# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2021 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_wv580 _database_code_depnum_ccdc_archive 'CCDC 2044215' loop_ _audit_author_name _audit_author_address 'Peter Mayer' ;LMU Muenchen Germany ; _audit_update_record ; 2020-11-13 deposited with the CCDC. 2021-02-09 downloaded from the CCDC. ; _chemical_name_common RM436 _chemical_compound_source ? _chemical_absolute_configuration ? _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.100 #?# in millimeters _exptl_crystal_size_mid 0.030 #?# in millimeters _exptl_crystal_size_min 0.020 #?# in millimeters _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_special_details ; ; _audit_creation_date ? #?# style: 18-Aug-1998 _diffrn_ambient_temperature 108.(2) #?# in K _diffrn_source_type 'Bruker TXS' _diffrn_source_power 2.5 #?# in kW _diffrn_source_voltage 50 #?# in kV _diffrn_source_current 50 #?# in mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode (TXS)' _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_collimation ? _diffrn_measurement_device 'fixed-chi three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture TXS' _diffrn_measurement_method 'mix of phi and omega scans' _diffrn_measurement_details ? _diffrn_detector_area_resol_mean 7.3910 _diffrn_special_details ? _diffrn_orient_matrix_type ? _diffrn_orient_matrix_UB_11 ? _diffrn_orient_matrix_UB_12 ? _diffrn_orient_matrix_UB_13 ? _diffrn_orient_matrix_UB_21 ? _diffrn_orient_matrix_UB_22 ? _diffrn_orient_matrix_UB_23 ? _diffrn_orient_matrix_UB_31 ? _diffrn_orient_matrix_UB_32 ? _diffrn_orient_matrix_UB_33 ? _cell_length_a 14.2681(7) _cell_length_b 3.9182(2) _cell_length_c 17.1782(10) _cell_angle_alpha 90 _cell_angle_beta 109.954(2) _cell_angle_gamma 90 _cell_volume 902.70(8) _cell_measurement_temperature 108.(2) #?# in K _cell_measurement_reflns_used 3311 _cell_measurement_theta_min 3.0378 _cell_measurement_theta_max 26.7428 _cell_special_details ? _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 1.00 _shelx_estimated_absorpt_T_min 0.991 _shelx_estimated_absorpt_T_max 0.998 _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _diffrn_reflns_number 8211 #xl _diffrn_reflns_av_R_equivalents 0.0394 #xl _diffrn_reflns_av_unetI/netI 0.0335 #xl _diffrn_reflns_limit_h_min -17 #xl _diffrn_reflns_limit_h_max 18 #xl _diffrn_reflns_limit_k_min -4 #xl _diffrn_reflns_limit_k_max 4 #xl _diffrn_reflns_limit_l_min -21 #xl _diffrn_reflns_limit_l_max 17 #xl _diffrn_reflns_theta_min 3.219 #xl _diffrn_reflns_theta_max 26.732 #xl _diffrn_measured_fraction_theta_max 0.998 #xl _diffrn_reflns_theta_full 25.242 #xl _diffrn_measured_fraction_theta_full 0.998 #xl _diffrn_reflns_Laue_measured_fraction_max 0.998 #xl _diffrn_reflns_Laue_measured_fraction_full 0.998 #xl _diffrn_reflns_point_group_measured_fraction_max 0.998 #xl _diffrn_reflns_point_group_measured_fraction_full 0.998 #xl _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' _space_group_IT_number 14 _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_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' N N 0.0061 0.0033 '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' _reflns_number_total 1897 #xl _reflns_number_gt 1521 #xl _reflns_threshold_expression 'I > 2\s(I)' #xl _reflns_Friedel_coverage 0.000 #xl _reflns_Friedel_fraction_max . #xl _reflns_Friedel_fraction_full . #xl _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. ; _refine_ls_structure_factor_coef Fsqd #xl _refine_ls_matrix_type full #xl _refine_ls_weighting_scheme calc #xl _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.5869P] where P=(Fo^2^+2Fc^2^)/3' #xl _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr #?# _refine_ls_extinction_method none #xl _refine_ls_extinction_coef . #xl _refine_ls_abs_structure_details ? #xl _refine_ls_abs_structure_Flack ? #xl _refine_ls_number_reflns 1897 #xl _refine_ls_number_parameters 136 #xl _refine_ls_number_restraints 0 #xl _refine_ls_R_factor_all 0.0598 #xl _refine_ls_R_factor_gt 0.0460 #xl _refine_ls_wR_factor_ref 0.1119 #xl _refine_ls_wR_factor_gt 0.1064 #xl _refine_ls_goodness_of_fit_ref 1.089 #xl _refine_ls_restrained_S_all 1.089 #xl _refine_ls_shift/su_max 0.000 #xl _refine_ls_shift/su_mean 0.000 #xl _refine_diff_density_max 0.243 #xl _refine_diff_density_min -0.243 #xl _refine_diff_density_rms 0.047 #xl _refine_special_details ; ; _computing_data_collection 'APEX3 v2016.5-0, Bruker AXS (2016)' _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 833)' _computing_publication_material ? 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 0.31101(9) 0.0642(4) 0.05504(7) 0.0248(3) Uani 1 1 d . . . . . N1 N 0.26954(10) 0.1378(4) 0.30372(8) 0.0173(3) Uani 1 1 d . . . . . N2 N 0.07342(12) 0.5432(5) 0.34323(10) 0.0304(4) Uani 1 1 d . . . . . C1 C 0.30786(13) 0.0533(5) 0.38599(10) 0.0211(4) Uani 1 1 d . . . . . H1 H 0.274181 0.118697 0.422753 0.025 Uiso 1 1 calc R U . . . C2 C 0.39413(13) -0.1242(5) 0.41418(11) 0.0235(4) Uani 1 1 d . . . . . H2 H 0.420674 -0.185373 0.471045 0.028 Uiso 1 1 calc R U . . . C3 C 0.44548(13) -0.2202(5) 0.36016(11) 0.0223(4) Uani 1 1 d . . . . . H3 H 0.506463 -0.342686 0.380718 0.027 Uiso 1 1 calc R U . . . C4 C 0.40656(12) -0.1350(5) 0.27801(10) 0.0191(4) Uani 1 1 d . . . . . H4 H 0.440437 -0.199465 0.241324 0.023 Uiso 1 1 calc R U . . . C5 C 0.31684(12) 0.0471(4) 0.24803(10) 0.0165(4) Uani 1 1 d . . . . . C6 C 0.25582(12) 0.1710(5) 0.17067(10) 0.0170(4) Uani 1 1 d . . . . . C7 C 0.25109(13) 0.1795(5) 0.08501(10) 0.0181(4) Uani 1 1 d . . . . . C8 C 0.15358(13) 0.3585(5) 0.03661(10) 0.0205(4) Uani 1 1 d . . . . . H8A H 0.110596 0.204472 -0.006574 0.025 Uiso 1 1 calc R U . . . H8B H 0.167262 0.565719 0.009284 0.025 Uiso 1 1 calc R U . . . C9 C 0.10074(12) 0.4565(5) 0.09892(10) 0.0193(4) Uani 1 1 d . . . . . H9A H 0.091010 0.706320 0.100100 0.023 Uiso 1 1 calc R U . . . H9B H 0.035338 0.341215 0.085192 0.023 Uiso 1 1 calc R U . . . C10 C 0.17288(12) 0.3303(4) 0.17978(10) 0.0170(4) Uani 1 1 d . . . . . C11 C 0.18063(12) 0.3136(5) 0.26170(10) 0.0186(4) Uani 1 1 d . . . . . C12 C 0.11997(13) 0.4397(5) 0.30575(10) 0.0219(4) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0250(7) 0.0347(8) 0.0186(6) -0.0014(6) 0.0123(5) 0.0009(6) N1 0.0193(7) 0.0186(8) 0.0147(7) -0.0018(6) 0.0069(6) -0.0018(6) N2 0.0330(9) 0.0391(10) 0.0236(8) 0.0024(8) 0.0154(7) 0.0118(8) C1 0.0248(9) 0.0253(10) 0.0139(8) -0.0018(7) 0.0075(7) -0.0040(8) C2 0.0251(9) 0.0272(10) 0.0153(8) 0.0022(7) 0.0030(7) -0.0033(8) C3 0.0189(9) 0.0232(10) 0.0226(9) 0.0011(8) 0.0043(7) -0.0009(8) C4 0.0197(9) 0.0184(9) 0.0207(9) -0.0018(7) 0.0090(7) -0.0027(7) C5 0.0181(8) 0.0174(9) 0.0162(8) -0.0037(7) 0.0085(7) -0.0042(7) C6 0.0172(8) 0.0185(9) 0.0165(8) -0.0029(7) 0.0072(7) -0.0039(7) C7 0.0202(8) 0.0179(9) 0.0175(8) -0.0012(7) 0.0081(7) -0.0042(7) C8 0.0247(9) 0.0222(10) 0.0158(8) 0.0013(7) 0.0082(7) -0.0004(8) C9 0.0177(8) 0.0213(9) 0.0191(8) 0.0011(7) 0.0065(7) -0.0002(7) C10 0.0178(8) 0.0162(9) 0.0185(8) -0.0018(7) 0.0081(7) -0.0027(7) C11 0.0184(8) 0.0207(9) 0.0185(8) -0.0015(7) 0.0086(7) -0.0001(7) C12 0.0225(9) 0.0271(10) 0.0159(8) 0.0012(7) 0.0064(7) 0.0024(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C7 1.225(2) . ? N1 C1 1.371(2) . ? N1 C5 1.392(2) . ? N1 C11 1.407(2) . ? N2 C12 1.145(2) . ? C1 C2 1.351(3) . ? C1 H1 0.9500 . ? C2 C3 1.415(3) . ? C2 H2 0.9500 . ? C3 C4 1.370(2) . ? C3 H3 0.9500 . ? C4 C5 1.401(2) . ? C4 H4 0.9500 . ? C5 C6 1.404(2) . ? C6 C10 1.393(2) . ? C6 C7 1.450(2) . ? C7 C8 1.526(2) . ? C8 C9 1.553(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.502(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.375(2) . ? C11 C12 1.419(2) . ? 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 N1 C5 122.04(15) . . ? C1 N1 C11 128.31(14) . . ? C5 N1 C11 109.64(13) . . ? C2 C1 N1 119.20(16) . . ? C2 C1 H1 120.4 . . ? N1 C1 H1 120.4 . . ? C1 C2 C3 120.91(16) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 119.48(17) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 120.07(16) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? N1 C5 C4 118.29(15) . . ? N1 C5 C6 105.83(14) . . ? C4 C5 C6 135.88(15) . . ? C10 C6 C5 108.96(14) . . ? C10 C6 C7 110.88(15) . . ? C5 C6 C7 140.15(16) . . ? O1 C7 C6 128.35(17) . . ? O1 C7 C8 125.28(15) . . ? C6 C7 C8 106.35(14) . . ? C7 C8 C9 107.74(13) . . ? C7 C8 H8A 110.2 . . ? C9 C8 H8A 110.2 . . ? C7 C8 H8B 110.2 . . ? C9 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? C10 C9 C8 102.43(13) . . ? C10 C9 H9A 111.3 . . ? C8 C9 H9A 111.3 . . ? C10 C9 H9B 111.3 . . ? C8 C9 H9B 111.3 . . ? H9A C9 H9B 109.2 . . ? C11 C10 C6 108.59(15) . . ? C11 C10 C9 138.79(16) . . ? C6 C10 C9 112.57(14) . . ? C10 C11 N1 106.97(14) . . ? C10 C11 C12 132.74(16) . . ? N1 C11 C12 120.27(15) . . ? N2 C12 C11 178.04(19) . . ? 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 C5 N1 C1 C2 -0.1(3) . . . . ? C11 N1 C1 C2 178.57(17) . . . . ? N1 C1 C2 C3 0.6(3) . . . . ? C1 C2 C3 C4 -0.7(3) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? C1 N1 C5 C4 -0.3(2) . . . . ? C11 N1 C5 C4 -179.18(15) . . . . ? C1 N1 C5 C6 179.13(15) . . . . ? C11 N1 C5 C6 0.22(19) . . . . ? C3 C4 C5 N1 0.2(3) . . . . ? C3 C4 C5 C6 -179.0(2) . . . . ? N1 C5 C6 C10 -0.56(19) . . . . ? C4 C5 C6 C10 178.69(19) . . . . ? N1 C5 C6 C7 -179.0(2) . . . . ? C4 C5 C6 C7 0.2(4) . . . . ? C10 C6 C7 O1 -179.99(18) . . . . ? C5 C6 C7 O1 -1.5(4) . . . . ? C10 C6 C7 C8 -1.1(2) . . . . ? C5 C6 C7 C8 177.4(2) . . . . ? O1 C7 C8 C9 179.07(17) . . . . ? C6 C7 C8 C9 0.11(19) . . . . ? C7 C8 C9 C10 0.78(19) . . . . ? C5 C6 C10 C11 0.7(2) . . . . ? C7 C6 C10 C11 179.64(15) . . . . ? C5 C6 C10 C9 -177.26(15) . . . . ? C7 C6 C10 C9 1.7(2) . . . . ? C8 C9 C10 C11 -178.6(2) . . . . ? C8 C9 C10 C6 -1.5(2) . . . . ? C6 C10 C11 N1 -0.5(2) . . . . ? C9 C10 C11 N1 176.6(2) . . . . ? C6 C10 C11 C12 178.0(2) . . . . ? C9 C10 C11 C12 -4.8(4) . . . . ? C1 N1 C11 C10 -178.62(17) . . . . ? C5 N1 C11 C10 0.2(2) . . . . ? C1 N1 C11 C12 2.6(3) . . . . ? C5 N1 C11 C12 -178.60(17) . . . . ? _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. ; _audit_block_code C12H8N2O_wv580_mayr _audit_creation_method 'APEX3 v2017.3-0' _shelxl_version_number ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H8 N2 O' _chemical_formula_sum 'C12 H8 N2 O' _chemical_formula_weight 196.20 #?# (Cohen, 1996) _chemical_melting_point ? #?# in K! _cell_formula_units_Z 4 #?# adjust to _chemical_formula_[] _exptl_crystal_density_diffrn 1.444 _exptl_crystal_F_000 408 #?# check! _shelx_res_file ; TITL wv580_0m_a.res in P2(1)/c wv580_0m_a.res created by SHELXL-2016/6 at 14:26:41 on 14-Nov-2018 REM Old TITL wv580_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.112, Rweak 0.003, Alpha 0.032, Orientation as input REM Formula found by SHELXT: C12 N2 O CELL 0.71073 14.2681 3.9182 17.1782 90.000 109.954 90.000 ZERR 4.000 0.0007 0.0002 0.0010 0.000 0.002 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O UNIT 48 32 8 4 TEMP -165 SIZE 0.02 0.03 0.10 L.S. 10 BOND $H LIST 4 CONF ACTA SHEL 9.0 0.79 OMIT 0 0 2 OMIT -1 0 2 FMAP 2 PLAN -20 WGHT 0.042600 0.586900 FVAR 0.95196 O1 4 0.311008 0.064181 0.055037 11.00000 0.02504 0.03471 = 0.01858 -0.00138 0.01233 0.00089 N1 3 0.269541 0.137841 0.303721 11.00000 0.01931 0.01856 = 0.01474 -0.00177 0.00690 -0.00178 N2 3 0.073418 0.543201 0.343235 11.00000 0.03300 0.03912 = 0.02356 0.00237 0.01537 0.01182 C1 1 0.307860 0.053310 0.385990 11.00000 0.02484 0.02535 = 0.01390 -0.00177 0.00746 -0.00397 AFIX 43 H1 2 0.274181 0.118697 0.422753 11.00000 -1.20000 AFIX 0 C2 1 0.394130 -0.124181 0.414184 11.00000 0.02507 0.02717 = 0.01534 0.00216 0.00302 -0.00330 AFIX 43 H2 2 0.420674 -0.185373 0.471045 11.00000 -1.20000 AFIX 0 C3 1 0.445482 -0.220161 0.360162 11.00000 0.01893 0.02322 = 0.02256 0.00109 0.00431 -0.00091 AFIX 43 H3 2 0.506463 -0.342686 0.380718 11.00000 -1.20000 AFIX 0 C4 1 0.406560 -0.134994 0.278010 11.00000 0.01972 0.01838 = 0.02068 -0.00179 0.00898 -0.00267 AFIX 43 H4 2 0.440437 -0.199465 0.241324 11.00000 -1.20000 AFIX 0 C5 1 0.316840 0.047104 0.248031 11.00000 0.01809 0.01736 = 0.01620 -0.00366 0.00848 -0.00417 C6 1 0.255820 0.170986 0.170673 11.00000 0.01719 0.01846 = 0.01645 -0.00285 0.00719 -0.00393 C7 1 0.251090 0.179526 0.085013 11.00000 0.02024 0.01789 = 0.01748 -0.00125 0.00812 -0.00420 C8 1 0.153585 0.358498 0.036605 11.00000 0.02468 0.02219 = 0.01577 0.00126 0.00821 -0.00039 AFIX 23 H8A 2 0.110596 0.204472 -0.006574 11.00000 -1.20000 H8B 2 0.167262 0.565719 0.009284 11.00000 -1.20000 AFIX 0 C9 1 0.100741 0.456454 0.098919 11.00000 0.01765 0.02131 = 0.01912 0.00106 0.00645 -0.00022 AFIX 23 H9A 2 0.091010 0.706320 0.100100 11.00000 -1.20000 H9B 2 0.035338 0.341215 0.085192 11.00000 -1.20000 AFIX 0 C10 1 0.172884 0.330345 0.179775 11.00000 0.01785 0.01623 = 0.01849 -0.00175 0.00809 -0.00269 C11 1 0.180625 0.313612 0.261696 11.00000 0.01836 0.02065 = 0.01854 -0.00154 0.00860 -0.00008 C12 1 0.119969 0.439731 0.305753 11.00000 0.02247 0.02707 = 0.01592 0.00123 0.00640 0.00245 HKLF 4 REM wv580_0m_a.res in P2(1)/c REM R1 = 0.0460 for 1521 Fo > 4sig(Fo) and 0.0598 for all 1897 data REM 136 parameters refined using 0 restraints END WGHT 0.0426 0.5869 REM Highest difference peak 0.243, deepest hole -0.243, 1-sigma level 0.047 Q1 1 0.2009 0.1674 0.1694 11.00000 0.05 0.24 Q2 1 0.4471 -0.0854 0.3266 11.00000 0.05 0.21 Q3 1 0.3701 -0.0891 0.1054 11.00000 0.05 0.20 Q4 1 0.2501 0.0686 0.1325 11.00000 0.05 0.20 Q5 1 0.2863 0.0676 0.2037 11.00000 0.05 0.19 Q6 1 0.3093 0.1817 0.2086 11.00000 0.05 0.19 Q7 1 0.2291 0.3182 0.1803 11.00000 0.05 0.19 Q8 1 0.3478 -0.1118 0.2607 11.00000 0.05 0.19 Q9 1 0.1297 0.3841 0.1429 11.00000 0.05 0.18 Q10 1 0.2756 0.2600 0.1418 11.00000 0.05 0.18 Q11 1 0.3728 0.0656 0.4002 11.00000 0.05 0.17 Q12 1 0.1327 0.3085 0.2688 11.00000 0.05 0.17 Q13 1 0.2785 0.0294 0.3404 11.00000 0.05 0.17 Q14 1 0.1590 0.2593 0.2115 11.00000 0.05 0.16 Q15 1 0.2891 0.1613 -0.0074 11.00000 0.05 0.16 Q16 1 0.1465 0.5600 0.3481 11.00000 0.05 0.15 Q17 1 0.1796 0.4151 0.2243 11.00000 0.05 0.15 Q18 1 0.2081 0.3213 0.0619 11.00000 0.05 0.14 Q19 1 0.2370 0.3390 0.2882 11.00000 0.05 0.14 Q20 1 0.2382 0.0889 0.3994 11.00000 0.05 0.14 ; _shelx_res_checksum 48689 _shelx_hkl_file ; 3 0 0 15.60 2.40 -3 0 0 16.60 2.50 3 0 0 17.60 2.40 -4 0 0 726.83 18.70 4 0 0 687.63 18.00 -4 0 0 686.93 18.10 4 0 0 701.33 18.40 5 0 0 1951.70 48.10 -5 0 0 2113.19 49.20 -5 0 0 1985.80 48.40 6 0 0 765.72 20.70 6 0 0 742.23 20.20 -6 0 0 734.73 21.10 -7 0 0 2057.39 50.39 7 0 0 1904.11 48.80 7 0 0 2060.09 49.70 7 0 0 1998.40 49.30 8 0 0 436.46 14.20 8 0 0 445.76 14.40 -8 0 0 438.96 15.40 8 0 0 455.55 14.90 9 0 0 263.97 11.10 -9 0 0 264.17 11.70 9 0 0 266.87 10.70 9 0 0 251.77 10.20 10 0 0 93.19 7.10 -10 0 0 91.89 8.20 10 0 0 92.79 7.50 10 0 0 96.29 7.00 -11 0 0 6.50 5.00 11 0 0 6.90 7.90 11 0 0 9.20 4.00 11 0 0 8.00 3.90 12 0 0 376.56 15.90 12 0 0 418.76 15.40 12 0 0 426.56 15.80 -12 0 0 421.76 17.60 13 0 0 63.29 7.40 -13 0 0 66.89 9.20 -14 0 0 766.32 27.00 14 0 0 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46.00 7.80 11 -1 -3 45.10 4.70 -11 1 3 46.70 5.00 11 1 -3 52.09 7.70 11 1 -3 72.59 9.80 -11 1 3 44.10 6.20 10 -1 -3 166.78 8.20 -10 -1 3 164.08 11.00 10 -1 -3 168.78 7.00 -10 1 3 169.98 7.20 10 1 -3 160.78 10.10 -10 1 3 170.78 8.70 10 1 -3 174.58 10.40 10 1 -3 179.58 10.60 9 -1 -3 5.10 3.00 9 -1 -3 4.00 2.00 -9 -1 3 3.60 4.20 9 1 -3 6.50 4.30 9 1 -3 5.10 4.70 -9 1 3 6.20 2.20 -9 1 3 8.90 3.50 -8 -1 3 23.50 5.20 -8 -1 3 19.80 4.90 8 -1 -3 21.70 3.80 -8 1 3 27.40 4.10 8 1 -3 32.50 5.60 8 1 -3 24.30 5.10 8 1 -3 26.90 5.00 7 -1 -3 703.23 19.40 -7 -1 3 667.93 21.90 -7 -1 3 693.63 22.10 -7 1 3 646.74 19.10 7 1 -3 713.63 21.70 7 1 -3 725.83 21.70 -6 -1 3 102.09 7.80 -6 -1 3 102.09 7.80 6 -1 -3 101.29 5.90 -6 1 3 98.59 5.80 6 1 -3 106.69 7.70 6 1 -3 109.29 7.50 -5 -1 3 26.60 4.90 5 -1 -3 31.60 4.10 -5 -1 3 18.90 4.20 5 1 -3 30.60 5.00 -5 1 3 26.70 3.60 5 1 -3 44.60 5.70 4 -1 -3 138.29 6.60 -4 -1 3 139.29 7.50 -4 -1 3 137.59 7.60 -4 1 3 143.59 6.30 4 1 -3 139.99 7.60 4 1 -3 153.08 7.70 -3 -1 3 3.20 2.70 3 -1 -3 7.50 1.50 -3 -1 3 7.00 3.30 3 -1 -3 4.50 2.70 -3 1 3 4.80 1.30 -3 1 3 5.70 2.50 3 1 -3 4.30 3.10 3 1 -3 7.10 2.80 2 -1 -3 1920.41 47.80 2 -1 -3 2005.60 46.20 -2 -1 3 1955.10 48.00 2 1 -3 1890.21 48.10 2 1 -3 1904.41 47.60 -2 1 3 2060.79 49.00 2 1 -3 1965.30 48.40 -2 1 3 1975.60 45.90 1 -1 -3 505.95 13.90 1 -1 -3 519.55 15.30 -1 -1 3 487.65 14.40 1 1 -3 486.15 14.20 1 1 -3 506.25 15.00 -1 1 3 504.25 14.90 -1 1 3 516.35 13.80 1 1 -3 498.25 14.90 0 -1 -3 2.50 2.40 0 -1 3 3.90 2.30 0 -1 -3 1.20 2.70 0 1 3 3.30 2.80 0 1 3 1.70 2.20 0 1 -3 3.60 2.00 0 1 -3 3.50 2.10 1 -1 3 2211.98 53.49 -1 -1 -3 2142.19 53.39 -1 -1 -3 2237.08 52.89 -1 1 -3 2030.80 51.19 1 1 3 2205.48 52.59 -1 1 -3 2223.58 52.29 1 1 3 2184.38 53.29 -1 1 -3 2125.29 50.89 -2 -1 -3 -2.20 2.90 -2 -1 -3 -4.40 2.40 -2 1 -3 -0.40 1.40 2 1 3 -1.20 2.70 2 1 3 1.10 2.60 -2 1 -3 0.60 1.80 -2 1 -3 1.20 1.30 -3 -1 -3 1530.75 40.40 -3 -1 -3 1540.95 40.40 3 -1 3 1558.64 38.80 3 1 3 1532.65 39.90 3 1 3 1565.54 40.30 -3 1 -3 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4 2 -18 18.40 6.30 3 -2 -18 2.90 6.40 3 -2 -18 1.90 4.80 3 2 -18 3.60 4.60 3 2 -18 1.00 4.80 2 -2 -18 -3.30 5.10 2 -2 -18 -0.60 5.50 2 2 -18 -1.10 4.60 2 2 -18 2.30 4.60 1 -2 -18 31.70 8.70 1 -2 -18 16.60 6.90 1 2 -18 22.20 5.70 1 2 -18 23.80 7.80 0 -2 -18 46.40 10.00 0 -2 -18 29.10 8.60 0 2 -18 41.30 8.80 0 2 -18 46.40 7.00 -1 -2 -18 4.30 6.90 -1 -2 -18 5.10 6.80 -1 2 -18 -4.30 5.20 -1 2 -18 16.10 4.60 13 0 -19 -4.70 7.10 13 0 -19 3.10 5.90 12 0 -19 -3.50 4.50 11 0 -19 -2.60 4.10 11 0 -19 3.50 4.80 10 0 -19 -0.30 4.70 10 0 -19 0.50 4.40 9 0 -19 -3.70 3.80 9 0 -19 1.00 4.80 8 0 -19 4.70 5.30 8 0 -19 0.10 6.60 7 0 -19 1.60 4.90 6 0 -19 6.30 5.70 6 0 -19 -2.60 4.80 5 0 -19 -2.10 3.70 4 0 -19 -6.00 3.90 4 0 -19 5.10 9.60 3 0 -19 2.00 4.60 3 0 -19 7.00 4.90 2 0 -19 -0.60 4.80 2 0 -19 3.30 5.00 1 0 -19 3.00 5.20 1 0 -19 -4.60 4.40 0 0 -19 6.60 5.30 0 0 -19 3.80 5.60 -1 0 -19 -0.30 5.40 -1 0 -19 -6.40 4.90 -2 0 -19 7.10 5.70 -2 0 -19 6.50 6.30 12 -1 -19 4.00 5.60 12 1 -19 2.40 5.60 12 1 -19 0.40 4.80 11 -1 -19 7.30 6.00 11 -1 -19 -4.60 3.60 11 1 -19 5.40 5.80 11 1 -19 5.50 5.30 10 -1 -19 11.50 5.00 10 -1 -19 10.50 6.40 10 1 -19 15.00 6.40 10 1 -19 21.20 6.90 9 -1 -19 73.59 8.60 9 -1 -19 75.69 10.20 9 1 -19 89.09 10.70 9 1 -19 90.79 10.20 8 -1 -19 74.19 8.60 8 -1 -19 77.19 11.40 8 1 -19 68.19 10.30 8 1 -19 66.99 9.80 7 -1 -19 26.90 6.50 7 -1 -19 42.40 9.20 7 1 -19 24.90 6.90 7 1 -19 28.60 7.10 6 -1 -19 27.90 7.90 6 -1 -19 28.80 7.10 6 1 -19 32.70 7.60 6 1 -19 26.60 7.40 5 -1 -19 3.90 5.80 5 1 -19 18.70 8.00 5 1 -19 7.80 5.30 4 -1 -19 -2.60 4.50 4 -1 -19 8.70 5.90 4 1 -19 -2.50 4.30 4 1 -19 3.60 4.90 3 -1 -19 95.29 11.20 3 -1 -19 116.19 12.00 3 1 -19 128.29 11.70 3 1 -19 121.89 10.80 2 -1 -19 86.89 10.90 2 -1 -19 77.29 10.70 2 1 -19 89.39 9.60 2 1 -19 72.89 10.40 1 -1 -19 5.90 6.40 1 -1 -19 5.60 6.30 1 1 -19 4.30 5.80 1 1 -19 11.90 5.30 0 -1 -19 7.00 6.40 0 -1 -19 9.70 6.70 0 1 -19 8.40 5.80 0 1 -19 17.70 5.80 -1 -1 -19 15.00 7.90 -1 -1 -19 22.90 8.30 -1 1 -19 22.80 7.80 -1 1 -19 35.60 6.50 -2 -1 -19 21.90 8.20 -2 -1 -19 39.60 8.40 -2 1 -19 37.80 6.90 -2 1 -19 12.20 7.10 10 -2 -19 17.80 7.30 10 -2 -19 1.60 4.80 10 2 -19 14.20 6.50 10 2 -19 7.20 5.60 9 -2 -19 13.10 6.10 9 -2 -19 2.40 4.90 9 2 -19 9.00 6.00 9 2 -19 20.70 6.90 8 -2 -19 4.30 5.50 8 -2 -19 -3.60 4.60 8 2 -19 -1.10 5.10 8 2 -19 -1.00 5.00 7 -2 -19 54.19 11.00 7 -2 -19 35.60 7.70 7 2 -19 46.20 9.00 7 2 -19 36.10 8.00 6 -2 -19 23.30 7.20 6 -2 -19 32.20 9.00 6 2 -19 27.30 7.90 6 2 -19 52.59 9.10 5 -2 -19 -3.60 5.30 5 -2 -19 6.30 5.90 5 2 -19 3.30 5.10 5 2 -19 0.00 4.90 4 -2 -19 38.20 8.40 4 -2 -19 46.80 9.80 4 2 -19 26.50 7.10 4 2 -19 49.20 11.50 3 -2 -19 -10.00 4.80 3 -2 -19 -7.80 4.80 3 2 -19 2.40 5.30 3 2 -19 11.00 5.30 2 -2 -19 17.30 7.50 2 -2 -19 -0.80 5.80 2 2 -19 15.80 5.00 2 2 -19 -3.00 4.80 1 -2 -19 26.60 8.20 1 -2 -19 42.70 9.80 1 2 -19 38.30 8.80 12 0 -20 12.90 6.60 12 0 -20 5.20 4.60 11 0 -20 143.89 12.40 11 0 -20 99.39 10.30 10 0 -20 75.89 10.30 10 0 -20 66.09 9.10 9 0 -20 165.08 12.60 9 0 -20 184.78 13.70 8 0 -20 70.29 11.00 8 0 -20 68.19 9.40 7 0 -20 11.20 5.80 7 0 -20 10.50 5.40 6 0 -20 -2.30 4.40 6 0 -20 7.00 5.00 5 0 -20 407.56 20.10 5 0 -20 434.36 20.80 4 0 -20 103.39 11.20 4 0 -20 150.58 12.60 3 0 -20 91.59 10.60 3 0 -20 101.49 11.40 2 0 -20 47.20 8.60 2 0 -20 49.60 9.20 1 0 -20 23.30 7.30 1 0 -20 20.10 7.60 0 0 -20 69.89 11.00 0 0 -20 49.10 9.80 -1 0 -20 12.60 7.30 11 -1 -20 35.20 6.80 11 -1 -20 28.00 7.90 11 1 -20 29.50 7.80 11 1 -20 40.40 8.50 10 -1 -20 2.50 5.30 10 -1 -20 -2.90 3.80 10 1 -20 9.90 5.70 10 1 -20 -3.00 4.80 9 -1 -20 20.40 7.20 9 -1 -20 20.40 6.80 9 1 -20 23.10 6.90 9 1 -20 23.20 7.00 8 -1 -20 15.00 6.70 8 1 -20 11.30 5.90 8 1 -20 9.00 5.70 7 -1 -20 1.00 4.60 7 -1 -20 1.70 4.90 7 1 -20 6.10 5.50 7 1 -20 1.40 4.70 6 -1 -20 27.00 7.80 6 -1 -20 6.10 5.30 6 1 -20 6.50 5.00 6 1 -20 15.00 6.40 5 -1 -20 -2.70 4.70 5 -1 -20 -3.20 5.20 5 1 -20 -1.80 4.50 5 1 -20 6.30 5.20 4 -1 -20 15.30 7.00 4 -1 -20 -1.40 5.10 4 1 -20 8.50 5.20 4 1 -20 10.20 6.20 3 -1 -20 5.20 6.00 3 -1 -20 -0.20 5.10 3 1 -20 2.20 4.80 2 -1 -20 12.50 6.70 2 -1 -20 9.80 6.70 2 1 -20 23.40 6.50 2 1 -20 10.60 6.50 1 -1 -20 5.80 6.70 1 -1 -20 11.70 6.90 1 1 -20 4.20 5.30 1 1 -20 26.60 6.50 0 -1 -20 27.30 8.10 0 -1 -20 28.90 8.80 0 1 -20 15.20 6.90 0 1 -20 21.50 6.00 10 0 -21 -1.00 5.40 10 0 -21 -2.80 4.30 9 0 -21 -0.80 4.40 9 0 -21 6.20 5.30 8 0 -21 5.20 5.40 8 0 -21 -3.90 4.10 7 0 -21 6.90 5.90 7 0 -21 -3.40 4.50 6 0 -21 -7.00 4.30 6 0 -21 2.50 5.10 5 0 -21 6.60 5.70 5 0 -21 0.90 4.80 4 0 -21 4.30 5.50 4 0 -21 3.60 5.30 3 0 -21 0.90 4.70 3 0 -21 -1.30 5.10 2 0 -21 4.60 5.50 2 0 -21 -6.90 4.80 8 -1 -21 8.50 6.00 8 -1 -21 16.80 6.90 8 1 -21 9.00 5.70 8 1 -21 7.40 5.40 7 -1 -21 525.95 22.80 7 -1 -21 559.64 25.60 7 1 -21 529.65 23.50 7 1 -21 513.75 23.80 6 -1 -21 -6.90 4.60 6 -1 -21 11.00 6.20 6 1 -21 17.50 6.30 6 1 -21 -1.80 4.70 5 -1 -21 120.39 12.60 5 -1 -21 113.69 12.20 5 1 -21 122.59 12.40 5 1 -21 145.59 11.90 4 -1 -21 2.60 5.80 4 -1 -21 3.20 5.60 4 1 -21 0.30 4.70 4 1 -21 10.80 5.