#------------------------------------------------------------------------------ #$Date: 2017-06-05 15:30:59 +0100 (Mon, 05 Jun 2017) $ #$Revision: 197524 $ #$URL: svn://www.crystallography.net/cod/cif/3/50/00/3500068.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_3500068 loop_ _publ_author_name 'Thierry Maris' _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _journal_name_full 'Personal communication to COD' _journal_year 2017 _chemical_formula_moiety 'C8 H10 O2' _chemical_formula_sum 'C8 H10 O2' _chemical_formula_weight 138.16 _chemical_melting_point 439 _chemical_name_common 1,2-Benzenedimethanol _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' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _audit_creation_date 2016-10-26 _audit_creation_method ; Olex2 1.2 (compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227) ; _cell_angle_alpha 90 _cell_angle_beta 117.3230(10) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 15.0049(6) _cell_length_b 7.5241(3) _cell_length_c 13.8287(9) _cell_measurement_reflns_used 9532 _cell_measurement_temperature 100 _cell_measurement_theta_max 60.662 _cell_measurement_theta_min 3.131 _cell_volume 1387.06(12) _computing_cell_refinement ; SAINT (2013) V8.37A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_collection ; APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_reduction ; SAINT (2013) V8.37A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173. ; _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 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 100 _diffrn_detector 'CMOS Area detector' _diffrn_detector_area_resol_mean 10.24 _diffrn_detector_type 'Bruker Photon 100 CMOS Detector' _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device 'k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker Venture Metaljet' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_collimation 'Focusing mirrors' _diffrn_radiation_monochromator 'Helios MX Mirror Optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_unetI/netI 0.0173 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 11438 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 60.631 _diffrn_reflns_theta_min 5.775 _diffrn_source 'Metal Jet' _diffrn_source_target Ga _diffrn_source_type 'Gallium Liquid Metal Jet Source' _exptl_absorpt_coefficient_mu 0.494 _exptl_absorpt_correction_T_max 0.7519 _exptl_absorpt_correction_T_min 0.6965 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1098 before and 0.0429 after correction. The Ratio of minimum to maximum transmission is 0.9263. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.323 _exptl_crystal_description block _exptl_crystal_F_000 592 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.075 _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Venture diffractometer equipped with a Photon 100 CMOS Detector, a Helios MX optics and a Kappa goniometer. The crystal-to-detector distance was 4.0 cm, and the data collection was carried out in 1024 x 1024 pixel mode. ; _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _refine_diff_density_max 0.316 _refine_diff_density_min -0.167 _refine_diff_density_rms 0.038 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 139 _refine_ls_number_reflns 1581 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0344 _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^)+(0.0542P)^2^+0.6946P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0923 _refine_ls_wR_factor_ref 0.0935 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1504 _reflns_number_total 1581 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file BENDIM.cif _cod_data_source_block bendim _cod_depositor_comments ; The following automatic conversions were performed: '_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_original_cell_volume 1387.05(12) _cod_database_code 3500068 _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 0.964 _shelx_estimated_absorpt_t_min 0.948 _olex2_refinement_description ; 