 1.14 -10 -4 -9 0.81 0.73 -10 4 -9 0.40 0.72 -10 -4 -10 62.82 2.95 -10 4 -10 61.64 2.90 -10 -4 -11 0.70 0.71 -10 4 -11 0.84 0.74 10 6 -13 26.96 1.37 10 6 -12 4.93 0.66 10 6 -11 3.93 0.61 -10 6 11 3.79 1.01 -10 -6 11 3.82 0.98 10 6 -10 22.82 1.15 10 -6 -10 21.01 1.61 -10 6 10 21.96 1.86 -10 -6 10 26.58 2.02 10 -6 -9 1.89 0.69 -10 6 9 2.26 0.86 -10 -6 9 3.02 0.95 10 -6 -8 0.79 0.61 -10 6 8 1.19 0.81 -10 -6 8 2.08 0.91 -10 6 7 13.23 1.45 -10 -6 7 12.45 1.37 -10 6 6 0.71 0.71 -10 -6 6 0.28 0.73 -10 -6 5 33.25 2.10 -10 6 5 32.92 2.12 -10 -6 4 1.21 0.67 -10 6 4 0.54 0.67 10 6 -4 0.55 0.56 -10 -6 3 128.61 4.39 -10 6 3 130.72 4.43 10 6 -3 135.17 3.86 -10 -6 2 71.11 3.06 -10 6 2 74.80 3.15 10 6 -2 74.70 2.74 -10 -6 1 122.54 4.19 -10 6 1 119.62 4.18 10 6 -1 122.18 3.80 10 6 0 1.23 0.73 -10 -6 0 3.11 0.79 -10 6 0 2.34 0.73 10 6 1 11.46 1.21 -10 -6 -1 13.50 1.32 -10 6 -1 14.44 1.39 -10 -6 -2 8.19 1.13 -10 6 -2 9.99 1.23 -10 -6 -3 9.95 1.21 -10 6 -3 10.04 1.19 -10 -6 -4 12.15 1.30 -10 6 -4 11.99 1.26 -10 -6 -5 7.67 1.07 -10 6 -5 7.09 1.04 -10 -6 -6 13.59 1.32 -10 6 -6 14.59 1.34 -10 -6 -7 1.81 0.73 -10 6 -7 2.27 0.75 -10 -6 -8 2.10 0.75 -10 6 -8 0.77 0.67 -10 -6 -9 0.80 0.71 -10 6 -9 0.40 0.65 -10 6 -10 2.83 0.91 -10 -6 -10 2.59 0.83 -10 8 10 11.66 1.44 -10 -8 10 11.20 1.44 -10 8 9 10.85 1.38 -10 -8 9 9.33 1.32 -10 8 8 0.87 0.82 -10 -8 8 1.03 0.86 -10 8 7 21.28 1.77 -10 -8 7 20.69 1.73 -10 8 6 2.67 0.95 -10 -8 6 3.23 0.95 -10 8 5 80.75 3.40 -10 -8 5 86.31 3.49 -10 8 4 1.90 0.79 -10 -8 4 1.89 0.78 -10 -8 3 53.98 2.63 -10 8 3 51.51 2.60 -10 -8 2 4.47 0.89 -10 8 2 6.08 1.02 -10 -8 1 2.30 0.80 -10 8 1 2.06 0.71 10 8 0 23.93 1.60 -10 8 0 28.88 1.87 -10 -8 0 29.97 1.91 -10 -8 -1 0.63 0.65 -10 8 -1 0.89 0.69 -10 -8 -2 19.91 1.58 -10 8 -2 19.87 1.60 -10 -8 -3 -0.25 0.66 -10 8 -3 0.12 0.63 -10 -8 -4 11.90 1.28 -10 8 -4 11.49 1.26 -10 -8 -5 10.94 1.26 -10 8 -5 10.97 1.21 -10 -8 -6 0.76 0.74 -10 8 -6 0.86 0.66 -10 -8 -7 21.08 1.66 -10 8 -7 23.71 1.71 -10 -8 -8 8.19 1.16 -10 8 -8 8.85 1.14 -10 -8 -9 20.51 1.66 -10 8 -9 19.91 1.64 -10 -10 9 6.45 1.11 -10 10 8 7.91 1.24 -10 -10 8 6.76 1.17 -10 10 7 1.25 0.84 -10 -10 7 0.42 0.76 -10 10 6 -0.41 0.86 -10 -10 6 -0.28 0.81 -10 10 5 9.27 1.27 -10 -10 5 9.37 1.25 -10 10 4 -0.26 1.05 -10 -10 4 -1.20 0.98 -10 -10 3 17.04 1.58 -10 10 3 15.50 1.54 -10 -10 2 7.69 1.17 -10 10 2 4.73 1.05 -10 -10 1 4.14 1.00 -10 10 1 5.26 1.03 -10 -10 0 13.06 1.39 -10 10 0 11.74 1.35 -10 10 -1 6.69 1.12 -10 -10 -1 8.24 1.19 -10 -10 -2 5.26 1.04 -10 10 -2 