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 4166 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_wv581 _database_code_depnum_ccdc_archive 'CCDC 2044217' loop_ _audit_author_name _audit_author_address 'Peter Mayer' ;LMU Muenchen Germany ; _audit_update_record ; 2020-11-13 deposited with the CCDC. 2021-02-09 downloaded from the CCDC. ; _chemical_name_common RM447 _chemical_compound_source ? _chemical_absolute_configuration ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.080 #?# in millimeters _exptl_crystal_size_mid 0.060 #?# in millimeters _exptl_crystal_size_min 0.050 #?# in millimeters _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_special_details ; ; _audit_creation_date ? #?# style: 18-Aug-1998 _diffrn_ambient_temperature 108.(2) #?# in K _diffrn_source_type 'Bruker TXS' _diffrn_source_power 2.5 #?# in kW _diffrn_source_voltage 50 #?# in kV _diffrn_source_current 50 #?# in mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode (TXS)' _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_collimation ? _diffrn_measurement_device 'fixed-chi three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture TXS' _diffrn_measurement_method 'mix of phi and omega scans' _diffrn_measurement_details ? _diffrn_detector_area_resol_mean 7.3910 _diffrn_special_details ? _diffrn_orient_matrix_type ? _diffrn_orient_matrix_UB_11 ? _diffrn_orient_matrix_UB_12 ? _diffrn_orient_matrix_UB_13 ? _diffrn_orient_matrix_UB_21 ? _diffrn_orient_matrix_UB_22 ? _diffrn_orient_matrix_UB_23 ? _diffrn_orient_matrix_UB_31 ? _diffrn_orient_matrix_UB_32 ? _diffrn_orient_matrix_UB_33 ? _cell_length_a 10.6358(4) _cell_length_b 9.5636(4) _cell_length_c 10.4269(4) _cell_angle_alpha 90 _cell_angle_beta 100.187(2) _cell_angle_gamma 90 _cell_volume 1043.87(7) _cell_measurement_temperature 108.(2) #?# in K _cell_measurement_reflns_used 4879 _cell_measurement_theta_min 2.8849 _cell_measurement_theta_max 27.0815 _cell_special_details ? _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.99 _shelx_estimated_absorpt_T_min 0.993 _shelx_estimated_absorpt_T_max 0.995 _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _diffrn_reflns_number 10661 #xl _diffrn_reflns_av_R_equivalents 0.0344 #xl _diffrn_reflns_av_unetI/netI 0.0279 #xl _diffrn_reflns_limit_h_min -13 #xl _diffrn_reflns_limit_h_max 13 #xl _diffrn_reflns_limit_k_min -12 #xl _diffrn_reflns_limit_k_max 12 #xl _diffrn_reflns_limit_l_min -13 #xl _diffrn_reflns_limit_l_max 11 #xl _diffrn_reflns_theta_min 2.885 #xl _diffrn_reflns_theta_max 27.081 #xl _diffrn_measured_fraction_theta_max 0.998 #xl _diffrn_reflns_theta_full 25.242 #xl _diffrn_measured_fraction_theta_full 0.997 #xl _diffrn_reflns_Laue_measured_fraction_max 0.998 #xl _diffrn_reflns_Laue_measured_fraction_full 0.997 #xl _diffrn_reflns_point_group_measured_fraction_max 0.998 #xl _diffrn_reflns_point_group_measured_fraction_full 0.997 #xl _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' _space_group_IT_number 14 _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_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' N N 0.0061 0.0033 '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' _reflns_number_total 2298 #xl _reflns_number_gt 1971 #xl _reflns_threshold_expression 'I > 2\s(I)' #xl _reflns_Friedel_coverage 0.000 #xl _reflns_Friedel_fraction_max . #xl _reflns_Friedel_fraction_full . #xl _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. ; _refine_ls_structure_factor_coef Fsqd #xl _refine_ls_matrix_type full #xl _refine_ls_weighting_scheme calc #xl _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.5066P] where P=(Fo^2^+2Fc^2^)/3' #xl _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr #?# _refine_ls_extinction_method none #xl _refine_ls_extinction_coef . #xl _refine_ls_abs_structure_details ? #xl _refine_ls_abs_structure_Flack ? #xl _refine_ls_number_reflns 2298 #xl _refine_ls_number_parameters 145 #xl _refine_ls_number_restraints 0 #xl _refine_ls_R_factor_all 0.0481 #xl _refine_ls_R_factor_gt 0.0401 #xl _refine_ls_wR_factor_ref 0.1025 #xl _refine_ls_wR_factor_gt 0.0976 #xl _refine_ls_goodness_of_fit_ref 1.036 #xl _refine_ls_restrained_S_all 1.036 #xl _refine_ls_shift/su_max 0.000 #xl _refine_ls_shift/su_mean 0.000 #xl _refine_diff_density_max 0.243 #xl _refine_diff_density_min -0.205 #xl _refine_diff_density_rms 0.043 #xl _refine_special_details ; ; _computing_data_collection 'APEX3 v2016.5-0, Bruker AXS (2016)' _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 833)' _computing_publication_material ? 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 0.41843(9) 0.68753(11) 0.87282(9) 0.0253(2) Uani 1 1 d . . . . . O2 O 0.44558(10) 0.85591(11) 0.73767(10) 0.0294(3) Uani 1 1 d . . . . . N1 N 0.06818(12) 0.29812(13) -0.00227(12) 0.0280(3) Uani 1 1 d . . . . . C1 C 0.38988(12) 0.74939(15) 0.75523(13) 0.0213(3) Uani 1 1 d . . . . . C2 C 0.29018(12) 0.68827(14) 0.65376(13) 0.0187(3) Uani 1 1 d . . . . . H2 H 0.250464 0.753760 0.583352 0.022 Uiso 1 1 calc R U . . . C3 C 0.30299(12) 0.53560(14) 0.61191(12) 0.0189(3) Uani 1 1 d . . . . . H3 H 0.378278 0.483473 0.660108 0.023 Uiso 1 1 calc R U . . . C4 C 0.20340(12) 0.57738(14) 0.69118(13) 0.0191(3) Uani 1 1 d . . . . . H4 H 0.113077 0.579213 0.643697 0.023 Uiso 1 1 calc R U . . . C5 C 0.22181(12) 0.54299(15) 0.83420(13) 0.0215(3) Uani 1 1 d . . . . . H5A H 0.191156 0.446738 0.845200 0.026 Uiso 1 1 calc R U . . . H5B H 0.170008 0.607803 0.877546 0.026 Uiso 1 1 calc R U . . . C6 C 0.36070(13) 0.55429(15) 0.89881(13) 0.0228(3) Uani 1 1 d . . . . . H6A H 0.366973 0.542953 0.994103 0.027 Uiso 1 1 calc R U . . . H6B H 0.409431 0.477235 0.867266 0.027 Uiso 1 1 calc R U . . . C7 C 0.26266(12) 0.49701(13) 0.47256(12) 0.0181(3) Uani 1 1 d . . . . . C8 C 0.15864(12) 0.56174(14) 0.39384(13) 0.0201(3) Uani 1 1 d . . . . . H8 H 0.117327 0.638107 0.427311 0.024 Uiso 1 1 calc R U . . . C9 C 0.11523(12) 0.51599(14) 0.26802(13) 0.0206(3) Uani 1 1 d . . . . . H9 H 0.045162 0.561274 0.215032 0.025 Uiso 1 1 calc R U . . . C10 C 0.17507(13) 0.40278(14) 0.21940(13) 0.0198(3) Uani 1 1 d . . . . . C11 C 0.28277(13) 0.34186(14) 0.29440(13) 0.0210(3) Uani 1 1 d . . . . . H11 H 0.326004 0.267846 0.259664 0.025 Uiso 1 1 calc R U . . . C12 C 0.32641(12) 0.38980(14) 0.41978(13) 0.0203(3) Uani 1 1 d . . . . . H12 H 0.400505 0.349218 0.470325 0.024 Uiso 1 1 calc R U . . . C13 C 0.11854(13) 0.34493(14) 0.09459(13) 0.0216(3) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0215(5) 0.0305(6) 0.0223(5) -0.0036(4) -0.0005(4) -0.0037(4) O2 0.0264(5) 0.0306(6) 0.0319(6) -0.0068(4) 0.0069(4) -0.0117(4) N1 0.0299(7) 0.0305(7) 0.0232(6) -0.0014(5) 0.0033(5) -0.0045(5) C1 0.0165(6) 0.0243(7) 0.0236(7) -0.0048(5) 0.0051(5) -0.0014(5) C2 0.0176(6) 0.0183(6) 0.0197(6) -0.0006(5) 0.0015(5) -0.0011(5) C3 0.0173(6) 0.0189(6) 0.0194(6) -0.0001(5) 0.0005(5) 0.0006(5) C4 0.0145(6) 0.0198(6) 0.0221(7) 0.0000(5) 0.0013(5) -0.0011(5) C5 0.0208(7) 0.0228(7) 0.0215(7) -0.0003(5) 0.0056(5) -0.0008(5) C6 0.0232(7) 0.0261(7) 0.0182(6) 0.0003(5) 0.0015(5) 0.0031(6) C7 0.0169(6) 0.0173(6) 0.0197(6) 0.0007(5) 0.0024(5) -0.0032(5) C8 0.0189(6) 0.0182(6) 0.0226(7) -0.0007(5) 0.0023(5) 0.0008(5) C9 0.0167(6) 0.0216(7) 0.0224(7) 0.0027(5) 0.0004(5) -0.0009(5) C10 0.0205(6) 0.0209(7) 0.0182(6) 0.0009(5) 0.0042(5) -0.0050(5) C11 0.0218(6) 0.0191(6) 0.0231(7) -0.0003(5) 0.0065(5) 0.0004(5) C12 0.0177(6) 0.0209(7) 0.0218(7) 0.0033(5) 0.0019(5) 0.0010(5) C13 0.0211(6) 0.0225(7) 0.0219(7) 0.0018(5) 0.0055(5) -0.0025(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.3468(17) . ? O1 C6 1.4606(17) . ? O2 C1 1.2086(17) . ? N1 C13 1.1472(18) . ? C1 C2 1.4794(18) . ? C2 C4 1.5021(18) . ? C2 C3 1.5368(18) . ? C2 H2 1.0000 . ? C3 C7 1.4869(18) . ? C3 C4 1.5081(18) . ? C3 H3 1.0000 . ? C4 C5 1.5056(18) . ? C4 H4 1.0000 . ? C5 C6 1.5151(18) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C12 1.3950(18) . ? C7 C8 1.4000(18) . ? C8 C9 1.3825(18) . ? C8 H8 0.9500 . ? C9 C10 1.3958(19) . ? C9 H9 0.9500 . ? C10 C11 1.3951(19) . ? C10 C13 1.4438(18) . ? C11 C12 1.3857(19) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 C6 121.17(10) . . ? O2 C1 O1 118.06(12) . . ? O2 C1 C2 122.23(13) . . ? O1 C1 C2 119.68(12) . . ? C1 C2 C4 119.26(11) . . ? C1 C2 C3 119.35(11) . . ? C4 C2 C3 59.50(8) . . ? C1 C2 H2 115.7 . . ? C4 C2 H2 115.7 . . ? C3 C2 H2 115.7 . . ? C7 C3 C4 119.48(11) . . ? C7 C3 C2 119.24(11) . . ? C4 C3 C2 59.11(8) . . ? C7 C3 H3 115.7 . . ? C4 C3 H3 115.7 . . ? C2 C3 H3 115.7 . . ? C2 C4 C5 115.67(11) . . ? C2 C4 C3 61.40(8) . . ? C5 C4 C3 120.27(11) . . ? C2 C4 H4 116.1 . . ? C5 C4 H4 116.1 . . ? C3 C4 H4 116.1 . . ? C4 C5 C6 111.75(11) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? O1 C6 C5 112.86(11) . . ? O1 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? O1 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C12 C7 C8 118.85(12) . . ? C12 C7 C3 119.45(12) . . ? C8 C7 C3 121.65(12) . . ? C9 C8 C7 120.87(12) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 119.53(12) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 120.15(12) . . ? C11 C10 C13 120.99(12) . . ? C9 C10 C13 118.73(12) . . ? C12 C11 C10 119.70(12) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C7 120.69(12) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? N1 C13 C10 176.65(14) . . ? 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 C6 O1 C1 O2 -176.32(12) . . . . ? C6 O1 C1 C2 5.35(18) . . . . ? O2 C1 C2 C4 -165.34(12) . . . . ? O1 C1 C2 C4 12.92(18) . . . . ? O2 C1 C2 C3 125.29(14) . . . . ? O1 C1 C2 C3 -56.45(17) . . . . ? C1 C2 C3 C7 -142.56(12) . . . . ? C4 C2 C3 C7 108.80(13) . . . . ? C1 C2 C3 C4 108.64(13) . . . . ? C1 C2 C4 C5 3.23(17) . . . . ? C3 C2 C4 C5 112.01(12) . . . . ? C1 C2 C4 C3 -108.78(13) . . . . ? C7 C3 C4 C2 -108.40(13) . . . . ? C7 C3 C4 C5 146.94(12) . . . . ? C2 C3 C4 C5 -104.66(13) . . . . ? C2 C4 C5 C6 -34.37(16) . . . . ? C3 C4 C5 C6 36.09(17) . . . . ? C1 O1 C6 C5 -38.18(16) . . . . ? C4 C5 C6 O1 51.48(15) . . . . ? C4 C3 C7 C12 -143.13(13) . . . . ? C2 C3 C7 C12 147.93(12) . . . . ? C4 C3 C7 C8 34.21(18) . . . . ? C2 C3 C7 C8 -34.73(18) . . . . ? C12 C7 C8 C9 3.3(2) . . . . ? C3 C7 C8 C9 -174.07(12) . . . . ? C7 C8 C9 C10 0.7(2) . . . . ? C8 C9 C10 C11 -3.94(19) . . . . ? C8 C9 C10 C13 172.04(12) . . . . ? C9 C10 C11 C12 3.1(2) . . . . ? C13 C10 C11 C12 -172.76(12) . . . . ? C10 C11 C12 C7 0.9(2) . . . . ? C8 C7 C12 C11 -4.1(2) . . . . ? C3 C7 C12 C11 173.31(12) . . . . ? _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. ; _audit_block_code C13H11NO2_wv581_mayr _audit_creation_method 'APEX3 v2017.3-0' _shelxl_version_number ? _chemical_name_systematic ? _chemical_formula_moiety 'C13 H11 N O2' _chemical_formula_sum 'C13 H11 N O2' _chemical_formula_weight 213.23 #?# (Cohen, 1996) _chemical_melting_point ? #?# in K! _cell_formula_units_Z 4 #?# adjust to _chemical_formula_[] _exptl_crystal_density_diffrn 1.357 _exptl_crystal_F_000 448 #?# check! _shelx_res_file ; TITL wv581_0ma_a.res in P2(1)/c wv581_0ma_a.res created by SHELXL-2016/6 at 15:09:54 on 14-Nov-2018 REM Old TITL wv581_0ma in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.103, Rweak 0.003, Alpha 0.017, Orientation as input REM Formula found by SHELXT: C13 N O2 CELL 0.71073 10.6358 9.5636 10.4269 90.000 100.187 90.000 ZERR 4.000 0.0004 0.0004 0.0004 0.000 0.002 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O UNIT 52 44 4 8 TEMP -165 SIZE 0.05 0.06 0.08 L.S. 10 BOND $H LIST 4 CONF ACTA SHEL 9.0 0.78 OMIT -2 0 2 OMIT 5 0 0 OMIT -6 3 3 FMAP 2 PLAN -20 WGHT 0.043300 0.506600 FVAR 1.10328 O1 4 0.418433 0.687534 0.872819 11.00000 0.02149 0.03049 = 0.02230 -0.00363 -0.00052 -0.00373 O2 4 0.445578 0.855914 0.737675 11.00000 0.02643 0.03060 = 0.03187 -0.00683 0.00694 -0.01170 N1 3 0.068177 0.298118 -0.002268 11.00000 0.02986 0.03046 = 0.02322 -0.00138 0.00333 -0.00447 C1 1 0.389878 0.749388 0.755226 11.00000 0.01652 0.02427 = 0.02355 -0.00478 0.00508 -0.00142 C2 1 0.290176 0.688265 0.653760 11.00000 0.01755 0.01825 = 0.01974 -0.00055 0.00149 -0.00109 AFIX 13 H2 2 0.250464 0.753760 0.583352 11.00000 -1.20000 AFIX 0 C3 1 0.302986 0.535601 0.611912 11.00000 0.01731 0.01892 = 0.01942 -0.00007 0.00052 0.00058 AFIX 13 H3 2 0.378278 0.483473 0.660108 11.00000 -1.20000 AFIX 0 C4 1 0.203395 0.577377 0.691184 11.00000 0.01451 0.01982 = 0.02213 0.00004 0.00127 -0.00110 AFIX 13 H4 2 0.113077 0.579213 0.643697 11.00000 -1.20000 AFIX 0 C5 1 0.221814 0.542993 0.834202 11.00000 0.02083 0.02282 = 0.02148 -0.00031 0.00558 -0.00084 AFIX 23 H5A 2 0.191156 0.446738 0.845200 11.00000 -1.20000 H5B 2 0.170008 0.607803 0.877546 11.00000 -1.20000 AFIX 0 C6 1 0.360698 0.554287 0.898805 11.00000 0.02317 0.02607 = 0.01823 0.00035 0.00148 0.00311 AFIX 23 H6A 2 0.366973 0.542953 0.994103 11.00000 -1.20000 H6B 2 0.409431 0.477235 0.867266 11.00000 -1.20000 AFIX 0 C7 1 0.262663 0.497012 0.472562 11.00000 0.01688 0.01728 = 0.01974 0.00066 0.00236 -0.00323 C8 1 0.158635 0.561739 0.393837 11.00000 0.01886 0.01821 = 0.02259 -0.00069 0.00226 0.00076 AFIX 43 H8 2 0.117327 0.638107 0.427311 11.00000 -1.20000 AFIX 0 C9 1 0.115225 0.515987 0.268021 11.00000 0.01665 0.02160 = 0.02243 0.00268 0.00042 -0.00092 AFIX 43 H9 2 0.045162 0.561274 0.215032 11.00000 -1.20000 AFIX 0 C10 1 0.175071 0.402784 0.219402 11.00000 0.02052 0.02095 = 0.01815 0.00094 0.00420 -0.00501 C11 1 0.282774 0.341860 0.294398 11.00000 0.02183 0.01912 = 0.02307 -0.00028 0.00652 0.00041 AFIX 43 H11 2 0.326004 0.267846 0.259664 11.00000 -1.20000 AFIX 0 C12 1 0.326408 0.389795 0.419782 11.00000 0.01771 0.02094 = 0.02180 0.00326 0.00190 0.00095 AFIX 43 H12 2 0.400505 0.349218 0.470325 11.00000 -1.20000 AFIX 0 C13 1 0.118538 0.344930 0.094593 11.00000 0.02107 0.02247 = 0.02192 0.00178 0.00552 -0.00250 HKLF 4 REM wv581_0ma_a.res in P2(1)/c REM R1 = 0.0401 for 1971 Fo > 4sig(Fo) and 0.0481 for all 2298 data REM 145 parameters refined using 0 restraints END WGHT 0.0433 0.5066 REM Highest difference peak 0.243, deepest hole -0.205, 1-sigma level 0.043 Q1 1 0.2225 0.3612 0.2661 11.00000 0.05 0.24 Q2 1 0.2888 0.5619 0.8592 11.00000 0.05 0.23 Q3 1 0.2452 0.3857 0.2457 11.00000 0.05 0.22 Q4 1 0.3356 0.7062 0.7042 11.00000 0.05 0.22 Q5 1 0.2478 0.5199 0.6557 11.00000 0.05 0.21 Q6 1 0.2137 0.5506 0.7594 11.00000 0.05 0.21 Q7 1 0.1627 0.3870 0.1512 11.00000 0.05 0.20 Q8 1 0.2775 0.5219 0.5413 11.00000 0.05 0.20 Q9 1 0.2042 0.5178 0.4379 11.00000 0.05 0.19 Q10 1 0.2269 0.6558 0.6849 11.00000 0.05 0.18 Q11 1 0.1371 0.4355 0.2563 11.00000 0.05 0.18 Q12 1 0.1586 0.4603 0.2422 11.00000 0.05 0.18 Q13 1 0.2840 0.4282 0.4582 11.00000 0.05 0.18 Q14 1 0.3719 0.5830 0.9827 11.00000 0.05 0.18 Q15 1 0.3030 0.4568 0.4432 11.00000 0.05 0.17 Q16 1 0.2785 0.3498 0.3699 11.00000 0.05 0.17 Q17 1 0.1546 0.5529 0.3240 11.00000 0.05 0.17 Q18 1 0.3161 0.3946 0.3419 11.00000 0.05 0.15 Q19 1 0.1444 0.5745 0.6526 11.00000 0.05 0.14 Q20 1 0.3234 0.6197 0.6258 11.00000 0.05 0.13 ; _shelx_res_checksum 4549 _shelx_hkl_file ; 0 0 -2 4101.09 133.89 0 0 3 0.80 1.00 0 0 3 1.00 1.40 0 0 -3 1.20 1.00 0 0 -3 1.20 1.60 0 0 -4 29.10 3.10 0 0 -4 28.80 2.90 0 0 4 28.90 3.60 0 0 4 28.20 2.40 0 0 -5 12.10 2.50 0 0 5 11.10 2.60 0 0 -5 10.50 2.20 0 0 5 12.50 2.20 0 0 -5 12.00 3.00 0 0 -6 761.52 26.60 0 0 -6 676.73 23.60 0 0 6 744.83 24.10 0 0 -6 725.03 26.10 0 0 7 12.70 2.40 0 0 -7 10.40 3.00 0 0 -7 8.90 2.20 0 0 -7 13.10 3.10 0 0 -8 1268.47 43.40 0 0 -8 1229.28 39.30 0 0 8 1228.58 39.60 0 0 -9 6.20 3.60 0 0 -9 -1.30 2.10 0 0 -9 2.80 2.00 0 0 -10 203.18 13.40 0 0 -10 184.78 9.40 0 0 -10 197.78 9.40 0 0 -11 2.40 3.20 0 0 -11 2.70 2.00 0 0 -11 -1.50 2.10 0 0 -12 64.99 4.50 0 0 -12 44.50 8.30 0 0 -12 57.79 4.70 0 0 -13 -2.90 4.00 0 -1 -1 663.13 21.10 0 -1 -1 667.33 21.40 0 -1 1 750.32 21.30 0 1 2 127.79 5.70 0 1 2 147.29 6.00 0 1 -2 139.69 5.80 0 1 -2 135.19 4.80 0 -1 2 126.49 5.70 0 -1 2 125.69 4.80 0 -1 -2 142.89 6.40 0 -1 -2 142.79 5.80 0 1 3 40.20 3.20 0 1 3 45.60 3.50 0 1 -3 47.00 3.40 0 1 -3 39.00 2.30 0 -1 -3 39.10 3.20 0 -1 3 41.00 2.40 0 -1 -3 35.10 3.20 0 -1 -3 43.20 3.10 0 -1 3 43.80 3.50 0 1 -4 571.64 17.50 0 1 -4 557.64 19.60 0 -1 4 545.05 19.40 0 -1 -4 517.95 19.20 0 -1 4 538.55 17.40 0 -1 -4 590.64 18.90 0 -1 -4 545.75 19.50 0 1 -5 0.30 2.40 0 1 5 0.10 1.60 0 -1 -5 3.00 2.00 0 -1 -5 1.10 1.90 0 -1 5 4.70 2.30 0 -1 5 2.90 1.40 0 -1 -5 3.00 1.80 0 1 -6 844.52 25.70 0 1 -6 849.41 29.10 0 1 6 797.32 27.20 0 -1 -6 774.62 26.90 0 -1 6 782.22 25.60 0 -1 -6 824.52 28.80 0 1 -7 80.89 4.70 0 1 -7 93.09 7.40 0 1 7 82.99 5.70 0 -1 -7 90.89 6.70 0 -1 7 85.99 6.80 0 -1 -7 89.19 6.00 0 -1 7 83.09 5.30 0 -1 -7 80.89 6.90 0 -1 -7 84.49 5.80 0 1 -8 48.10 6.80 0 1 -8 48.00 3.80 0 -1 8 54.89 4.00 0 -1 -8 52.39 4.80 0 -1 -8 45.70 6.50 0 -1 -8 45.10 4.80 0 1 -9 4.80 2.00 0 1 -9 -0.50 3.30 0 -1 -9 2.10 2.60 0 -1 -9 5.50 2.30 0 -1 -9 0.40 3.20 0 -1 9 2.80 1.80 0 1 -10 66.39 4.50 0 1 -10 62.89 8.70 0 1 -10 62.39 4.40 0 -1 -10 61.69 5.90 0 -1 -10 70.09 9.10 0 -1 -10 66.89 5.60 0 1 -11 2.40 1.60 0 1 -11 1.30 3.80 0 1 -11 1.30 1.50 0 -1 -11 -3.90 2.60 0 -1 -11 -0.90 2.90 0 1 -12 11.80 5.20 0 -1 -12 15.20 5.90 0 -1 -12 7.60 3.60 0 1 -13 94.19 11.00 0 -1 -13 79.69 6.50 0 -1 -13 66.49 11.20 0 -2 0 1647.04 49.60 0 2 -1 6612.34 215.08 0 2 1 6461.65 201.88 0 -2 1 6342.87 213.18 0 -2 -1 6570.54 202.18 0 2 -2 8.80 1.60 0 2 2 4.70 1.60 0 2 -2 11.30 2.10 0 -2 2 9.10 2.00 0 -2 2 7.90 1.50 0 -2 -2 8.90 2.20 0 -2 -2 6.70 2.00 0 -2 -2 12.00 2.70 0 2 -3 2277.97 69.29 0 2 -3 2457.95 70.99 0 2 3 2374.46 70.89 0 -2 3 2181.78 70.59 0 -2 -3 2444.46 71.19 0 -2 -3 2376.06 71.29 0 -2 -3 2421.66 70.89 0 -2 3 2300.47 69.19 0 2 4 522.05 18.90 0 2 -4 529.35 19.00 0 2 -4 514.05 16.90 0 -2 4 563.84 19.10 0 -2 4 511.05 16.80 0 -2 -4 529.35 18.90 0 -2 -4 505.85 18.70 0 -2 -4 503.65 18.80 0 2 -5 731.33 26.20 0 -2 -5 740.93 25.70 0 -2 -5 752.72 25.70 0 -2 -5 770.72 26.20 0 -2 -5 708.03 26.00 0 -2 5 733.13 26.10 0 -2 5 764.22 23.40 0 2 -6 16.40 2.20 0 2 -6 19.90 4.10 0 -2 -6 15.60 3.10 0 -2 6 15.30 3.30 0 -2 6 14.50 2.20 0 -2 -6 16.30 3.30 0 -2 -6 18.90 3.60 0 -2 -6 13.90 3.50 0 2 -7 20.90 4.20 0 2 -7 21.70 2.40 0 -2 -7 21.50 4.30 0 -2 7 23.70 2.50 0 -2 -7 28.50 5.00 0 -2 -7 20.60 3.90 0 -2 -7 27.70 4.10 0 2 -8 126.59 5.90 0 2 -8 123.09 9.50 0 -2 -8 127.69 9.40 0 -2 -8 136.39 8.20 0 -2 8 129.89 6.00 0 -2 -8 129.99 8.30 0 2 -9 256.97 14.70 0 2 -9 259.67 9.60 0 -2 -9 256.57 12.70 0 -2 -9 251.27 14.60 0 -2 -9 248.98 12.60 0 -2 9 254.67 9.90 0 2 -10 75.19 8.70 0 2 -10 85.59 4.50 0 -2 -10 93.19 9.60 0 -2 -10 88.49 7.30 0 -2 -10 94.29 7.00 0 2 -11 78.09 3.30 0 2 -11 68.39 9.80 0 -2 -11 96.89 6.90 0 -2 -11 70.99 9.90 0 2 -12 24.10 6.60 0 -2 -12 20.60 5.00 0 -2 -12 23.50 6.10 0 3 0 0.50 1.60 0 3 0 0.10 1.30 0 -3 0 1.10 1.40 0 -3 0 -0.80 1.40 0 3 -1 2156.18 62.29 0 3 1 2045.00 62.19 0 3 1 2025.00 63.19 0 3 -1 2036.40 62.49 0 -3 -1 2049.89 62.09 0 -3 1 2105.19 62.49 0 -3 -1 2072.59 63.19 0 -3 1 2052.49 62.09 0 3 2 54.79 4.00 0 3 -2 49.99 4.00 0 3 -2 53.79 3.80 0 -3 -2 48.80 3.80 0 -3 2 43.50 3.70 0 -3 -2 48.20 4.30 0 -3 2 49.90 4.00 0 -3 -2 48.10 4.50 0 3 -3 431.86 15.80 0 3 -3 430.56 14.70 0 3 3 418.96 15.60 0 -3 3 416.56 15.60 0 -3 -3 420.66 16.50 0 -3 -3 404.66 15.50 0 -3 3 410.56 14.50 0 -3 -3 413.46 16.20 0 3 4 10.00 2.80 0 3 -4 8.30 1.90 0 3 -4 10.30 2.90 0 -3 -4 12.00 3.20 0 -3 4 8.20 2.00 0 -3 -4 9.50 2.80 0 -3 4 6.70 2.60 0 -3 -4 10.60 2.70 0 3 -5 43.20 4.90 0 3 -5 49.80 3.40 0 3 5 59.49 5.00 0 -3 5 47.20 4.80 0 -3 5 47.00 3.60 0 -3 -5 53.89 5.10 0 -3 -5 47.80 4.70 0 -3 -5 54.19 4.90 0 3 -6 59.79 7.60 0 3 6 47.90 4.90 0 3 -6 44.40 3.30 0 -3 -6 45.70 4.90 0 -3 -6 44.90 5.00 0 -3 6 46.60 5.20 0 -3 -6 54.09 5.30 0 -3 -6 39.90 4.40 0 -3 6 49.80 3.50 0 3 -7 26.20 5.00 0 3 -7 21.70 2.50 0 -3 -7 20.30 4.10 0 -3 -7 24.10 4.30 0 -3 -7 22.00 4.50 0 -3 7 26.10 2.80 0 3 -8 4.30 2.80 0 3 -8 5.80 1.60 0 -3 -8 5.40 3.50 0 -3 -8 6.40 3.40 0 -3 8 2.90 1.50 0 -3 -8 6.10 2.90 0 3 -9 844.62 33.00 0 -3 -9 866.81 31.30 0 -3 9 849.32 26.30 0 -3 -9 817.12 32.70 0 -3 -9 816.02 33.20 0 3 -10 3.60 4.00 0 3 -10 9.10 1.40 0 -3 -10 7.90 4.30 0 -3 -10 8.20 4.00 0 3 -11 47.00 8.10 0 -3 -11 46.20 7.70 0 -3 -11 34.20 6.10 0 3 -12 3.40 4.70 0 -3 -12 9.30 5.00 0 -3 -12 4.30 4.20 0 4 0 1.20 2.20 0 4 0 5.30 2.10 0 -4 0 1.70 2.20 0 -4 0 2.60 1.90 0 4 1 3.50 2.50 0 4 -1 1.20 1.90 0 4 -1 -1.00 1.80 0 4 1 2.80 2.00 0 -4 -1 2.70 1.90 0 -4 1 3.10 2.20 0 -4 -1 2.10 1.70 0 -4 1 -1.00 1.50 0 4 -2 312.17 12.80 0 4 -2 334.37 13.00 0 4 2 301.37 12.60 0 -4 -2 316.47 12.70 0 -4 2 309.47 12.60 0 -4 -2 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197.48 11.80 -4 6 -1 997.30 36.00 -4 6 -1 951.40 31.50 4 6 1 960.80 35.00 4 -6 1 952.40 31.30 -4 -6 -1 969.70 36.10 -4 6 -2 228.98 10.70 -4 6 -2 245.28 13.70 4 6 2 241.98 13.30 4 -6 2 270.27 11.10 -4 -6 -2 238.68 14.30 4 6 3 41.50 6.40 -4 6 -3 46.90 4.70 -4 6 -3 37.70 6.30 4 -6 3 41.50 4.40 -4 -6 -3 44.00 7.40 4 6 4 171.98 11.10 -4 6 -4 167.68 11.10 -4 6 -4 170.98 9.60 4 -6 4 152.18 9.10 -4 -6 -4 183.98 12.80 -4 6 -5 -0.30 2.20 -4 6 -5 1.70 3.40 4 6 5 2.20 3.30 -4 -6 -5 0.70 3.90 4 -6 5 1.50 2.50 4 6 6 30.10 6.10 -4 6 -6 32.50 5.30 -4 6 -6 22.70 5.00 -4 -6 -6 22.70 6.30 -4 6 -7 106.89 8.80 -4 6 -7 113.09 9.10 4 6 7 112.39 10.30 -4 -6 -7 94.19 10.60 -4 6 -8 12.30 4.10 -4 6 -8 0.50 3.60 4 6 8 18.10 5.70 4 6 9 -4.80 3.10 -4 6 -9 11.10 5.00 -4 6 -9 4.30 3.20 -4 -6 -9 11.30 6.10 -4 6 -10 5.40 5.00 -4 6 -10 8.30 3.70 -4 -6 -10 -1.90 5.00 -4 -6 -10 4.50 4.60 4 7 -10 44.40 8.20 4 7 -9 -1.50 3.70 4 -7 -9 1.40 4.10 4 -7 -9 -0.10 2.80 4 7 -8 35.70 7.30 -4 -7 8 40.50 3.50 4 -7 -8 41.00 6.30 4 -7 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5 106.49 9.70 -10 -3 -5 118.89 12.60 -10 3 -6 5.60 5.00 10 3 6 -1.40 3.60 -10 3 -6 -2.50 3.30 -10 -3 -6 -5.20 5.20 -10 4 9 92.39 9.70 10 4 -9 87.59 9.60 -10 -4 9 101.29 5.50 10 -4 -9 79.69 6.70 -10 4 8 133.89 11.20 10 4 -8 117.59 8.50 10 -4 -8 111.49 6.70 -10 -4 8 138.59 7.90 10 -4 -8 112.69 6.50 10 4 -7 85.29 7.80 -10 4 7 120.39 10.30 10 4 -7 96.19 9.20 -10 -4 7 111.89 8.00 10 -4 -7 84.49 5.90 10 -4 -7 110.39 6.00 -10 4 6 77.39 9.50 10 4 -6 83.59 8.30 -10 -4 6 85.19 7.70 -10 4 5 -2.00 3.60 10 4 -5 0.10 3.30 -10 -4 5 3.50 3.50 10 4 -4 167.58 11.00 -10 4 4 159.58 12.80 -10 -4 4 167.18 11.90 -10 4 3 3.40 3.80 10 4 -3 3.50 3.60 -10 -4 3 8.30 5.00 -10 4 2 193.78 13.90 10 4 -2 172.18 11.30 -10 -4 2 178.38 13.10 -10 4 1 67.09 9.70 10 4 -1 52.59 7.40 -10 -4 1 52.09 8.50 10 4 0 30.90 5.60 -10 4 0 37.40 7.40 -10 -4 0 32.90 7.50 10 4 1 -2.00 2.80 -10 -4 -1 -3.70 4.10 -10 4 -2 122.39 11.80 10 4 2 139.99 10.30 -10 -4 -2 117.89 12.30 10 4 3 37.60 6.50 -10 4 -3 35.70 7.50 -10 4 -3 33.10 2.90 -10 -4 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4 5.80 4.10 -10 -5 -4 3.60 6.20 -10 5 -5 14.10 3.10 -10 5 -5 14.70 5.30 10 5 5 17.70 5.30 -10 -5 -5 4.00 6.20 -10 6 7 231.48 16.40 10 6 -7 195.68 14.60 -10 -6 7 204.18 12.10 -10 6 6 59.29 9.70 10 6 -6 62.29 9.20 -10 -6 6 45.90 7.20 10 6 -5 46.70 7.80 -10 6 5 64.59 9.70 -10 -6 5 37.80 7.00 -10 6 4 151.88 13.30 -10 -6 4 141.09 11.80 -10 6 3 28.70 7.20 10 6 -3 19.30 5.10 -10 -6 3 23.00 6.20 10 6 -2 18.00 4.80 -10 6 2 22.20 6.40 -10 -6 2 15.70 6.70 10 6 -1 52.09 7.60 -10 6 1 36.10 8.10 -10 6 0 5.40 4.00 -10 -6 0 2.20 5.20 -10 6 -1 8.00 5.00 10 6 1 1.00 3.80 -10 -6 -1 6.30 6.00 -10 6 -2 12.90 5.20 10 6 2 8.40 4.40 -10 -6 -2 4.20 5.60 -10 6 -3 136.39 13.10 10 6 3 136.89 11.60 -10 -6 -3 145.09 14.30 -10 6 -4 252.37 9.90 10 6 4 254.67 16.60 -10 6 -4 297.27 19.20 -10 -6 -4 263.37 19.40 10 7 -6 33.60 7.30 -10 7 6 42.10 8.90 -10 -7 6 19.90 6.20 10 7 -5 18.20 5.90 -10 7 5 19.90 6.60 10 7 -4 8.70 4.50 -10 7 4 8.60 5.20 -10 -7 4 2.50 4.70 -10 7 3 12.80 5.50 10 7 -3 3.90 4.20 -10 -7 3 8.50 5.60 10 7 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43.10 3.90 -11 -2 7 49.70 6.00 11 -2 -7 41.60 4.20 -11 2 6 3.10 4.00 11 2 -6 1.60 3.00 -11 -2 6 7.60 4.10 11 -2 -6 5.30 1.50 11 2 -5 63.99 6.50 -11 2 5 62.59 7.70 -11 -2 5 66.59 7.50 -11 2 4 70.99 9.00 11 2 -4 70.79 6.40 -11 -2 4 61.19 7.60 -11 2 3 0.90 3.80 11 2 -3 7.00 2.90 -11 -2 3 4.10 4.00 11 2 -2 88.99 7.20 -11 2 2 87.69 9.60 -11 -2 2 77.09 10.40 -11 -2 2 87.49 8.40 11 2 -1 71.79 6.50 -11 2 1 88.49 9.50 -11 -2 1 78.19 9.10 11 2 0 6.70 2.90 -11 -2 0 10.20 5.40 -11 2 -1 16.00 5.30 11 2 1 20.80 4.50 -11 2 -1 19.10 2.00 -11 -2 -1 23.40 7.00 -11 2 -2 6.70 2.30 -11 2 -2 13.50 5.40 -11 2 -2 10.80 2.50 11 2 2 10.70 3.80 -11 -2 -2 9.60 5.10 -11 2 -3 161.28 9.00 11 2 3 196.08 11.90 -11 2 -3 187.08 9.40 -11 2 -3 208.68 15.20 -11 -2 -3 194.48 15.40 -11 2 -4 10.50 5.00 11 2 4 9.00 4.30 -11 2 -4 14.00 6.00 -11 -2 -4 10.80 6.00 -11 2 -5 30.70 7.20 -11 2 -5 18.00 4.60 -11 -2 -5 34.10 6.50 -11 -2 -5 37.60 8.80 -11 3 8 421.46 21.30 11 3 -8 394.26 20.50 -11 -3 8 444.76 18.60 11 -3 -8 419.96 15.80 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4 25.00 6.60 -11 -4 4 23.20 6.10 -11 4 3 30.20 6.70 11 4 -3 30.10 5.50 -11 -4 3 24.70 6.60 -11 4 2 222.18 15.80 11 4 -2 212.78 12.70 -11 -4 2 203.78 15.10 -11 4 1 22.90 6.40 11 4 -1 25.40 5.10 11 4 0 14.60 4.00 -11 4 0 21.30 6.60 -11 -4 0 23.70 7.00 11 4 1 2.30 3.40 -11 4 -1 4.00 4.10 -11 -4 -1 -0.10 6.00 11 4 2 246.98 15.10 -11 4 -2 303.37 18.70 -11 -4 -2 252.47 18.20 -11 4 -3 72.29 10.60 -11 -4 -3 56.79 10.60 11 4 4 17.10 4.70 -11 4 -4 12.80 5.80 -11 4 -4 10.50 2.60 -11 -4 -4 11.80 7.00 11 5 -7 24.70 6.00 -11 5 7 29.60 7.20 -11 -5 7 23.00 4.80 -11 5 6 74.29 10.50 11 5 -6 52.19 8.50 -11 -5 6 50.99 7.50 -11 5 5 17.80 6.20 11 5 -5 27.50 7.40 -11 -5 5 11.70 4.90 11 5 -4 90.09 8.90 -11 5 4 127.49 11.90 -11 -5 4 92.39 10.10 11 5 -3 10.20 3.90 -11 5 3 -1.30 3.30 -11 -5 3 5.60 5.10 11 5 -2 53.49 7.80 -11 5 2 38.10 7.70 11 5 -1 9.20 3.90 -11 5 1 0.10 4.10 -11 -5 1 -4.00 4.30 -11 5 0 315.37 20.00 11 5 0 312.27 17.20 -11 -5 0 324.27 20.10 -11 5 -1 441.26 24.30 -11 -5 -1 434.06 24.40 11 5 2 294.07 17.30 -11 5 -2 328.17 20.40 -11 -5 -2 325.17 20.80 11 5 3 96.59 9.80 -11 5 -3 93.49 11.20 -11 -5 -3 81.59 12.50 -11 6 6 27.50 7.10 11 6 -6 23.40 6.50 -11 -6 6 15.10 5.40 -11 6 5 43.20 8.70 11 6 -5 51.09 8.80 -11 -6 5 41.50 8.00 -11 6 4 170.18 14.70 11 6 -4 189.48 13.70 -11 -6 4 186.38 14.00 -11 6 3 140.79 12.60 11 6 -3 123.29 11.10 11 6 -2 -1.10 3.00 -11 6 2 9.50 4.60 -11 -6 2 -5.90 4.80 -11 6 1 -2.90 3.00 11 6 -1 9.40 4.30 -11 -6 1 6.60 5.90 -11 6 0 16.80 6.20 11 6 0 7.30 3.60 -11 -6 0 1.70 5.20 11 6 1 23.30 5.30 -11 6 -1 16.80 6.00 -11 -6 -1 23.70 7.90 -11 6 -2 11.30 5.10 11 6 2 7.00 4.60 -11 -6 -2 -0.10 5.40 11 7 -3 13.50 5.00 -11 7 3 16.90 6.60 -11 -7 3 -2.80 5.70 11 7 -2 41.10 7.60 -11 7 2 49.80 9.40 -11 -7 2 34.40 8.60 -11 7 1 57.09 9.70 11 7 -1 62.79 9.30 -11 -7 1 47.30 10.10 -11 7 0 7.50 5.40 11 7 0 4.90 4.60 -11 -7 0 2.80 5.90 12 0 -8 8.60 3.50 -12 0 8 6.90 3.70 12 0 -7 -0.20 2.40 -12 0 7 7.10 3.40 12 0 -6 3.40 2.20 -12 0 6 12.80 4.80 -12 0 5 -4.90 2.50 -12 0 5 0.10 3.50 12 0 -5 -2.60 1.60 12 0 -4 65.09 4.80 -12 0 4 55.39 5.30 -12 0 4 64.59 7.90 12 0 -3 2.30 1.80 -12 0 3 -3.10 2.20 -12 0 3 -0.20 3.90 12 0 -2 386.56 14.40 -12 0 2 365.86 20.90 -12 0 2 361.06 14.30 12 0 -1 0.50 1.80 -12 0 1 -1.20 3.80 -12 0 0 135.39 12.00 -12 0 0 118.69 7.50 12 0 0 143.29 7.60 -12 0 -1 0.60 3.90 -12 0 -1 2.50 2.50 -12 0 -2 207.18 11.50 -12 0 -2 193.68 11.80 -12 0 -2 226.58 16.40 -12 0 -3 4.50 5.10 -12 0 -4 17.40 6.50 -12 0 -4 2.60 3.70 -12 1 8 18.10 4.50 12 1 -8 13.70 4.10 -12 -1 8 20.10 4.30 12 1 -7 2.40 3.30 -12 1 7 3.80 3.50 -12 -1 7 16.80 4.90 12 -1 -7 6.00 2.50 -12 1 6 8.50 3.10 -12 1 6 21.10 5.50 12 1 -6 9.90 3.60 12 -1 -6 15.40 2.50 -12 -1 6 19.80 4.60 -12 1 5 291.87 16.80 -12 1 5 236.88 9.90 12 1 -5 266.37 12.50 -12 -1 5 224.88 12.50 -12 -1 5 299.27 16.70 12 -1 -5 254.57 9.80 12 1 -4 123.39 11.10 -12 1 4 141.69 12.30 -12 -1 4 140.79 11.60 -12 -1 4 124.19 8.70 12 1 -3 287.57 13.30 -12 -1 3 319.17 13.80 -12 -1 3 311.77 18.00 -12 1 2 242.28 16.10 12 1 -2 244.48 11.50 -12 -1 2 228.78 11.40 -12 -1 2 207.68 17.80 12 1 -1 29.10 4.40 -12 1 1 27.50 6.70 -12 1 1 21.30 2.50 -12 -1 1 29.10 7.50 -12 -1 1 16.20 3.60 -12 1 0 -2.60 3.40 12 1 0 -0.10 2.40 -12 1 0 -1.60 1.40 -12 -1 0 -3.60 2.40 -12 -1 0 2.40 4.50 -12 1 -1 130.49 7.10 -12 1 -1 136.09 12.70 -12 1 -1 158.48 7.70 12 1 1 158.78 9.50 -12 -1 -1 158.88 13.70 -12 1 -2 -4.60 4.10 -12 1 -2 -4.20 2.00 12 1 2 3.80 2.60 -12 1 -2 2.60 4.00 -12 -1 -2 5.10 5.30 -12 1 -3 0.80 4.10 -12 -1 -3 -4.70 4.00 -12 -1 -3 2.50 3.10 -12 1 -4 121.09 8.80 -12 1 -4 132.89 12.90 -12 -1 -4 125.19 9.80 -12 -1 -4 106.19 12.40 -12 2 7 6.90 4.50 12 2 -7 5.60 3.70 12 -2 -7 5.60 1.60 -12 -2 7 14.00 4.30 -12 2 6 11.70 4.50 12 2 -6 13.80 4.20 -12 -2 6 14.30 4.60 12 2 -5 53.09 6.00 -12 -2 5 64.99 8.90 -12 2 4 11.60 5.00 12 2 -4 7.00 3.20 -12 -2 4 11.00 4.50 12 2 -3 4.60 2.60 -12 2 3 5.00 3.60 -12 -2 3 13.70 5.20 -12 2 2 1.40 4.60 12 2 -2 6.30 2.80 -12 -2 2 2.20 4.10 -12 2 1 10.60 4.80 12 2 -1 2.00 2.90 -12 -2 1 7.00 5.10 -12 2 0 0.90 4.10 12 2 0 7.70 3.20 -12 -2 0 -1.50 4.20 -12 2 -1 33.10 7.70 12 2 1 39.10 6.00 -12 -2 -1 30.70 7.90 12 2 2 16.70 4.50 -12 2 -2 10.90 5.90 -12 2 -2 13.00 2.40 -12 -2 -2 17.20 6.60 12 2 3 37.40 6.00 -12 2 -3 33.30 4.10 -12 2 -3 33.60 8.40 -12 -2 -3 30.30 7.80 12 3 -7 22.50 5.40 -12 3 7 22.30 5.90 -12 -3 7 24.90 5.10 12 3 -6 9.80 4.20 -12 3 6 19.80 5.70 -12 -3 6 21.10 5.20 -12 3 5 86.09 9.50 12 3 -5 77.79 7.60 -12 -3 5 86.19 9.20 12 3 -4 4.00 3.30 -12 3 4 4.20 4.00 -12 -3 4 3.30 3.90 12 3 -3 86.59 7.80 -12 3 3 87.79 10.10 12 3 -2 31.30 5.30 -12 3 2 43.90 8.40 -12 -3 2 30.10 7.50 12 3 -1 25.10 5.00 -12 3 1 31.00 7.00 -12 -3 1 28.10 7.20 12 3 0 16.30 4.40 -12 3 0 14.80 5.80 -12 -3 0 7.90 5.60 12 3 1 20.20 5.10 -12 3 -1 29.10 8.00 -12 -3 -1 27.40 7.70 12 3 2 22.40 5.00 -12 3 -2 23.70 7.20 -12 -3 -2 13.20 7.00 12 3 3 2.00 3.20 -12 3 -3 19.10 6.70 -12 -3 -3 -9.70 4.10 -12 4 6 11.60 5.00 12 4 -6 15.80 5.10 -12 -4 6 2.10 3.50 -12 4 5 124.49 12.10 -12 -4 5 120.49 10.70 12 4 -4 16.50 4.30 -12 4 4 19.10 6.10 -12 -4 4 8.70 5.30 12 4 -3 17.30 4.60 -12 4 3 21.30 6.70 -12 -4 3 20.80 6.70 12 4 -2 5.10 3.60 -12 4 2 11.40 5.00 -12 -4 2 3.20 5.60 -12 4 1 18.30 5.40 12 4 -1 12.60 4.10 -12 -4 1 5.60 5.40 12 4 0 7.30 3.90 -12 4 0 12.40 5.30 -12 -4 0 2.20 5.80 -12 4 -1 30.00 7.70 12 4 1 39.40 7.00 -12 -4 -1 29.50 8.50 12 4 2 67.59 10.30 -12 4 -2 95.89 11.30 -12 -4 -2 93.09 13.30 -12 5 5 57.59 9.70 12 5 -5 70.19 8.20 -12 -5 5 53.69 8.30 -12 5 4 37.60 7.70 12 5 -4 39.10 6.80 -12 -5 4 25.70 6.70 12 5 -3 0.30 3.30 -12 5 3 -3.50 3.60 -12 -5 3 -8.30 4.40 -12 5 2 42.50 9.00 -12 -5 2 28.80 8.20 -12 5 1 109.69 12.20 12 5 -1 94.79 9.40 -12 -5 1 115.29 12.60 -12 5 0 39.00 8.10 12 5 0 44.80 7.60 -12 -5 0 36.00 8.90 -12 5 -1 22.40 6.50 12 5 1 11.70 4.60 -12 -5 -1 10.60 6.80 13 0 -6 20.20 3.60 -13 0 6 26.70 5.80 13 0 -5 4.60 2.10 -13 0 5 4.40 4.60 -13 0 4 52.79 8.70 13 0 -4 43.80 4.10 -13 0 3 5.70 4.30 13 0 -3 2.80 1.90 -13 0 2 53.99 9.40 13 0 -2 59.79 4.40 13 0 -1 -1.20 1.80 -13 0 1 -0.40 3.60 -13 0 0 21.20 6.50 -13 0 0 12.20 2.90 -13 0 -1 -4.30 2.20 -13 0 -1 0.80 4.10 -13 1 6 80.29 9.00 13 1 -6 49.80 5.60 13 1 -5 264.47 13.00 -13 1 5 278.77 17.70 -13 -1 5 288.37 17.00 -13 1 4 9.90 5.00 -13 -1 4 9.90 5.30 -13 1 3 118.09 11.70 -13 -1 3 131.29 11.80 -13 1 2 1.40 4.00 -13 -1 2 2.40 4.70 -13 1 1 58.99 9.80 -13 -1 1 66.09 10.10 13 1 0 27.40 4.40 -13 1 0 36.00 8.20 -13 -1 0 40.50 8.60 -13 1 -1 137.49 7.00 13 1 1 154.08 9.50 -13 1 -1 139.39 13.40 -13 -1 -1 167.28 14.60 -13 2 5 40.40 7.60 13 2 -5 34.40 5.20 -13 -2 5 35.00 6.80 13 2 -4 535.65 22.20 -13 2 4 562.04 27.70 -13 -2 4 560.64 26.50 13 2 -3 3.60 2.90 -13 2 3 6.40 4.50 -13 -2 3 1.20 4.10 -13 2 2 57.49 9.80 13 2 -2 57.69 6.10 -13 -2 2 48.10 8.80 13 2 -1 14.00 3.60 -13 2 1 11.00 5.20 -13 -2 1 8.00 5.30 -13 2 0 30.30 7.20 13 2 0 10.60 3.80 -13 -2 0 17.00 6.50 -13 2 -1 111.29 11.80 13 2 1 109.39 8.40 -13 -2 -1 133.69 13.30 13 3 -4 38.20 6.30 -13 3 4 48.60 9.00 -13 -3 4 42.80 8.10 13 3 -3 11.90 4.30 -13 3 3 17.50 6.40 -13 -3 3 31.50 7.20 -13 3 2 83.29 10.10 13 3 -2 82.19 7.70 -13 -3 2 87.49 10.50 13 3 -1 124.29 9.70 -13 3 1 136.19 13.00 -13 -3 1 138.09 13.30 -13 3 0 307.97 20.50 -13 -3 0 330.87 21.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 31543 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_yv471 _database_code_depnum_ccdc_archive 'CCDC 2044216' loop_ _audit_author_name _audit_author_address 'Peter Mayer' ;LMU Muenchen Germany ; _audit_update_record ; 2020-11-13 deposited with the CCDC. 2021-02-09 downloaded from the CCDC. ; _chemical_name_common RNH389f2 _chemical_compound_source ? _chemical_absolute_configuration ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.120 #?# in millimeters _exptl_crystal_size_mid 0.100 #?# in millimeters _exptl_crystal_size_min 0.090 #?# in millimeters _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_special_details ; ; _audit_creation_date ? #?# style: 18-Aug-1998 _diffrn_ambient_temperature 102.(2) #?# in K _diffrn_source_type 'Bruker TXS' _diffrn_source_power 2.5 #?# in kW _diffrn_source_voltage 50 #?# in kV _diffrn_source_current 50 #?# in mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode (TXS)' _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_collimation ? _diffrn_measurement_device 'fixed-chi three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture TXS' _diffrn_measurement_method 'mix of phi and omega scans' _diffrn_measurement_details ? _diffrn_detector_area_resol_mean 7.3910 _diffrn_special_details ? _diffrn_orient_matrix_type ? _diffrn_orient_matrix_UB_11 ? _diffrn_orient_matrix_UB_12 ? _diffrn_orient_matrix_UB_13 ? _diffrn_orient_matrix_UB_21 ? _diffrn_orient_matrix_UB_22 ? _diffrn_orient_matrix_UB_23 ? _diffrn_orient_matrix_UB_31 ? _diffrn_orient_matrix_UB_32 ? _diffrn_orient_matrix_UB_33 ? _cell_length_a 10.8844(9) _cell_length_b 9.9707(7) _cell_length_c 9.1680(7) _cell_angle_alpha 90 _cell_angle_beta 91.835(3) _cell_angle_gamma 90 _cell_volume 994.45(13) _cell_measurement_temperature 102.(2) #?# in K _cell_measurement_reflns_used 7361 _cell_measurement_theta_min 2.7711 _cell_measurement_theta_max 28.2542 _cell_special_details ? _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.99 _shelx_estimated_absorpt_T_min 0.990 _shelx_estimated_absorpt_T_max 0.992 _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _diffrn_reflns_number 17273 #xl _diffrn_reflns_av_R_equivalents 0.0482 #xl _diffrn_reflns_av_unetI/netI 0.0321 #xl _diffrn_reflns_limit_h_min -14 #xl _diffrn_reflns_limit_h_max 14 #xl _diffrn_reflns_limit_k_min -13 #xl _diffrn_reflns_limit_k_max 13 #xl _diffrn_reflns_limit_l_min -12 #xl _diffrn_reflns_limit_l_max 12 #xl _diffrn_reflns_theta_min 3.019 #xl _diffrn_reflns_theta_max 28.282 #xl _diffrn_measured_fraction_theta_max 0.998 #xl _diffrn_reflns_theta_full 25.242 #xl _diffrn_measured_fraction_theta_full 0.997 #xl _diffrn_reflns_Laue_measured_fraction_max 0.998 #xl _diffrn_reflns_Laue_measured_fraction_full 0.997 #xl _diffrn_reflns_point_group_measured_fraction_max 0.998 #xl _diffrn_reflns_point_group_measured_fraction_full 0.997 #xl _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' _space_group_IT_number 14 _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_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' N N 0.0061 0.0033 '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' _reflns_number_total 2461 #xl _reflns_number_gt 2059 #xl _reflns_threshold_expression 'I > 2\s(I)' #xl _reflns_Friedel_coverage 0.000 #xl _reflns_Friedel_fraction_max . #xl _reflns_Friedel_fraction_full . #xl _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. ; _refine_ls_structure_factor_coef Fsqd #xl _refine_ls_matrix_type full #xl _refine_ls_weighting_scheme calc #xl _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.4815P] where P=(Fo^2^+2Fc^2^)/3' #xl _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr #?# _refine_ls_extinction_method none #xl _refine_ls_extinction_coef . #xl _refine_ls_abs_structure_details ? #xl _refine_ls_abs_structure_Flack ? #xl _refine_ls_number_reflns 2461 #xl _refine_ls_number_parameters 141 #xl _refine_ls_number_restraints 0 #xl _refine_ls_R_factor_all 0.0529 #xl _refine_ls_R_factor_gt 0.0415 #xl _refine_ls_wR_factor_ref 0.1163 #xl _refine_ls_wR_factor_gt 0.1046 #xl _refine_ls_goodness_of_fit_ref 1.043 #xl _refine_ls_restrained_S_all 1.043 #xl _refine_ls_shift/su_max 0.000 #xl _refine_ls_shift/su_mean 0.000 #xl _refine_diff_density_max 0.241 #xl _refine_diff_density_min -0.214 #xl _refine_diff_density_rms 0.046 #xl _refine_special_details ; The O-atom is disordered. The sof ratio of the two parts refined to 0.966/0.034. ; _computing_data_collection 'APEX3 v2016.5-0, Bruker AXS (2016)' _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 924)' _computing_publication_material ? 