1. Others Fixed Sof: H1B(0.5) H2A(0.5) H2B(0.5) H1A(0.5) ; _shelx_res_file ; TITL bendim_a.res in C2/c bendim.res created by SHELXL-2016/6 at 17:02:23 on 26-Oct-2016 REM Old TITL BENDIM in C2/c #15 REM SHELXT solution in C2/c REM R1 0.114, Rweak 0.002, Alpha 0.023, Orientation as input REM Formula found by SHELXT: C8 O2 CELL 1.34139 15.0049 7.5241 13.8287 90 117.323 90 ZERR 8 0.0006 0.0003 0.0009 0 0.001 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H O DISP C 0.014 0.007 57.748 DISP H -0 0 0.648 DISP O 0.039 0.025 193.954 UNIT 64 80 16 EQIV $1 1-X,1-Y,1-Z EQIV $2 1-X,+Y,0.5-Z EQIV $3 1-X,-Y,1-Z L.S. 45 PLAN 8 SIZE 0.075 0.1 0.11 TEMP 0 HTAB C7 O2 HTAB O1 O2_$1 HTAB O2 O2_$2 HTAB O2 O1_$1 HTAB O1 O1_$3 BOND $H LIST 4 MORE -1 CONF HTAB fmap 2 acta REM REM REM WGHT 0.054200 0.694600 FVAR 0.87077 O1 3 0.468344 0.171766 0.484513 11.00000 0.02685 0.01971 = 0.02875 -0.00266 0.01737 -0.00604 O2 3 0.555336 0.654814 0.357296 11.00000 0.02628 0.02240 = 0.02399 0.00347 0.01376 0.00644 C1 1 0.622874 0.339873 0.523301 11.00000 0.01714 0.01543 = 0.01795 -0.00099 0.00948 0.00212 C2 1 0.667082 0.275209 0.629305 11.00000 0.02184 0.02359 = 0.02034 0.00300 0.01237 0.00553 C3 1 0.764119 0.325143 0.703914 11.00000 0.02314 0.03327 = 0.01728 -0.00083 0.00815 0.01027 C4 1 0.818165 0.439968 0.672287 11.00000 0.01789 0.02815 = 0.02512 -0.01015 0.00617 0.00297 C5 1 0.774965 0.504662 0.566361 11.00000 0.01935 0.01809 = 0.03014 -0.00517 0.01238 -0.00092 C6 1 0.677828 0.456686 0.491448 11.00000 0.01838 0.01478 = 0.02032 -0.00144 0.01090 0.00179 C7 1 0.517878 0.283635 0.441353 11.00000 0.01866 0.01919 = 0.01959 0.00038 0.00964 -0.00192 C8 1 0.634660 0.530921 0.377922 11.00000 0.02344 0.02025 = 0.02390 0.00280 0.01527 0.00293 H7A 2 0.475250 0.390182 0.411174 11.00000 0.01864 H7B 2 0.521703 0.217240 0.381042 11.00000 0.02339 H2 2 0.631866 0.194368 0.652171 11.00000 0.02983 H8A 2 0.687774 0.591924 0.366630 11.00000 0.02940 H8B 2 0.606432 0.435627 0.322310 11.00000 0.02604 H5 2 0.812825 0.584354 0.542565 11.00000 0.02922 H3 2 0.791744 0.277994 0.776497 11.00000 0.03349 H4 2 0.885449 0.478991 0.724479 11.00000 0.03916 PART 2 H1B 2 0.460528 0.223569 0.535129 10.50000 0.02639 PART 0 PART 1 H2A 2 0.522206 0.673821 0.292319 10.50000 0.02895 PART 0 PART 2 H2B 2 0.554709 0.708157 0.409665 10.50000 0.03006 PART 0 PART 1 H1A 2 0.486578 0.066589 0.491229 10.50000 0.03212 HKLF 4 REM bendim_a.res in C2/c REM R1 = 0.0344 for 1504 Fo > 4sig(Fo) and 0.0355 for all 1581 data REM 139 parameters refined using 0 restraints END WGHT 0.0552 0.6699 REM Instructions for potential hydrogen bonds HTAB C7 O2 HTAB O1 O2_$1 HTAB O2 O2_$2 HTAB O2 O1_$1 HTAB O1 O1_$3 REM Highest difference peak 0.316, deepest hole -0.167, 1-sigma level 0.038 Q1 1 0.6540 0.4963 0.4343 11.00000 0.05 0.32 Q2 1 0.5712 0.3158 0.4848 11.00000 0.05 0.30 Q3 1 0.6495 0.3967 0.5057 11.00000 0.05 0.27 Q4 1 0.6477 0.2999 0.5766 11.00000 0.05 0.26 Q5 1 0.7957 0.4545 0.6196 11.00000 0.05 0.26 Q6 1 0.7296 0.4653 0.5259 11.00000 0.05 0.25 Q7 1 0.7199 0.2859 0.6593 11.00000 0.05 0.22 Q8 1 0.7883 0.3783 0.6868 11.00000 0.05 0.21 ; _shelx_res_checksum 22497 _shelx_hkl_file ; -2 0 2 10.70 1.30 2 0 -2 11.20 1.30 -4 0 4 3347.77 118.09 -6 0 6 54.09 2.10 -6 0 6 53.19 2.50 -6 0 6 48.20 2.10 -6 0 6 57.09 2.30 6 0 -6 52.09 2.00 -6 0 6 55.29 2.10 8 0 -8 893.71 31.10 -8 0 8 874.11 31.10 -8 0 8 914.11 31.10 8 0 -8 866.21 31.10 -8 0 8 896.01 31.10 -8 0 8 888.91 31.20 -8 0 8 854.21 31.10 -10 0 10 254.07 9.20 -10 0 10 254.27 9.30 -10 0 10 261.97 9.20 -10 0 10 247.08 9.10 -10 0 10 253.17 9.20 10 0 -10 267.77 9.10 -10 0 10 223.18 9.90 -12 0 12 2.40 0.60 12 0 -12 3.00 0.60 -12 0 12 2.30 0.50 -12 0 12 3.20 0.60 -12 0 12 3.30 0.60 -14 0 14 1.60 0.60 -14 0 14 2.60 0.70 14 0 -14 1.30 0.90 -14 0 14 2.20 0.70 -14 0 14 2.20 0.60 1 1 -1 364.56 12.70 -1 1 1 287.47 12.50 -1 -1 1 362.56 12.70 1 -1 -1 348.67 12.60 -5 1 5 516.55 19.80 -5 1 5 512.05 18.20 -5 1 5 537.45 18.70 -5 1 5 487.45 18.20 -5 1 5 508.25 18.20 5 1 -5 532.25 