7.13 1.14 -10 -10 -3 -0.24 0.88 -10 10 -3 0.12 0.75 -10 -10 -4 5.88 1.01 -10 10 -4 3.05 0.85 -10 10 -5 2.18 0.84 -10 -10 -5 2.45 0.77 -10 -10 -6 50.67 2.52 -10 10 -6 56.36 2.62 -10 10 -7 1.70 0.74 -10 -10 -7 0.62 0.64 -10 -10 -8 15.40 1.44 -10 10 -8 14.32 1.39 11 1 -15 -0.22 0.65 11 1 -14 27.05 1.73 11 1 -13 21.78 1.54 11 -1 -13 20.65 1.59 11 1 -12 48.79 2.25 11 -1 -12 51.31 2.37 11 -1 -11 18.96 1.46 11 1 -11 20.74 1.44 11 1 -10 37.04 1.85 11 -1 -10 35.50 1.91 11 -1 -9 2.94 0.74 11 1 -9 2.50 0.65 -11 -1 8 0.16 0.78 -11 -1 7 5.62 1.07 -11 -1 6 1.41 0.79 -11 -1 5 4.60 0.99 -11 -1 4 -0.15 0.71 -11 -1 3 2.39 0.82 -11 -1 2 24.88 1.93 -11 -1 1 3.83 0.91 -11 -1 0 14.03 1.45 -11 -1 0 11.12 1.04 -11 -1 -1 1.67 0.63 -11 -1 -1 1.88 0.79 -11 -1 -2 6.02 0.84 -11 -1 -2 5.03 1.02 -11 -1 -3 2.09 0.64 -11 -1 -3 2.72 0.91 -11 -1 -4 21.71 1.79 -11 -1 -4 24.64 1.48 -11 -1 -5 2.00 0.81 -11 -1 -5 -0.08 0.56 -11 -1 -6 37.23 1.81 -11 -1 -6 37.80 2.28 -11 -1 -7 9.04 1.23 11 3 -16 19.87 1.51 11 3 -15 1.97 0.79 11 3 -14 23.81 1.54 11 3 -13 7.04 0.91 11 3 -12 2.34 0.70 11 -3 -11 0.46 0.59 11 3 -11 -0.17 0.55 11 -3 -10 -0.11 0.61 11 3 -10 0.94 0.55 11 -3 -9 10.90 1.17 -11 3 8 1.15 0.82 -11 -3 8 0.81 0.78 -11 3 7 14.39 1.57 -11 -3 7 14.70 1.54 -11 -3 6 -0.78 0.92 -11 3 6 0.63 0.84 -11 -3 5 2.60 0.91 -11 3 5 2.63 0.90 -11 -3 4 30.96 2.10 -11 3 4 31.78 2.16 -11 -3 3 28.54 1.98 -11 3 3 27.90 1.97 -11 -3 2 49.14 2.62 -11 3 2 51.60 2.70 -11 -3 1 29.99 2.02 -11 3 1 30.69 2.06 -11 -3 0 7.02 1.07 -11 3 0 5.64 0.95 -11 -3 -1 8.11 1.20 -11 3 -1 10.27 1.28 -11 -3 -2 0.14 0.76 -11 3 -2 1.13 0.75 -11 -3 -3 3.88 0.94 -11 3 -3 2.39 0.80 -11 -3 -4 0.72 0.63 -11 3 -4 -0.28 0.66 -11 -3 -5 116.94 4.24 -11 3 -5 111.33 4.09 -11 -3 -6 1.29 0.66 -11 3 -6 0.70 0.67 -11 -3 -7 3.59 0.90 -11 3 -7 5.52 1.05 -11 -5 7 28.67 2.14 -11 5 7 26.46 2.10 -11 5 6 4.42 1.07 -11 -5 6 3.42 0.99 -11 -5 5 24.03 1.91 -11 5 5 24.05 1.93 -11 5 4 13.39 1.48 -11 -5 4 15.01 1.52 -11 -5 3 54.41 2.79 -11 5 3 52.98 2.77 -11 5 2 0.88 0.68 -11 -5 2 1.46 0.81 -11 -5 1 45.94 2.54 -11 5 1 43.67 2.47 -11 -5 0 0.72 0.68 -11 5 0 1.15 0.72 -11 -5 -1 28.84 1.99 -11 5 -1 29.67 2.02 -11 -5 -2 1.00 0.72 -11 5 -2 0.84 0.71 -11 -5 -3 16.74 1.61 -11 5 -3 17.85 1.63 -11 -5 -4 2.85 0.93 -11 5 -4 4.31 0.99 -11 -5 -5 4.01 0.98 -11 5 -5 5.42 1.04 -11 -5 -6 0.29 0.63 -11 5 -6 0.70 0.79 -11 7 5 7.96 1.26 -11 -7 5 9.08 1.34 -11 -7 4 -0.44 0.90 -11 7 4 -0.15 0.94 -11 -7 3 23.19 1.84 -11 7 3 28.45 2.04 -11 -7 2 0.43 0.75 -11 7 2 -0.29 0.77 -11 -7 1 32.64 2.15 -11 7 1 33.60 2.15 -11 -7 0 10.43 1.35 -11 7 0 14.28 1.47 -11 -7 -1 37.40 2.30 -11 7 -1 37.72 2.30 -11 -7 -2 1.13 0.72 -11 7 -2 0.97 0.80 -11 -7 -3 15.70 1.51 -11 7 -3 15.99 1.55 -11 -7 -4 1.41 0.79 -11 7 -4 0.82 0.69 -11 9 2 16.38 1.64 -11 9 1 15.57 1.53 -11 9 0 0.28 0.91 -11 9 -1 59.51 2.90 12 2 -13 13.22 1.23 12 2 -12 25.23 1.57 0 0 0 0.00 0.00 TITL haneda_AD_auto in C2/c REM C2/c (#15 in standard setting) CELL 0.71073 9.311543 13.034363 19.639717 90.0000 91.5602 90.0000 ZERR 4.00 0.000313 0.000432 0.000657 0.0000 0.0030 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H O P UNIT 88.00 176.00 16.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 64887 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 1.455 _oxdiff_exptl_absorpt_empirical_full_min 0.565 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 P1 P 0.500000 0.45535(3) 0.750000 0.01520(10) Uani 1 2 d S T P . . O2 O 0.99753(8) 0.26969(6) 0.68682(4) 0.02050(17) Uani 1 1 d . . . . . O1 O 0.75950(8) 0.24197(5) 0.68281(4) 0.02102(17) Uani 1 1 d . . . . . C11 C 0.87482(11) 0.25562(7) 0.65536(5) 0.01633(19) Uani 1 1 d . . . . . C3 C 0.87658(11) 0.57962(8) 0.67438(5) 0.0197(2) Uani 1 1 d . . . . . H3A H 0.831249 0.630799 0.643367 0.024 Uiso 1 1 calc R U . . . H3B H 0.902331 0.614778 0.717698 0.024 Uiso 1 1 calc R U . . . C5 C 0.43157(11) 0.37348(7) 0.68320(5) 0.0179(2) Uani 1 1 d . . . . . H5A H 0.506487 0.322952 0.671686 0.022 Uiso 1 1 calc R U . . . H5B H 0.347967 0.335026 0.699997 0.022 Uiso 1 1 calc R U . . . C9 C 0.74192(11) 0.25212(8) 0.53859(5) 0.0205(2) Uani 1 1 d . . . . . H9A H 0.685264 0.313666 0.550169 0.025 Uiso 1 1 calc R U . . . H9B H 0.687592 0.191065 0.553263 0.025 Uiso 1 1 calc R U . . . C2 C 0.76832(10) 0.49466(7) 0.68836(5) 0.0174(2) Uani 1 1 d . . . . . H2A H 0.740438 0.459740 0.645232 0.021 Uiso 1 1 calc R U . . . H2B H 0.812321 0.443206 0.719588 0.021 Uiso 1 1 calc R U . . . C1 C 0.63593(10) 0.54092(7) 0.72035(5) 0.0183(2) Uani 1 1 d . . . . . H1A H 0.590087 0.587586 0.686450 0.022 Uiso 1 1 calc R U . . . H1B H 0.668918 0.583659 0.759404 0.022 Uiso 1 1 calc R U . . . C10 C 0.88490(11) 0.25562(8) 0.57773(5) 0.0215(2) Uani 1 1 d . . . . . H10A H 0.937137 0.318089 0.563944 0.026 Uiso 1 1 calc R U . . . H10B H 0.942821 0.195666 0.564184 0.026 Uiso 1 1 calc R U . . . C6 C 0.38570(11) 0.43193(8) 0.61857(5) 0.0217(2) Uani 1 1 d . . . . . H6A H 0.319578 0.488091 0.630733 0.026 Uiso 1 1 calc R U . . . H6B H 0.471463 0.463125 0.598220 0.026 Uiso 1 1 calc R U . . . C4 C 