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 C1 C 0.17780(11) 0.53214(12) 0.61837(13) 0.0205(3) Uani 1 1 d . . . . . H1 H 0.095694 0.489786 0.632110 0.025 Uiso 1 1 calc R U . A 1 O1 O 0.03318(9) 0.82127(10) 0.75894(11) 0.0289(3) Uani 0.966(3) 1 d . . P B 1 C2 C 0.25328(12) 0.55600(13) 0.75574(14) 0.0237(3) Uani 0.966(3) 1 d . . P B 1 H2 H 0.344638 0.546312 0.753440 0.028 Uiso 0.966(3) 1 calc R U P B 1 C3 C 0.19274(11) 0.67459(12) 0.68012(14) 0.0219(3) Uani 0.966(3) 1 d . . P B 1 H3 H 0.243381 0.742536 0.628879 0.026 Uiso 0.966(3) 1 calc R U P B 1 C4 C 0.09006(11) 0.71763(12) 0.77171(13) 0.0215(3) Uani 0.966(3) 1 d . . P B 1 C5 C 0.06892(12) 0.61088(13) 0.88615(14) 0.0246(3) Uani 0.966(3) 1 d . . P B 1 H5A H -0.000356 0.551829 0.855603 0.029 Uiso 0.966(3) 1 calc R U P B 1 H5AB H 0.050222 0.652535 0.980922 0.029 Uiso 0.966(3) 1 calc R U P B 1 C6 C 0.18925(13) 0.53098(14) 0.89841(14) 0.0287(3) Uani 0.966(3) 1 d . . P B 1 H6A H 0.240802 0.562589 0.982447 0.034 Uiso 0.966(3) 1 calc R U P B 1 H6AB H 0.172303 0.434197 0.911103 0.034 Uiso 0.966(3) 1 calc R U P B 1 O1B O 0.191(3) 0.451(4) 0.980(4) 0.044(10) Uiso 0.034(3) 1 d . . P B 2 C2B C 0.25328(12) 0.55600(13) 0.75574(14) 0.0237(3) Uani 0.034(3) 1 d . . P B 2 H2B H 0.344638 0.546312 0.753440 0.028 Uiso 0.034(3) 1 calc R U P B 2 C3B C 0.19274(11) 0.67459(12) 0.68012(14) 0.0219(3) Uani 0.034(3) 1 d . . P B 2 H3B H 0.243381 0.742536 0.628879 0.026 Uiso 0.034(3) 1 calc R U P B 2 C4B C 0.09006(11) 0.71763(12) 0.77171(13) 0.0215(3) Uani 0.034(3) 1 d . . P B 2 H4A H 0.014526 0.730111 0.710159 0.026 Uiso 0.034(3) 1 calc R U P B 2 H4AB H 0.110498 0.804112 0.819670 0.026 Uiso 0.034(3) 1 calc R U P B 2 C5B C 0.06892(12) 0.61088(13) 0.88615(14) 0.0246(3) Uani 0.034(3) 1 d . . P B 2 H5C H -0.000356 0.551829 0.855603 0.029 Uiso 0.034(3) 1 calc R U P B 2 H5D H 0.050222 0.652535 0.980922 0.029 Uiso 0.034(3) 1 calc R U P B 2 C6B C 0.18925(13) 0.53098(14) 0.89841(14) 0.0287(3) Uani 0.034(3) 1 d . . P B 2 C7 C 0.23924(11) 0.49492(12) 0.48162(13) 0.0197(3) Uani 1 1 d . . . . . C8 C 0.19527(12) 0.38377(13) 0.40315(14) 0.0229(3) Uani 1 1 d . . . . . H8 H 0.125212 0.337079 0.435817 0.027 Uiso 1 1 calc R U . . . C9 C 0.25211(12) 0.34051(13) 0.27848(14) 0.0240(3) Uani 1 1 d . . . . . H9 H 0.221921 0.264079 0.226885 0.029 Uiso 1 1 calc R U . . . C10 C 0.35405(11) 0.41011(13) 0.22934(13) 0.0224(3) Uani 1 1 d . . . . . C11 C 0.39732(12) 0.52298(13) 0.30443(14) 0.0248(3) Uani 1 1 d . . . . . H11 H 0.465399 0.571720 0.269568 0.030 Uiso 1 1 calc R U . . . C12 C 0.34065(11) 0.56392(13) 0.43025(14) 0.0241(3) Uani 1 1 d . . . . . H12 H 0.371289 0.639968 0.482156 0.029 Uiso 1 1 calc R U . . . C13 C 0.41650(12) 0.36449(13) 0.10175(14) 0.0251(3) Uani 1 1 d . . . . . N1 N 0.46719(12) 0.32889(13) 0.00087(13) 0.0330(3) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0215(6) 0.0201(6) 0.0201(6) -0.0001(4) 0.0027(4) -0.0015(4) O1 0.0333(6) 0.0223(5) 0.0314(6) 0.0009(4) 0.0049(4) 0.0082(4) C2 0.0241(6) 0.0241(6) 0.0227(6) -0.0015(5) -0.0006(5) 0.0042(5) C3 0.0227(6) 0.0192(6) 0.0238(6) 0.0000(5) 0.0032(5) -0.0007(5) C4 0.0233(6) 0.0204(6) 0.0206(6) -0.0024(5) -0.0008(4) -0.0003(5) C5 0.0317(7) 0.0228(6) 0.0195(6) -0.0002(5) 0.0046(5) 0.0022(5) C6 0.0407(8) 0.0261(7) 0.0192(6) 0.0003(5) -0.0005(5) 0.0097(6) C2B 0.0241(6) 0.0241(6) 0.0227(6) -0.0015(5) -0.0006(5) 0.0042(5) C3B 0.0227(6) 0.0192(6) 0.0238(6) 0.0000(5) 0.0032(5) -0.0007(5) C4B 0.0233(6) 0.0204(6) 0.0206(6) -0.0024(5) -0.0008(4) -0.0003(5) C5B 0.0317(7) 0.0228(6) 0.0195(6) -0.0002(5) 0.0046(5) 0.0022(5) C6B 0.0407(8) 0.0261(7) 0.0192(6) 0.0003(5) -0.0005(5) 0.0097(6) C7 0.0196(5) 0.0205(6) 0.0190(6) 0.0011(4) 0.0010(4) 0.0011(4) C8 0.0239(6) 0.0217(6) 0.0231(6) 0.0014(5) 0.0030(5) -0.0032(5) C9 0.0274(6) 0.0228(6) 0.0217(6) -0.0011(5) 0.0006(5) -0.0007(5) C10 0.0219(6) 0.0253(6) 0.0200(6) 0.0020(5) 0.0017(4) 0.0057(5) C11 0.0211(6) 0.0270(6) 0.0266(6) 0.0013(5) 0.0050(5) 0.0003(5) C12 0.0231(6) 0.0236(6) 0.0258(6) -0.0026(5) 0.0033(5) -0.0027(5) C13 0.0247(6) 0.0255(6) 0.0253(6) 0.0013(5) 0.0013(5) 0.0038(5) N1 0.0359(7) 0.0331(7) 0.0306(6) -0.0023(5) 0.0088(5) 0.0050(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 C1 C7 1.4868(16) . ? C1 C2 1.5004(17) . ? C1 C2B 1.5004(17) . ? C1 C3 1.5357(17) . ? C1 C3B 1.5357(17) . ? C1 H1 1.0000 . ? O1 C4 1.2084(15) . ? C2 C3 1.5112(17) . ? C2 C6 1.5222(18) . ? C2 H2 1.0000 . ? C3 C4 1.4827(17) . ? C3 H3 1.0000 . ? C4 C5 1.5172(17) . ? C5 C6 1.5341(19) . ? C5 H5A 0.9900 . ? C5 H5AB 0.9900 . ? C6 H6A 0.9900 . ? C6 H6AB 0.9900 . ? O1B C6B 1.09(4) . ? C2B C3B 1.5112(17) . ? C2B C6B 1.5222(18) . ? C2B H2B 1.0000 . ? C3B C4B 1.4827(17) . ? C3B H3B 1.0000 . ? C4B C5B 1.5172(17) . ? C4B H4A 0.9900 . ? C4B H4AB 0.9900 . ? C5B C6B 1.5341(19) . ? C5B H5C 0.9900 . ? C5B H5D 0.9900 . ? C7 C12 1.3953(17) . ? C7 C8 1.3974(17) . ? C8 C9 1.3858(17) . ? C8 H8 0.9500 . ? C9 C10 1.3956(18) . ? C9 H9 0.9500 . ? C10 C11 1.3934(18) . ? C10 C13 1.4450(17) . ? C11 C12 1.3868(17) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 N1 1.1482(18) . ? 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 C7 C1 C2 119.89(10) . . ? C7 C1 C2B 119.89(10) . . ? C7 C1 C3 119.77(10) . . ? C2 C1 C3 59.69(8) . . ? C7 C1 C3B 119.77(10) . . ? C2B C1 C3B 59.69(8) . . ? C7 C1 H1 115.4 . . ? C2 C1 H1 115.4 . . ? C3 C1 H1 115.4 . . ? C1 C2 C3 61.32(8) . . ? C1 C2 C6 116.22(11) . . ? C3 C2 C6 108.52(10) . . ? C1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C6 C2 H2 119.0 . . ? C4 C3 C2 106.99(10) . . ? C4 C3 C1 113.80(10) . . ? C2 C3 C1 59.00(8) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C1 C3 H3 120.5 . . ? O1 C4 C3 125.85(12) . . ? O1 C4 C5 125.34(12) . . ? C3 C4 C5 108.81(10) . . ? C4 C5 C6 105.48(11) . . ? C4 C5 H5A 110.6 . . ? C6 C5 H5A 110.6 . . ? C4 C5 H5AB 110.6 . . ? C6 C5 H5AB 110.6 . . ? H5A C5 H5AB 108.8 . . ? C2 C6 C5 105.38(10) . . ? C2 C6 H6A 110.7 . . ? C5 C6 H6A 110.7 . . ? C2 C6 H6AB 110.7 . . ? C5 C6 H6AB 110.7 . . ? H6A C6 H6AB 108.8 . . ? C1 C2B C3B 61.32(8) . . ? C1 C2B C6B 116.22(11) . . ? C3B C2B C6B 108.52(10) . . ? C1 C2B H2B 119.0 . . ? C3B C2B H2B 119.0 . . ? C6B C2B H2B 119.0 . . ? C4B C3B C2B 106.99(10) . . ? C4B C3B C1 113.80(10) . . ? C2B C3B C1 59.00(8) . . ? C4B C3B H3B 120.5 . . ? C2B C3B H3B 120.5 . . ? C1 C3B H3B 120.5 . . ? C3B C4B C5B 108.81(10) . . ? C3B C4B H4A 109.9 . . ? C5B C4B H4A 109.9 . . ? C3B C4B H4AB 109.9 . . ? C5B C4B H4AB 109.9 . . ? H4A C4B H4AB 108.3 . . ? C4B C5B C6B 105.48(11) . . ? C4B C5B H5C 110.6 . . ? C6B C5B H5C 110.6 . . ? C4B C5B H5D 110.6 . . ? C6B C5B H5D 110.6 . . ? H5C C5B H5D 108.8 . . ? O1B C6B C2B 135.4(19) . . ? O1B C6B C5B 114.9(18) . . ? C2B C6B C5B 105.38(10) . . ? C12 C7 C8 118.61(11) . . ? C12 C7 C1 122.93(11) . . ? C8 C7 C1 118.44(11) . . ? C9 C8 C7 121.12(11) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.47(12) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C11 C10 C9 120.12(11) . . ? C11 C10 C13 119.59(12) . . ? C9 C10 C13 120.28(12) . . ? C12 C11 C10 119.76(12) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C7 120.89(12) . . ? C11 C12 H12 119.6 . . ? C7 C12 H12 119.6 . . ? N1 C13 C10 179.31(15) . . ? 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 C7 C1 C2 C3 109.11(12) . . . . ? C7 C1 C2 C6 -153.19(11) . . . . ? C3 C1 C2 C6 97.70(12) . . . . ? C1 C2 C3 C4 107.98(11) . . . . ? C6 C2 C3 C4 -2.38(14) . . . . ? C6 C2 C3 C1 -110.36(12) . . . . ? C7 C1 C3 C4 154.53(11) . . . . ? C2 C1 C3 C4 -96.17(12) . . . . ? C7 C1 C3 C2 -109.31(12) . . . . ? C2 C3 C4 O1 167.57(12) . . . . ? C1 C3 C4 O1 -129.42(13) . . . . ? C2 C3 C4 C5 -11.62(13) . . . . ? C1 C3 C4 C5 51.38(14) . . . . ? O1 C4 C5 C6 -158.28(13) . . . . ? C3 C4 C5 C6 20.92(14) . . . . ? C1 C2 C6 C5 -51.40(15) . . . . ? C3 C2 C6 C5 15.06(14) . . . . ? C4 C5 C6 C2 -21.64(14) . . . . ? C7 C1 C2B C3B 109.11(12) . . . . ? C7 C1 C2B C6B -153.19(11) . . . . ? C3B C1 C2B C6B 97.70(12) . . . . ? C1 C2B C3B C4B 107.98(11) . . . . ? C6B C2B C3B C4B -2.38(14) . . . . ? C6B C2B C3B C1 -110.36(12) . . . . ? C7 C1 C3B C4B 154.53(11) . . . . ? C2B C1 C3B C4B -96.17(12) . . . . ? C7 C1 C3B C2B -109.31(12) . . . . ? C2B C3B C4B C5B -11.62(13) . . . . ? C1 C3B C4B C5B 51.38(14) . . . . ? C3B C4B C5B C6B 20.92(14) . . . . ? C1 C2B C6B O1B 103(3) . . . . ? C3B C2B C6B O1B 169(3) . . . . ? C1 C2B C6B C5B -51.40(15) . . . . ? C3B C2B C6B C5B 15.06(14) . . . . ? C4B C5B C6B O1B 178(2) . . . . ? C4B C5B C6B C2B -21.64(14) . . . . ? C2 C1 C7 C12 -48.35(17) . . . . ? C2B C1 C7 C12 -48.35(17) . . . . ? C3 C1 C7 C12 21.66(18) . . . . ? C3B C1 C7 C12 21.66(18) . . . . ? C2 C1 C7 C8 129.98(12) . . . . ? C2B C1 C7 C8 129.98(12) . . . . ? C3 C1 C7 C8 -160.01(11) . . . . ? C3B C1 C7 C8 -160.01(11) . . . . ? C12 C7 C8 C9 1.33(19) . . . . ? C1 C7 C8 C9 -177.07(12) . . . . ? C7 C8 C9 C10 -0.84(19) . . . . ? C8 C9 C10 C11 -0.66(19) . . . . ? C8 C9 C10 C13 178.39(12) . . . . ? C9 C10 C11 C12 1.63(19) . . . . ? C13 C10 C11 C12 -177.43(12) . . . . ? C10 C11 C12 C7 -1.1(2) . . . . ? C8 C7 C12 C11 -0.34(19) . . . . ? C1 C7 C12 C11 177.98(12) . . . . ? _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. ; _audit_block_code C13H11NO_yv471_ofial _audit_creation_method 'APEX3 v2018.7-2' _shelxl_version_number ? _chemical_name_systematic ? _chemical_formula_moiety 'C13 H11 N O' _chemical_formula_sum 'C13 H11 N O' _chemical_formula_weight 197.23 #?# (Cohen, 1996) _chemical_melting_point ? #?# in K! _cell_formula_units_Z 4 #?# adjust to _chemical_formula_[] _exptl_crystal_density_diffrn 1.317 _exptl_crystal_F_000 416 #?# check! _shelx_res_file ; TITL yv471_0ma_a.res in P2(1)/c yv471.res created by SHELXL-2018/3 at 12:34:57 on 18-Aug-2020 REM Old TITL yv471_0ma in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.113, Rweak 0.002, Alpha 0.015, Orientation as input REM Formula found by SHELXT: C13 N O CELL 0.71073 10.8844 9.9707 9.1680 90.000 91.835 90.000 ZERR 4.000 0.0009 0.0007 0.0007 0.000 0.003 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O UNIT 52 44 4 4 TEMP -171 SIZE 0.09 0.10 0.12 L.S. 10 BOND $H LIST 4 CONF ACTA OMIT 1 1 0 ! 0.70 157.13 14.98 0.103 7.35 OMIT 6 3 0 ! 32.55 2.69 8.80 0.014 1.59 OMIT 6 3 3 ! 133.55 38.92 8.73 0.052 1.40 OMIT 3 6 6 ! 46.29 12.62 6.73 0.029 1.07 SHEL 9.0 0.75 FMAP 2 PLAN -20 EXYZ C2 C2B EADP C2 C2B EXYZ C3 C3B EADP C3 C3B EXYZ C4 C4B EADP C4 C4B EXYZ C5 C5B EADP C5 C5B EXYZ C6 C6B EADP C6 C6B WGHT 0.048300 0.481500 FVAR 0.84956 0.96559 C1 1 0.177795 0.532143 0.618370 11.00000 0.02148 0.02009 = 0.02014 -0.00005 0.00275 -0.00151 AFIX 13 H1 2 0.095694 0.489786 0.632110 11.00000 -1.20000 AFIX 0 PART 1 21.0 O1 4 0.033183 0.821274 0.758937 21.00000 0.03329 0.02234 = 0.03139 0.00093 0.00487 0.00823 C2 1 0.253275 0.555998 0.755736 21.00000 0.02412 0.02414 = 0.02269 -0.00146 -0.00059 0.00417 AFIX 13 H2 2 0.344638 0.546312 0.753440 21.00000 -1.20000 AFIX 0 C3 1 0.192742 0.674594 0.680122 21.00000 0.02272 0.01925 = 0.02382 0.00004 0.00323 -0.00074 AFIX 13 H3 2 0.243381 0.742536 0.628879 21.00000 -1.20000 AFIX 0 C4 1 0.090057 0.717629 0.771713 21.00000 0.02333 0.02040 = 0.02063 -0.00237 -0.00080 -0.00032 C5 1 0.068916 0.610881 0.886152 21.00000 0.03172 0.02277 = 0.01948 -0.00022 0.00465 0.00221 AFIX 23 H5A 2 -0.000356 0.551829 0.855603 21.00000 -1.20000 H5AB 2 0.050222 0.652535 0.980922 21.00000 -1.20000 AFIX 0 C6 1 0.189253 0.530976 0.898408 21.00000 0.04066 0.02610 = 0.01921 0.00027 -0.00046 0.00973 AFIX 23 H6A 2 0.240802 0.562589 0.982447 21.00000 -1.20000 H6AB 2 0.172303 0.434197 0.911103 21.00000 -1.20000 AFIX 0 PART 2 -21.0 O1B 4 0.190676 0.451213 0.980098 -21.00000 0.04362 C2B 1 0.253275 0.555998 0.755736 -21.00000 0.02412 0.02414 = 0.02269 -0.00146 -0.00059 0.00417 AFIX 13 H2B 2 0.344638 0.546312 0.753440 -21.00000 -1.20000 AFIX 0 C3B 1 0.192742 0.674594 0.680122 -21.00000 0.02272 0.01925 = 0.02382 0.00004 0.00323 -0.00074 AFIX 13 H3B 2 0.243381 0.742536 0.628879 -21.00000 -1.20000 AFIX 0 C4B 1 0.090057 0.717629 0.771713 -21.00000 0.02333 0.02040 = 0.02063 -0.00237 -0.00080 -0.00032 AFIX 23 H4A 2 0.014526 0.730111 0.710159 -21.00000 -1.20000 H4AB 2 0.110498 0.804112 0.819670 -21.00000 -1.20000 AFIX 0 C5B 1 0.068916 0.610881 0.886152 -21.00000 0.03172 0.02277 = 0.01948 -0.00022 0.00465 0.00221 AFIX 23 H5C 2 -0.000356 0.551829 0.855603 -21.00000 -1.20000 H5D 2 0.050222 0.652535 0.980922 -21.00000 -1.20000 AFIX 0 C6B 1 0.189253 0.530976 0.898408 -21.00000 0.04066 0.02610 = 0.01921 0.00027 -0.00046 0.00973 PART 0 C7 1 0.239239 0.494921 0.481619 11.00000 0.01959 0.02046 = 0.01900 0.00107 0.00101 0.00107 C8 1 0.195266 0.383775 0.403148 11.00000 0.02393 0.02170 = 0.02314 0.00135 0.00305 -0.00322 AFIX 43 H8 2 0.125212 0.337079 0.435817 11.00000 -1.20000 AFIX 0 C9 1 0.252107 0.340508 0.278484 11.00000 0.02741 0.02282 = 0.02168 -0.00114 0.00057 -0.00066 AFIX 43 H9 2 0.221921 0.264079 0.226885 11.00000 -1.20000 AFIX 0 C10 1 0.354052 0.410106 0.229341 11.00000 0.02193 0.02533 = 0.02002 0.00196 0.00170 0.00570 C11 1 0.397323 0.522984 0.304433 11.00000 0.02112 0.02704 = 0.02656 0.00127 0.00504 0.00028 AFIX 43 H11 2 0.465399 0.571720 0.269568 11.00000 -1.20000 AFIX 0 C12 1 0.340651 0.563919 0.430245 11.00000 0.02310 0.02356 = 0.02585 -0.00260 0.00331 -0.00269 AFIX 43 H12 2 0.371289 0.639968 0.482156 11.00000 -1.20000 AFIX 0 C13 1 0.416502 0.364490 0.101752 11.00000 0.02469 0.02548 = 0.02525 0.00131 0.00131 0.00379 N1 3 0.467188 0.328890 0.000874 11.00000 0.03588 0.03310 = 0.03061 -0.00232 0.00879 0.00502 HKLF 4 REM yv471_0ma_a.res in P2(1)/c REM wR2 = 0.116341, GooF = S = 1.04275, Restrained GooF = 1.04275 for all data REM R1 = 0.041538 for 2059 Fo > 4sig(Fo) and 0.052872 for all 2461 data REM 141 parameters refined using 0 restraints END WGHT 0.0483 0.4815 REM Highest difference peak 0.241, deepest hole -0.214, 1-sigma level 0.046 Q1 1 0.2188 0.5468 0.8212 11.00000 0.05 0.24 Q2 1 0.0775 0.6681 0.8353 11.00000 0.05 0.23 Q3 1 0.3044 0.3854 0.2553 11.00000 0.05 0.23 Q4 1 0.2098 0.5189 0.5415 11.00000 0.05 0.22 Q5 1 0.2444 0.3524 0.3596 11.00000 0.05 0.22 Q6 1 0.3441 0.5555 0.3425 11.00000 0.05 0.21 Q7 1 0.2212 0.5151 0.6865 11.00000 0.05 0.21 Q8 1 0.1994 0.4596 0.4164 11.00000 0.05 0.20 Q9 1 0.1267 0.6877 0.7015 11.00000 0.05 0.20 Q10 1 0.2806 0.5386 0.4524 11.00000 0.05 0.20 Q11 1 0.1326 0.5785 0.8917 11.00000 0.05 0.19 Q12 1 0.3837 0.4525 0.2781 11.00000 0.05 0.18 Q13 1 0.2408 0.6423 0.7572 11.00000 0.05 0.17 Q14 1 0.2410 0.4192 0.4559 11.00000 0.05 0.17 Q15 1 0.3830 0.3835 0.1635 11.00000 0.05 0.16 Q16 1 0.1641 0.6131 0.6135 11.00000 0.05 0.15 Q17 1 -0.0155 0.5988 0.8142 11.00000 0.05 0.15 Q18 1 0.2183 0.4979 1.0037 11.00000 0.05 0.14 Q19 1 0.2595 0.5857 0.9603 11.00000 0.05 0.13 Q20 1 0.1323 0.8684 0.6633 11.00000 0.05 0.13 ; _shelx_res_checksum 16640 _shelx_hkl_file ; 0 0 1 -0.10 0.10 0 0 1 0.00 0.10 0 0 -2 1732.03 119.89 0 0 2 1713.63 116.09 0 0 3 0.30 0.40 0 0 -3 0.30 0.50 0 0 -3 0.10 0.30 0 0 3 0.30 0.50 0 0 3 0.30 0.60 0 0 -3 0.50 0.40 0 0 4 875.91 39.00 0 0 -4 831.92 37.60 0 0 4 899.41 37.80 0 0 -4 871.01 38.70 0 0 -4 823.22 38.70 0 0 -5 3.70 1.10 0 0 -5 3.50 0.70 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7 2 19.80 2.60 1 -7 2 16.80 2.60 -1 -7 -2 18.90 2.50 1 -7 2 14.50 3.30 1 -7 2 16.30 3.20 1 7 3 43.50 4.30 1 7 3 33.30 3.40 1 7 3 36.80 3.20 -1 7 -3 41.10 3.90 1 7 3 43.10 3.80 -1 7 -3 39.10 4.60 1 7 3 42.80 3.80 1 -7 3 40.50 3.80 1 -7 3 41.50 4.90 -1 -7 -3 41.00 3.70 1 -7 3 43.30 4.70 1 7 4 82.29 5.40 1 7 4 75.89 5.80 1 7 4 73.69 4.80 -1 7 -4 68.89 5.70 1 7 4 71.79 5.50 1 7 4 67.39 5.80 1 7 4 95.09 5.60 1 -7 4 70.29 7.10 1 -7 4 75.09 6.10 1 -7 4 91.49 7.10 1 7 5 5.50 1.40 1 7 5 2.30 1.40 1 7 5 7.30 2.00 1 7 5 3.90 1.00 1 7 5 4.00 1.30 1 -7 5 6.90 2.10 1 -7 5 5.60 1.90 -1 -7 -5 6.60 2.20 1 -7 5 2.50 2.10 1 7 6 86.39 7.00 1 7 6 86.29 5.90 1 7 6 84.49 4.50 -1 7 -6 72.89 6.30 1 7 6 89.29 6.40 1 7 6 87.59 4.60 1 -7 6 81.79 7.40 1 -7 6 103.29 7.50 1 -7 6 93.79 8.80 1 7 7 19.60 3.70 1 7 7 17.50 3.20 1 7 7 15.40 2.60 1 -7 7 19.50 3.80 1 -7 7 16.70 3.50 1 -7 7 16.90 4.40 1 7 8 8.10 2.50 1 7 8 5.80 2.10 1 7 8 7.90 2.20 1 -7 8 7.70 2.40 1 -7 8 9.90 3.10 1 -7 8 6.70 3.00 1 7 9 49.70 4.90 1 7 9 39.80 5.80 1 -7 9 49.99 5.90 1 -7 9 45.90 7.90 1 -7 9 52.19 6.00 1 7 10 1.90 2.90 -1 7 -10 6.20 3.30 1 7 10 7.80 2.20 1 -7 10 2.30 3.10 1 -7 10 4.70 2.50 1 -7 10 9.40 3.10 -1 8 9 -2.00 1.40 -1 8 9 0.00 1.90 -1 -8 9 -1.80 1.70 -1 -8 9 -3.30 2.10 -1 -8 9 -2.30 1.20 -1 8 8 2.90 2.00 -1 8 8 3.70 1.70 -1 -8 8 0.40 2.40 -1 -8 8 5.00 1.90 -1 -8 8 6.20 2.50 -1 8 7 2.00 0.70 -1 8 7 -0.40 1.20 -1 8 7 0.40 0.60 1 8 -7 4.80 1.40 -1 8 7 2.50 1.80 -1 -8 7 3.50 2.00 -1 -8 7 1.90 2.60 -1 -8 7 3.00 1.60 -1 8 6 7.80 1.80 -1 8 6 2.00 1.60 -1 8 6 5.20 1.30 -1 8 6 4.80 2.10 -1 8 6 5.40 2.20 1 8 -6 4.70 1.60 -1 -8 6 4.60 1.80 -1 -8 6 0.70 2.30 -1 -8 6 6.70 2.50 -1 8 5 -1.20 0.90 -1 8 5 0.40 1.40 -1 8 5 0.70 0.80 -1 8 5 1.40 1.10 1 8 -5 -1.40 0.80 -1 8 5 3.60 1.60 -1 -8 5 0.50 1.70 -1 -8 5 -0.20 1.00 -1 -8 5 2.20 1.20 -1 8 4 -2.00 1.00 -1 8 4 0.60 1.30 -1 8 4 -0.40 1.10 -1 8 4 0.30 0.90 1 8 -4 -0.30 0.90 -1 8 4 0.80 1.30 -1 -8 4 -1.60 1.20 -1 -8 4 -1.90 1.30 -1 -8 4 0.00 0.80 -1 8 3 30.20 3.70 -1 8 3 22.90 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-1 -13 -1 17.80 4.00 1 13 2 -1.10 1.30 1 13 2 1.50 2.00 -1 13 -2 2.70 1.50 -1 13 -2 -0.90 2.30 1 -13 2 -1.80 2.40 -2 0 12 1.60 2.40 -2 0 12 0.70 3.00 2 0 -11 -0.10 1.30 -2 0 11 -2.10 2.10 -2 0 11 -1.50 2.40 -2 0 11 0.00 1.00 -2 0 10 169.78 12.40 2 0 -10 177.68 9.40 -2 0 10 159.88 11.70 -2 0 10 170.38 9.40 -2 0 9 -0.80 1.50 2 0 -9 0.10 1.00 -2 0 9 -0.70 1.40 -2 0 9 -0.30 0.80 -2 0 8 404.86 18.50 2 0 -8 360.56 18.30 -2 0 8 400.86 21.10 -2 0 8 368.36 20.20 -2 0 7 0.60 1.10 -2 0 7 -0.30 1.10 2 0 -7 -1.00 1.00 2 0 -7 -0.90 0.60 2 0 -7 0.20 0.90 -2 0 7 0.00 0.70 -2 0 6 202.38 10.50 2 0 -6 211.48 12.20 2 0 -6 207.68 10.50 2 0 -6 247.08 11.90 -2 0 6 196.98 12.00 -2 0 6 192.98 11.50 2 0 -5 -0.50 0.80 -2 0 5 0.50 0.50 2 0 -5 0.20 0.70 2 0 -5 -1.00 0.40 -2 0 5 0.30 0.70 -2 0 5 1.00 1.00 -2 0 4 29.60 2.30 2 0 -4 25.60 2.90 2 0 -4 30.10 2.70 -2 0 4 28.50 3.00 2 0 -4 28.50 2.30 -2 0 4 28.30 2.70 2 0 -3 0.20 0.40 2 0 -3 0.30 0.70 -2 0 3 1.10 0.60 -2 0 3 -0.30 0.40 2 0 -3 0.50 0.50 -2 0 3 0.80 0.60 2 0 -2 52.89 3.20 -2 0 2 52.79 3.30 2 0 -2 54.79 3.30 -2 0 2 58.19 3.60 -2 0 2 53.59 3.20 2 0 -2 54.19 3.50 2 0 -1 0.30 0.50 2 0 -1 0.40 0.50 -2 0 1 0.20 0.40 -2 0 1 0.40 0.50 2 0 -1 0.20 0.40 -2 0 1 0.70 0.50 -2 0 0 1843.22 120.89 2 0 1 0.30 0.50 2 0 1 0.00 0.50 -2 0 -1 0.30 0.50 -2 0 -1 -0.40 0.50 2 0 1 -0.30 0.40 -2 0 -1 0.00 0.40 2 0 2 229.18 11.00 -2 0 -2 232.68 11.20 -2 0 -2 216.58 10.70 2 0 2 237.98 11.40 2 0 2 254.27 10.90 -2 0 -2 210.08 10.80 2 0 3 0.70 0.70 -2 0 -3 0.00 0.40 -2 0 -3 0.50 0.50 2 0 3 0.70 0.90 -2 0 -3 0.10 0.60 -2 0 -3 0.10 0.70 -2 0 -4 403.36 19.40 2 0 4 390.76 19.20 -2 0 -4 407.06 18.30 2 0 4 370.56 19.50 -2 0 -4 424.66 18.40 -2 0 -4 410.96 19.10 -2 0 -5 2.20 0.70 -2 0 -5 2.80 1.10 2 0 5 2.00 1.30 2 0 5 2.20 1.00 -2 0 -5 1.90 1.00 -2 0 -6 1.80 1.10 2 0 6 1.90 1.20 -2 0 -6 0.70 0.60 -2 0 -6 1.90 1.10 2 0 6 1.00 1.10 -2 0 -6 0.40 0.50 -2 0 -7 -0.50 0.90 2 0 7 -0.30 0.90 2 0 7 -0.80 1.50 -2 0 -7 -0.30 0.50 -2 0 -7 0.00 0.50 -2 0 -8 126.29 8.90 2 0 8 126.39 9.80 -2 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5 7 2.20 0.50 -2 5 7 3.70 1.70 -2 5 7 2.00 1.50 -2 5 7 3.10 0.70 2 5 -7 1.50 1.20 -2 -5 7 3.00 1.70 -2 -5 7 1.80 1.70 -2 -5 7 1.60 1.40 2 5 -6 62.79 4.70 -2 5 6 71.59 4.10 -2 5 6 68.89 5.80 2 5 -6 69.69 6.10 -2 5 6 66.39 5.70 -2 5 6 61.59 3.90 -2 -5 6 61.19 6.10 -2 -5 6 64.59 5.70 -2 -5 6 67.79 5.20 -2 5 5 690.43 31.50 -2 5 5 705.43 33.20 2 5 -5 628.44 33.30 -2 5 5 678.33 33.30 2 5 -5 690.43 32.80 -2 5 5 712.93 31.50 2 5 -5 715.33 31.60 -2 5 5 701.53 33.00 -2 -5 5 687.33 34.10 -2 -5 5 678.63 32.00 2 -5 -5 731.23 33.70 -2 -5 5 698.73 33.20 2 5 -4 5.10 1.20 -2 5 4 5.10 1.50 -2 5 4 7.00 1.40 -2 5 4 2.30 1.20 -2 5 4 4.80 1.10 2 5 -4 4.60 1.60 2 5 -4 6.20 1.90 2 -5 -4 5.80 1.90 -2 -5 4 5.90 2.00 -2 -5 4 3.70 1.50 -2 -5 4 4.50 1.20 -2 5 3 127.19 8.20 2 5 -3 124.69 7.80 2 5 -3 123.09 7.50 -2 5 3 127.69 7.10 -2 5 3 97.49 6.80 -2 5 3 122.19 8.40 2 5 -3 128.99 6.20 -2 5 3 120.39 7.70 -2 -5 3 116.99 7.60 -2 -5 3 116.79 8.00 -2 -5 3 125.89 6.40 -2 5 2 239.38 12.00 -2 5 2 191.08 11.70 2 5 -2 231.48 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168.48 9.10 2 -5 2 171.18 11.40 2 -5 2 182.28 11.40 -2 -5 -2 179.88 9.60 -2 -5 -2 186.58 9.60 2 -5 2 194.98 10.50 2 5 3 128.69 6.30 -2 5 -3 120.99 8.30 2 5 3 117.39 6.50 -2 5 -3 108.09 7.50 2 5 3 115.69 7.00 -2 5 -3 120.19 7.70 -2 -5 -3 121.29 6.60 2 -5 3 125.79 7.80 -2 -5 -3 127.29 7.20 2 -5 3 119.29 8.50 2 -5 3 119.39 7.90 2 5 4 16.10 1.60 -2 5 -4 21.20 3.10 2 5 4 19.80 2.10 2 5 4 17.70 1.80 -2 5 -4 19.70 3.10 2 5 4 18.20 3.20 -2 -5 -4 20.10 1.80 2 -5 4 19.60 3.60 -2 -5 -4 16.00 2.30 2 -5 4 23.70 3.20 2 5 5 190.28 9.20 -2 5 -5 172.68 10.50 2 5 5 183.48 10.50 -2 5 -5 188.88 11.70 -2 5 -5 173.28 11.30 2 5 5 161.98 8.20 2 -5 5 181.58 11.00 -2 -5 -5 182.68 10.40 2 -5 5 162.48 11.50 2 -5 5 162.28 10.70 2 5 6 2.80 1.70 -2 5 -6 1.80 1.40 2 5 6 2.50 1.10 -2 5 -6 1.60 1.30 2 -5 6 5.90 2.10 2 -5 6 3.10 1.90 -2 -5 -6 3.40 1.30 2 -5 6 5.10 2.20 2 5 7 105.29 6.80 2 5 7 96.39 7.90 -2 -5 -7 119.99 7.10 2 -5 7 105.39 9.20 2 -5 7 99.19 8.30 2 -5 7 98.29 7.80 2 5 8 9.20 3.40 -2 5 -8 6.50 2.50 2 5 8 8.70 2.00 2 -5 8 4.80 2.10 2 -5 8 10.80 2.90 -2 -5 -8 5.20 1.90 2 -5 8 7.20 2.70 2 5 9 22.80 4.70 -2 5 -9 24.40 4.50 2 5 9 16.30 3.10 2 -5 9 27.80 5.00 2 -5 9 19.40 4.60 -2 -5 -9 19.30 3.30 2 5 10 -0.70 1.50 -2 