18.20 -5 1 5 505.15 18.20 -5 -1 5 537.75 18.20 -5 -1 5 530.45 18.40 -5 -1 5 516.85 18.20 -5 -1 5 483.35 18.20 5 -1 -5 530.55 18.10 -5 -1 5 525.15 18.20 -7 1 7 247.28 8.40 -7 1 7 215.88 9.10 -7 1 7 235.28 8.40 7 1 -7 250.47 8.40 -7 1 7 231.68 8.40 -7 1 7 237.58 8.60 -7 1 7 242.98 8.40 -7 -1 7 236.18 8.40 -7 -1 7 235.08 8.40 -7 -1 7 238.88 8.60 7 -1 -7 231.98 8.30 -7 -1 7 206.98 8.70 -7 -1 7 243.38 8.50 -7 -1 7 241.58 8.50 -7 -1 7 237.18 8.50 -7 -1 7 228.48 8.40 9 1 -9 73.89 3.00 9 1 -9 75.99 2.90 -9 1 9 74.99 2.90 -9 1 9 63.79 3.80 -9 1 9 79.59 3.10 -9 1 9 74.89 2.90 -9 1 9 72.89 3.00 -9 1 9 78.09 3.00 -9 -1 9 72.59 3.00 -9 -1 9 75.19 3.10 -9 -1 9 75.19 3.00 -9 -1 9 74.19 3.00 -11 1 11 541.15 22.50 -11 1 11 631.94 21.80 -11 1 11 593.24 21.60 -11 1 11 617.54 21.60 -11 1 11 596.94 21.60 -11 -1 11 622.14 21.60 11 -1 -11 619.54 21.60 -11 -1 11 610.84 21.80 -11 -1 11 616.04 21.60 -11 -1 11 619.54 21.60 -13 1 13 37.40 2.10 -13 1 13 36.60 1.90 -13 1 13 37.90 1.90 13 1 -13 35.40 2.00 -13 1 13 35.90 1.80 -13 -1 13 37.20 1.90 -13 -1 13 37.20 2.00 -13 -1 13 35.80 1.80 13 -1 -13 36.00 1.80 -13 -1 13 37.80 1.90 -15 1 15 29.60 1.60 -15 1 15 25.80 1.80 -15 -1 15 28.00 1.70 -15 -1 15 25.60 2.00 15 -1 -15 25.10 1.90 -15 -1 15 26.00 1.60 0 2 0 571.94 20.30 -4 2 4 8.80 1.90 -4 2 4 5.50 0.50 -4 2 4 5.50 0.50 -4 -2 4 4.60 0.50 -4 -2 4 6.40 0.50 -4 -2 4 6.60 0.50 -6 2 6 159.38 5.90 -6 2 6 157.48 5.80 -6 2 6 164.38 5.90 6 2 -6 170.08 5.90 -6 2 6 162.38 5.90 -6 2 6 158.88 5.90 -6 2 6 154.78 6.00 -6 2 6 136.99 6.50 -6 -2 6 159.48 6.00 -6 -2 6 162.38 5.90 -6 -2 6 172.18 5.90 -6 -2 6 170.08 6.00 -6 -2 6 163.68 5.90 -6 -2 6 178.58 6.10 -6 -2 6 166.68 5.90 -8 2 8 140.39 5.00 -8 2 8 138.79 5.10 8 2 -8 142.59 5.00 -8 2 8 135.29 5.00 -8 2 8 122.49 5.90 -8 2 8 136.69 5.20 -8 -2 8 115.69 5.60 -8 -2 8 131.09 5.10 -8 -2 8 132.79 5.00 -8 -2 8 141.79 5.10 -8 -2 8 140.49 5.00 -8 -2 8 138.69 5.10 -8 -2 8 137.39 5.10 -10 2 10 10.70 0.90 10 2 -10 11.10 1.00 -10 2 10 12.30 1.10 -10 2 10 9.20 0.90 -10 2 10 9.70 1.90 -10 -2 10 10.50 1.00 -10 -2 10 8.70 1.00 12 2 -12 9.30 1.10 -12 2 12 8.20 1.10 -12 2 12 8.00 2.00 -12 2 12 8.40 1.00 -12 2 12 10.00 1.10 -12 -2 12 9.10 1.00 -12 -2 12 9.80 1.00 -12 -2 12 12.80 1.80 12 -2 -12 9.60 0.90 -14 2 14 1.80 0.70 -14 2 14 0.00 0.60 14 -2 -14 1.40 0.60 -14 -2 14 1.60 0.60 -14 -2 14 1.60 0.70 -14 -2 14 0.70 0.60 -1 3 1 12.50 1.90 1 3 -1 11.20 0.60 1 3 -1 10.40 0.80 -1 3 1 10.60 0.60 -1 3 1 10.20 1.00 1 3 -1 10.20 0.90 -1 -3 1 9.80 0.60 1 -3 -1 9.20 0.60 -1 -3 1 10.60 0.60 3 3 -3 28.90 1.40 -3 3 3 26.50 1.80 -3 3 3 31.80 1.20 -3 3 3 29.70 1.30 -3 3 3 30.00 1.30 -3 3 3 34.10 2.80 -3 3 3 31.60 1.40 -3 -3 3 32.50 1.30 -3 -3 3 32.00 1.30 5 3 -5 2408.36 80.29 -5 3 5 2293.37 80.29 -5 3 5 2103.99 81.09 -5 3 5 2363.56 80.29 -5 -3 5 2294.27 80.39 -7 3 7 7.60 1.50 -7 3 7 9.00 0.80 7 3 -7 9.20 0.90 -7 3 7 8.80 0.90 -7 3 7 9.00 0.90 -7 3 7 8.50 0.70 -7 3 7 9.30 0.80 -7 -3 7 8.90 0.70 -7 -3 7 9.10 0.90 -7 -3 7 9.20 0.80 -7 -3 7 8.50 0.90 -7 -3 7 8.80 0.80 -9 3 9 1.80 0.60 -9 3 9 3.10 1.40 9 3 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403.16 15.00 -2 4 -5 422.86 15.00 2 4 5 423.66 15.50 2 4 5 428.66 15.00 2 -4 5 440.66 15.10 2 -4 5 410.86 15.00 2 -4 5 413.76 15.00 2 -4 5 437.46 15.40 -2 -4 -5 423.96 15.00 0 4 7 209.68 7.50 0 4 7 188.98 11.40 0 4 7 198.48 7.40 0 4 -7 203.48 7.40 0 -4 7 213.58 7.80 0 -4 7 211.48 7.50 0 -4 7 193.78 7.30 0 -4 7 199.48 7.40 2 4 -9 275.97 9.40 -2 4 9 260.07 10.10 -2 4 9 259.87 9.40 -2 4 9 229.68 13.80 -2 -4 9 267.27 9.80 -2 -4 9 252.47 9.40 4 4 -11 0.70 0.40 -4 4 11 1.20 0.50 -4 4 11 1.20 0.90 -4 4 11 4.00 2.90 -4 -4 11 1.20 0.60 -4 -4 11 0.90 0.50 -4 -4 11 2.20 0.60 -4 -4 11 0.50 0.50 6 4 -13 17.30 1.10 -6 4 13 17.50 2.00 -6 4 13 16.70 1.30 -6 4 13 19.60 4.00 -6 -4 13 17.90 1.20 -6 -4 13 17.00 1.40 -6 -4 13 18.50 1.50 8 4 -15 23.50 1.40 -8 4 15 25.00 1.50 -8 -4 15 27.00 1.60 -8 -4 15 25.30 1.50 15 5 -8 6.70 1.50 -15 5 8 7.80 0.90 -15 5 8 5.70 2.30 -15 -5 8 9.10 0.90 15 -5 -8 7.30 1.00 -15 -5 8 