1.01267(12) 0.53935(9) 0.64267(6) 0.0270(2) Uani 1 1 d . . . . . H4A H 0.990126 0.514386 0.596539 0.040 Uiso 1 1 calc R U . . . H4B H 1.051974 0.483004 0.670459 0.040 Uiso 1 1 calc R U . . . H4C H 1.083624 0.594716 0.640570 0.040 Uiso 1 1 calc R U . . . C7 C 0.31157(14) 0.36249(9) 0.56640(6) 0.0299(3) Uani 1 1 d . . . . . H7A H 0.225617 0.331474 0.586678 0.036 Uiso 1 1 calc R U . . . H7B H 0.377576 0.306210 0.554320 0.036 Uiso 1 1 calc R U . . . C8 C 0.26656(17) 0.42061(12) 0.50220(7) 0.0441(3) Uani 1 1 d . . . . . H8A H 0.214951 0.374197 0.470828 0.066 Uiso 1 1 calc R U . . . H8B H 0.352077 0.447359 0.480241 0.066 Uiso 1 1 calc R U . . . H8C H 0.203623 0.477737 0.514144 0.066 Uiso 1 1 calc R U . . . H2 H 0.992(4) 0.272(2) 0.7270(13) 0.031(8) Uiso 0.5 1 d . . P . . 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 P1 0.01567(18) 0.01460(17) 0.01523(17) 0.000 -0.00131(12) 0.000 O2 0.0219(4) 0.0260(4) 0.0132(4) 0.0002(3) -0.0064(3) 0.0016(3) O1 0.0240(4) 0.0242(4) 0.0147(3) 0.0026(3) -0.0020(3) -0.0027(3) C11 0.0233(5) 0.0129(4) 0.0125(4) 0.0008(3) -0.0047(4) 0.0018(3) C3 0.0205(5) 0.0207(5) 0.0176(5) 0.0015(3) -0.0017(4) -0.0042(4) C5 0.0188(5) 0.0181(4) 0.0169(4) -0.0013(3) -0.0021(4) -0.0021(3) C9 0.0222(5) 0.0276(5) 0.0113(5) 0.0013(4) -0.0039(4) -0.0028(4) C2 0.0175(5) 0.0168(4) 0.0179(4) -0.0004(3) -0.0010(4) -0.0010(3) C1 0.0185(5) 0.0150(4) 0.0213(5) -0.0006(3) -0.0001(4) -0.0017(3) C10 0.0219(5) 0.0303(5) 0.0122(5) 0.0000(4) -0.0035(4) -0.0001(4) C6 0.0213(5) 0.0258(5) 0.0178(5) 0.0018(4) -0.0031(4) -0.0018(4) C4 0.0212(5) 0.0314(6) 0.0284(6) 0.0027(4) 0.0030(4) -0.0046(4) C7 0.0336(6) 0.0354(6) 0.0202(5) -0.0033(4) -0.0069(4) -0.0031(5) C8 0.0560(9) 0.0547(9) 0.0209(6) -0.0015(5) -0.0139(6) 0.0019(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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 -16 12 0.0715 -13 -2 -2 0.0097 -4 4 26 0.1224 -1 16 -14 0.0470 8 -10 -17 0.0955 13 1 1 0.0710 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 C5 P1 C5 107.03(6) . 2_656 ? C5 P1 C1 111.53(5) 2_656 . ? C5 P1 C1 111.82(4) 2_656 2_656 ? C5 P1 C1 111.81(4) . . ? C5 P1 C1 111.53(5) . 2_656 ? C1 P1 C1 103.21(6) . 2_656 ? C11 O2 H2 114(2) . . ? O2 C11 C10 113.42(9) . . ? O1 C11 O2 125.53(9) . . ? O1 C11 C10 121.05(9) . . ? H3A C3 H3B 107.8 . . ? C2 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? C4 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? C4 C3 C2 112.63(8) . . ? P1 C5 H5A 108.9 . . ? P1 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C6 C5 P1 113.31(7) . . ? C6 C5 H5A 108.9 . . ? C6 C5 H5B 108.9 . . ? C9 C9 H9A 108.9 7_656 . ? C9 C9 H9B 108.9 7_656 . ? H9A C9 H9B 107.7 . . ? C10 C9 C9 113.21(11) . 