5 -10 0.40 1.30 2 5 10 0.10 2.30 2 -5 10 -0.30 2.00 2 -5 10 0.50 2.30 2 5 11 -0.10 1.90 2 5 11 -4.70 1.90 -2 5 -11 0.30 2.30 2 -5 11 2.60 2.60 2 -5 11 -2.10 2.90 -2 6 10 -2.00 1.20 -2 6 10 -1.30 1.60 -2 -6 10 3.20 2.90 -2 -6 10 -2.90 1.00 -2 -6 10 -0.20 2.50 -2 6 9 70.79 7.20 -2 6 9 71.79 7.00 -2 -6 9 69.29 6.80 -2 -6 9 72.89 6.70 -2 -6 9 69.79 8.30 -2 6 8 1.20 1.50 -2 6 8 1.40 1.20 2 6 -8 0.50 1.30 -2 -6 8 1.40 1.60 -2 -6 8 6.40 2.20 -2 -6 8 2.20 2.30 -2 6 7 1.50 1.70 -2 6 7 0.60 1.10 -2 6 7 0.40 0.60 -2 6 7 1.10 0.60 2 6 -7 0.30 0.90 -2 -6 7 -1.40 1.20 -2 -6 7 -0.40 1.50 -2 -6 7 0.40 1.20 -2 6 6 18.30 2.10 -2 6 6 14.10 3.00 -2 6 6 18.50 3.30 2 6 -6 18.90 2.30 -2 6 6 20.40 2.10 -2 -6 6 23.80 4.00 2 -6 -6 13.60 3.00 -2 -6 6 19.90 4.10 -2 -6 6 20.40 2.80 -2 6 5 163.98 9.80 -2 6 5 143.49 9.90 -2 6 5 151.08 8.20 -2 6 5 142.59 8.00 -2 6 5 126.49 9.00 2 6 -5 150.38 8.00 -2 -6 5 149.99 9.80 -2 -6 5 153.48 10.50 -2 -6 5 134.19 8.20 -2 6 4 19.50 2.50 -2 6 4 20.20 3.50 -2 6 4 20.20 2.30 2 6 -4 22.70 3.00 -2 6 4 22.70 3.00 -2 6 4 23.10 3.00 2 6 -4 13.70 2.70 2 6 -4 21.40 3.10 -2 6 4 27.70 3.40 -2 -6 4 18.50 3.50 -2 -6 4 16.50 2.10 -2 -6 4 20.80 3.40 -2 6 3 11.30 2.30 -2 6 3 10.20 2.70 -2 6 3 7.90 2.20 -2 6 3 10.00 2.10 2 6 -3 9.20 2.10 -2 6 3 11.50 2.10 -2 6 3 11.70 2.50 2 6 -3 9.00 1.20 2 6 -3 9.80 2.30 -2 -6 3 6.90 2.20 -2 -6 3 10.40 1.30 -2 -6 3 8.40 2.00 -2 6 2 23.20 2.70 -2 6 2 28.50 3.40 2 6 -2 25.70 3.90 2 6 -2 24.90 2.90 2 6 -2 23.50 1.90 -2 6 2 27.10 3.50 -2 6 2 29.70 3.30 -2 6 2 24.90 2.90 -2 6 2 29.10 3.60 -2 -6 2 29.60 3.50 -2 -6 2 24.70 3.10 -2 -6 2 27.80 1.90 -2 6 1 431.06 20.60 2 6 -1 406.96 18.60 2 6 -1 412.76 20.20 2 6 -1 411.86 20.30 -2 6 1 436.76 20.90 -2 6 1 408.86 21.40 -2 6 1 405.16 20.60 2 6 -1 408.66 18.70 -2 -6 1 420.46 20.70 2 -6 -1 406.96 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6 4 453.55 22.00 2 6 4 444.86 21.10 -2 -6 -4 462.25 20.90 2 -6 4 465.85 23.20 2 -6 4 454.55 22.70 -2 -6 -4 449.26 22.00 2 -6 4 440.86 24.00 2 6 5 121.99 6.90 2 6 5 138.89 6.70 -2 6 -5 130.39 8.80 2 6 5 129.99 7.20 2 6 5 125.19 7.60 2 6 5 147.69 8.90 -2 -6 -5 130.69 8.60 2 -6 5 128.49 10.00 2 -6 5 149.88 9.70 2 -6 5 134.99 9.20 2 6 6 121.19 7.20 2 6 6 121.39 8.20 -2 6 -6 108.29 8.20 2 6 6 110.29 6.70 2 -6 6 99.89 8.10 2 -6 6 114.69 9.50 2 -6 6 110.19 8.50 2 6 7 171.08 9.80 2 -6 7 172.28 11.50 2 -6 7 174.28 11.80 -2 -6 -7 177.08 10.20 -2 6 -8 41.70 5.20 2 6 8 43.10 5.30 2 6 8 38.30 3.90 2 -6 8 28.30 5.00 2 -6 8 36.80 6.40 2 -6 8 50.59 5.40 2 6 9 1.70 1.40 2 6 9 0.20 1.80 -2 6 -9 3.50 2.20 2 -6 9 3.10 2.30 2 -6 9 -1.50 2.30 -2 -6 -9 1.70 1.60 2 6 10 52.09 5.20 -2 6 -10 45.00 5.90 2 6 10 53.59 6.90 2 -6 10 38.30 7.20 2 -6 10 50.49 6.50 -2 7 10 11.90 3.80 -2 7 10 7.60 2.90 -2 -7 10 17.90 3.60 -2 -7 10 15.70 4.40 -2 -7 10 9.00 4.20 -2 7 9 71.09 6.80 -2 7 9 69.99 7.20 -2 -7 9 83.79 7.80 -2 -7 9 73.89 6.80 -2 -7 9 72.79 8.80 -2 7 8 43.90 5.30 2 7 -8 44.90 4.30 -2 7 8 38.90 4.70 -2 -7 8 48.20 4.80 -2 -7 8 41.60 5.30 -2 -7 8 41.80 6.00 -2 7 7 0.50 1.30 -2 7 7 -0.10 0.60 -2 7 7 0.80 1.50 2 7 -7 0.00 0.90 -2 -7 7 0.00 1.20 -2 -7 7 -0.10 1.80 -2 -7 7 1.10 1.50 -2 7 6 128.89 7.30 -2 7 6 127.99 9.10 2 7 -6 130.59 7.40 -2 7 6 118.29 7.00 -2 7 6 131.49 8.90 -2 -7 6 115.39 7.70 -2 -7 6 124.19 9.40 -2 -7 6 120.09 9.90 -2 7 5 232.18 13.60 -2 7 5 224.28 14.00 -2 7 5 224.28 13.40 -2 7 5 236.68 12.10 -2 7 5 204.98 12.10 2 7 -5 241.48 11.70 -2 -7 5 230.18 14.00 -2 -7 5 246.38 12.20 -2 -7 5 243.38 15.00 2 7 -4 255.37 15.20 -2 7 4 246.58 13.90 -2 7 4 252.97 13.70 -2 7 4 255.17 14.90 -2 7 4 307.87 15.20 -2 7 4 285.67 15.70 -2 -7 4 268.17 15.30 -2 -7 4 244.08 15.60 -2 -7 4 269.37 13.10 -2 7 3 5.10 1.50 -2 7 3 3.00 1.60 -2 7 3 5.70 1.80 2 7 -3 5.00 1.00 -2 7 3 8.60 2.60 2 7 -3 6.10 2.00 -2 7 3 4.70 1.70 -2 -7 3 7.80 1.30 -2 -7 3 5.00 2.10 -2 -7 3 3.20 1.80 2 7 -2 4.00 1.60 2 7 -2 4.70 1.00 -2 7 2 6.80 2.30 -2 7 2 4.20 1.60 2 7 -2 3.50 1.50 -2 7 2 5.10 1.60 -2 7 2 4.30 1.70 -2 7 2 5.40 2.00 -2 7 2 6.10 1.90 -2 -7 2 4.60 0.90 -2 -7 2 2.10 1.50 -2 -7 2 4.50 1.70 -2 7 1 242.18 13.90 2 7 -1 224.28 12.60 2 7 -1 214.28 12.50 -2 7 1 219.38 13.10 -2 7 1 231.08 12.80 -2 7 1 224.08 13.60 2 7 -1 227.48 11.10 -2 7 1 229.98 12.90 2 7 -1 240.18 10.90 2 -7 -1 241.98 12.80 2 -7 -1 251.47 13.90 -2 -7 1 224.18 13.00 -2 -7 1 229.38 13.10 -2 7 0 15.60 2.70 2 7 0 13.50 2.50 2 7 0 12.40 2.30 2 7 0 12.50 1.50 2 7 0 13.30 1.60 -2 7 0 12.30 3.30 -2 7 0 11.00 2.20 -2 7 0 16.60 3.00 2 -7 0 10.00 2.60 -2 -7 0 12.50 2.40 -2 -7 0 12.90 2.60 -2 7 -1 50.29 5.20 2 7 1 47.50 3.90 2 7 1 49.90 3.40 2 7 1 51.19 4.10 -2 7 -1 44.30 4.70 -2 7 -1 43.30 4.30 2 7 1 46.00 3.60 -2 7 -1 42.60 4.40 2 -7 1 51.99 5.20 2 -7 1 42.40 4.90 2 -7 1 44.50 4.50 -2 -7 -1 48.60 4.30 -2 -7 -1 48.40 4.00 2 7 2 36.30 3.30 -2 7 -2 39.00 3.90 2 7 2 33.80 3.20 2 7 2 40.30 3.30 -2 7 -2 38.70 4.60 -2 7 -2 36.40 3.90 2 7 2 38.80 3.20 2 7 2 38.00 3.40 2 -7 2 35.20 4.20 -2 -7 -2 42.40 3.80 2 -7 2 36.50 4.70 2 7 3 72.79 5.10 2 7 3 74.99 5.20 2 7 3 82.39 5.50 2 7 3 85.39 5.10 -2 7 -3 79.19 6.10 2 7 3 76.09 5.50 -2 -7 -3 75.59 5.50 2 -7 3 85.89 6.90 2 -7 3 72.79 7.20 2 -7 3 78.49 6.10 -2 7 -4 77.89 7.20 2 7 4 67.79 4.60 2 7 4 75.39 5.00 2 7 4 65.69 5.40 2 7 4 68.59 4.60 2 -7 4 77.39 6.10 -2 -7 -4 70.59 6.20 2 -7 4 71.69 7.10 2 -7 4 82.49 6.80 -2 -7 -4 71.89 5.00 2 7 5 17.60 2.10 2 7 5 15.60 2.40 2 7 5 23.40 3.20 2 7 5 21.30 2.10 2 7 5 21.40 2.20 -2 7 -5 22.90 3.80 -2 -7 -5 22.30 3.50 2 -7 5 21.90 4.50 2 -7 5 17.80 3.40 2 -7 5 20.90 3.90 2 7 6 74.99 6.30 2 7 6 68.59 3.90 2 7 6 80.99 3.90 2 7 6 76.79 5.50 2 7 6 63.19 4.70 2 -7 6 74.29 6.50 2 -7 6 71.49 6.80 2 -7 6 83.79 9.20 2 7 7 3.20 1.80 2 7 7 10.10 2.00 2 7 7 8.00 2.00 2 -7 7 10.30 3.00 2 -7 7 8.10 3.20 2 7 8 -2.40 1.30 -2 7 -8 0.30 1.90 2 7 8 -0.30 1.80 2 7 8 -2.30 1.40 2 -7 8 2.10 1.60 2 -7 8 2.80 2.00 2 7 9 18.30 4.30 2 7 9 15.30 2.80 2 7 9 15.10 3.20 -2 7 -9 16.80 4.10 2 -7 9 14.60 3.40 2 -7 9 12.20 4.20 2 7 10 -3.30 1.60 2 7 10 -0.60 2.30 -2 7 -10 -2.30 2.20 2 -7 10 2.20 2.40 -2 8 9 35.50 6.00 -2 -8 9 29.90 6.60 -2 -8 9 32.50 5.40 -2 -8 9 48.80 5.20 2 8 -8 1.00 1.60 -2 8 8 1.60 1.80 -2 8 8 2.60 1.90 -2 -8 8 3.70 2.40 -2 -8 8 1.40 1.50 -2 -8 8 1.50 2.00 -2 8 7 60.69 5.70 -2 8 7 53.79 3.80 2 8 -7 51.19 4.30 -2 8 7 51.29 3.70 -2 8 7 55.39 5.90 -2 -8 7 58.39 4.90 -2 -8 7 49.70 6.10 -2 -8 7 57.29 7.10 -2 8 6 -0.30 1.50 -2 8 6 2.20 0.90 -2 8 6 -0.60 1.30 -2 8 6 0.80 1.00 2 8 -6 1.00 0.80 -2 -8 6 1.30 1.10 -2 -8 6 -0.20 1.70 -2 8 5 7.70 1.80 -2 8 5 7.90 2.30 -2 8 5 10.40 2.70 2 8 -5 9.10 1.50 -2 -8 5 8.70 1.70 -2 -8 5 8.50 2.80 -2 -8 5 11.80 3.00 -2 8 4 261.97 14.50 -2 8 4 231.38 14.60 -2 8 4 221.58 13.60 -2 8 4 230.68 12.90 -2 8 4 221.98 13.20 -2 -8 4 249.08 14.80 -2 -8 4 244.88 11.90 -2 -8 4 249.97 15.30 -2 8 3 103.99 7.30 2 8 -3 97.99 5.30 -2 8 3 91.59 7.90 -2 8 3 89.59 7.40 -2 8 3 93.49 7.00 2 8 -3 85.79 7.10 -2 -8 3 99.69 7.80 -2 -8 3 99.29 5.40 -2 -8 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19.80 3.40 2 8 2 24.50 2.70 2 -8 2 16.70 4.00 2 -8 2 21.90 3.40 2 -8 2 16.00 3.30 -2 -8 -2 23.20 3.10 2 8 3 1.90 1.20 2 8 3 2.50 1.10 -2 8 -3 2.00 1.40 2 8 3 -0.90 0.90 2 8 3 1.70 1.10 2 8 3 -0.50 0.90 2 -8 3 0.80 1.30 -2 -8 -3 0.70 1.20 2 -8 3 1.10 1.30 2 -8 3 1.60 2.00 2 8 4 0.60 0.90 -2 8 -4 0.40 1.60 2 8 4 1.20 1.40 2 8 4 1.50 1.10 2 8 4 -1.60 1.10 2 8 4 1.40 0.80 2 -8 4 1.30 1.30 2 -8 4 -0.90 1.40 2 -8 4 4.70 2.10 -2 -8 -4 0.40 1.00 2 8 5 6.70 1.70 2 8 5 3.20 1.20 2 8 5 4.60 1.50 2 8 5 7.20 2.20 2 8 5 3.90 1.20 2 -8 5 5.00 2.20 2 -8 5 3.20 1.70 2 -8 5 1.50 2.30 2 8 6 52.39 3.60 2 8 6 50.59 4.00 2 8 6 59.79 4.70 2 8 6 48.30 3.50 2 8 6 54.59 5.30 2 -8 6 55.59 6.10 2 -8 6 53.29 5.50 2 -8 6 49.60 6.70 2 8 7 4.30 2.30 2 8 7 2.70 1.40 -2 8 -7 6.40 2.80 2 8 7 4.60 1.80 2 -8 7 6.10 2.60 2 -8 7 1.20 2.50 2 -8 7 8.30 2.40 -2 8 -8 64.69 7.20 2 8 8 68.89 5.50 2 -8 8 44.60 7.80 2 -8 8 62.39 6.90 2 -8 8 57.39 6.50 2 8 9 10.00 2.20 2 8 9 7.40 3.20 -2 8 -9 9.50 3.90 2 -8 9 14.60 3.50 -2 9 8 1.20 2.10 -2 9 8 1.20 1.80 -2 -9 8 5.80 3.40 -2 -9 8 -1.10 1.80 -2 -9 8 4.20 2.50 -2 9 7 27.80 4.10 -2 9 7 31.10 3.10 -2 9 7 33.40 3.00 -2 9 7 37.40 5.00 -2 -9 7 28.40 5.30 -2 -9 7 34.40 3.80 -2 -9 7 30.00 6.10 -2 9 6 16.80 3.80 -2 9 6 24.60 3.00 -2 9 6 23.80 3.10 -2 9 6 29.60 3.70 -2 -9 6 21.90 2.80 -2 -9 6 27.90 5.00 -2 -9 6 26.20 5.40 -2 9 5 82.59 8.20 2 9 -5 92.69 5.50 -2 9 5 96.89 7.00 -2 9 5 86.69 6.30 -2 9 5 89.79 7.50 -2 -9 5 103.49 5.90 -2 -9 5 85.69 8.10 -2 9 4 124.69 9.20 -2 9 4 123.39 8.80 -2 9 4 126.19 8.20 -2 -9 4 120.69 6.80 -2 -9 4 113.69 9.40 -2 -9 4 128.69 10.10 -2 9 3 83.69 7.40 -2 9 3 106.69 7.90 -2 9 3 136.09 9.10 2 9 -3 109.09 5.90 -2 9 3 103.19 7.40 -2 -9 3 104.29 8.60 -2 -9 3 118.09 9.20 2 9 -2 200.88 9.80 2 9 -2 191.18 9.90 -2 9 2 191.58 12.70 -2 9 2 198.18 12.50 2 9 -2 206.58 12.40 -2 9 2 200.88 12.00 -2 -9 2 201.38 12.90 -2 -9 2 206.78 13.20 -2 9 1 2.20 1.30 2 9 -1 1.80 1.80 2 9 -1 1.90 0.80 -2 9 1 2.20 1.70 -2 9 1 0.10 1.60 -2 9 1 4.90 2.10 -2 -9 1 3.90 1.80 -2 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3.20 -2 9 -6 8.40 3.10 2 9 6 11.10 2.00 2 9 6 12.10 2.00 2 9 6 7.50 1.50 2 9 6 8.80 1.70 2 9 6 12.70 2.90 2 -9 6 13.50 3.50 2 -9 6 8.70 3.10 2 -9 6 12.60 3.10 -2 9 -7 25.40 5.40 2 9 7 23.50 3.10 2 9 7 20.80 2.80 2 9 7 20.20 4.10 2 -9 7 25.70 5.70 2 -9 7 19.50 3.90 2 -9 7 23.40 4.70 -2 9 -8 22.30 5.10 2 9 8 15.00 3.90 2 -9 8 18.70 3.70 2 -9 8 19.00 5.30 -2 10 7 27.20 4.20 -2 10 7 23.30 4.60 -2 -10 7 17.50 4.20 -2 -10 7 21.50 5.50 -2 10 6 96.59 8.00 -2 10 6 93.69 6.80 2 10 -6 83.69 5.40 -2 10 6 88.99 6.30 -2 10 6 77.89 7.30 -2 -10 6 87.19 8.80 -2 -10 6 94.79 9.50 -2 -10 6 89.59 5.70 2 10 -5 19.20 2.20 -2 10 5 16.40 3.40 -2 10 5 20.70 3.50 -2 10 5 30.00 4.60 -2 -10 5 26.60 5.00 -2 -10 5 23.80 2.40 -2 -10 5 23.10 4.90 -2 10 4 0.90 1.50 -2 10 4 -0.40 1.40 -2 10 4 -1.40 1.00 -2 -10 4 0.40 0.70 -2 -10 4 -0.70 1.50 2 10 -3 490.45 22.90 -2 10 3 458.05 25.50 -2 10 3 506.45 26.20 -2 10 3 574.64 27.40 -2 -10 3 499.55 27.50 -2 -10 3 514.05 27.40 -2 10 2 224.78 13.70 2 10 -2 216.28 10.40 -2 10 2 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14.80 3.60 -4 -4 8 19.10 3.40 4 -4 -8 12.40 2.20 4 4 -7 -0.10 0.90 -4 4 7 1.50 0.90 -4 4 7 1.30 1.60 -4 4 7 -0.20 1.20 -4 -4 7 3.00 1.70 -4 -4 7 1.50 1.40 4 -4 -7 1.60 0.90 -4 -4 7 0.00 1.70 -4 4 6 2.10 1.60 -4 4 6 4.80 1.40 4 4 -6 2.80 1.20 4 4 -6 3.00 1.50 -4 4 6 3.80 1.70 -4 -4 6 4.60 1.50 -4 -4 6 4.80 2.00 -4 -4 6 4.40 1.90 4 -4 -6 1.70 1.00 4 4 -5 10.80 1.70 -4 4 5 10.50 2.00 -4 4 5 12.30 2.60 4 4 -5 9.30 2.40 -4 4 5 17.00 3.10 4 4 -5 11.60 2.30 -4 4 5 12.10 2.60 -4 -4 5 14.30 2.90 4 -4 -5 14.70 3.00 4 -4 -5 11.50 2.10 -4 -4 5 8.60 2.20 -4 -4 5 13.40 2.00 -4 4 4 2.50 1.00 -4 4 4 -0.60 0.60 4 4 -4 0.60 0.90 -4 4 4 1.10 1.00 -4 4 4 0.30 1.10 4 4 -4 0.20 0.50 4 4 -4 -1.10 0.70 -4 -4 4 0.30 1.00 4 -4 -4 1.10 1.00 -4 -4 4 1.40 1.10 -4 -4 4 0.90 0.70 -4 4 3 26.10 3.30 -4 4 3 28.10 2.90 -4 4 3 19.80 2.90 -4 4 3 27.40 3.10 4 4 -3 25.50 2.80 4 4 -3 23.50 2.80 -4 -4 3 25.10 1.70 4 -4 -3 21.50 3.20 -4 -4 3 26.00 2.90 -4 -4 3 26.90 1.80 4 -4 -3 16.90 2.40 -4 -4 3 27.50 3.10 4 4 -2 562.24 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-4 3 2.10 1.40 4 -4 3 1.60 1.50 -4 -4 -3 0.40 0.60 -4 4 -4 6.70 2.10 4 4 4 6.70 1.90 -4 4 -4 4.80 1.70 -4 4 -4 5.70 1.70 4 4 4 3.80 1.10 -4 4 -4 6.90 2.20 -4 -4 -4 6.80 1.20 4 -4 4 6.80 2.20 -4 -4 -4 3.60 1.20 4 -4 4 5.30 2.20 -4 4 -5 209.58 12.70 4 4 5 215.88 12.30 -4 4 -5 209.78 12.50 4 4 5 216.28 10.30 4 4 5 206.18 10.00 -4 4 -5 200.18 12.80 -4 4 -5 214.38 12.20 4 -4 5 200.78 13.20 4 -4 5 186.58 12.60 -4 -4 -5 216.48 10.10 -4 -4 -5 199.88 11.70 -4 -4 -5 244.58 10.10 4 4 6 11.10 2.70 4 4 6 9.90 1.60 -4 4 -6 11.20 2.50 -4 4 -6 10.70 2.70 4 -4 6 11.20 3.10 4 -4 6 8.50 2.90 -4 4 -7 53.09 5.40 4 4 7 66.79 6.30 4 4 7 55.59 4.30 -4 4 -7 60.39 5.30 4 -4 7 59.69 6.50 4 -4 7 67.49 6.90 -4 -4 -7 53.29 4.10 4 4 8 5.90 2.90 4 4 8 7.40 1.90 -4 4 -8 6.20 2.40 4 -4 8 8.60 3.40 -4 -4 -8 12.20 2.10 4 -4 8 8.50 3.10 4 4 9 -2.00 2.00 -4 4 -9 -1.90 1.50 4 4 9 -0.60 1.20 4 -4 9 0.90 2.40 4 -4 9 0.40 2.50 -4 -4 -9 -0.10 1.70 4 4 10 2.00 1.80 4 4 10 -2.20 2.80 -4 4 -10 2.40 1.70 4 -4 10 3.90 2.30 -4 -4 -10 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2.80 -4 5 4 55.49 4.30 -4 -5 4 51.09 3.00 4 -5 -4 42.70 4.90 4 -5 -4 44.40 4.00 -4 -5 4 46.50 4.50 -4 -5 4 42.80 4.60 -4 5 3 67.29 5.60 -4 5 3 71.29 5.60 -4 5 3 65.39 5.60 4 5 -3 58.59 4.90 4 5 -3 57.29 4.90 -4 5 3 65.09 5.10 -4 -5 3 61.89 5.20 -4 -5 3 69.39 5.50 4 -5 -3 70.89 5.20 4 5 -2 14.50 2.00 -4 5 2 13.00 2.40 -4 5 2 15.20 2.80 -4 5 2 17.30 3.30 -4 5 2 22.10 3.00 -4 5 2 14.00 2.50 4 5 -2 13.30 2.30 4 -5 -2 16.70 2.70 -4 -5 2 12.70 2.40 4 -5 -2 17.40 2.50 -4 -5 2 11.20 2.20 -4 5 1 118.89 8.30 -4 5 1 129.09 8.20 -4 5 1 131.19 9.10 4 5 -1 131.19 7.30 4 5 -1 141.29 8.00 -4 5 1 117.39 8.60 4 -5 -1 130.29 8.30 -4 -5 1 136.49 8.10 -4 -5 1 134.69 7.60 -4 5 0 430.16 22.80 4 5 0 429.46 19.30 -4 5 0 454.25 22.20 4 5 0 443.46 19.30 4 5 0 431.76 21.20 -4 5 0 509.15 22.50 4 5 0 440.56 20.20 -4 5 0 406.86 21.70 4 -5 0 434.66 22.70 -4 -5 0 426.26 21.20 4 -5 0 435.96 22.00 -4 -5 0 440.96 20.50 4 5 1 169.98 8.50 -4 5 -1 157.38 10.10 -4 5 -1 175.18 10.30 -4 5 -1 164.98 10.80 4 5 1 173.58 8.00 -4 5 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85.69 7.80 4 -5 7 83.09 8.20 4 5 8 64.99 6.70 -4 5 -8 64.89 6.40 4 5 8 57.19 4.60 4 -5 8 61.19 6.80 4 -5 8 67.29 7.70 4 5 9 6.20 3.10 4 5 9 4.10 1.60 -4 5 -9 7.50 2.60 -4 -5 -9 6.10 1.90 4 -5 9 3.90 2.80 4 -5 9 6.10 2.80 4 5 10 111.99 10.60 -4 5 -10 93.79 8.80 4 5 10 121.29 8.10 4 -5 10 132.59 11.30 4 -5 10 114.79 11.30 -4 6 10 -1.30 2.20 -4 6 10 1.10 1.80 -4 -6 10 -0.60 1.80 -4 -6 10 -1.10 1.40 -4 6 9 0.70 0.70 -4 6 9 3.90 1.80 -4 6 9 -0.50 1.40 -4 -6 9 -1.90 1.40 -4 -6 9 0.70 1.60 -4 -6 9 0.90 1.60 -4 6 8 38.40 3.10 -4 6 8 34.70 3.20 4 6 -8 40.70 4.00 -4 6 8 34.40 4.80 -4 6 8 44.20 5.30 -4 -6 8 42.40 5.10 -4 -6 8 36.40 4.20 -4 -6 8 26.20 5.40 -4 6 7 0.70 0.90 -4 6 7 0.70 1.40 -4 6 7 0.70 1.10 -4 6 7 1.40 1.50 4 6 -7 0.30 0.90 -4 -6 7 -0.40 1.00 -4 -6 7 -0.20 1.70 -4 -6 7 1.00 1.40 -4 6 6 6.90 1.60 -4 6 6 7.90 1.80 4 6 -6 8.20 1.60 -4 6 6 3.70 2.10 -4 6 6 8.10 2.40 -4 -6 6 6.40 1.60 -4 -6 6 7.00 2.50 -4 -6 6 6.00 2.50 -4 6 5 88.69 7.30 -4 6 5 99.19 9.20 -4 6 5 92.59 6.20 4 6 -5 91.49 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753.92 37.30 -4 7 3 235.78 13.60 4 7 -3 243.08 13.40 -4 7 3 216.38 13.60 -4 7 3 251.17 13.50 -4 -7 3 227.98 13.80 -4 -7 3 233.68 13.80 4 7 -2 -1.00 0.60 -4 7 2 0.00 1.40 -4 7 2 -1.70 0.80 -4 7 2 -1.10 1.10 -4 7 2 0.40 1.50 -4 7 2 -1.40 0.80 -4 -7 2 -0.40 1.20 -4 -7 2 -0.10 1.30 4 -7 -2 0.20 1.00 -4 7 1 82.59 7.20 -4 7 1 77.49 7.10 -4 7 1 72.09 6.30 -4 7 1 84.59 6.50 4 7 -1 75.99 5.90 -4 7 1 72.09 6.40 4 7 -1 79.39 5.50 4 -7 -1 78.89 6.40 -4 -7 1 80.49 5.90 -4 -7 1 72.19 6.00 -4 7 0 206.68 13.90 4 7 0 215.48 9.70 4 7 0 208.68 12.10 4 7 0 217.78 11.20 -4 7 0 211.18 13.10 -4 7 0 214.68 12.90 -4 7 0 230.48 13.20 4 7 0 227.08 9.90 -4 -7 0 224.98 11.80 4 -7 0 223.48 13.90 -4 -7 0 221.68 12.50 4 -7 0 205.28 12.70 4 7 1 32.70 3.40 4 7 1 35.50 2.70 4 7 1 32.60 2.60 4 7 1 30.90 2.50 -4 7 -1 41.70 4.40 -4 7 -1 35.30 4.00 -4 -7 -1 30.10 2.70 4 -7 1 35.50 4.50 -4 -7 -1 32.90 3.60 4 -7 1 34.80 4.10 4 7 2 3.40 1.20 -4 7 -2 3.10 1.80 4 7 2 4.90 1.30 -4 7 -2 6.00 1.90 4 7 2 2.60 0.60 4 7 2 3.10 0.70 4 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0 5.70 1.80 5 4 1 76.29 4.20 5 4 1 83.99 5.60 -5 4 -1 85.19 6.80 5 4 1 89.09 5.10 -5 4 -1 78.39 6.30 -5 4 -1 86.59 6.50 -5 -4 -1 85.09 4.70 5 -4 1 93.89 6.50 5 -4 1 88.89 6.60 -5 -4 -1 90.19 5.70 5 -4 1 87.09 6.90 -5 4 -2 0.30 1.00 -5 4 -2 -1.80 0.80 5 4 2 2.50 1.00 -5 4 -2 0.90 1.00 -5 4 -2 1.10 1.10 -5 -4 -2 1.50 0.70 5 -4 2 -0.10 0.80 -5 -4 -2 0.90 1.00 5 -4 2 1.00 1.10 5 4 3 16.20 2.70 5 4 3 13.20 2.10 -5 4 -3 14.20 3.30 -5 4 -3 13.20 3.40 -5 4 -3 14.90 3.00 -5 4 -3 14.80 2.80 5 -4 3 13.10 3.00 -5 -4 -3 16.70 2.00 -5 -4 -3 15.10 2.00 5 -4 3 16.20 3.10 5 4 4 58.69 4.20 -5 4 -4 61.69 5.50 -5 4 -4 55.59 5.60 -5 4 -4 54.49 5.50 5 4 4 60.99 5.20 -5 4 -4 57.39 5.20 5 -4 4 63.59 5.80 -5 -4 -4 63.79 4.10 -5 -4 -4 59.19 4.60 5 -4 4 63.39 6.20 -5 4 -5 88.79 7.00 5 4 5 101.69 6.00 5 4 5 95.99 7.20 -5 4 -5 81.79 6.60 -5 -4 -5 90.59 5.20 5 -4 5 88.29 7.90 -5 -4 -5 92.89 6.50 5 -4 5 74.49 7.10 5 4 6 37.00 2.50 5 4 6 25.40 4.20 -5 4 -6 25.80 4.40 5 4 6 29.30 2.30 -5 4 -6 23.60 3.80 -5 -4 -6 28.20 2.10 -5 -4 -6 27.40 2.00 5 -4 6 25.90 4.70 5 -4 6 28.10 4.90 5 4 7 107.19 6.30 -5 4 -7 101.49 7.90 5 4 7 113.99 8.80 5 -4 7 110.19 9.30 5 -4 7 101.69 9.00 -5 -4 -7 99.09 7.20 5 4 8 41.80 5.40 5 4 8 43.50 3.90 -5 4 -8 45.80 4.90 5 -4 8 42.60 5.90 5 -4 8 52.99 6.40 5 4 9 0.50 2.60 5 4 9 0.30 1.30 -5 4 -9 -0.60 1.40 5 -4 9 -1.60 2.00 -5 -4 -9 0.40 1.30 5 -4 9 1.20 1.50 5 4 10 -3.70 2.60 -5 4 -10 2.70 1.90 5 4 10 1.70 1.70 5 -4 10 3.20 2.70 5 -4 10 1.20 2.70 -5 5 10 16.70 4.10 -5 5 10 17.90 2.10 -5 5 10 23.30 4.70 -5 -5 10 23.50 4.40 -5 -5 10 25.40 4.30 -5 -5 10 12.70 4.10 -5 5 9 26.30 3.00 -5 5 9 20.40 4.40 -5 5 9 22.20 2.50 -5 5 9 27.60 4.70 -5 -5 9 17.90 4.70 -5 -5 9 21.70 3.80 -5 -5 9 21.50 4.00 -5 5 8 24.10 4.40 -5 5 8 26.90 4.50 5 5 -8 29.70 3.40 -5 -5 8 27.40 4.50 5 -5 -8 25.80 3.30 -5 -5 8 34.00 4.90 -5 -5 8 26.50 3.90 -5 5 7 16.80 3.70 5 5 -7 16.10 2.30 -5 5 7 13.60 3.20 -5 5 7 21.20 2.70 -5 -5 7 16.40 4.50 -5 -5 7 14.70 3.00 5 -5 -7 17.90 2.90 -5 -5 7 13.40 2.60 -5 5 6 14.20 3.20 -5 5 6 13.50 3.20 -5 5 6 17.80 2.80 -5 -5 6 16.50 2.40 -5 -5 6 13.60 3.00 5 -5 -6 14.90 2.80 -5 -5 6 20.60 2.10 -5 -5 6 13.00 3.20 -5 5 5 41.90 4.10 -5 5 5 45.40 5.10 -5 5 5 41.10 4.70 -5 -5 5 53.79 5.10 -5 -5 5 49.80 3.40 -5 -5 5 51.09 3.30 -5 -5 5 46.80 5.10 5 -5 -5 51.29 4.50 -5 5 4 40.40 4.40 -5 5 4 36.80 4.50 -5 5 4 37.40 3.90 -5 5 4 38.50 5.50 5 5 -4 35.90 4.00 -5 -5 4 37.60 2.40 -5 -5 4 42.50 4.50 -5 -5 4 42.50 2.40 5 -5 -4 40.20 5.60 5 -5 -4 34.90 3.80 -5 -5 4 38.60 4.20 -5 5 3 6.60 2.20 -5 5 3 7.00 2.10 5 5 -3 5.60 1.60 -5 5 3 8.70 2.60 -5 5 3 7.50 2.10 -5 5 3 4.80 1.80 5 5 -3 5.20 1.60 -5 -5 3 4.00 1.70 5 -5 -3 7.90 2.10 5 -5 -3 4.90 1.60 -5 -5 3 5.10 1.80 5 5 -2 31.10 3.10 5 5 -2 30.70 3.30 -5 5 2 32.80 3.90 -5 5 2 31.50 4.20 -5 5 2 35.40 3.90 -5 5 2 39.80 4.40 5 -5 -2 30.80 3.50 5 -5 -2 33.10 3.70 -5 -5 2 32.30 3.50 -5 -5 2 37.50 3.50 -5 5 1 323.27 16.20 -5 5 1 278.47 15.00 5 5 -1 269.17 13.40 -5 5 1 240.98 15.40 -5 5 1 267.17 15.00 5 -5 -1 281.57 15.00 -5 -5 1 267.37 13.60 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59.89 5.10 -5 6 6 56.39 6.00 -5 6 6 53.99 4.80 -5 -6 6 64.39 5.00 -5 -6 6 64.39 6.50 -5 -6 6 60.49 5.80 -5 -6 6 50.79 3.90 -5 6 5 88.79 7.70 -5 6 5 92.09 6.70 -5 6 5 90.59 7.40 -5 -6 5 81.79 4.70 -5 -6 5 87.29 7.50 -5 -6 5 89.69 7.20 -5 -6 5 89.39 4.60 -5 6 4 5.80 2.10 5 6 -4 5.90 2.00 -5 6 4 4.70 2.10 -5 6 4 6.80 2.10 -5 6 4 5.70 1.80 -5 -6 4 9.10 2.30 -5 -6 4 6.40 2.20 -5 6 3 96.89 7.20 -5 6 3 77.09 7.00 -5 6 3 65.79 6.00 5 6 -3 77.99 5.90 -5 6 3 79.99 6.20 -5 -6 3 79.59 6.40 -5 -6 3 98.09 6.80 -5 6 2 162.18 10.50 -5 6 2 179.38 12.00 5 6 -2 166.88 9.70 -5 6 2 164.38 10.70 5 6 -2 169.08 11.40 -5 6 2 167.98 11.20 5 -6 -2 177.78 10.90 -5 -6 2 190.38 10.50 -5 -6 2 175.78 10.60 -5 6 1 12.30 2.80 -5 6 1 11.40 3.00 5 6 -1 9.90 2.10 -5 6 1 6.80 2.30 -5 6 1 13.40 3.20 -5 6 1 8.60 2.30 5 6 -1 8.40 1.60 5 -6 -1 8.80 2.40 -5 -6 1 9.60 2.00 -5 -6 1 9.60 2.20 -5 6 0 280.17 14.80 -5 6 0 238.08 15.00 -5 6 0 235.68 14.30 5 6 0 255.97 12.20 -5 6 0 230.58 15.00 -5 6 0 225.28 13.90 5 6 0 242.08 13.40 -5 -6 0 251.07 12.60 -5 -6 0 255.67 13.70 5 -6 0 255.67 15.30 5 -6 0 271.07 14.60 5 6 1 107.09 5.60 5 6 1 110.99 7.30 5 6 1 111.99 6.10 -5 6 -1 108.69 8.70 -5 6 -1 109.59 8.20 -5 6 -1 118.39 8.30 -5 6 -1 113.49 8.40 -5 -6 -1 121.39 7.60 5 -6 1 121.99 9.20 -5 -6 -1 111.99 5.90 -5 -6 -1 113.29 5.80 5 -6 1 112.49 8.20 -5 6 -2 28.10 4.00 5 6 2 31.40 3.20 -5 6 -2 19.20 3.70 5 6 2 28.90 2.90 5 -6 2 31.80 4.60 5 -6 2 34.40 4.10 -5 -6 -2 29.80 2.50 -5 -6 -2 32.10 3.30 5 6 3 78.89 5.40 5 6 3 86.29 5.80 -5 6 -3 68.19 6.50 5 -6 3 72.49 7.30 5 -6 3 83.69 7.00 -5 -6 -3 78.59 5.40 -5 -6 -3 67.79 5.00 -5 6 -4 0.00 1.50 5 6 4 -0.20 0.80 5 6 4 2.20 1.40 -5 -6 -4 -1.00 