9.60 1.20 13 5 -6 147.29 6.30 -13 5 6 151.98 5.90 -13 5 6 132.89 9.20 -13 5 6 164.68 6.00 -13 5 6 161.08 6.10 -13 -5 6 154.08 6.00 13 -5 -6 153.48 5.80 -13 -5 6 162.78 6.00 -11 5 4 31.80 1.80 -11 5 4 31.30 1.80 11 5 -4 30.60 2.20 -11 5 4 28.30 3.20 -11 -5 4 29.20 1.80 11 -5 -4 29.90 1.50 -11 -5 4 29.60 1.80 -11 -5 4 31.70 1.70 -9 5 2 0.80 1.30 -9 5 2 0.00 0.50 9 5 -2 1.80 0.90 -9 -5 2 0.30 0.60 -9 -5 2 0.00 0.50 -9 -5 2 0.60 0.60 -7 5 0 486.85 18.50 -7 5 0 498.25 17.40 -7 5 0 479.45 17.30 7 5 0 463.05 17.70 7 5 0 486.35 17.90 -7 -5 0 507.05 17.50 5 5 2 40.30 2.20 -5 5 -2 39.50 1.80 5 5 2 37.80 2.60 5 5 2 40.10 2.40 -5 5 -2 34.70 2.70 -5 -5 -2 42.10 1.90 5 -5 2 40.00 1.80 3 5 4 83.69 4.10 3 5 4 91.59 3.50 -3 5 -4 92.69 3.50 3 5 4 82.89 7.10 3 5 4 94.49 4.00 3 -5 4 83.39 3.80 3 -5 4 88.69 3.50 -3 -5 -4 91.09 3.50 1 5 6 179.68 6.70 1 5 6 195.28 7.40 1 5 6 173.88 10.70 -1 5 -6 182.38 6.60 1 -5 6 174.78 6.80 1 -5 6 184.78 7.10 -1 -5 -6 183.38 6.70 1 -5 6 166.38 6.60 1 -5 6 181.18 6.60 -1 5 8 100.89 3.90 1 5 -8 99.29 3.90 -1 5 8 109.29 4.70 -1 5 8 91.29 7.90 -1 -5 8 101.39 4.00 -1 -5 8 100.69 3.90 -1 -5 8 99.59 3.90 -1 -5 8 98.19 4.30 -3 5 10 87.39 7.70 3 5 -10 102.89 4.00 -3 5 10 110.49 4.90 -3 5 10 105.29 4.10 -3 -5 10 100.39 4.10 -3 -5 10 103.39 4.10 -3 -5 10 100.89 4.40 -3 -5 10 107.79 4.50 -3 -5 10 101.79 4.00 5 5 -12 1.70 0.50 -5 5 12 3.00 0.70 -5 5 12 4.10 2.50 -5 -5 12 2.60 0.70 -5 -5 12 1.50 0.60 -5 -5 12 4.20 0.80 -7 5 14 4.60 0.80 7 5 -14 4.10 0.60 -7 5 14 3.70 1.40 -7 -5 14 4.20 0.70 -7 -5 14 3.50 1.00 -7 -5 14 3.00 0.70 -14 6 7 8.30 2.40 14 6 -7 7.70 1.80 -14 6 7 9.20 1.10 14 -6 -7 9.20 1.00 -14 -6 7 10.50 1.10 -14 -6 7 10.90 1.20 -12 6 5 53.89 4.50 -12 6 5 62.49 2.80 12 6 -5 53.69 3.30 -12 -6 5 59.39 2.70 12 -6 -5 57.49 2.60 -12 -6 5 61.19 2.80 -10 6 3 15.60 3.00 10 6 -3 15.70 2.00 -10 6 3 17.00 1.30 -10 -6 3 16.80 1.40 -10 -6 3 18.20 1.40 10 -6 -3 16.90 1.20 -8 6 1 148.29 5.40 -8 6 1 133.09 6.90 -8 6 1 149.59 5.60 8 6 -1 143.79 6.10 -8 -6 1 144.29 5.60 6 6 1 878.51 34.10 -6 6 -1 964.00 33.60 -6 6 -1 960.50 33.50 -6 -6 -1 995.60 33.70 4 6 3 780.92 27.70 4 6 3 789.32 28.30 -4 6 -3 791.62 27.80 4 -6 3 774.62 27.80 4 -6 3 782.12 28.20 -4 -6 -3 786.22 28.00 2 6 5 129.29 9.50 2 6 5 152.58 5.70 2 6 5 154.68 6.40 -2 6 -5 154.28 5.70 -2 -6 -5 154.88 5.80 2 -6 5 157.38 6.20 2 -6 5 148.89 5.80 0 6 7 208.18 8.10 0 6 -7 205.08 7.30 0 6 7 169.38 10.90 0 6 7 202.08 7.30 0 -6 7 199.78 7.30 0 -6 7 190.58 7.70 0 -6 7 200.88 7.50 -2 6 9 5.50 0.80 2 6 -9 6.50 0.80 -2 6 9 7.40 3.00 -2 6 9 8.00 1.40 -2 -6 9 4.90 0.90 -2 -6 9 4.90 0.80 -2 -6 9 7.30 0.90 -4 6 11 85.49 4.30 4 6 -11 80.69 3.30 -4 6 11 83.69 3.40 -4 -6 11 83.29 3.70 -4 -6 11 83.79 3.40 -4 -6 11 81.09 3.50 6 6 -13 0.20 0.50 -6 6 13 -0.20 0.70 -6 6 13 -0.40 1.30 -6 -6 13 -0.20 0.60 -6 -6 13 0.20 0.60 -6 -6 13 0.40 0.80 -13 7 6 7.70 1.10 -13 -7 6 9.10 1.10 -13 -7 6 8.60 1.10 -11 7 4 73.09 3.10 11 7 -4 61.89 3.80 -11 7 4 68.89 5.10 -11 -7 4 74.29 3.00 -11 -7 4 60.69 3.70 9 7 -2 80.99 4.30 -9 7 2 90.89 3.60 -9 7 2 83.19 5.50 -9 -7 2 86.99 3.70 -9 -7 2 87.19 3.60 -7 7 0 5.50 0.70 -7 -7 0 7.60 1.00 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0 8 7 82.99 3.30 0 8 -7 82.09 3.30 0 8 7 78.49 4.20 0 -8 7 80.29 3.40 0 -8 7 79.19 3.60 -2 8 9 105.09 4.10 2 8 -9 102.69 4.00 -2 -8 9 106.79 4.10 -2 -8 9 98.89 4.20 -5 9 -2 1.20 0.70 5 -9 2 3.50 1.10 -3 9 -4 1188.88 41.30 3 -9 4 1158.98 41.50 -18 0 10 30.80 1.70 -18 0 10 33.20 1.70 -18 0 10 27.50 2.00 18 0 -10 29.00 1.90 16 0 -8 85.29 3.60 -16 0 8 85.69 3.50 -16 0 8 83.59 5.10 -16 0 8 82.79 3.60 -16 0 8 83.79 3.50 -12 0 4 39.40 1.90 12 0 -4 38.80 2.20 12 0 -4 41.30 1.90 -12 0 4 43.10 1.90 -12 0 4 41.50 1.90 -10 0 2 151.98 5.70 10 0 -2 155.38 5.90 -10 0 2 157.78 5.80 10 0 -2 156.08 5.80 -10 0 2 156.58 5.70 8 0 0 13.30 0.90 -8 0 0 13.10 0.80 8 0 0 13.90 0.90 -8 0 0 13.10 0.90 -8 0 0 11.10 0.90 8 0 0 12.70 0.80 4 0 4 228.18 8.20 4 0 4 214.58 8.10 -4 0 -4 222.98 8.00 4 0 4 212.78 8.10 4 0 4 242.88 10.60 4 0 4 225.88 8.10 