7_656 ? C10 C9 H9A 108.9 . . ? C10 C9 H9B 108.9 . . ? C3 C2 H2A 109.8 . . ? C3 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? C1 C2 C3 109.43(8) . . ? C1 C2 H2A 109.8 . . ? C1 C2 H2B 109.8 . . ? P1 C1 H1A 107.7 . . ? P1 C1 H1B 107.7 . . ? C2 C1 P1 118.25(7) . . ? C2 C1 H1A 107.7 . . ? C2 C1 H1B 107.7 . . ? H1A C1 H1B 107.1 . . ? C11 C10 H10A 108.5 . . ? C11 C10 H10B 108.5 . . ? C9 C10 C11 115.29(9) . . ? C9 C10 H10A 108.5 . . ? C9 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C5 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C7 C6 C5 111.97(9) . . ? C7 C6 H6A 109.2 . . ? C7 C6 H6B 109.2 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C6 C7 C8 111.88(10) . . ? H7A C7 H7B 107.9 . . ? C8 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 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 P1 C5 1.7946(10) . ? P1 C5 1.7947(10) 2_656 ? P1 C1 1.7959(10) 2_656 ? P1 C1 1.7959(10) . ? O2 C11 1.2972(12) . ? O2 H2 0.79(3) . ? O1 C11 1.2275(13) . ? C11 C10 1.5300(13) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C2 1.5274(13) . ? C3 C4 1.5206(15) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.5311(14) . ? C9 C9 1.5285(18) 7_656 ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.5198(14) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C1 1.5232(13) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C7 1.5189(15) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.5200(17) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 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 P1 C5 C6 C7 -172.96(8) . . . . ? O2 C11 C10 C9 -173.04(9) . . . . ? O1 C11 C10 C9 7.84(14) . . . . ? C3 C2 C1 P1 -173.59(7) . . . . ? C5 P1 C5 C6 -172.97(9) 2_656 . . . ? C5 P1 C1 C2 -57.65(9) . . . . ? C5 P1 C1 C2 62.15(9) 2_656 . . . ? C5 C6 C7 C8 -179.82(10) . . . . ? C9 C9 C10 C11 -177.67(10) 7_656 . . . ? C1 P1 C5 C6 64.44(8) 2_656 . . . ? C1 P1 C5 C6 -50.56(8) . . . . ? C1 P1 C1 C2 -177.65(9) 2_656 . . . ? C4 C3 C2 C1 179.67(8) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 1.2563 -16.4485 12.0018 0.2224 0.9274 -0.3008 -13.0191 -1.5578 -1.9468 0.9518 -0.2283 0.2050 -3.8833 4.2453 25.8757 0.1069 0.4451 0.8891 -0.9658 15.9125 -13.6558 -0.2267 -0.9455 0.2338 7.9328 -9.9350 -16.6682 -0.2984 0.0714 -0.9518 13.0938 0.8724 0.8157 -0.9393 0.2252 -0.2590