0.90 5 -6 4 0.60 1.60 -5 -6 -4 1.40 0.80 5 -6 4 0.60 1.80 5 6 5 17.60 2.20 5 6 5 14.20 3.10 -5 6 -5 14.10 3.30 -5 -6 -5 17.10 2.00 -5 -6 -5 13.90 2.70 5 -6 5 10.80 3.20 5 -6 5 14.90 3.60 5 6 6 12.50 3.40 5 6 6 14.70 1.80 -5 6 -6 20.90 4.10 5 -6 6 8.40 3.10 -5 -6 -6 14.10 1.60 -5 6 -7 9.10 3.30 5 6 7 10.30 3.00 5 -6 7 8.20 3.20 5 -6 7 11.30 3.40 -5 6 -8 -1.50 1.40 5 6 8 -1.50 2.10 5 -6 8 4.20 1.90 5 -6 8 -1.00 1.70 -5 6 -9 6.20 2.90 5 6 9 7.80 1.60 5 6 9 1.30 2.90 5 -6 9 9.20 3.60 5 -6 9 2.20 2.80 -5 7 9 25.00 2.70 -5 7 9 31.00 5.20 -5 -7 9 30.20 5.90 -5 -7 9 28.40 5.00 -5 -7 9 27.90 4.10 -5 7 8 94.49 6.60 -5 7 8 110.09 7.20 -5 -7 8 121.09 9.60 -5 -7 8 111.19 10.20 -5 -7 8 106.79 8.30 -5 7 7 43.70 4.20 -5 7 7 48.10 4.50 -5 7 7 47.40 5.60 -5 -7 7 37.60 3.40 -5 -7 7 43.90 5.50 -5 -7 7 42.50 3.30 -5 -7 7 38.80 5.70 -5 7 6 12.80 2.50 -5 7 6 16.60 2.80 -5 7 6 9.10 3.40 -5 7 6 11.20 3.00 -5 -7 6 17.60 3.80 -5 -7 6 13.50 1.50 -5 -7 6 10.50 3.30 -5 -7 6 15.00 1.40 -5 7 5 64.69 5.30 -5 7 5 57.69 5.20 -5 7 5 61.39 6.40 -5 7 5 61.49 7.00 -5 -7 5 58.59 6.20 -5 7 4 67.89 6.30 -5 7 4 55.29 6.20 -5 7 4 69.59 5.90 -5 7 4 69.49 5.90 -5 -7 4 70.19 6.40 -5 -7 4 66.49 6.10 -5 7 3 15.00 3.10 -5 7 3 18.80 3.50 -5 7 3 21.80 3.60 -5 7 3 17.80 3.80 5 7 -3 16.50 3.20 -5 -7 3 15.20 3.20 -5 -7 3 17.80 3.50 5 7 -2 5.10 1.60 -5 7 2 8.60 2.80 -5 7 2 9.40 2.60 -5 -7 2 9.50 2.60 5 -7 -2 8.80 2.40 -5 7 1 147.79 9.40 5 7 -1 114.69 7.10 -5 7 1 114.59 9.20 5 -7 -1 115.69 8.60 -5 -7 1 120.79 7.70 -5 -7 1 110.59 8.10 5 7 0 190.68 11.10 -5 7 0 189.68 12.90 5 7 0 188.28 9.70 -5 7 0 198.48 12.20 5 -7 0 173.98 12.50 5 -7 0 173.88 11.70 -5 -7 0 201.68 10.30 -5 -7 0 183.48 11.20 -5 7 -1 291.97 17.00 5 7 1 298.47 13.80 5 7 1 308.17 13.80 5 7 1 297.17 13.90 5 7 1 307.97 15.80 -5 -7 -1 281.67 15.70 5 -7 1 271.87 17.40 -5 -7 -1 302.17 14.00 5 -7 1 288.47 16.70 -5 7 -2 125.69 9.30 5 7 2 124.39 8.00 5 7 2 132.29 7.30 5 -7 2 109.79 8.80 5 -7 2 119.19 9.90 -5 -7 -2 125.19 8.00 -5 -7 -2 123.39 6.90 5 7 3 0.10 0.80 -5 7 -3 1.20 1.50 5 7 3 2.70 1.50 -5 -7 -3 0.00 1.00 -5 -7 -3 -0.30 0.80 5 -7 3 0.50 1.20 5 -7 3 0.20 1.60 -5 7 -4 3.90 1.90 5 7 4 4.00 1.30 5 7 4 2.70 1.70 5 -7 4 1.00 2.00 5 -7 4 4.10 1.90 -5 -7 -4 5.60 1.60 -5 -7 -4 2.60 1.30 5 7 5 183.88 11.20 -5 7 -5 179.18 12.40 5 7 5 160.28 9.40 5 -7 5 179.88 12.30 -5 -7 -5 174.28 10.70 -5 -7 -5 176.38 9.60 5 -7 5 188.88 14.00 5 7 6 2.60 1.80 -5 7 -6 6.00 2.50 5 7 6 2.00 2.10 5 -7 6 5.80 2.20 -5 -7 -6 2.90 1.00 5 -7 6 3.30 2.10 5 7 7 -0.40 2.00 -5 7 -7 6.00 2.40 5 -7 7 3.00 2.10 5 -7 7 5.30 3.00 5 7 8 25.50 4.90 -5 7 -8 17.40 4.10 5 -7 8 19.90 4.90 5 -7 8 26.90 5.20 5 7 9 -4.60 2.20 -5 7 -9 1.30 2.40 5 -7 9 1.30 2.70 -5 8 8 19.80 2.60 -5 8 8 12.70 3.60 -5 8 8 11.50 3.70 -5 -8 8 19.90 2.70 -5 -8 8 15.80 4.10 -5 -8 8 20.00 4.90 -5 8 7 27.60 3.80 -5 8 7 38.70 5.20 -5 8 7 37.30 4.20 -5 8 7 36.90 5.10 -5 -8 7 33.70 5.80 -5 -8 7 36.80 2.50 -5 -8 7 40.20 2.60 -5 -8 7 31.00 5.30 -5 8 6 6.70 2.80 -5 8 6 3.90 1.80 -5 8 6 8.70 2.60 -5 8 6 6.20 2.20 -5 -8 6 7.50 2.70 -5 -8 6 8.20 2.90 -5 8 5 1.40 1.60 -5 8 5 0.40 1.60 -5 -8 5 -0.90 1.40 -5 -8 5 1.20 1.30 -5 8 4 93.59 7.10 -5 8 4 75.09 7.50 -5 -8 4 78.89 7.50 -5 -8 4 81.69 7.40 -5 8 3 17.20 3.80 5 8 -3 11.60 2.40 -5 8 3 13.20 3.10 -5 8 3 12.90 3.10 -5 -8 3 14.70 3.40 -5 -8 3 17.50 3.40 5 8 -2 37.50 4.00 -5 8 2 37.00 4.70 -5 8 2 41.30 5.40 -5 -8 2 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11.20 2.90 -7 -6 5 10.30 2.80 -7 6 4 8.20 2.90 -7 6 4 18.00 3.40 -7 6 4 14.80 3.50 -7 -6 4 14.70 3.10 -7 -6 4 11.60 2.70 -7 6 3 34.60 4.50 -7 6 3 35.50 4.80 7 6 -3 36.60 3.90 -7 -6 3 32.60 4.00 -7 -6 3 38.50 4.50 7 -6 -3 35.10 4.40 -7 6 2 14.80 3.60 -7 6 2 10.90 3.00 7 6 -2 15.80 2.20 -7 -6 2 10.00 2.50 -7 -6 2 10.30 3.00 7 -6 -2 15.30 3.20 -7 6 1 102.09 8.80 7 6 -1 106.49 6.70 -7 6 1 98.49 8.20 7 -6 -1 112.39 8.60 -7 -6 1 113.59 7.00 -7 -6 1 117.49 8.00 -7 6 0 42.10 4.90 -7 6 0 61.99 6.40 7 6 0 46.90 4.50 -7 -6 0 41.70 4.50 7 -6 0 42.40 5.10 -7 -6 0 47.40 3.60 -7 6 -1 43.20 5.70 -7 6 -1 34.30 4.80 7 6 1 44.00 3.10 7 -6 1 34.90 4.60 -7 -6 -1 40.80 2.70 7 -6 1 36.60 5.00 -7 -6 -1 42.50 4.20 -7 6 -2 139.39 10.30 7 6 2 138.99 9.00 7 6 2 148.09 8.20 -7 -6 -2 139.39 8.80 -7 -6 -2 139.69 7.60 7 -6 2 129.89 10.60 7 -6 2 128.69 10.00 7 6 3 18.70 3.20 -7 6 -3 19.90 4.10 7 6 3 22.70 3.10 -7 -6 -3 20.30 2.80 7 -6 3 21.90 4.70 -7 -6 -3 19.30 2.50 7 -6 3 20.90 4.20 7 6 4 3.80 1.70 -7 6 -4 0.20 1.60 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51.99 4.40 8 -5 3 51.69 6.20 8 5 4 15.90 2.90 8 5 4 16.80 3.40 -8 5 -4 20.50 4.20 8 -5 4 18.40 4.10 8 -5 4 17.50 5.00 -8 -5 -4 24.30 3.00 -8 -5 -4 18.90 3.00 8 5 5 152.88 10.40 8 -5 5 145.79 11.40 -8 -5 -5 140.79 8.70 8 5 6 1.50 1.40 -8 5 -6 0.60 1.90 8 5 6 0.50 2.00 8 -5 6 1.70 2.40 -8 -5 -6 3.80 1.20 8 -5 6 0.00 2.00 8 5 7 29.80 3.20 -8 5 -7 39.60 6.20 8 5 7 39.30 5.50 8 -5 7 30.40 5.70 -8 -5 -7 37.90 3.10 8 -5 7 32.10 6.20 -8 5 -8 10.70 3.40 8 5 8 5.90 3.20 -8 -5 -8 8.10 1.70 8 -5 8 6.60 3.30 8 -5 8 10.10 3.60 -8 6 8 4.80 2.20 -8 6 8 9.00 3.40 -8 6 8 8.30 2.80 -8 -6 8 2.50 2.40 -8 -6 8 2.70 1.90 -8 -6 8 1.90 2.50 -8 6 7 5.60 2.30 -8 6 7 7.00 2.30 -8 -6 7 4.40 2.00 -8 -6 7 4.30 2.80 -8 6 6 4.40 2.00 -8 6 6 3.20 2.60 -8 6 6 4.80 2.10 -8 -6 6 2.30 2.40 -8 -6 6 4.90 2.50 -8 6 5 32.40 4.90 -8 6 5 24.40 4.90 -8 6 5 26.30 4.70 -8 -6 5 31.00 4.50 -8 -6 5 25.40 4.50 -8 6 4 13.60 3.20 -8 6 4 15.40 3.60 -8 6 4 15.10 3.80 -8 -6 4 14.50 3.40 -8 -6 4 9.70 2.80 8 6 -3 38.80 4.30 -8 6 3 43.70 7.60 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47.70 4.90 -10 -1 4 51.49 6.50 -10 -1 4 50.49 4.70 -10 1 3 347.77 18.90 -10 1 3 326.37 18.90 10 1 -3 353.66 17.80 -10 -1 3 323.57 18.50 -10 -1 3 334.17 18.60 -10 -1 3 322.57 17.90 10 -1 -3 338.87 18.30 -10 -1 3 323.77 17.60 10 1 -2 4.10 1.70 -10 1 2 5.90 2.20 -10 1 2 2.40 1.90 -10 -1 2 3.00 1.50 -10 -1 2 0.30 1.30 -10 -1 2 2.70 1.90 10 -1 -2 3.20 1.90 10 1 -1 112.79 8.00 -10 1 1 126.89 9.10 -10 1 1 116.09 8.70 -10 -1 1 113.19 8.60 -10 -1 1 117.99 8.20 -10 -1 1 109.39 8.20 -10 -1 1 111.39 8.40 10 -1 -1 116.39 8.50 -10 1 0 -0.10 1.30 -10 1 0 0.10 1.80 10 1 0 1.70 1.40 -10 1 0 -0.20 1.30 -10 -1 0 -1.90 1.30 -10 -1 0 1.20 1.50 10 -1 0 0.80 1.50 -10 -1 0 -0.10 1.40 -10 -1 0 1.30 1.30 -10 1 -1 37.40 4.60 -10 1 -1 37.00 4.90 10 1 1 36.10 4.50 -10 1 -1 39.30 4.80 10 -1 1 44.20 5.10 -10 -1 -1 38.70 4.50 -10 -1 -1 41.90 4.50 -10 -1 -1 41.40 4.10 -10 -1 -1 50.89 5.10 10 1 2 20.20 3.70 -10 1 -2 14.60 3.40 -10 1 -2 17.90 3.60 -10 1 -2 19.50 3.70 -10 -1 -2 15.80 3.20 -10 -1 -2 20.50 3.10 10 -1 2 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1.70 10 -2 1 5.40 2.10 -10 -2 -1 2.00 2.00 -10 -2 -1 1.50 1.30 -10 -2 -1 5.10 1.60 10 2 2 6.30 2.20 -10 2 -2 9.40 2.70 -10 2 -2 6.90 2.50 -10 -2 -2 10.00 2.70 -10 -2 -2 6.00 2.50 10 -2 2 5.80 2.50 -10 -2 -2 7.10 1.70 -10 -2 -2 9.90 2.10 -10 2 -3 69.49 6.60 -10 2 -3 61.69 6.30 10 2 3 71.99 6.60 -10 -2 -3 72.49 5.20 -10 -2 -3 62.59 5.70 10 -2 3 67.59 7.00 -10 -2 -3 62.19 4.70 -10 2 -4 21.80 4.30 -10 2 -4 25.00 4.40 10 2 4 27.30 4.50 -10 -2 -4 21.80 2.50 -10 -2 -4 22.00 2.70 10 -2 4 22.50 4.50 -10 -2 -4 28.90 3.80 -10 2 -5 136.29 10.00 -10 2 -5 121.59 9.90 -10 -2 -5 121.69 8.30 10 -2 5 120.69 9.50 -10 -2 -5 112.49 7.00 10 -2 5 137.59 10.80 -10 -2 -5 121.39 7.00 -10 2 -6 5.10 2.70 10 2 6 3.50 2.10 -10 -2 -6 1.20 1.40 -10 -2 -6 5.80 1.50 10 -2 6 3.40 2.60 10 -2 6 2.50 2.30 -10 -2 -6 8.90 2.10 10 2 7 10.90 3.70 -10 2 -7 11.40 3.20 -10 -2 -7 8.60 1.70 10 -2 7 15.80 3.60 10 -2 7 16.90 4.50 -10 -2 -7 9.80 2.70 -10 2 -8 5.70 2.40 10 2 8 -2.20 2.50 -10 -2 -8 -2.00 2.60 10 -2 8 1.10 1.80 10 -2 8 7.00 3.60 -10 -2 -8 3.40 1.70 -10 3 8 -3.70 1.70 -10 3 8 -0.80 1.40 -10 -3 8 -1.20 1.90 -10 -3 8 -0.70 1.50 -10 -3 8 -1.10 2.70 -10 3 7 73.69 7.10 -10 3 7 76.69 8.40 -10 3 7 69.99 7.10 -10 -3 7 79.29 8.20 -10 -3 7 84.99 7.60 -10 -3 7 82.79 6.20 -10 3 6 5.00 2.20 -10 3 6 5.00 2.70 -10 3 6 3.00 2.10 -10 -3 6 2.40 1.50 -10 -3 6 2.10 2.50 -10 -3 6 6.30 2.00 -10 -3 6 5.80 2.40 -10 3 5 22.70 4.60 -10 3 5 31.60 4.80 -10 3 5 19.70 4.00 -10 -3 5 18.90 3.10 -10 -3 5 23.80 4.20 -10 -3 5 22.10 2.90 -10 -3 5 24.20 4.80 -10 3 4 11.70 3.30 -10 3 4 8.80 2.70 -10 -3 4 10.60 2.70 -10 -3 4 10.20 2.20 -10 -3 4 10.10 2.80 -10 3 3 198.28 15.10 -10 -3 3 183.68 11.00 -10 -3 3 197.08 12.40 -10 -3 3 197.28 10.70 -10 -3 3 197.78 12.10 10 -3 -3 198.88 12.70 10 3 -2 37.10 3.50 10 3 -2 37.70 4.40 -10 3 2 38.60 4.80 -10 3 2 40.10 5.30 10 -3 -2 35.40 4.40 -10 -3 2 35.90 3.70 -10 -3 2 39.30 5.20 -10 -3 2 37.20 4.10 10 3 -1 -0.80 1.20 -10 3 1 0.00 1.50 -10 3 1 3.90 2.00 10 3 -1 0.30 1.10 -10 -3 1 -0.80 1.20 -10 -3 1 1.80 1.50 10 -3 -1 2.30 1.70 -10 -3 1 2.60 1.30 -10 3 0 8.80 2.80 10 3 0 11.50 2.40 -10 3 0 15.20 3.30 -10 -3 0 9.00 2.00 10 -3 0 12.70 3.20 -10 -3 0 12.40 2.60 -10 -3 0 10.40 2.50 -10 -3 0 15.40 3.30 10 3 1 149.09 9.30 -10 3 -1 146.79 10.50 -10 3 -1 132.99 10.40 10 -3 1 154.68 10.90 -10 -3 -1 143.89 8.20 -10 -3 -1 147.79 10.70 -10 -3 -1 134.29 8.60 -10 -3 -1 141.99 9.60 -10 3 -2 10.90 3.00 -10 3 -2 5.50 2.60 10 3 2 11.00 2.70 -10 -3 -2 7.70 2.30 10 -3 2 7.70 2.70 -10 -3 -2 6.00 2.20 -10 -3 -2 12.80 1.60 -10 -3 -2 9.70 1.90 -10 3 -3 -0.50 1.60 10 3 3 2.20 1.80 -10 -3 -3 1.60 0.80 10 -3 3 0.30 1.50 -10 -3 -3 -0.30 0.80 -10 -3 -3 -1.70 0.90 10 3 4 49.00 5.40 -10 3 -4 49.90 6.00 -10 3 -4 45.90 5.60 -10 -3 -4 42.30 4.50 -10 -3 -4 51.79 2.90 -10 -3 -4 43.90 2.70 10 -3 4 49.30 6.00 10 3 5 3.20 1.80 -10 3 -5 4.30 2.20 10 -3 5 1.40 1.00 -10 -3 -5 1.30 1.50 10 -3 5 2.20 1.70 -10 3 -6 12.20 2.70 10 3 6 6.50 2.80 10 -3 6 10.40 3.10 10 -3 6 10.00 3.40 -10 -3 -6 6.90 2.20 10 3 7 17.80 4.40 -10 3 -7 24.50 4.20 10 -3 7 28.40 5.60 -10 -3 -7 15.00 2.60 10 -3 7 16.80 3.80 10 3 8 86.09 9.10 -10 3 -8 92.29 8.40 10 -3 8 80.29 8.10 10 -3 8 87.49 9.40 -10 -3 -8 78.19 6.20 -10 4 8 -0.20 2.60 -10 4 8 -2.50 1.70 -10 4 8 -1.40 1.70 -10 -4 8 -0.90 1.60 -10 -4 8 -2.80 2.00 -10 -4 8 -0.30 1.80 -10 4 7 0.50 2.10 -10 4 7 1.40 2.20 -10 4 7 -0.80 1.70 -10 -4 7 3.00 1.50 -10 -4 7 0.50 2.30 -10 -4 7 0.50 1.70 -10 4 6 11.40 3.20 -10 4 6 11.20 3.60 -10 4 6 10.40 2.90 -10 -4 6 13.20 2.50 -10 -4 6 9.90 3.30 -10 -4 6 9.20 2.90 -10 4 5 4.80 2.40 -10 4 5 9.80 2.70 -10 4 5 4.00 1.80 -10 -4 5 4.90 2.00 -10 -4 5 6.20 1.50 -10 -4 5 10.80 2.00 -10 4 4 2.30 2.30 -10 4 4 -0.50 1.40 -10 4 4 1.50 1.40 -10 -4 4 -1.40 0.80 -10 -4 4 -0.10 1.10 -10 -4 4 -1.10 1.40 -10 -4 4 0.90 1.50 -10 4 3 82.89 7.70 -10 4 3 68.89 7.00 -10 -4 3 75.39 4.90 -10 -4 3 80.29 6.70 -10 -4 3 77.49 5.30 10 -4 -3 75.69 7.10 -10 -4 3 78.49 6.90 10 4 -2 283.07 16.70 -10 4 2 339.67 18.60 -10 -4 2 304.97 15.30 -10 -4 2 303.37 16.60 -10 -4 2 306.17 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56.69 6.60 -10 -4 -6 55.79 5.00 10 -4 6 59.09 7.20 10 -4 6 58.89 7.20 -10 4 -7 5.50 2.60 10 4 7 3.80 3.10 -10 -4 -7 -0.10 1.60 10 -4 7 6.90 3.70 -10 5 7 12.10 3.30 -10 5 7 9.10 2.90 -10 -5 7 10.00 3.20 -10 -5 7 10.70 3.70 -10 -5 7 8.50 2.20 -10 5 6 4.10 2.60 -10 5 6 2.10 1.90 -10 5 6 2.40 2.10 -10 -5 6 0.40 1.90 -10 -5 6 0.00 1.00 -10 -5 6 0.90 1.60 -10 -5 6 2.60 1.90 -10 5 5 7.20 2.70 -10 5 5 2.50 2.10 -10 5 5 7.10 2.60 -10 -5 5 3.70 2.10 -10 -5 5 5.10 2.90 -10 -5 5 3.70 1.20 -10 -5 5 1.90 0.90 -10 5 4 89.49 8.00 -10 5 4 69.79 7.10 -10 5 4 72.59 7.80 -10 -5 4 75.99 4.00 -10 -5 4 83.69 7.20 -10 -5 4 76.89 7.10 -10 -5 4 69.19 4.10 -10 5 3 9.50 3.10 -10 5 3 7.90 2.70 -10 -5 3 9.70 1.10 -10 -5 3 7.00 1.20 -10 -5 3 9.80 2.50 -10 -5 3 8.60 2.60 10 -5 -3 12.30 3.00 -10 5 2 12.20 3.70 -10 5 2 13.10 3.40 -10 -5 2 12.80 3.30 -10 -5 2 15.80 3.00 -10 -5 2 10.80 1.30 10 -5 -2 11.90 3.40 -10 -5 2 10.20 1.40 -10 5 1 87.49 8.10 -10 5 1 71.19 7.00 10 5 -1 57.89 5.30 10 -5 -1 72.99 7.30 -10 -5 1 69.79 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7.80 2.60 -11 -1 6 6.50 2.40 -11 -1 6 6.20 2.90 -11 -1 6 5.40 2.00 -11 1 5 53.19 6.30 -11 1 5 48.20 5.60 -11 -1 5 50.79 5.10 -11 -1 5 48.80 5.50 -11 -1 5 46.80 5.70 -11 1 4 8.80 2.60 -11 1 4 10.80 3.10 -11 1 4 7.60 2.60 -11 -1 4 8.20 2.40 -11 -1 4 7.60 2.80 -11 1 3 0.30 1.50 -11 1 3 -0.10 1.60 11 1 -3 0.70 1.20 -11 -1 3 0.10 1.30 11 -1 -3 -0.80 1.10 -11 -1 3 -0.20 1.30 -11 -1 3 0.90 1.50 11 1 -2 227.28 13.10 -11 1 2 237.38 14.30 -11 1 2 216.68 13.90 -11 -1 2 209.78 13.30 11 -1 -2 207.18 13.40 -11 -1 2 226.58 14.00 -11 1 1 11.90 3.10 -11 1 1 15.80 3.30 11 1 -1 8.90 2.70 11 -1 -1 11.10 2.90 -11 -1 1 12.10 3.00 -11 -1 1 11.10 3.10 11 1 0 2.50 1.40 -11 1 0 -0.30 1.40 -11 1 0 3.40 1.80 -11 -1 0 3.20 1.70 -11 -1 0 3.30 2.10 11 -1 0 1.90 1.80 -11 -1 0 2.40 1.70 -11 1 -1 6.40 2.20 -11 1 -1 3.50 2.10 11 1 1 2.90 1.80 11 -1 1 6.60 2.40 -11 -1 -1 6.20 2.30 -11 -1 -1 5.40 2.00 11 1 2 21.20 4.10 -11 1 -2 18.60 4.00 -11 1 -2 26.00 3.90 -11 -1 -2 21.60 4.00 11 -1 2 21.30 4.20 -11 -1 -2 24.60 4.20 -11 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-3 1 127.89 9.20 -12 -3 1 147.09 10.50 12 -3 -1 150.08 11.10 -12 -3 1 132.79 9.10 12 3 0 48.90 4.70 -12 3 0 47.30 5.90 -12 3 0 40.90 5.50 12 -3 0 45.50 5.60 -12 -3 0 40.50 4.30 -12 -3 0 45.00 5.30 -12 -3 0 40.20 5.00 -12 3 -1 0.90 1.90 12 3 1 0.30 1.30 -12 3 -1 -2.10 1.50 -12 -3 -1 0.40 1.30 -12 -3 -1 2.40 1.90 12 -3 1 1.00 1.50 -12 -3 -1 -1.40 1.40 -12 3 -2 8.70 3.30 -12 3 -2 7.30 2.40 12 3 2 7.50 2.30 12 -3 2 8.20 3.00 -12 -3 -2 2.70 2.00 -12 -3 -2 8.10 2.40 -12 -3 -2 4.40 1.50 -12 3 -3 30.20 5.70 12 3 3 29.30 4.10 -12 3 -3 29.10 5.10 12 -3 3 24.70 5.10 -12 -3 -3 25.60 3.00 -12 -3 -3 28.10 4.50 -12 3 -4 33.30 5.80 12 3 4 35.20 4.90 -12 3 -4 27.20 5.00 -12 -3 -4 34.70 2.90 -12 -3 -4 32.40 2.90 -12 -3 -4 35.10 4.50 12 -3 4 50.09 6.50 -12 3 -5 33.50 4.80 -12 3 -5 20.80 4.90 12 3 5 37.30 4.80 -12 -3 -5 37.90 4.60 12 -3 5 24.70 5.40 -12 4 6 11.50 3.80 -12 4 6 9.70 3.10 -12 4 6 9.60 4.00 -12 -4 6 6.10 2.30 -12 -4 6 10.80 3.30 -12 -4 6 6.80 3.10 -12 4 5 18.80 4.60 -12 4 5 7.70 3.20 -12 4 5 11.70 3.50 -12 -4 5 8.80 2.40 -12 -4 5 6.20 2.90 -12 -4 5 14.30 3.70 -12 4 4 32.10 6.00 -12 4 4 26.00 5.10 -12 4 4 28.90 4.90 -12 -4 4 17.00 3.90 -12 -4 4 29.10 4.20 -12 4 3 10.10 3.70 -12 4 3 7.80 3.20 -12 -4 3 9.90 2.80 12 -4 -3 12.60 3.20 -12 -4 3 11.40 3.30 -12 -4 3 2.90 2.10 -12 4 2 -0.70 1.90 -12 4 2 -1.10 1.60 12 -4 -2 4.10 1.90 -12 -4 2 2.90 2.00 -12 -4 2 3.80 1.90 -12 -4 2 -1.60 1.90 -12 4 1 30.10 5.60 -12 4 1 24.30 4.80 12 4 -1 35.20 3.40 -12 -4 1 26.30 4.30 -12 -4 1 28.80 3.60 12 -4 -1 35.90 5.10 -12 -4 1 22.50 3.50 -12 -4 1 28.00 4.60 12 4 0 12.00 2.50 -12 4 0 15.10 4.00 -12 4 0 13.80 3.90 12 -4 0 16.10 3.60 -12 -4 0 14.30 2.90 -12 -4 0 15.70 3.50 -12 -4 0 6.20 2.30 -12 -4 0 12.40 2.30 12 4 1 4.20 1.50 -12 4 -1 -0.50 1.90 -12 4 -1 2.40 2.50 -12 -4 -1 1.90 1.50 -12 -4 -1 -0.20 1.00 12 -4 1 0.40 1.90 -12 -4 -1 -3.30 1.70 -12 -4 -1 -0.90 1.60 -12 4 -2 -2.70 1.90 -12 4 -2 -3.60 1.50 12 4 2 0.70 1.60 -12 -4 -2 -1.80 1.10 12 -4 2 -2.30 1.70 -12 -4 -2 0.50 1.00 12 4 3 13.40 2.90 -12 4 -3 10.90 3.80 -12 4 -3 12.90 3.70 12 -4 3 8.70 3.00 -12 -4 -3 13.20 3.20 -12 4 -4 -4.30 2.40 -12 4 -4 11.00 3.70 12 4 4 6.50 2.10 12 -4 4 9.80 3.40 -12 -4 -4 3.20 1.60 -12 4 -5 21.20 5.00 12 4 5 17.10 4.00 -12 4 -5 19.10 5.00 12 -4 5 29.30 5.60 -12 -4 -5 18.10 3.50 -12 5 5 -3.60 1.90 -12 5 5 1.90 2.00 -12 -5 5 -0.10 2.40 -12 -5 5 2.80 2.40 -12 5 4 61.59 7.20 -12 5 4 47.90 7.80 -12 5 4 60.19 7.20 -12 -5 4 51.59 5.90 -12 -5 4 71.09 8.40 -12 5 3 43.60 5.80 -12 5 3 38.70 6.70 12 -5 -3 31.70 5.50 -12 -5 3 37.30 5.00 -12 -5 3 39.30 3.00 -12 -5 3 51.39 6.00 -12 5 2 1.30 2.40 -12 5 2 0.00 2.60 12 -5 -2 -0.60 1.60 -12 -5 2 -1.50 1.50 -12 -5 2 1.40 0.90 -12 -5 2 3.10 2.20 -12 5 1 233.08 15.60 -12 5 1 210.38 15.60 -12 -5 1 206.98 11.40 12 -5 -1 216.28 15.30 -12 -5 1 227.98 13.40 -12 -5 1 225.38 11.50 -12 -5 1 233.38 12.70 -12 -5 1 216.58 14.40 -12 5 0 -1.40 1.80 -12 5 0 7.20 3.00 -12 -5 0 -2.90 1.50 -12 -5 0 0.70 1.90 12 -5 0 -0.10 2.00 -12 -5 0 3.90 2.10 -12 -5 0 2.90 1.40 -12 5 -1 29.90 5.70 12 5 1 23.90 3.20 -12 5 -1 14.80 4.40 -12 -5 -1 20.60 2.10 12 -5 1 24.80 5.20 -12 -5 -1 19.20 3.50 -12 -5 -1 13.60 3.90 12 5 2 33.80 4.10 -12 5 -2 30.80 6.10 -12 5 -2 33.40 6.10 -12 -5 -2 31.70 5.00 12 -5 2 35.90 6.20 -12 5 -3 -0.60 2.40 -12 5 -3 3.20 2.80 12 5 3 5.50 1.90 -12 -5 -3 -1.10 1.60 12 -5 3 2.70 2.70 -12 5 -4 3.90 2.60 -12 5 -4 2.20 3.30 12 5 4 6.60 2.40 -12 -5 -4 1.90 2.10 12 -5 4 1.50 2.90 -12 6 4 6.80 3.60 -12 6 4 11.30 3.80 -12 6 4 6.90 3.50 -12 -6 4 8.70 3.20 -12 -6 4 9.40 3.30 -12 6 3 60.49 7.20 -12 -6 3 56.29 5.80 12 -6 -3 58.59 8.20 -12 6 2 12.40 3.50 -12 6 2 14.80 4.50 -12 -6 2 23.40 4.60 -12 -6 2 13.90 3.00 12 -6 -2 18.00 4.10 -12 6 1 6.00 3.40 -12 6 1 2.70 2.70 -12 -6 1 3.60 2.40 -12 -6 1 1.20 1.70 12 -6 -1 1.20 2.10 -12 6 0 5.50 3.40 -12 6 0 4.20 2.90 -12 -6 0 5.70 1.60 12 -6 0 9.30 3.30 -12 -6 0 5.00 2.60 12 6 1 15.50 2.50 -12 6 -1 27.00 5.70 -12 6 -1 17.50 4.10 -12 -6 -1 19.30 4.20 12 -6 1 12.30 3.60 12 6 2 3.40 1.60 -12 6 -2 0.50 3.00 -12 -6 -2 -1.20 1.80 12 -6 2 6.00 3.50 -12 6 -3 6.20 3.60 12 6 3 11.90 2.40 -12 6 -3 8.00 3.50 12 -6 3 8.80 4.10 -12 7 2 4.30 2.90 -12 7 2 3.60 2.90 12 -7 -2 7.90 3.50 -12 -7 2 10.60 3.40 -12 -7 2 5.10 2.30 -12 7 1 -0.80 2.10 -12 7 1 0.20 2.30 -12 -7 1 2.50 2.30 -12 -7 1 -2.90 1.70 12 -7 -1 -1.40 1.30 -12 7 0 165.08 13.20 -12 -7 0 141.79 11.20 12 -7 0 154.68 12.70 -12 7 -1 19.00 4.50 12 -7 1 8.20 3.60 -12 -7 -1 21.60 4.50 -12 7 -2 7.10 3.70 -12 7 -2 16.80 4.30 -12 -7 -2 17.40 3.70 12 -7 2 19.20 4.50 -13 0 5 0.60 2.20 -13 0 5 -2.70 1.30 -13 0 4 153.68 11.90 -13 0 4 154.38 10.90 -13 0 4 158.68 11.90 -13 0 3 -0.50 1.40 13 0 -3 -2.20 1.20 -13 0 3 -2.20 1.50 -13 0 3 -0.90 1.20 13 0 -2 37.00 4.60 -13 0 2 36.30 5.10 -13 0 2 43.30 5.70 13 0 -1 1.60 1.00 -13 0 1 -0.60 2.00 -13 0 0 95.39 8.30 13 0 0 101.99 8.60 -13 0 0 105.09 9.00 -13 0 -1 -3.30 1.40 13 0 1 3.00 1.70 -13 0 -1 0.30 1.70 13 0 2 24.20 4.50 -13 0 -2 17.40 3.50 -13 0 -2 24.20 4.90 13 0 3 -1.10 1.70 -13 0 -3 -1.50 1.70 -13 0 -3 -3.50 1.60 -13 0 -4 1.40 1.80 -13 0 -4 -0.40 2.20 13 0 4 2.40 2.20 -13 0 -5 1.10 1.90 -13 0 -5 -1.90 2.00 13 0 5 3.30 2.90 -13 1 5 23.20 5.10 -13 1 5 15.10 3.50 -13 1 5 23.10 7.60 -13 -1 5 20.70 4.60 -13 -1 5 16.90 3.20 -13 1 4 0.00 2.00 -13 1 4 -0.80 2.30 -13 1 4 1.90 1.80 -13 -1 4 2.50 1.80 -13 -1 4 -3.40 1.70 -13 -1 4 -1.90 1.60 -13 1 3 2.60 1.90 -13 1 3 2.70 2.50 -13 -1 3 -3.10 1.40 13 -1 -3 -1.60 1.20 -13 -1 3 -0.80 1.80 -13 -1 3 -0.60 1.40 13 1 -2 4.80 2.20 -13 1 2 0.20 1.50 -13 1 2 4.30 2.10 -13 -1 2 3.80 2.10 -13 -1 2 1.30 2.00 13 -1 -2 6.60 2.40 -13 1 1 0.70 2.00 -13 1 1 0.70 1.80 13 1 -1 3.00 1.60 -13 -1 1 0.00 1.90 13 -1 -1 0.30 1.40 -13 -1 1 -1.90 1.40 13 1 0 9.20 2.50 -13 1 0 2.00 1.90 -13 1 0 -0.40 2.00 -13 -1 0 4.20 2.40 -13 -1 0 3.90 1.50 13 -1 0 7.90 2.50 -13 1 -1 3.90 2.40 13 1 1 7.20 2.40 -13 -1 -1 3.90 2.00 13 -1 1 8.20 3.00 -13 -1 -1 6.00 2.30 13 1 2 40.30 4.70 -13 1 -2 37.80 5.00 -13 1 -2 35.50 5.90 13 -1 2 46.80 5.80 -13 -1 -2 40.70 5.40 -13 -1 -2 34.90 4.40 -13 1 -3 12.80 3.60 13 1 3 6.90 2.60 -13 1 -3 5.90 2.80 -13 -1 -3 15.20 3.80 13 -1 3 10.40 3.50 -13 -1 -3 9.00 2.50 -13 1 -4 19.50 3.70 13 1 4 31.90 5.30 -13 1 -4 24.60 5.20 -13 -1 -4 22.80 4.50 13 -1 4 34.10 6.00 -13 -1 -4 28.10 3.90 13 1 5 11.30 3.70 -13 1 -5 5.90 3.10 -13 1 -5 5.20 3.80 -13 -1 -5 5.40 2.60 -13 -1 -5 6.40 2.80 -13 2 5 61.59 6.80 -13 2 5 73.19 9.40 -13 -2 5 58.89 6.80 -13 -2 5 54.89 6.90 -13 -2 5 58.19 5.50 -13 2 4 5.20 2.10 -13 2 4 0.90 2.40 -13 2 4 -2.10 1.80 -13 -2 4 0.90 2.20 -13 -2 4 -0.70 1.60 -13 -2 4 3.00 2.50 -13 2 3 -1.30 1.80 -13 2 3 1.30 2.50 -13 -2 3 -0.60 1.80 -13 -2 3 0.70 1.70 13 -2 -3 3.10 2.20 -13 -2 3 -0.90 1.40 13 2 -2 3.70 1.60 -13 2 2 1.90 1.90 -13 2 2 -0.90 1.40 -13 -2 2 2.20 1.40 -13 -2 2 -1.40 1.40 13 -2 -2 1.80 1.90 -13 2 1 72.39 7.70 13 2 -1 89.19 6.80 -13 2 1 79.99 8.00 -13 -2 1 74.49 7.60 -13 -2 1 81.79 6.90 13 -2 -1 84.19 7.90 -13 2 0 -1.00 1.40 -13 2 0 0.30 2.10 13 2 0 0.50 1.50 -13 -2 0 0.90 1.70 -13 -2 0 1.20 2.10 13 -2 0 3.00 2.00 -13 2 -1 -1.60 1.50 13 2 1 1.10 1.60 -13 2 -1 -0.30 1.90 -13 -2 -1 0.50 2.60 -13 -2 -1 1.30 1.90 13 -2 1 3.20 2.00 -13 -2 -1 -2.30 1.70 13 2 2 1.40 1.80 -13 2 -2 2.70 2.20 -13 2 -2 -0.40 2.50 13 -2 2 0.90 2.20 -13 -2 -2 0.50 1.50 -13 -2 -2 -1.50 1.70 13 2 3 0.80 1.50 -13 2 -3 -4.10 1.70 13 -2 3 