2 0 6 37.80 1.70 2 0 6 34.30 1.80 2 0 6 37.90 1.70 2 0 6 40.00 1.70 2 0 6 37.90 1.90 2 0 6 37.50 1.50 2 0 6 35.60 3.90 0 0 8 839.62 30.30 0 0 8 879.61 30.40 0 0 8 881.91 30.30 0 0 8 850.51 30.50 0 0 8 864.41 30.20 0 0 8 826.12 33.80 0 0 8 880.21 30.30 0 0 8 871.91 30.40 0 0 8 846.42 30.20 -2 0 10 9.00 0.80 -2 0 10 8.30 0.80 -2 0 10 8.80 1.00 -2 0 10 8.10 0.70 -2 0 10 5.50 2.60 -2 0 10 7.70 1.10 -2 0 10 8.50 0.80 -4 0 12 1519.55 53.39 -4 0 12 1569.74 53.69 -4 0 12 1417.16 57.89 -4 0 12 1549.74 53.49 -4 0 12 1545.75 53.39 -4 0 12 1524.75 53.49 -6 0 14 13.70 1.10 -6 0 14 12.90 3.50 -6 0 14 13.80 1.10 -6 0 14 14.50 1.30 -8 0 16 240.78 8.80 -8 0 16 224.88 8.50 -19 1 11 25.00 1.50 -19 -1 11 24.70 1.40 -17 1 9 1122.79 41.70 -17 1 9 1191.48 41.90 17 1 -9 1175.28 42.00 -17 1 9 1196.18 41.70 17 -1 -9 1182.48 41.80 -17 -1 9 1204.38 41.70 -17 -1 9 1201.98 41.90 15 1 -7 432.36 15.70 -15 1 7 420.06 16.00 -15 1 7 415.96 15.60 -15 1 7 419.76 15.60 -15 1 7 462.95 17.00 15 -1 -7 441.56 15.60 -15 -1 7 430.86 15.70 -15 -1 7 432.16 16.10 -15 -1 7 430.76 15.60 -15 -1 7 433.56 16.60 13 1 -5 70.29 3.00 -13 1 5 69.89 3.00 -13 1 5 71.09 3.00 -13 -1 5 66.79 2.90 13 -1 -5 74.39 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295.27 10.90 5 -1 3 284.07 10.90 5 -1 3 312.17 11.00 -5 -1 -3 301.77 10.90 3 1 5 1536.35 53.09 3 1 5 1562.94 52.79 3 1 5 1548.65 55.89 3 1 5 1523.85 52.79 -3 1 -5 1467.95 52.59 3 1 5 1422.56 52.79 3 1 5 1373.66 52.89 -3 -1 -5 1431.26 52.69 3 -1 5 1449.95 52.79 3 -1 5 1601.44 52.89 3 -1 5 1559.24 52.79 3 -1 5 1546.05 55.49 3 -1 5 1495.35 52.69 3 -1 5 1489.15 52.79 3 -1 5 1560.24 52.89 3 -1 5 1516.25 52.89 1 1 7 381.46 13.00 1 1 7 351.86 12.90 1 1 7 361.36 12.90 1 1 7 354.86 13.00 1 1 7 382.56 13.10 1 1 7 339.57 13.00 -1 1 -7 357.46 12.90 1 1 7 374.76 13.30 1 1 7 358.66 16.40 1 -1 7 355.56 13.00 1 -1 7 363.76 13.20 1 -1 7 384.06 13.10 1 -1 7 377.56 12.90 1 -1 7 347.27 15.80 1 -1 7 363.66 13.00 1 -1 7 382.66 13.10 -1 1 9 149.69 5.70 -1 1 9 151.68 5.50 -1 1 9 147.99 5.90 -1 1 9 156.58 5.70 -1 1 9 142.99 9.20 -1 1 9 152.48 5.50 -1 1 9 151.58 5.60 -1 -1 9 150.28 5.80 -1 -1 9 161.78 5.90 -1 -1 9 152.88 5.60 -1 -1 9 144.89 8.80 -1 -1 9 150.38 5.50 -1 -1 9 156.28 5.70 -1 -1 9 150.78 5.60 -1 -1 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569.84 19.70 -16 -2 8 534.95 19.60 16 -2 -8 555.64 19.70 -16 -2 8 542.45 19.70 -14 2 6 1.30 0.60 -14 2 6 2.50 1.50 -14 2 6 1.10 0.60 -14 2 6 1.10 0.50 14 2 -6 2.60 0.70 14 -2 -6 2.10 0.60 -14 -2 6 1.80 0.60 -14 -2 6 1.00 0.70 -14 -2 6 2.40 0.70 -14 -2 6 0.40 0.50 -12 2 4 3158.98 110.59 12 2 -4 2952.60 110.69 -12 2 4 3203.88 110.49 -12 2 4 3142.69 110.49 12 2 -4 3301.07 110.69 -12 -2 4 3176.88 110.39 -12 -2 4 3174.88 110.49 -12 -2 4 3205.78 110.59 -12 -2 4 3071.49 110.49 -10 2 2 5.30 0.60 10 2 -2 4.40 0.70 10 2 -2 3.80 0.80 10 2 -2 4.90 2.30 -10 2 2 6.50 0.70 -10 -2 2 3.10 0.50 -10 -2 2 3.70 0.50 10 -2 -2 4.20 0.50 -10 -2 2 4.80 0.60 10 -2 -2 4.40 0.70 10 -2 -2 4.50 0.70 -10 -2 2 3.70 0.60 8 2 0 85.19 3.40 -8 2 0 80.89 3.20 8 2 0 88.69 3.40 -8 2 0 79.39 3.20 8 2 0 92.19 5.70 -8 2 0 83.79 3.20 8 -2 0 82.29 3.20 8 -2 0 74.39 3.20 -8 -2 0 82.79 3.20 8 -2 0 85.59 3.10 -8 -2 0 80.59 3.20 8 -2 0 82.49 3.30 8 -2 0 85.29 3.30 -8 -2 0 83.69 3.20 6 2 2 969.50 36.20 6 2 2 945.31 33.30 -6 2 -2 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-3 16.80 1.30 13 3 3 17.10 2.00 13 3 3 17.70 1.40 13 -3 3 15.10 4.30 -13 -3 -3 17.80 1.50 -11 3 -5 75.89 3.10 11 3 5 67.29 4.10 11 3 5 62.89 9.40 11 3 5 77.69 3.20 -11 -3 -5 74.09 3.20 11 -3 5 73.49 3.50 11 -3 5 70.59 7.70 -9 3 -7 9.90 1.10 9 3 7 12.20 4.60 9 3 7 10.50 1.20 9 -3 7 9.00 4.30 9 -3 7 11.90 1.60 -9 -3 -7 10.80 1.20 9 -3 7 8.90 1.10 7 3 9 2.40 3.60 7 3 9 0.00 0.60 7 -3 9 1.30 0.90 7 -3 9 0.30 0.70 -7 -3 -9 0.20 0.70 7 -3 9 -1.00 4.50 7 -3 9 -0.30 0.60 5 3 11 171.08 12.10 5 3 11 188.38 6.80 5 3 11 182.38 7.00 -5 3 -11 182.88 6.80 5 -3 11 185.08 6.70 5 -3 11 182.18 7.00 5 -3 11 176.38 6.80 3 3 13 4.70 4.00 3 3 13 3.80 0.70 3 -3 13 2.90 0.60 3 -3 13 5.10 0.80 3 -3 13 2.60 0.90 14 4 2 21.40 2.80 -14 4 -2 23.20 1.50 14 4 2 23.30 1.50 14 -4 2 19.30 5.60 -14 -4 -2 22.70 1.60 14 -4 2 21.30 2.20 -12 4 -4 2.30 0.70 12 4 4 4.80 0.90 12 4 4 2.10 1.60 -12 -4 -4 3.30 0.80 12 -4 4 4.10 1.10 12 -4 4 0.60 3.90 -10 4 -6 8.10 0.90 10 4 6 8.60 4.80 10 4 6 8.90 1.20 10 -4 6 6.60 4.80 -10 -4 -6 9.20 1.00 10 -4 6 7.10 1.20 8 4 8 16.30 5.10 -8 4 -8 19.60 1.40 8 4 8 21.40 1.40 8 -4 8 19.30 1.80 -8 -4 -8 18.20 1.50 8 -4 8 17.60 1.50 6 4 10 200.78 13.10 -6 4 -10 224.28 8.00 6 4 10 220.88 7.90 6 -4 10 205.28 8.00 6 -4 10 222.88 8.20 -4 4 -12 98.89 4.00 4 4 12 92.69 8.70 4 -4 12 107.79 4.10 4 -4 12 97.59 3.80 4 -4 12 95.29 3.90 13 5 3 115.99 4.50 13 -5 3 114.39 4.70 -13 -5 -3 112.59 4.50 -11 5 -5 -0.60 0.60 11 5 5 0.70 0.70 -11 -5 -5 0.80 0.80 11 -5 5 1.00 0.90 9 5 7 1.20 0.80 -9 5 -7 1.30 0.70 9 -5 7 3.20 0.90 -9 -5 -7 0.40 0.90 -7 5 -9 171.48 6.50 7 -5 9 176.58 6.70 16 0 1 -0.30 0.90 -16 0 -1 -0.80 0.90 -16 0 -1 -1.00 1.10 16 0 1 -1.30 3.60 -16 0 -1 -0.40 0.70 14 0 3 0.90 0.70 -14 0 -3 2.20 0.70 14 0 3 -1.60 3.10 -14 0 -3 0.40 0.70 -12 0 -5 -0.30 0.60 12 0 5 -0.90 3.20 12 0 5 0.30 1.40 -12 0 -5 -0.30 0.90 12 0 5 0.70 0.60 12 0 5 0.30 1.60 10 0 7 0.30 3.20 10 0 7 -0.70 1.40 10 0 7 3.30 1.30 10 0 7 0.20 0.60 10 0 7 1.30 0.80 -10 0 -7 2.10 0.70 8 0 9 0.20 3.40 8 0 9 -0.50 1.10 8 0 9 -0.40 1.40 8 0 9 0.20 0.60 8 0 9 0.30 0.70 6 0 11 -0.80 1.70 6 0 11 0.10 0.60 6 0 11 -0.10 3.70 6 0 11 0.60 1.30 6 0 11 1.30 0.70 4 0 13 0.60 0.70 -4 0 -13 1.00 0.90 4 0 13 -0.30 0.50 4 0 13 1.70 4.30 2 0 15 2.20 0.80 2 0 15 0.00 0.50 -17 1 0 13.30 1.40 17 1 0 11.80 1.20 17 -1 0 7.90 4.10 15 1 2 4.20 3.80 15 1 2 3.10 0.80 -15 1 -2 3.70 0.80 -15 1 -2 4.00 0.90 -15 -1 -2 3.60 0.90 15 -1 2 4.40 3.50 -15 -1 -2 4.40 0.90 15 -1 2 4.50 0.90 13 1 4 101.79 9.00 13 1 4 110.69 4.50 -13 1 -4 111.19 4.40 -13 1 -4 107.29 4.30 13 -1 4 107.99 4.30 13 -1 4 112.39 9.10 -13 -1 -4 111.79 4.40 -13 -1 -4 108.29 4.40 11 1 6 34.40 2.30 11 1 6 36.00 1.90 11 1 6 35.30 6.30 11 1 6 32.40 2.50 11 -1 6 34.70 2.40 11 -1 6 36.00 6.30 11 -1 6 32.20 2.90 11 -1 6 34.60 1.80 -11 -1 -6 36.70 1.90 9 1 8 2.20 0.70 9 1 8 6.00 1.50 9 1 8 3.30 3.70 9 1 8 1.70 1.20 9 1 8 2.20 0.70 9 -1 8 2.50 1.60 9 -1 8 2.00 1.30 -9 -1 -8 1.50 0.70 9 -1 8 3.50 3.70 9 -1 8 2.80 0.70 9 -1 8 3.40 0.80 7 1 10 168.88 6.30 7 1 10 171.58 6.30 7 1 10 156.68 6.50 7 1 10 156.78 6.70 7 1 10 169.38 17.30 -7 -1 -10 172.38 6.30 7 -1 10 164.58 6.30 7 -1 10 152.08 6.80 7 -1 10 169.98 6.20 7 -1 10 166.38 6.50 7 -1 10 160.88 11.70 5 1 12 2.90 4.00 5 1 12 3.20 0.70 5 1 12 4.40 0.70 5 -1 12 3.20 0.60 5 -1 12 4.60 4.60 5 -1 12 2.40 0.70 -5 -1 -12 1.80 0.90 3 1 14 100.79 9.40 3 1 14 110.39 4.40 3 1 14 117.99 4.80 3 -1 14 110.39 4.40 3 -1 14 119.89 4.40 -16 2 -1 53.19 2.50 -16 -2 -1 54.19 2.50 16 -2 1 55.19 6.60 -14 2 -3 35.70 1.90 -14 2 -3 36.30 2.00 14 2 3 36.60 7.00 14 2 3 40.20 2.00 14 -2 3 31.40 5.80 -14 -2 -3 40.50 2.00 12 2 5 -2.20 3.40 12 2 5 0.50 0.60 -12 2 -5 0.80 0.60 12 -2 5 0.00 0.70 12 -2 5 -2.00 3.20 -12 -2 -5 0.30 0.70 10 2 7 45.50 2.10 -10 2 -7 41.80 2.10 10 2 7 38.80 2.50 10 2 7 40.80 2.60 10 -2 7 41.90 2.00 10 -2 7 39.50 6.90 -10 -2 -7 44.20 2.10 8 2 9 45.10 2.20 8 2 9 45.00 2.80 -8 2 -9 43.40 2.20 8 2 9 41.70 2.50 8 2 9 44.40 2.70 8 2 9 42.60 6.90 8 -2 9 39.80 7.00 8 -2 9 44.10 2.10 -8 -2 -9 45.80 2.40 8 -2 9 44.00 2.20 6 2 11 0.70 0.70 6 2 11 0.20 0.60 6 2 11 1.20 3.60 6 -2 11 0.90 0.60 6 -2 11 0.60 0.70 -6 -2 -11 0.70 0.80 6 -2 11 -1.20 4.70 4 2 13 84.09 3.50 4 2 13 82.39 8.60 4 -2 13 85.09 3.50 4 -2 13 84.89 3.40 -15 3 -2 21.60 1.50 15 3 2 23.40 2.00 15 -3 2 22.10 5.60 -15 -3 -2 20.90 1.50 13 3 4 35.90 7.80 13 3 4 37.60 2.00 -13 3 -4 35.50 2.00 -13 3 -4 36.90 1.90 -13 -3 -4 38.20 2.00 13 -3 4 34.60 6.00 11 3 6 71.19 8.40 -11 3 -6 76.49 3.20 11 3 6 80.19 3.30 -11 -3 -6 78.09 3.30 11 -3 6 73.39 7.90 -9 3 -8 1.70 0.70 9 3 8 -0.20 0.60 9 3 8 1.00 3.80 9 -3 8 -0.70 4.30 9 -3 8 1.70 0.70 -9 -3 -8 1.70 0.80 7 3 10 224.08 13.90 -7 3 -10 234.18 8.60 7 3 10 