2.50 2.40 -13 -2 -3 -3.40 1.30 -13 2 -4 4.00 2.50 13 2 4 8.20 2.30 -13 2 -4 4.50 2.90 -13 -2 -4 5.40 2.50 13 -2 4 14.70 4.30 -13 3 5 36.90 6.90 -13 3 5 54.89 6.80 -13 3 5 50.29 6.40 -13 -3 5 57.69 6.90 -13 -3 5 51.19 6.50 -13 -3 5 49.80 4.80 -13 3 4 4.50 2.60 -13 3 4 -1.90 2.20 -13 3 4 -2.10 1.90 -13 -3 4 1.20 2.00 -13 -3 4 -2.20 1.30 -13 -3 4 0.60 1.40 -13 3 3 -1.00 1.90 -13 3 3 -3.70 1.70 13 -3 -3 -1.80 1.70 -13 -3 3 -2.50 1.30 -13 -3 3 -2.00 1.40 -13 3 2 6.20 2.40 -13 3 2 1.00 2.80 -13 -3 2 3.00 1.90 13 -3 -2 5.10 2.60 -13 -3 2 5.10 2.60 -13 -3 2 2.90 2.20 -13 3 1 90.49 8.90 13 3 -1 104.19 7.20 -13 3 1 83.59 8.60 13 -3 -1 97.09 8.80 -13 -3 1 94.69 7.40 -13 -3 1 87.29 8.20 13 3 0 7.40 2.10 -13 3 0 9.80 3.00 -13 3 0 3.10 2.80 -13 -3 0 5.70 2.60 13 -3 0 8.50 2.90 -13 -3 0 8.50 2.40 -13 -3 0 10.70 3.80 -13 3 -1 5.40 2.50 -13 3 -1 4.00 2.50 13 -3 1 6.60 2.70 -13 -3 -1 4.50 2.60 -13 -3 -1 4.50 1.70 13 3 2 3.20 1.80 -13 3 -2 1.00 1.80 -13 3 -2 -0.60 1.40 13 -3 2 -1.30 1.70 -13 -3 -2 -2.40 1.40 13 3 3 1.30 1.70 -13 3 -3 -0.80 2.10 -13 3 -3 -0.10 2.70 -13 -3 -3 5.20 2.50 -13 -3 -3 -2.20 1.20 13 -3 3 2.40 2.10 -13 3 -4 -1.80 2.30 13 3 4 3.90 2.10 -13 3 -4 4.80 2.30 -13 -3 -4 -1.40 2.00 -13 4 4 12.30 3.80 -13 4 4 4.10 3.50 -13 4 4 8.70 3.70 -13 -4 4 4.90 3.00 -13 -4 4 4.20 2.30 -13 -4 4 5.10 2.90 -13 4 3 87.39 10.40 -13 4 3 94.09 9.50 13 -4 -3 89.89 8.80 -13 -4 3 89.89 6.30 -13 4 2 19.90 4.60 -13 4 2 19.80 4.90 -13 -4 2 18.80 3.70 13 -4 -2 16.90 4.10 -13 -4 2 15.30 2.70 -13 -4 2 21.80 4.60 -13 4 1 41.50 5.80 13 4 -1 31.50 3.40 -13 4 1 20.50 4.60 13 -4 -1 20.80 4.70 -13 -4 1 26.20 5.00 -13 -4 1 23.20 3.70 13 4 0 53.59 5.10 -13 4 0 50.89 6.60 -13 4 0 50.59 7.00 -13 -4 0 53.89 6.30 -13 -4 0 51.29 4.80 13 -4 0 55.79 6.90 13 4 1 2.70 1.60 -13 4 -1 0.40 2.10 -13 4 -1 -0.50 1.90 13 -4 1 2.80 1.70 -13 -4 -1 -1.00 1.70 -13 -4 -1 0.80 1.40 -13 4 -2 0.80 2.40 13 4 2 2.90 1.60 -13 4 -2 -3.80 2.00 13 -4 2 0.90 2.20 -13 -4 -2 1.10 2.00 -13 4 -3 -0.70 2.60 13 4 3 4.10 2.30 -13 -4 -3 0.80 2.20 13 -4 3 3.20 3.60 -13 5 3 51.39 6.90 -13 5 3 50.29 7.40 13 -5 -3 43.40 7.00 -13 -5 3 60.49 7.00 -13 5 2 70.79 9.60 -13 5 2 64.49 7.70 -13 -5 2 67.09 7.50 -13 -5 2 62.09 6.10 -13 5 1 -1.60 2.20 -13 5 1 2.80 2.90 -13 -5 1 2.60 1.90 -13 -5 1 5.30 2.90 13 -5 -1 5.80 3.30 -13 -5 1 -1.50 1.80 -13 5 0 144.69 12.20 13 5 0 153.98 8.70 -13 5 0 120.59 11.50 13 -5 0 130.09 12.90 -13 -5 0 133.99 10.70 -13 5 -1 7.60 3.60 -13 5 -1 24.30 5.00 13 5 1 13.50 2.60 -13 -5 -1 16.50 3.90 -13 5 -2 4.70 3.10 13 5 2 8.70 2.20 -13 5 -2 2.80 3.10 -13 -5 -2 8.60 3.10 13 -5 2 6.10 3.20 -14 0 3 0.60 2.40 -14 0 3 -1.30 2.70 -14 0 3 -0.20 1.90 -14 0 2 18.30 4.50 14 0 -2 21.80 4.30 -14 0 2 26.30 4.80 14 0 -1 1.10 1.50 -14 0 1 3.40 1.50 -14 0 0 123.19 10.90 14 0 0 145.89 10.70 -14 0 0 146.29 10.50 -14 0 -1 0.20 1.60 14 0 1 -0.50 1.60 -14 0 -1 -1.20 1.30 -14 0 -2 0.20 2.10 -14 0 -2 1.50 2.10 14 0 2 0.00 2.20 -14 1 3 73.79 8.00 -14 1 3 67.69 7.10 -14 1 3 77.89 8.20 -14 -1 3 72.59 6.70 -14 -1 3 69.09 7.70 -14 -1 3 72.49 7.40 -14 1 2 4.10 2.30 14 1 -2 9.00 2.40 -14 1 2 7.20 3.20 -14 -1 2 6.70 2.80 14 -1 -2 7.00 2.60 -14 -1 2 3.70 2.80 14 1 -1 7.80 2.40 -14 1 1 6.10 3.60 -14 1 1 8.70 2.80 -14 -1 1 8.00 2.80 14 -1 -1 5.50 2.70 -14 1 0 6.30 2.70 14 1 0 9.00 2.40 -14 -1 0 7.70 3.10 -14 -1 0 2.10 2.50 14 -1 0 11.00 3.30 14 1 1 40.10 5.50 -14 1 -1 42.30 5.70 -14 -1 -1 36.90 5.90 14 -1 1 48.80 6.20 -14 -1 -1 47.40 5.20 -14 1 -2 17.20 4.00 14 1 2 20.10 3.90 14 -1 2 23.20 5.00 -14 -1 -2 18.10 4.20 -14 -1 -2 19.60 3.80 -14 2 3 1.10 2.00 -14 2 3 -0.70 2.40 -14 -2 3 -2.80 1.70 -14 -2 3 -2.60 1.80 -14 -2 3 -1.30 1.70 -14 2 2 13.50 3.90 -14 2 2 20.40 4.90 14 2 -2 12.90 2.60 -14 -2 2 18.60 3.50 -14 -2 2 16.10 4.00 14 -2 -2 17.60 4.20 -14 2 1 6.60 3.30 -14 2 1 14.40 3.60 -14 -2 1 10.60 4.10 14 -2 -1 12.80 3.60 -14 2 0 7.30 3.00 -14 2 0 10.80 3.50 14 2 0 11.40 2.50 -14 -2 0 8.50 2.60 14 -2 0 12.00 3.50 14 2 1 0.90 1.80 -14 2 -1 -0.70 1.80 -14 2 -1 -3.10 1.20 14 -2 1 4.30 2.30 -14 -2 -1 0.00 2.30 -14 2 -2 25.00 5.00 -14 2 -2 16.90 4.10 14 2 2 29.30 4.10 14 -2 2 24.60 5.10 -14 -2 -2 25.00 4.70 -14 -2 -2 30.70 4.10 -14 3 2 22.90 5.10 -14 3 2 26.90 5.20 -14 -3 2 23.00 4.70 -14 -3 2 29.60 4.00 -14 -3 2 26.50 4.30 14 -3 -2 20.50 4.70 -14 3 1 8.30 3.10 14 3 -1 9.80 2.20 -14 3 1 8.60 4.20 -14 -3 1 2.90 2.10 -14 -3 1 4.20 2.80 14 -3 -1 10.30 3.30 -14 3 0 8.90 3.60 -14 3 0 9.10 3.40 14 3 0 15.10 3.20 -14 -3 0 5.80 3.20 14 -3 0 6.50 3.40 -14 -3 0 5.30 2.20 14 3 1 5.90 2.70 -14 3 -1 1.90 2.20 -14 3 -1 -0.20 2.50 14 -3 1 0.30 2.70 -14 -3 -1 -1.30 1.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 26488 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_wv638 _database_code_depnum_ccdc_archive 'CCDC 2044219' loop_ _audit_author_name _audit_author_address 'Peter Mayer' ;LMU Muenchen Germany ; _audit_update_record ; 2020-11-13 deposited with the CCDC. 2021-02-09 downloaded from the CCDC. ; _chemical_name_common RNH142F1 _chemical_compound_source ? _chemical_absolute_configuration ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.080 #?# in millimeters _exptl_crystal_size_mid 0.030 #?# in millimeters _exptl_crystal_size_min 0.030 #?# in millimeters _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_special_details ; ; _audit_creation_date ? #?# style: 18-Aug-1998 _diffrn_ambient_temperature 112.(2) #?# in K _diffrn_source_type 'Bruker TXS' _diffrn_source_power 2.5 #?# in kW _diffrn_source_voltage 50 #?# in kV _diffrn_source_current 50 #?# in mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode (TXS)' _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_collimation ? _diffrn_measurement_device 'fixed-chi three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture TXS' _diffrn_measurement_method 'mix of phi and omega scans' _diffrn_measurement_details ? _diffrn_detector_area_resol_mean 7.3910 _diffrn_special_details ? _diffrn_orient_matrix_type ? _diffrn_orient_matrix_UB_11 ? _diffrn_orient_matrix_UB_12 ? _diffrn_orient_matrix_UB_13 ? _diffrn_orient_matrix_UB_21 ? _diffrn_orient_matrix_UB_22 ? _diffrn_orient_matrix_UB_23 ? _diffrn_orient_matrix_UB_31 ? _diffrn_orient_matrix_UB_32 ? _diffrn_orient_matrix_UB_33 ? _cell_length_a 11.6656(4) _cell_length_b 9.4061(4) _cell_length_c 10.7626(5) _cell_angle_alpha 90 _cell_angle_beta 97.797(2) _cell_angle_gamma 90 _cell_volume 1170.04(8) _cell_measurement_temperature 112.(2) #?# in K _cell_measurement_reflns_used 3795 _cell_measurement_theta_min 2.7920 _cell_measurement_theta_max 27.0609 _cell_special_details ? _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 1.00 _shelx_estimated_absorpt_T_min 0.993 _shelx_estimated_absorpt_T_max 0.997 _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _diffrn_reflns_number 11194 #xl _diffrn_reflns_av_R_equivalents 0.0421 #xl _diffrn_reflns_av_unetI/netI 0.0367 #xl _diffrn_reflns_limit_h_min -14 #xl _diffrn_reflns_limit_h_max 14 #xl _diffrn_reflns_limit_k_min -11 #xl _diffrn_reflns_limit_k_max 11 #xl _diffrn_reflns_limit_l_min -13 #xl _diffrn_reflns_limit_l_max 13 #xl _diffrn_reflns_theta_min 3.246 #xl _diffrn_reflns_theta_max 26.363 #xl _diffrn_measured_fraction_theta_max 0.998 #xl _diffrn_reflns_theta_full 25.242 #xl _diffrn_measured_fraction_theta_full 0.998 #xl _diffrn_reflns_Laue_measured_fraction_max 0.998 #xl _diffrn_reflns_Laue_measured_fraction_full 0.998 #xl _diffrn_reflns_point_group_measured_fraction_max 0.998 #xl _diffrn_reflns_point_group_measured_fraction_full 0.998 #xl _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' _space_group_IT_number 14 _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_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' N N 0.0061 0.0033 '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' _reflns_number_total 2388 #xl _reflns_number_gt 1856 #xl _reflns_threshold_expression 'I > 2\s(I)' #xl _reflns_Friedel_coverage 0.000 #xl _reflns_Friedel_fraction_max . #xl _reflns_Friedel_fraction_full . #xl _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. ; _refine_ls_structure_factor_coef Fsqd #xl _refine_ls_matrix_type full #xl _refine_ls_weighting_scheme calc #xl _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.5952P] where P=(Fo^2^+2Fc^2^)/3' #xl _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr #?# _refine_ls_extinction_method none #xl _refine_ls_extinction_coef . #xl _refine_ls_abs_structure_details ? #xl _refine_ls_abs_structure_Flack ? #xl _refine_ls_number_reflns 2388 #xl _refine_ls_number_parameters 154 #xl _refine_ls_number_restraints 0 #xl _refine_ls_R_factor_all 0.0622 #xl _refine_ls_R_factor_gt 0.0434 #xl _refine_ls_wR_factor_ref 0.1005 #xl _refine_ls_wR_factor_gt 0.0933 #xl _refine_ls_goodness_of_fit_ref 1.032 #xl _refine_ls_restrained_S_all 1.032 #xl _refine_ls_shift/su_max 0.000 #xl _refine_ls_shift/su_mean 0.000 #xl _refine_diff_density_max 0.226 #xl _refine_diff_density_min -0.199 #xl _refine_diff_density_rms 0.042 #xl _refine_special_details ; ; _computing_data_collection 'APEX3 v2016.5-0, Bruker AXS (2016)' _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 833)' _computing_publication_material ? 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 -0.05132(10) 0.36380(13) 0.39951(11) 0.0268(3) Uani 1 1 d . . . . . O2 O 0.02727(11) 0.52940(13) 0.29661(11) 0.0289(3) Uani 1 1 d . . . . . N1 N 0.66389(13) 0.36602(18) 0.95272(14) 0.0318(4) Uani 1 1 d . . . . . C1 C 0.15686(14) 0.35263(17) 0.39032(15) 0.0205(4) Uani 1 1 d . . . . . C2 C 0.24985(15) 0.4006(2) 0.31534(16) 0.0255(4) Uani 1 1 d . . . . . H2A H 0.311817 0.331844 0.303840 0.031 Uiso 1 1 calc R U . . . H2B H 0.226531 0.463335 0.242449 0.031 Uiso 1 1 calc R U . . . C3 C 0.24952(14) 0.46241(18) 0.44309(15) 0.0222(4) Uani 1 1 d . . . . . H3 H 0.219949 0.562243 0.442147 0.027 Uiso 1 1 calc R U . . . C4 C 0.04119(14) 0.42045(18) 0.35694(15) 0.0217(4) Uani 1 1 d . . . . . C5 C 0.16002(14) 0.20441(17) 0.44420(16) 0.0227(4) Uani 1 1 d . . . . . H5A H 0.238126 0.183476 0.488708 0.027 Uiso 1 1 calc R U . . . H5B H 0.141863 0.133913 0.376066 0.027 Uiso 1 1 calc R U . . . C6 C 0.07108(15) 0.19565(18) 0.53474(16) 0.0257(4) Uani 1 1 d . . . . . H6A H 0.071592 0.099301 0.571842 0.031 Uiso 1 1 calc R U . . . H6B H 0.090027 0.265174 0.603517 0.031 Uiso 1 1 calc R U . . . C7 C -0.04614(15) 0.22745(18) 0.46444(17) 0.0278(4) Uani 1 1 d . . . . . H7A H -0.067538 0.151045 0.402345 0.033 Uiso 1 1 calc R U . . . H7B H -0.103721 0.227239 0.524069 0.033 Uiso 1 1 calc R U . . . C8 C 0.33718(14) 0.42991(17) 0.55293(15) 0.0206(4) Uani 1 1 d . . . . . C9 C 0.43804(15) 0.35389(18) 0.54323(16) 0.0247(4) Uani 1 1 d . . . . . H9 H 0.449621 0.314697 0.464536 0.030 Uiso 1 1 calc R U . . . C10 C 0.52159(15) 0.33433(18) 0.64571(16) 0.0242(4) Uani 1 1 d . . . . . H10 H 0.590046 0.282517 0.637412 0.029 Uiso 1 1 calc R U . . . C11 C 0.50463(14) 0.39121(17) 0.76127(15) 0.0210(4) Uani 1 1 d . . . . . C12 C 0.40296(15) 0.46443(18) 0.77374(16) 0.0241(4) Uani 1 1 d . . . . . H12 H 0.390563 0.501262 0.853016 0.029 Uiso 1 1 calc R U . . . C13 C 0.32038(14) 0.48320(18) 0.67047(16) 0.0232(4) Uani 1 1 d . . . . . H13 H 0.251119 0.533040 0.679320 0.028 Uiso 1 1 calc R U . . . C14 C 0.59359(15) 0.37645(18) 0.86744(16) 0.0237(4) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0201(6) 0.0295(7) 0.0302(7) 0.0009(5) 0.0014(5) 0.0030(5) O2 0.0326(7) 0.0306(7) 0.0227(7) 0.0064(5) 0.0003(5) 0.0083(6) N1 0.0241(8) 0.0455(10) 0.0256(9) 0.0017(7) 0.0025(7) -0.0017(7) C1 0.0197(8) 0.0231(8) 0.0183(8) -0.0018(7) 0.0017(6) 0.0026(7) C2 0.0232(9) 0.0342(10) 0.0194(9) 0.0021(7) 0.0039(7) 0.0014(7) C3 0.0221(8) 0.0214(8) 0.0229(9) 0.0010(7) 0.0020(7) -0.0014(7) C4 0.0227(9) 0.0266(9) 0.0149(8) -0.0041(7) -0.0003(6) 0.0019(7) C5 0.0213(9) 0.0210(8) 0.0243(9) -0.0021(7) -0.0023(7) 0.0022(7) C6 0.0320(10) 0.0211(8) 0.0236(9) 0.0013(7) 0.0022(7) -0.0030(7) C7 0.0256(9) 0.0248(9) 0.0337(10) -0.0010(8) 0.0062(8) -0.0033(7) C8 0.0207(8) 0.0187(8) 0.0221(9) 0.0003(7) 0.0015(7) -0.0040(7) C9 0.0262(9) 0.0261(9) 0.0214(9) -0.0039(7) 0.0024(7) 0.0016(7) C10 0.0205(9) 0.0249(9) 0.0270(10) -0.0011(7) 0.0030(7) 0.0018(7) C11 0.0201(8) 0.0217(8) 0.0208(9) 0.0023(7) 0.0016(7) -0.0044(7) C12 0.0253(9) 0.0273(9) 0.0200(9) -0.0030(7) 0.0047(7) -0.0013(7) C13 0.0197(8) 0.0241(9) 0.0256(9) -0.0018(7) 0.0028(7) 0.0022(7) C14 0.0220(9) 0.0269(9) 0.0232(9) 0.0008(7) 0.0066(7) -0.0022(7) 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 C4 1.339(2) . ? O1 C7 1.458(2) . ? O2 C4 1.212(2) . ? N1 C14 1.149(2) . ? C1 C4 1.492(2) . ? C1 C2 1.506(2) . ? C1 C5 1.508(2) . ? C1 C3 1.546(2) . ? C2 C3 1.493(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.486(2) . ? C3 H3 1.0000 . ? C5 C6 1.519(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.500(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.393(2) . ? C8 C13 1.399(2) . ? C9 C10 1.382(2) . ? C9 H9 0.9500 . ? C10 C11 1.393(2) . ? C10 H10 0.9500 . ? C11 C12 1.394(2) . ? C11 C14 1.442(2) . ? C12 C13 1.380(2) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? 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 C4 O1 C7 122.09(13) . . ? C4 C1 C2 115.89(14) . . ? C4 C1 C5 117.51(14) . . ? C2 C1 C5 120.06(14) . . ? C4 C1 C3 111.55(14) . . ? C2 C1 C3 58.56(11) . . ? C5 C1 C3 119.78(14) . . ? C3 C2 C1 62.06(11) . . ? C3 C2 H2A 117.6 . . ? C1 C2 H2A 117.6 . . ? C3 C2 H2B 117.6 . . ? C1 C2 H2B 117.6 . . ? H2A C2 H2B 114.6 . . ? C8 C3 C2 124.39(15) . . ? C8 C3 C1 121.74(14) . . ? C2 C3 C1 59.38(11) . . ? C8 C3 H3 113.6 . . ? C2 C3 H3 113.6 . . ? C1 C3 H3 113.6 . . ? O2 C4 O1 117.66(15) . . ? O2 C4 C1 122.79(16) . . ? O1 C4 C1 119.48(14) . . ? C1 C5 C6 108.28(14) . . ? C1 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? C1 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? C7 C6 C5 108.71(14) . . ? C7 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? C7 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? O1 C7 C6 113.13(14) . . ? O1 C7 H7A 109.0 . . ? C6 C7 H7A 109.0 . . ? O1 C7 H7B 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C13 118.37(15) . . ? C9 C8 C3 122.89(15) . . ? C13 C8 C3 118.68(15) . . ? C10 C9 C8 121.34(16) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 119.44(16) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C10 C11 C12 120.12(15) . . ? C10 C11 C14 119.76(15) . . ? C12 C11 C14 120.11(15) . . ? C13 C12 C11 119.74(15) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C8 120.95(16) . . ? C12 C13 H13 119.5 . . ? C8 C13 H13 119.5 . . ? N1 C14 C11 179.2(2) . . ? 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 C4 C1 C2 C3 100.48(16) . . . . ? C5 C1 C2 C3 -108.59(17) . . . . ? C1 C2 C3 C8 109.62(17) . . . . ? C4 C1 C3 C8 138.08(16) . . . . ? C2 C1 C3 C8 -113.93(18) . . . . ? C5 C1 C3 C8 -4.9(2) . . . . ? C4 C1 C3 C2 -107.99(16) . . . . ? C5 C1 C3 C2 109.06(17) . . . . ? C7 O1 C4 O2 175.09(15) . . . . ? C7 O1 C4 C1 -8.0(2) . . . . ? C2 C1 C4 O2 -17.2(2) . . . . ? C5 C1 C4 O2 -168.85(15) . . . . ? C3 C1 C4 O2 47.3(2) . . . . ? C2 C1 C4 O1 166.06(14) . . . . ? C5 C1 C4 O1 14.4(2) . . . . ? C3 C1 C4 O1 -129.51(15) . . . . ? C4 C1 C5 C6 -40.39(19) . . . . ? C2 C1 C5 C6 169.13(14) . . . . ? C3 C1 C5 C6 100.43(17) . . . . ? C1 C5 C6 C7 59.85(18) . . . . ? C4 O1 C7 C6 29.4(2) . . . . ? C5 C6 C7 O1 -55.47(19) . . . . ? C2 C3 C8 C9 9.5(2) . . . . ? C1 C3 C8 C9 81.9(2) . . . . ? C2 C3 C8 C13 -173.40(16) . . . . ? C1 C3 C8 C13 -100.99(19) . . . . ? C13 C8 C9 C10 -1.8(2) . . . . ? C3 C8 C9 C10 175.30(16) . . . . ? C8 C9 C10 C11 0.2(3) . . . . ? C9 C10 C11 C12 1.4(2) . . . . ? C9 C10 C11 C14 -177.37(16) . . . . ? C10 C11 C12 C13 -1.5(2) . . . . ? C14 C11 C12 C13 177.29(16) . . . . ? C11 C12 C13 C8 -0.1(3) . . . . ? C9 C8 C13 C12 1.7(2) . . . . ? C3 C8 C13 C12 -175.50(15) . . . . ? _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. ; _audit_block_code C14H13NO2_wv638_mayr _audit_creation_method 'APEX3 v2017.3-0' _shelxl_version_number ? _chemical_name_systematic ? _chemical_formula_moiety 'C14 H13 N O2' _chemical_formula_sum 'C14 H13 N O2' _chemical_formula_weight 227.25 #?# (Cohen, 1996) _chemical_melting_point ? #?# in K! _cell_formula_units_Z 4 #?# adjust to _chemical_formula_[] _exptl_crystal_density_diffrn 1.290 _exptl_crystal_F_000 480 #?# check! _shelx_res_file ; TITL wv638_0ma_a.res in P2(1)/c wv638_0ma_a.res created by SHELXL-2016/6 at 10:37:03 on 05-Dec-2018 REM Old TITL wv638_0ma in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.122, Rweak 0.006, Alpha 0.018, Orientation as input REM Formula found by SHELXT: C14 N O2 CELL 0.71073 11.6656 9.4061 10.7626 90.000 97.797 90.000 ZERR 4.000 0.0004 0.0004 0.0005 0.000 0.002 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O UNIT 56 52 4 8 TEMP -161 SIZE 0.03 0.03 0.08 L.S. 10 BOND $H LIST 4 CONF ACTA OMIT 0 1 1 SHEL 9.0 0.80 FMAP 2 PLAN -20 WGHT 0.036000 0.595200 FVAR 0.79229 O1 4 -0.051316 0.363800 0.399513 11.00000 0.02009 0.02948 = 0.03016 0.00091 0.00144 0.00301 O2 4 0.027274 0.529398 0.296608 11.00000 0.03261 0.03056 = 0.02271 0.00637 0.00033 0.00833 N1 3 0.663893 0.366020 0.952716 11.00000 0.02412 0.04548 = 0.02559 0.00167 0.00252 -0.00165 C1 1 0.156860 0.352628 0.390319 11.00000 0.01975 0.02310 = 0.01831 -0.00182 0.00171 0.00264 C2 1 0.249852 0.400575 0.315345 11.00000 0.02317 0.03421 = 0.01939 0.00212 0.00389 0.00136 AFIX 23 H2A 2 0.311817 0.331844 0.303840 11.00000 -1.20000 H2B 2 0.226531 0.463335 0.242449 11.00000 -1.20000 AFIX 0 C3 1 0.249521 0.462408 0.443087 11.00000 0.02206 0.02138 = 0.02293 0.00096 0.00199 -0.00136 AFIX 13 H3 2 0.219949 0.562243 0.442147 11.00000 -1.20000 AFIX 0 C4 1 0.041188 0.420453 0.356945 11.00000 0.02271 0.02665 = 0.01494 -0.00411 -0.00028 0.00195 C5 1 0.160017 0.204411 0.444197 11.00000 0.02130 0.02105 = 0.02429 -0.00209 -0.00230 0.00221 AFIX 23 H5A 2 0.238126 0.183476 0.488708 11.00000 -1.20000 H5B 2 0.141863 0.133913 0.376066 11.00000 -1.20000 AFIX 0 C6 1 0.071077 0.195646 0.534739 11.00000 0.03196 0.02111 = 0.02359 0.00134 0.00220 -0.00298 AFIX 23 H6A 2 0.071592 0.099301 0.571842 11.00000 -1.20000 H6B 2 0.090027 0.265174 0.603517 11.00000 -1.20000 AFIX 0 C7 1 -0.046138 0.227446 0.464437 11.00000 0.02559 0.02477 = 0.03368 -0.00101 0.00618 -0.00326 AFIX 23 H7A 2 -0.067538 0.151045 0.402345 11.00000 -1.20000 H7B 2 -0.103721 0.227239 0.524069 11.00000 -1.20000 AFIX 0 C8 1 0.337181 0.429905 0.552930 11.00000 0.02066 0.01868 = 0.02212 0.00027 0.00149 -0.00396 C9 1 0.438042 0.353893 0.543227 11.00000 0.02623 0.02613 = 0.02145 -0.00393 0.00243 0.00156 AFIX 43 H9 2 0.449621 0.314697 0.464536 11.00000 -1.20000 AFIX 0 C10 1 0.521595 0.334333 0.645711 11.00000 0.02053 0.02492 = 0.02695 -0.00106 0.00301 0.00176 AFIX 43 H10 2 0.590046 0.282517 0.637412 11.00000 -1.20000 AFIX 0 C11 1 0.504627 0.391211 0.761274 11.00000 0.02013 0.02171 = 0.02082 0.00229 0.00164 -0.00438 C12 1 0.402963 0.464425 0.773738 11.00000 0.02535 0.02731 = 0.01997 -0.00304 0.00468 -0.00126 AFIX 43 H12 2 0.390563 0.501262 0.853016 11.00000 -1.20000 AFIX 0 C13 1 0.320380 0.483204 0.670474 11.00000 0.01966 0.02414 = 0.02562 -0.00184 0.00283 0.00220 AFIX 43 H13 2 0.251119 0.533040 0.679320 11.00000 -1.20000 AFIX 0 C14 1 0.593594 0.376449 0.867442 11.00000 0.02200 0.02688 = 0.02320 0.00079 0.00657 -0.00218 HKLF 4 REM wv638_0ma_a.res in P2(1)/c REM R1 = 0.0434 for 1856 Fo > 4sig(Fo) and 0.0622 for all 2388 data REM 154 parameters refined using 0 restraints END WGHT 0.0360 0.5952 REM Highest difference peak 0.226, deepest hole -0.199, 1-sigma level 0.042 Q1 1 0.1608 0.2795 0.3996 11.00000 0.05 0.23 Q2 1 0.1883 0.3995 0.4502 11.00000 0.05 0.21 Q3 1 0.1786 0.3514 0.3255 11.00000 0.05 0.20 Q4 1 0.1062 0.3970 0.3914 11.00000 0.05 0.17 Q5 1 0.4832 0.4720 0.7543 11.00000 0.05 0.16 Q6 1 -0.0456 0.5919 0.2990 11.00000 0.05 0.15 Q7 1 0.1843 0.5276 0.4585 11.00000 0.05 0.15 Q8 1 -0.1267 0.2407 0.4884 11.00000 0.05 0.15 Q9 1 0.1040 0.5479 0.2508 11.00000 0.05 0.15 Q10 1 0.5243 0.3903 0.6971 11.00000 0.05 0.14 Q11 1 -0.0599 0.1801 0.3640 11.00000 0.05 0.14 Q12 1 0.5010 0.3809 0.5837 11.00000 0.05 0.14 Q13 1 0.1178 0.4525 0.5081 11.00000 0.05 0.14 Q14 1 0.4792 0.3631 0.4639 11.00000 0.05 0.14 Q15 