245.28 8.60 -7 -3 -10 236.08 8.60 7 -3 10 230.08 8.50 7 -3 10 226.08 8.60 5 3 12 16.20 5.00 5 3 12 16.50 1.20 5 -3 12 16.40 1.20 5 -3 12 16.10 1.30 14 4 3 29.60 1.60 -14 -4 -3 29.00 1.80 -12 4 -5 2.00 0.70 12 4 5 0.30 0.90 -12 -4 -5 -0.10 0.80 10 4 7 24.00 6.00 -10 4 -7 27.60 1.60 -10 -4 -7 26.40 1.70 10 -4 7 26.70 2.10 -8 4 -9 113.99 4.40 8 4 9 116.09 4.30 8 4 9 97.59 9.50 8 -4 9 116.29 4.60 -8 -4 -9 108.19 4.40 6 4 11 133.29 5.00 6 4 11 123.59 13.00 6 -4 11 135.89 5.20 6 -4 11 127.89 5.30 16 0 2 17.00 1.30 16 0 2 12.80 4.60 14 0 4 -3.80 3.40 -14 0 -4 -0.70 0.80 -14 0 -4 0.00 0.70 14 0 4 -0.40 0.60 12 0 6 9.70 1.10 12 0 6 10.40 4.20 -12 0 -6 8.10 1.10 -12 0 -6 11.40 1.20 -10 0 -8 1269.57 42.90 10 0 8 1289.67 42.90 10 0 8 1167.38 48.60 10 0 8 1133.29 42.80 8 0 10 -0.30 0.60 8 0 10 -0.40 0.70 8 0 10 0.80 3.70 -8 0 -10 0.30 0.70 6 0 12 2.80 4.20 6 0 12 5.00 0.70 6 0 12 5.40 0.80 -6 0 -12 5.00 0.90 -15 1 -3 26.90 1.70 -15 1 -3 27.00 1.80 15 1 3 29.50 6.40 15 -1 3 25.60 1.60 15 -1 3 21.30 5.70 -15 -1 -3 27.70 1.70 13 1 5 123.79 4.80 13 1 5 121.69 9.70 -13 1 -5 120.39 4.80 -13 1 -5 126.99 4.80 -13 -1 -5 127.59 4.80 13 -1 5 120.59 4.70 13 -1 5 118.19 9.50 11 1 7 61.99 7.40 -11 1 -7 63.99 2.90 11 1 7 67.59 2.90 -11 1 -7 65.09 2.90 11 -1 7 70.69 7.80 11 -1 7 64.19 2.80 -11 -1 -7 67.49 2.90 9 1 9 36.90 1.90 9 1 9 32.00 1.90 9 1 9 42.70 6.90 9 -1 9 35.90 1.80 9 -1 9 34.10 6.60 -9 -1 -9 37.20 1.90 9 -1 9 33.90 1.90 7 1 11 85.59 8.80 7 1 11 95.59 3.70 7 1 11 93.19 3.70 7 -1 11 89.09 3.70 -7 -1 -11 97.39 3.80 7 -1 11 81.79 8.90 7 -1 11 96.29 3.70 5 1 13 75.69 2.90 5 1 13 57.79 8.20 5 1 13 70.99 3.00 5 -1 13 78.49 2.90 5 -1 13 70.29 3.00 14 2 4 20.00 1.40 -14 2 -4 23.00 1.60 -14 2 -4 22.10 1.50 14 2 4 16.30 5.30 14 -2 4 19.30 5.00 -14 -2 -4 21.40 1.50 12 2 6 119.99 9.90 -12 2 -6 135.29 5.00 12 2 6 130.89 5.00 -12 2 -6 120.49 4.90 12 -2 6 125.09 5.00 12 -2 6 125.79 9.70 -12 -2 -6 133.39 5.00 10 2 8 1.80 0.60 -10 2 -8 2.30 0.80 10 2 8 -0.10 3.80 10 -2 8 1.20 4.00 -10 -2 -8 1.10 0.70 10 -2 8 1.90 0.70 -8 2 -10 99.19 4.60 8 2 10 95.59 8.90 8 2 10 107.69 4.00 8 -2 10 91.59 4.00 8 -2 10 99.49 3.90 8 -2 10 94.29 9.50 -8 -2 -10 102.39 4.00 6 2 12 82.59 3.20 6 2 12 75.19 8.30 6 2 12 79.09 3.30 6 -2 12 77.19 3.30 6 -2 12 80.69 3.20 13 3 5 60.49 2.50 -13 3 -5 55.89 2.60 -13 3 -5 55.99 2.90 13 -3 5 50.09 11.60 -13 -3 -5 56.59 2.60 11 3 7 2.00 4.50 -11 3 -7 2.60 0.80 -11 -3 -7 4.10 0.90 11 -3 7 3.80 5.50 -9 3 -9 37.50 2.00 9 3 9 38.80 1.90 9 3 9 39.10 7.00 9 -3 9 35.00 1.90 -9 -3 -9 38.10 2.10 7 3 11 144.39 11.20 7 3 11 164.78 5.80 7 -3 11 149.69 5.70 -14 0 -5 0.90 0.80 14 0 5 1.10 0.60 14 0 5 -2.50 3.80 12 0 7 0.30 0.70 -12 0 -7 -0.30 0.70 12 0 7 1.10 3.90 -10 0 -9 -0.20 0.70 10 0 9 -0.40 4.10 8 0 11 -0.70 4.70 -8 0 -11 -0.10 0.80 8 0 11 -0.80 0.50 8 0 11 -0.70 1.10 -13 1 -6 282.97 10.10 13 1 6 289.97 10.10 13 1 6 253.07 14.80 13 -1 6 281.37 10.00 -13 -1 -6 295.37 10.10 13 -1 6 256.27 14.80 11 1 8 44.20 6.90 -11 1 -8 52.69 2.30 11 -1 8 46.00 7.00 11 -1 8 48.40 2.20 -11 -1 -8 50.99 2.30 9 1 10 5.50 0.70 9 1 10 5.90 4.40 -9 1 -10 6.20 0.90 -9 -1 -10 6.30 0.90 9 -1 10 4.80 0.70 9 -1 10 4.60 5.10 12 2 7 0.80 0.60 -12 2 -7 0.90 0.80 -12 -2 -7 1.10 0.80 12 -2 7 -0.20 0.80 10 2 9 161.98 14.30 10 2 9 181.38 6.50 10 -2 9 170.28 6.40 -10 -2 -9 175.98 6.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 23483 _shelx_shelxl_version_number 2016/6 _olex2_submission_special_instructions 'No special instructions were received' 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 O1 O 0.46834(5) 0.17177(9) 0.48451(6) 0.02331(19) Uani 1 1 d . . . . . O2 O 0.55534(5) 0.65481(9) 0.35730(6) 0.02337(19) Uani 1 1 d . . . . . C1 C 0.62287(6) 0.33987(11) 0.52330(7) 0.0163(2) Uani 1 1 d . . . . . C2 C 0.66708(7) 0.27521(12) 0.62931(7) 0.0209(2) Uani 1 1 d . . . . . C3 C 0.76412(7) 0.32514(13) 0.70391(7) 0.0250(2) Uani 1 1 d . . . . . C4 C 0.81817(7) 0.43997(13) 0.67229(8) 0.0252(2) Uani 1 1 d . . . . . C5 C 0.77497(6) 0.50466(12) 0.56636(8) 0.0221(2) Uani 1 1 d . . . . . C6 C 0.67783(6) 0.45669(11) 0.49145(7) 0.0170(2) Uani 1 1 d . . . . . C7 C 0.51788(6) 0.28363(12) 0.44135(7) 0.0188(2) Uani 1 1 d . . . . . C8 C 0.63466(7) 0.53092(12) 0.37792(7) 0.0208(2) Uani 1 1 d . . . . . H7A H 0.4753(8) 0.3902(15) 0.4112(9) 0.019(3) Uiso 1 1 d . . . . . H7B H 0.5217(8) 0.2172(16) 0.3810(10) 0.023(3) Uiso 1 1 d . . . . . H2 H 0.6319(9) 0.1944(17) 0.6522(10) 0.030(3) Uiso 1 1 d . . . . . H8A H 0.6878(9) 0.5919(17) 0.3666(10) 0.029(3) Uiso 1 1 d . . . . . H8B H 0.6064(9) 0.4356(17) 0.3223(10) 0.026(3) Uiso 1 1 d . . . . . H5 H 0.8128(9) 0.5844(17) 0.5426(10) 0.029(3) Uiso 1 1 d . . . . . H3 H 0.7917(9) 0.2780(18) 0.7765(11) 0.033(3) Uiso 1 1 d . . . . . H4 H 0.8854(10) 0.4790(18) 0.7245(11) 0.039(4) Uiso 1 1 d . . . . . H1B H 0.4605(18) 0.224(4) 0.535(2) 0.026(6) Uiso 0.5 1 d . . P A 2 H2A H 0.522(2) 0.674(3) 0.292(2) 0.029(6) Uiso 0.5 1 d . . P B 1 H2B H 0.555(2) 0.708(4) 0.410(2) 0.030(6) Uiso 0.5 1 d . . P C 2 H1A H 0.487(2) 0.067(4) 0.491(2) 0.032(7) Uiso 0.5 1 d . . P D 1 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 0.0268(4) 0.0197(3) 0.0287(4) -0.0027(3) 0.0174(3) -0.0060(3) O2 0.0263(4) 0.0224(4) 0.0240(4) 0.0035(3) 0.0138(3) 0.0064(3) C1 0.0171(4) 0.0154(4) 0.0180(4) -0.0010(3) 0.0095(3) 0.0021(3) C2 0.0218(4) 0.0236(4) 0.0203(4) 0.0030(3) 0.0124(3) 0.0055(3) C3 0.0231(5) 0.0333(5) 0.0173(4) -0.0008(3) 0.0081(4) 0.0103(4) C4 0.0179(4) 0.0281(5) 0.0251(5) -0.0102(4) 0.0062(3) 0.0030(3) C5 0.0194(4) 0.0181(4) 0.0301(5) -0.0052(3) 0.0124(4) -0.0009(3) C6 0.0184(4) 0.0148(4) 0.0203(4) -0.0014(3) 0.0109(3) 0.0018(3) C7 0.0187(4) 0.0192(4) 0.0196(4) 0.0004(3) 0.0096(3) -0.0019(3) C8 0.0234(4) 0.0203(4) 0.0239(4) 0.0028(3) 0.0153(4) 0.0029(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0140 0.0070 '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 0.0390 0.0250 '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 C7 O1 H1B 111.6(17) . . C7 O1 H1A 113.8(19) . . C8 O2 H2A 111.3(19) . . C8 O2 H2B 118.7(19) . . C2 C1 C6 118.95(8) . . C2 C1 C7 121.25(8) . . C6 C1 C7 119.78(7) . . C1 C2 C3 121.09(9) . . C1 C2 H2 120.4(8) . . C3 C2 H2 118.5(8) . . C2 C3 H3 118.5(8) . . C4 C3 C2 119.85(9) . . C4 C3 H3 121.7(8) . . C3 C4 C5 119.58(8) . . C3 C4 H4 120.6(8) . . C5 C4 H4 119.8(8) . . C4 C5 C6 121.03(9) . . C4 C5 H5 120.4(7) . . C6 C5 H5 118.6(7) . . C1 C6 C8 121.68(8) . . C5 C6 C1 119.50(8) . . C5 C6 C8 118.82(8) . . O1 C7 C1 114.49(7) . . O1 C7 H7A 107.2(6) . . O1 C7 H7B 107.2(7) . . C1 C7 H7A 109.7(7) . . C1 C7 H7B 109.0(7) . . H7A C7 H7B 109.1(10) . . O2 C8 C6 111.69(7) . . O2 C8 H8A 108.7(7) . . O2 C8 H8B 107.2(7) . . C6 C8 H8A 110.1(7) . . C6 C8 H8B 111.5(7) . . H8A C8 H8B 107.5(10) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O1 C7 1.4228(10) . O1 H1B 0.85(3) . O1 H1A 0.83(3) . O2 C8 1.4336(10) . O2 H2A 0.82(2) . O2 H2B 0.83(3) . C1 C2 1.3903(12) . C1 C6 1.4071(12) . C1 C7 1.5187(11) . C2 C3 1.3952(13) . C2 H2 0.950(13) . C3 C4 1.3860(15) . C3 H3 0.961(13) . C4 C5 1.3897(14) . C4 H4 0.979(14) . C5 C6 1.3935(12) . C5 H5 0.981(13) . C6 C8 1.5042(12) . C7 H7A 0.990(11) . C7 H7B 0.996(12) . C8 H8A 0.992(13) . C8 H8B 0.993(12) . 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 C7 H7A O2 0.990(11) 2.605(11) 3.1728(11) 116.5(8) . O1 H1B O2 0.85(3) 1.85(3) 2.7070(10) 178(3) 5_666 O2 H2A O2 0.82(2) 1.86(2) 2.6533(15) 165(2) 2_655 O2 H2B O1 0.83(3) 1.88(3) 2.7070(10) 171(3) 5_666 O1 H1A O1 0.83(3) 1.89(3) 2.7191(14) 177(3) 5_656 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 C1 C2 C3 C4 -0.50(14) . . . . C1 C6 C8 O2 69.42(10) . . . . C2 C1 C6 C5 0.10(12) . . . . C2 C1 C6 C8 179.74(7) . . . . C2 C1 C7 O1 4.03(12) . . . . C2 C3 C4 C5 0.13(14) . . . . C3 C4 C5 C6 0.36(13) . . . . C4 C5 C6 C1 -0.47(13) . . . . C4 C5 C6 C8 179.87(8) . . . . C5 C6 C8 O2 -110.93(9) . . . . C6 C1 C2 C3 0.38(13) . . . . C6 C1 C7 O1 -177.32(7) . . . . C7 C1 C2 C3 179.05(8) . . . . C7 C1 C6 C5 -178.58(7) . . . . C7 C1 C6 C8 1.06(12) . . . . _cod_database_fobs_code 3500068