1 0.3402 0.4789 0.6014 11.00000 0.05 0.14 Q16 1 0.2928 0.2445 0.6027 11.00000 0.05 0.13 Q17 1 0.5516 0.3989 0.8002 11.00000 0.05 0.13 Q18 1 0.3011 0.4457 0.4926 11.00000 0.05 0.13 Q19 1 0.2773 0.4743 0.3634 11.00000 0.05 0.13 Q20 1 0.4555 0.1346 0.5392 11.00000 0.05 0.12 ; _shelx_res_checksum 38455 _shelx_hkl_file ; 0 0 2 1021.80 23.60 0 0 2 944.71 21.00 0 0 -2 935.71 21.90 0 0 -2 972.50 22.00 0 0 3 0.50 2.40 0 0 3 -1.50 2.30 0 0 -3 0.40 2.20 0 0 -3 0.60 1.80 0 0 -4 29.80 4.70 0 0 -4 36.00 4.50 0 0 4 29.40 3.90 0 0 4 31.20 4.70 0 0 -5 -1.40 3.60 0 0 5 2.00 3.80 0 0 -5 3.50 3.60 0 0 5 -0.30 3.80 0 0 6 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5 14.90 3.40 1 5 -5 13.60 4.70 1 5 -5 8.00 4.10 -1 -5 5 13.40 5.20 1 -5 -5 15.80 5.50 -1 -5 5 10.90 4.00 1 5 -4 46.10 5.90 -1 5 4 56.39 4.30 -1 5 4 56.29 7.10 1 5 -4 54.89 5.50 -1 5 4 52.09 4.50 1 -5 -4 49.40 6.40 -1 -5 4 47.90 5.50 -1 -5 4 58.19 6.90 1 5 -3 3.80 2.90 -1 5 3 1.50 3.30 1 5 -3 4.80 3.90 -1 5 3 3.10 1.90 -1 5 3 5.70 1.90 -1 -5 3 2.70 3.10 1 -5 -3 3.50 3.60 -1 -5 3 4.20 3.90 -1 5 2 112.89 4.20 -1 5 2 103.29 7.80 1 5 -2 101.19 6.20 1 5 -2 108.39 7.50 -1 5 2 104.99 4.20 1 -5 -2 101.49 8.10 -1 -5 2 99.59 6.00 -1 -5 2 109.19 7.80 1 5 -1 141.79 6.60 -1 5 1 149.88 4.50 1 5 -1 130.79 7.50 -1 5 1 143.79 8.50 -1 5 1 143.89 4.50 -1 -5 1 138.89 6.50 -1 -5 1 147.39 8.30 1 -5 -1 138.09 8.70 1 5 0 402.76 11.70 -1 5 0 397.46 14.50 -1 5 0 404.26 9.80 1 5 0 413.16 13.30 -1 -5 0 396.06 11.70 1 -5 0 415.76 14.80 1 -5 0 399.36 9.90 -1 -5 0 398.96 13.50 -1 5 -1 1728.03 36.10 1 5 1 1701.93 39.30 -1 5 -1 1703.93 41.10 1 5 1 1747.53 37.30 1 -5 1 1724.13 36.00 -1 -5 -1 1743.63 39.60 -1 -5 -1 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9 41.30 9.90 -1 -5 -9 39.70 7.20 1 5 10 47.90 9.60 1 5 10 51.39 9.20 -1 5 -10 52.49 9.20 1 -5 10 32.70 10.00 -1 -5 -10 54.19 8.70 1 5 11 93.19 12.10 -1 5 -11 113.89 11.40 1 -5 11 82.09 13.80 1 5 12 12.20 6.10 1 5 12 0.30 6.80 -1 5 -12 6.10 6.10 -1 -5 -12 8.30 5.90 1 -5 12 -6.10 8.60 1 6 -11 7.10 5.70 -1 6 11 1.10 6.30 -1 -6 11 -12.50 6.90 1 -6 -11 6.60 5.30 1 6 -10 36.90 7.90 -1 6 10 23.70 9.90 1 -6 -10 33.60 6.90 -1 -6 10 9.50 8.40 1 6 -9 11.20 5.70 -1 6 9 9.10 5.10 -1 6 9 6.10 5.90 1 -6 -9 8.30 4.60 -1 -6 9 7.20 7.60 -1 6 8 13.80 4.70 -1 6 8 9.40 4.60 1 6 -8 10.60 5.40 -1 -6 8 12.10 7.50 1 -6 -8 15.20 6.40 -1 6 7 19.30 5.00 -1 6 7 20.00 4.60 1 6 -7 14.80 6.00 1 -6 -7 13.70 6.40 -1 -6 7 18.40 7.30 -1 6 6 102.89 6.80 -1 6 6 120.69 7.90 1 6 -6 124.99 9.30 -1 -6 6 119.49 10.90 1 -6 -6 121.99 10.50 -1 6 5 90.49 5.90 1 6 -5 90.69 8.50 -1 6 5 82.79 6.00 1 6 -5 96.89 8.60 -1 -6 5 83.79 9.10 -1 -6 5 76.89 6.80 1 -6 -5 92.29 9.00 -1 6 4 14.70 4.60 -1 6 4 6.60 2.60 1 6 -4 2.80 4.10 -1 6 4 9.10 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69.89 11.30 2 -5 12 56.19 13.20 -2 6 11 71.89 13.20 2 6 -11 74.09 11.00 2 -6 -11 51.59 8.20 -2 -6 11 57.59 11.70 -2 6 10 20.10 7.60 2 6 -10 24.50 7.40 2 -6 -10 14.00 5.10 -2 -6 10 13.40 10.40 2 6 -9 145.29 11.70 2 -6 -9 156.98 13.70 -2 -6 9 136.29 13.50 2 -6 -9 152.58 10.00 2 6 -8 20.30 6.30 -2 6 8 20.50 4.60 2 -6 -8 24.70 8.00 -2 -6 8 22.40 7.70 2 -6 -8 27.00 6.20 2 6 -7 5.00 4.90 -2 6 7 8.70 3.80 2 -6 -7 8.40 4.00 2 -6 -7 7.90 6.00 -2 -6 7 5.20 6.10 -2 6 6 -1.70 2.70 -2 6 6 0.70 3.00 2 6 -6 -6.00 3.90 2 -6 -6 -1.50 4.50 -2 -6 6 7.10 6.30 2 6 -5 47.90 7.00 2 6 -5 40.10 7.00 -2 6 5 47.90 4.20 -2 6 5 41.60 4.40 -2 -6 5 46.60 6.70 2 -6 -5 45.90 8.60 2 6 -4 -3.20 3.10 -2 6 4 0.00 1.80 -2 6 4 -2.50 3.90 -2 6 4 2.80 3.00 2 6 -4 3.10 3.60 -2 -6 4 0.40 3.00 2 -6 -4 7.30 4.60 -2 -6 4 -1.20 4.70 -2 6 3 42.90 2.40 2 6 -3 47.10 5.60 -2 6 3 49.20 7.20 -2 6 3 43.80 2.50 2 6 -3 43.10 5.70 -2 -6 3 39.60 5.30 -2 -6 3 51.39 6.80 2 6 -2 -0.60 3.10 2 6 -2 -1.20 2.90 -2 6 2 2.80 3.70 -2 -6 2 0.20 2.80 2 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6.10 4.60 2 6 6 8.80 4.40 2 -6 6 11.30 7.90 -2 -6 -6 11.70 5.70 2 -6 6 0.90 3.80 2 6 7 0.60 4.50 -2 6 -7 -0.40 3.90 2 6 7 -2.80 4.00 2 -6 7 0.30 6.60 2 6 8 48.90 8.90 2 6 8 34.10 7.70 -2 6 -8 35.10 6.90 2 -6 8 35.50 10.60 2 6 9 3.40 5.00 -2 6 -9 -1.10 4.60 2 6 9 1.10 4.70 2 -6 9 -7.90 7.00 -2 6 -10 4.30 5.00 2 6 10 9.00 5.40 2 6 10 7.30 6.20 2 -6 10 -4.40 8.70 2 6 11 1.80 5.90 2 6 11 3.40 6.60 -2 6 -11 9.50 6.40 2 -6 11 -19.10 7.30 -2 7 11 12.20 5.50 -2 7 11 9.50 7.40 2 7 -11 7.10 6.00 -2 -7 11 -8.40 8.10 2 7 -10 50.39 9.30 -2 7 10 39.80 10.30 -2 7 10 54.99 7.90 -2 -7 10 45.00 12.00 2 7 -9 23.00 6.50 -2 7 9 15.80 5.00 -2 -7 9 -0.20 8.00 2 -7 -9 17.20 11.90 -2 7 8 6.20 3.80 2 7 -8 5.80 5.20 2 -7 -8 8.10 6.20 -2 -7 8 0.80 6.90 -2 7 7 21.90 4.70 -2 7 7 21.40 4.20 2 7 -7 11.40 5.30 2 -7 -7 18.00 7.10 -2 -7 7 20.70 7.60 2 7 -6 19.20 6.20 -2 7 6 22.70 4.20 -2 7 6 17.30 3.60 2 -7 -6 22.10 7.20 -2 -7 6 27.00 8.10 -2 7 5 27.30 3.70 2 7 -5 41.10 6.80 -2 7 5 33.70 3.90 -2 -7 5 40.60 8.20 2 -7 -5 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319.97 7.60 4 -3 -1 308.67 8.10 -4 -3 1 324.37 11.70 -4 3 0 26.30 5.50 4 3 0 27.90 4.90 4 -3 0 25.40 3.10 -4 -3 0 26.80 4.80 4 -3 0 20.00 2.70 4 -3 0 17.70 5.10 4 3 1 36.00 2.00 4 3 1 41.60 2.00 4 3 1 40.70 5.60 -4 3 -1 50.39 6.80 -4 -3 -1 46.50 5.40 4 -3 1 35.90 4.10 4 -3 1 47.50 6.60 4 3 2 0.00 3.50 -4 3 -2 2.50 2.50 4 3 2 2.60 2.10 -4 3 -2 5.60 4.30 4 3 2 -1.60 1.60 -4 -3 -2 -1.00 3.10 4 -3 2 -2.60 2.40 4 -3 2 -3.10 2.80 4 -3 2 2.00 4.40 -4 3 -3 112.79 8.40 4 3 3 117.79 7.50 4 3 3 123.79 6.10 -4 3 -3 122.09 6.60 4 3 3 119.29 6.10 4 3 3 115.69 7.80 4 -3 3 111.49 6.40 4 -3 3 116.39 9.00 4 3 4 42.70 6.40 4 3 4 43.90 4.80 4 3 4 39.40 4.70 -4 3 -4 46.10 6.90 -4 3 -4 50.59 6.10 4 3 4 35.80 5.90 4 -3 4 43.40 7.10 4 -3 4 44.20 5.50 4 3 5 153.08 10.10 -4 3 -5 178.98 9.70 4 3 5 159.58 8.90 -4 3 -5 161.18 10.90 4 3 5 165.38 9.00 4 3 5 158.48 9.40 4 -3 5 173.68 10.40 4 -3 5 165.98 11.10 -4 3 -6 6.70 4.50 4 3 6 8.50 4.30 4 3 6 10.80 4.20 4 3 6 6.10 4.70 4 -3 6 8.40 4.20 4 -3 6 2.90 5.50 4 3 7 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310.37 9.30 -4 4 -2 311.67 9.90 4 4 2 313.27 9.10 4 -4 2 299.67 9.80 -4 -4 -2 314.07 12.60 4 -4 2 292.07 13.60 4 4 3 63.09 6.30 -4 4 -3 62.69 7.40 -4 4 -3 73.59 5.40 4 4 3 59.39 4.60 4 4 3 67.89 6.00 4 4 3 64.69 4.80 4 -4 3 60.09 7.50 4 -4 3 68.79 5.30 4 4 4 5.00 3.40 -4 4 -4 5.70 3.40 4 4 4 8.00 3.00 -4 4 -4 1.30 4.10 4 4 4 6.40 2.80 4 4 4 10.10 4.20 4 -4 4 7.60 5.40 4 -4 4 7.20 3.10 -4 4 -5 -0.90 3.00 4 4 5 -0.40 3.40 4 4 5 1.10 4.10 4 4 5 -3.00 2.80 4 4 5 2.50 3.00 4 -4 5 -2.70 3.30 4 -4 5 0.80 5.20 4 4 6 45.90 6.10 4 4 6 51.49 7.00 -4 4 -6 46.00 6.50 4 4 6 44.80 7.60 4 -4 6 52.59 9.10 4 -4 6 44.40 6.40 -4 4 -7 8.40 4.80 4 4 7 2.70 5.10 4 4 7 8.90 4.30 4 4 7 4.20 4.40 4 -4 7 4.60 6.60 -4 4 -8 294.97 15.00 4 4 8 287.27 15.30 4 4 8 296.47 16.40 4 -4 8 244.38 16.80 -4 4 -9 18.50 6.60 4 4 9 26.50 7.20 4 4 9 24.20 7.90 4 -4 9 22.90 9.10 4 4 10 -0.40 5.40 -4 4 -10 -1.90 4.30 4 4 10 2.90 6.20 4 -4 10 -9.80 7.80 -4 4 -11 0.50 4.70 4 4 11 12.40 7.90 4 4 11 -2.60 6.60 4 -4 11 4.60 9.10 4 5 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1208.78 28.20 -4 5 2 1208.78 33.20 4 5 -2 1211.68 30.40 -4 -5 2 1181.68 30.50 -4 -5 2 1264.87 28.10 4 -5 -2 1200.88 34.10 -4 5 1 14.40 4.80 4 5 -1 17.00 2.80 4 5 -1 15.50 4.00 -4 -5 1 20.00 4.20 4 -5 -1 15.00 5.20 -4 -5 1 15.40 2.70 4 5 0 275.37 8.20 4 5 0 273.47 11.10 -4 5 0 271.07 12.90 4 -5 0 287.47 13.60 -4 -5 0 284.77 11.60 4 5 1 36.10 3.40 -4 5 -1 45.90 7.20 4 5 1 43.10 6.00 -4 -5 -1 50.79 6.40 4 -5 1 41.90 7.90 -4 -5 -1 46.80 3.80 4 -5 1 42.10 3.30 4 -5 1 47.80 3.20 -4 5 -2 3.90 2.30 4 5 2 6.40 3.60 4 5 2 6.40 2.60 -4 5 -2 8.30 5.00 4 -5 2 9.60 5.00 -4 -5 -2 11.50 4.00 -4 -5 -2 4.80 2.30 4 -5 2 5.20 2.40 4 5 3 149.99 7.00 4 5 3 152.38 8.70 4 5 3 130.89 8.60 -4 5 -3 150.88 7.20 4 5 3 128.99 7.00 4 -5 3 152.38 10.60 -4 -5 -3 130.09 8.80 4 -5 3 148.79 7.10 4 5 4 549.74 19.10 4 5 4 563.54 17.30 -4 5 -4 578.14 17.30 4 5 4 550.04 16.80 4 5 4 518.35 18.30 4 -5 4 540.25 16.70 4 -5 4 561.24 21.60 4 5 5 332.07 13.70 -4 5 -5 355.66 13.60 4 5 5 342.07 15.10 4 5 5 340.17 13.40 4 -5 5 315.77 17.00 4 -5 5 346.77 13.50 -4 5 -6 2.40 3.90 4 5 6 -0.60 3.50 4 5 6 0.00 4.50 4 -5 6 -0.20 6.20 4 5 7 75.19 9.70 4 5 7 55.79 7.50 4 5 7 72.99 7.70 -4 5 -7 74.69 7.90 4 -5 7 73.29 11.40 -4 5 -8 186.58 12.60 4 5 8 170.28 12.00 4 5 8 165.58 13.10 4 -5 8 151.28 14.80 4 5 9 -5.20 5.00 4 5 9 5.60 5.20 -4 5 -9 4.70 5.20 4 -5 9 0.00 8.20 4 5 10 2.50 5.00 -4 5 -10 7.00 5.50 4 5 10 -2.60 5.40 4 -5 10 -9.30 7.80 -4 5 -11 3.10 4.70 4 5 11 7.00 6.30 4 5 11 -6.90 5.40 4 -5 11 -17.80 6.80 -4 6 11 95.99 14.80 4 6 -11 107.39 11.90 4 -6 -11 101.69 9.20 -4 -6 11 92.79 14.00 4 6 -10 -5.00 5.50 4 -6 -10 -2.10 3.70 -4 -6 10 -9.30 5.60 4 -6 -10 -9.30 5.30 4 6 -9 20.80 7.20 -4 -6 9 12.10 7.70 4 -6 -9 12.00 4.60 4 6 -8 -2.30 4.90 -4 -6 8 -7.50 5.60 4 -6 -8 1.40 3.10 4 -6 -8 -2.60 5.20 -4 6 7 31.50 4.60 4 6 -7 28.70 7.30 4 -6 -7 27.30 7.80 4 -6 -7 29.90 4.60 -4 -6 7 29.20 8.10 4 6 -6 137.89 10.30 -4 6 6 135.39 6.70 4 6 -6 167.88 11.40 -4 -6 6 165.88 11.50 4 -6 -6 146.89 6.80 4 -6 -6 149.69 12.40 4 6 -5 6.10 4.90 4 -6 -5 3.00 5.00 -4 -6 5 1.40 4.70 4 6 -4 79.69 7.70 4 6 -4 69.39 6.60 -4 -6 4 70.09 7.30 4 -6 -4 68.49 8.90 4 6 -3 44.00 5.40 4 6 -3 54.49 6.90 4 -6 -3 50.29 8.30 -4 -6 3 55.19 6.80 -4 -6 3 49.10 6.00 4 6 -2 243.88 9.80 4 6 -2 249.78 11.30 4 -6 -2 252.87 13.80 -4 -6 2 255.57 9.90 -4 -6 2 246.58 11.30 4 6 -1 328.97 11.00 4 6 -1 355.76 13.30 -4 -6 1 339.67 13.40 -4 -6 1 329.97 10.90 4 -6 -1 332.97 15.90 4 6 0 23.80 4.80 4 6 0 31.40 4.00 4 -6 0 16.90 6.10 -4 -6 0 28.30 3.80 4 6 1 172.18 9.40 4 6 1 180.98 7.60 -4 -6 -1 170.68 9.90 4 -6 1 183.28 5.50 4 -6 1 189.88 12.20 -4 -6 -1 197.28 7.90 4 -6 1 187.08 6.30 4 6 2 62.99 6.40 4 6 2 53.29 4.90 -4 6 -2 58.89 4.20 4 -6 2 51.79 4.10 4 -6 2 61.69 9.00 -4 -6 -2 57.79 6.40 -4 -6 -2 59.29 5.30 4 6 3 12.10 4.50 -4 6 -3 18.90 3.80 4 6 3 20.80 6.30 4 6 3 18.40 3.80 4 -6 3 15.90 3.50 4 -6 3 13.90 6.50 -4 -6 -3 19.50 4.30 4 6 4 35.90 5.40 -4 6 -4 45.50 5.70 4 6 4 38.40 6.70 4 6 4 50.49 5.80 4 -6 4 20.80 7.50 4 -6 4 38.20 5.20 -4 6 -5 369.66 14.30 4 6 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9.70 4 7 -5 101.69 8.80 4 -7 -5 95.89 10.90 4 7 -4 155.28 9.80 4 7 -4 163.18 11.20 4 -7 -4 159.18 13.10 -4 -7 4 164.48 10.30 4 7 -3 88.99 7.40 4 7 -3 98.79 8.30 -4 -7 3 102.89 8.00 4 -7 -3 89.09 10.20 4 7 -2 5.30 4.10 4 7 -2 11.50 4.00 -4 -7 2 3.70 3.70 4 -7 -2 10.70 6.10 -4 -7 2 6.90 4.10 4 7 -1 202.08 9.20 4 7 -1 205.08 12.30 -4 -7 1 215.38 9.30 -4 -7 1 190.28 10.70 4 -7 -1 198.48 13.30 4 7 0 -0.80 3.20 -4 -7 0 -1.10 3.30 4 -7 0 -5.60 4.80 -4 -7 0 -0.70 2.90 4 7 1 64.09 5.90 -4 -7 -1 71.19 6.10 -4 -7 -1 63.29 6.60 4 -7 1 64.89 9.60 4 7 2 222.78 9.70 4 7 2 234.78 11.50 -4 -7 -2 242.28 10.40 -4 -7 -2 227.68 12.20 4 -7 2 226.98 14.60 4 7 3 40.40 6.50 4 7 3 44.40 5.40 -4 7 -3 42.60 4.50 4 -7 3 42.10 4.70 -4 -7 -3 46.90 6.20 4 -7 3 25.70 7.90 4 7 4 188.28 9.60 -4 7 -4 182.88 8.90 4 7 4 174.58 11.20 4 -7 4 156.38 14.50 4 -7 4 175.18 8.60 -4 -7 -4 174.58 10.20 -4 7 -5 130.29 8.50 4 7 5 119.99 9.60 4 7 5 152.38 10.20 4 7 5 138.19 9.60 4 -7 5 141.99 13.50 4 -7 5 109.89 8.20 4 7 6 65.99 9.10 4 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215.38 12.00 -5 4 4 235.78 7.90 5 4 -4 233.78 9.90 5 4 -4 252.77 11.70 5 -4 -4 227.28 12.70 5 -4 -4 230.98 8.00 -5 -4 4 231.98 11.10 -5 -4 4 236.08 9.80 -5 4 3 8.00 4.20 -5 4 3 15.40 2.40 5 4 -3 18.80 4.60 -5 -4 3 14.00 4.40 -5 -4 3 16.40 3.30 5 -4 -3 13.90 5.20 5 -4 -3 15.70 2.40 5 4 -2 512.05 16.80 -5 4 2 508.95 18.30 -5 4 2 526.85 12.40 -5 -4 2 521.15 13.10 5 -4 -2 522.05 12.70 5 -4 -2 513.05 18.80 5 4 -1 3.60 3.60 -5 -4 1 1.20 3.20 5 -4 -1 1.20 1.60 5 -4 -1 -0.90 3.80 5 -4 -1 2.40 1.50 5 4 0 90.39 7.00 5 -4 0 83.99 4.10 5 -4 0 87.19 4.30 5 -4 0 81.99 7.90 -5 -4 0 77.29 6.60 -5 4 -1 40.70 6.60 5 4 1 36.70 5.50 5 -4 1 37.00 3.70 -5 -4 -1 43.40 6.70 5 -4 1 36.00 3.50 5 -4 1 33.40 6.30 -5 4 -2 -5.20 3.80 5 4 2 0.30 3.40 5 4 2 0.20 1.40 5 4 2 -0.40 1.30 5 -4 2 0.30 2.60 5 -4 2 -1.50 4.10 -5 -4 -2 2.80 3.40 5 -4 2 -2.00 2.10 5 4 3 305.37 9.60 5 4 3 284.87 12.40 -5 4 -3 270.67 13.80 5 -4 3 289.87 10.80 5 -4 3 302.67 11.80 5 -4 3 285.57 14.30 -5 -4 -3 285.07 13.30 5 4 4 237.68 12.90 5 4 4 204.38 11.60 5 4 4 202.88 8.80 -5 4 -4 218.88 10.10 5 4 4 208.38 9.00 5 -4 4 207.78 9.90 5 -4 4 199.18 12.60 5 4 5 154.88 10.90 5 4 5 159.18 8.90 5 4 5 178.08 9.30 -5 4 -5 172.98 10.00 5 -4 5 167.78 12.40 5 -4 5 159.78 9.10 5 4 6 255.77 12.40 -5 4 -6 266.67 12.80 5 4 6 259.57 12.10 5 4 6 277.77 14.70 5 -4 6 252.77 15.70 5 4 7 32.40 6.80 5 4 7 48.70 8.60 -5 4 -7 45.30 7.60 5 4 7 51.99 6.50 5 -4 7 39.50 10.10 -5 4 -8 161.58 11.60 5 4 8 163.68 11.80 5 4 8 144.69 12.60 5 -4 8 136.09 13.80 5 4 9 4.20 5.10 5 4 9 -0.40 6.70 -5 4 -9 1.30 5.00 5 -4 9 -11.60 6.10 5 4 10 2.00 6.30 5 4 10 1.90 5.80 -5 4 -10 3.80 5.30 5 -4 10 -8.40 7.40 5 4 11 13.20 7.30 -5 4 -11 11.60 6.10 5 4 11 13.20 7.70 5 -4 11 -10.00 8.20 5 5 -12 19.80 7.40 -5 5 12 1.80 6.50 5 -5 -12 23.00 5.80 -5 -5 12 3.90 7.40 -5 5 11 -5.30 4.80 5 5 -11 4.60 5.90 5 -5 -11 3.70 4.40 -5 -5 11 -8.10 5.80 5 5 -10 37.30 8.60 5 -5 -10 36.70 9.50 5 -5 -10 37.60 6.50 -5 -5 10 18.90 8.00 5 5 -9 2.40 5.80 5 -5 -9 6.60 4.10 -5 -5 9 3.90 6.10 5 -5 -9 -3.30 4.90 5 5 -8 161.08 12.30 -5 5 8 145.99 8.70 -5 -5 8 167.38 12.10 5 -5 -8 158.18 13.60 5 -5 -8 162.68 9.20 -5 5 7 22.80 4.40 5 5 -7 31.20 7.30 5 -5 -7 30.50 4.80 -5 -5 7 29.70 6.60 5 -5 -7 32.50 8.30 5 5 -6 17.30 4.90 5 5 -6 13.30 5.80 -5 5 6 9.60 3.30 5 -5 -6 20.20 3.70 5 -5 -6 15.60 6.60 -5 -5 6 16.70 5.50 5 5 -5 248.58 11.70 5 5 -5 273.77 13.40 -5 5 5 257.37 8.60 5 -5 -5 262.77 8.80 -5 -5 5 271.57 12.30 5 -5 -5 289.37 15.60 -5 5 4 297.87 8.30 5 5 -4 288.37 11.50 5 5 -4 285.47 13.10 5 -5 -4 292.87 15.30 -5 -5 4 302.27 11.80 5 -5 -4 285.27 8.20 5 5 -3 55.29 4.70 5 5 -3 48.80 6.60 -5 5 3 51.99 2.30 -5 -5 3 60.59 7.30 5 -5 -3 52.19 8.20 5 -5 -3 55.69 2.30 -5 -5 3 56.39 5.10 5 5 -2 73.09 7.70 5 5 -2 81.09 4.60 -5 5 2 74.29 7.30 -5 -5 2 78.89 6.90 5 -5 -2 74.19 8.20 -5 -5 2 84.49 4.70 5 5 -1 20.70 2.20 -5 5 1 20.80 5.50 5 5 -1 26.60 5.00 5 -5 -1 15.60 5.40 -5 -5 1 17.70 2.20 -5 -5 1 17.90 4.60 -5 5 0 4.40 4.20 5 5 0 3.70 3.60 5 -5 0 -2.00 3.90 5 -5 0 1.30 1.30 5 -5 0 2.60 1.40 -5 -5 0 1.00 3.10 5 5 1 7.90 4.10 -5 5 -1 15.40 5.70 5 5 1 10.00 1.40 5 5 1 11.60 1.40 5 -5 1 6.30 2.40 5 -5 1 8.60 2.40 5 -5 1 8.10 5.20 -5 -5 -1 1.90 3.50 5 5 2 28.50 2.90 5 -5 2 27.30 4.20 5 -5 2 25.20 6.40 5 -5 2 32.10 4.00 -5 -5 -2 17.00 4.90 5 5 3 214.68 11.00 5 5 3 252.57 11.50 5 5 3 235.58 12.00 5 5 3 229.58 8.60 -5 5 -3 225.08 9.30 5 -5 3 232.78 9.50 5 -5 3 226.78 10.10 5 -5 3 224.88 13.70 -5 -5 -3 215.08 12.00 5 5 4 694.33 23.20 5 5 4 689.43 19.50 -5 5 -4 727.93 20.70 5 5 4 708.03 19.40 5 -5 4 712.23 20.40 5 -5 4 720.23 25.60 -5 5 -5 124.59 8.40 5 5 5 143.29 11.10 5 5 5 137.69 8.50 5 5 5 134.69 8.20 5 -5 5 130.09 12.10 5 -5 5 133.79 8.70 -5 5 -6 213.48 11.80 5 5 6 233.58 11.50 5 5 6 216.68 11.50 5 5 6 212.78 13.70 5 -5 6 217.78 15.30 5 5 7 43.70 7.30 5 5 7 48.30 8.60 -5 5 -7 56.29 7.90 5 -5 7 40.90 10.20 -5 5 -8 199.38 12.80 5 5 8 182.28 13.60 5 5 8 166.48 11.80 -5 5 -9 12.90 5.80 5 5 9 10.30 6.10 5 5 9 1.40 5.90 5 -5 9 0.10 8.30 -5 5 -10 34.30 7.60 5 5 10 26.50 8.00 5 5 10 25.40 8.20 5 -5 10 9.80 10.90 5 6 -11 13.00 7.20 -5 6 11 13.90 7.80 5 -6 -11 13.90 5.20 -5 -6 11 5.70 7.70 5 -6 -11 9.50 7.40 5 6 -10 4.80 5.90 5 -6 -10 15.70 4.70 -5 -6 10 7.90 7.50 5 -6 -10 12.80 6.70 -5 6 9 -4.60 3.50 5 6 -9 0.10 5.10 5 -6 -9 -1.20 5.30 -5 -6 9 -1.30 6.60 5 -6 -9 5.50 3.70 5 6 -8 -0.40 5.10 -5 6 8 -0.70 3.60 5 -6 -8 -3.00 5.30 -5 -6 8 5.10 6.30 5 -6 -8 3.80 3.40 -5 6 7 3.10 3.00 5 6 -7 5.20 5.60 5 -6 -7 1.30 2.70 -5 -6 7 3.80 5.80 5 -6 -7 7.30 5.90 5 6 -6 105.09 8.90 5 6 -6 106.89 10.00 -5 6 6 98.79 5.60 5 -6 -6 98.69 5.70 5 -6 -6 96.09 11.10 5 6 -5 896.11 27.10 5 6 -5 833.92 25.20 -5 6 5 851.61 19.20 5 -6 -5 859.81 19.40 -5 -6 5 870.51 25.00 5 -6 -5 871.91 30.30 5 6 -4 188.38 9.80 5 6 -4 221.98 12.50 -5 -6 4 206.68 10.30 5 -6 -4 202.58 13.60 5 6 -3 259.97 10.50 5 6 -3 282.57 13.10 -5 -6 3 271.57 10.60 5 -6 -3 268.67 15.10 5 6 -2 67.39 8.10 5 6 -2 71.99 5.00 -5 -6 2 80.99 7.40 -5 -6 2 65.49 5.10 5 -6 -2 68.09 8.70 5 6 -1 12.50 2.60 5 6 -1 15.80 4.70 -5 -6 1 11.90 4.50 5 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-10 6.20 6.10 5 -7 -10 2.00 6.60 -5 -7 10 0.70 7.00 5 -7 -10 6.30 3.60 -5 7 9 9.00 4.50 5 7 -9 24.20 7.50 -5 -7 9 15.70 8.50 5 -7 -9 24.20 8.40 5 7 -8 -2.60 5.90 -5 -7 8 12.20 7.30 5 -7 -8 17.00 3.60 5 -7 -8 10.40 7.20 -5 7 7 -1.20 2.60 5 7 -7 3.70 5.90 -5 -7 7 -3.90 5.50 5 -7 -7 -1.90 5.10 -5 7 6 5.70 2.30 -5 7 6 4.40 2.80 5 7 -6 1.20 5.00 5 7 -6 5.90 4.00 -5 -7 6 0.10 5.20 5 -7 -6 -0.80 5.70 5 7 -5 208.98 11.60 5 7 -5 227.18 13.10 -5 -7 5 210.38 12.00 5 -7 -5 209.78 15.00 5 7 -4 17.10 4.50 5 7 -4 13.60 5.80 5 -7 -4 8.70 6.30 -5 -7 4 7.10 4.60 5 7 -3 972.80 26.20 5 7 -3 1022.60 29.10 -5 -7 3 1022.70 26.10 5 -7 -3 982.30 33.10 5 7 -2 167.88 10.50 5 7 -2 162.08 8.00 5 -7 -2 161.58 12.80 -5 -7 2 180.38 8.30 5 7 -1 133.99 6.70 5 7 -1 132.89 9.40 -5 -7 1 138.09 6.90 5 -7 -1 126.99 11.60 5 7 0 19.40 5.20 5 -7 0 20.70 7.20 -5 -7 0 24.00 3.60 5 7 1 120.59 9.60 -5 -7 -1 121.69 6.50 5 -7 1 140.09 11.90 5 7 2 80.79 5.70 5 7 2 100.79 8.70 -5 -7 -2 93.59 6.30 5 -7 2 89.89 5.20 5 -7 2 86.69 6.90 5 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7.30 -6 4 5 66.99 5.20 6 -4 -5 77.59 5.70 -6 -4 5 74.29 7.40 6 -4 -5 67.69 8.70 -6 -4 5 69.59 6.80 -6 4 4 3.00 2.30 6 4 -4 7.30 4.50 6 -4 -4 5.70 2.50 6 -4 -4 7.60 4.80 -6 -4 4 3.00 3.20 -6 -4 4 5.00 3.10 6 4 -3 3.20 4.00 -6 4 3 6.70 4.00 -6 4 3 4.20 2.20 6 -4 -3 6.30 2.40 -6 -4 3 8.10 2.70 6 -4 -3 7.90 4.80 -6 -4 3 7.80 4.00 6 4 -2 382.86 16.70 -6 4 2 391.96 16.10 -6 4 2 388.86 11.70 -6 -4 2 388.86 9.50 6 -4 -2 402.36 18.80 -6 -4 2 403.76 9.70 6 -4 -2 414.36 10.70 -6 -4 2 375.16 14.90 -6 4 1 27.30 5.80 6 -4 -1 27.10 3.10 -6 -4 1 21.80 5.00 -6 4 0 10.40 4.90 6 -4 0 12.00 2.60 -6 -4 0 15.60 4.40 6 -4 0 11.30 2.70 6 4 1 90.99 7.70 -6 4 -1 80.29 8.30 6 -4 1 88.49 5.60 6 -4 1 84.49 5.20 6 -4 1 90.79 8.60 -6 -4 -1 81.39 7.30 -6 4 -2 71.69 8.10 6 4 2 68.79 7.40 6 -4 2 80.29 5.60 6 -4 2 75.59 8.30 -6 -4 -2 83.49 7.60 6 -4 2 67.19 5.90 6 4 3 24.10 3.10 6 4 3 16.10 2.70 6 4 3 16.70 5.40 6 -4 3 15.70 6.30 6 -4 3 6.00 3.90 6 -4 3 17.50 4.10 6 4 4 288.07 10.40 6 4 4 275.77 14.10 6 4 4 281.87 10.30 6 -4 4 277.07 13.20 6 -4 4 276.57 15.30 6 -4 4 263.17 12.50 6 4 5 52.49 5.90 -6 4 -5 57.29 6.50 6 4 5 55.99 5.80 6 4 5 48.60 8.20 6 -4 5 59.49 8.00 6 -4 5 46.10 9.50 6 -4 5 53.49 6.90 6 4 6 21.50 5.10 6 4 6 25.30 5.20 -6 4 -6 29.20 5.90 6 4 6 29.70 7.50 6 -4 6 30.10 8.70 -6 4 -7 41.20 7.50 6 4 7 55.89 7.00 6 4 7 33.00 7.40 6 4 7 48.60 9.00 6 -4 7 42.70 10.30 -6 4 -8 227.58 13.70 6 4 8 203.48 12.80 6 4 8 217.08 15.20 6 -4 8 205.68 16.30 6 4 9 31.40 8.40 6 4 9 17.40 6.50 6 -4 9 30.00 10.10 -6 4 -10 15.10 6.50 6 4 10 15.90 6.70 6 4 10 13.50 7.00 6 -4 10 15.90 9.60 6 5 -11 5.40 6.60 -6 5 11 6.00 7.20 6 -5 -11 8.60 4.60 -6 -5 11 -2.80 7.00 6 5 -10 4.20 6.10 6 -5 -10 9.60 4.70 6 -5 -10 2.00 6.40 -6 -5 10 -4.90 5.80 6 -5 -9 60.69 6.70 -6 -5 9 40.00 8.60 6 -5 -9 48.90 12.10 6 5 -8 15.10 6.80 -6 5 8 13.80 4.40 -6 -5 8 22.50 7.00 6 -5 -8 18.80 4.60 6 -5 -8 22.70 7.60 -6 5 7 31.70 4.90 6 5 -7 26.20 7.70 -6 -5 7 44.30 7.30 -6 -5 7 22.80 6.30 6 -5 -7 31.90 4.80 6 -5 -7 29.20 7.90 -6 5 6 753.62 19.70 6 5 -6 742.13 25.30 6 -5 -6 777.62 20.10 -6 -5 6 780.42 23.90 6 -5 -6 755.42 28.40 6 5 -5 32.80 7.10 -6 5 5 32.20 3.80 -6 -5 5 34.20 5.80 -6 -5 5 43.10 6.10 6 -5 -5 36.50 4.10 6 -5 -5 24.10 6.90 6 5 -4 285.27 13.80 -6 5 4 273.17 9.30 -6 -5 4 298.27 11.20 -6 -5 4 296.87 11.60 6 -5 -4 298.97 8.70 6 -5 -4 291.77 15.80 -6 5 3 103.89 4.20 6 5 -3 110.49 8.80 6 -5 -3 97.49 9.60 -6 -5 3 121.79 9.20 -6 -5 3 100.69 5.90 6 5 -2 31.90 6.00 6 -5 -2 28.40 2.20 -6 -5 2 31.80 2.70 6 -5 -2 32.10 6.50 -6 -5 2 30.10 3.10 6 -5 -2 30.30 2.30 6 5 -1 -1.30 3.70 6 -5 -1 0.30 1.40 6 -5 -1 -4.90 3.70 6 -5 -1 2.20 1.60 -6 -5 1 4.20 4.20 6 5 0 47.40 6.80 -6 -5 0 39.60 6.30 6 -5 0 46.50 3.50 6 -5 0 41.70 3.30 6 -5 0 42.00 7.50 6 5 1 22.90 5.60 6 -5 1 21.10 6.40 6 -5 1 18.40 3.10 6 -5 1 21.50 3.40 6 5 2 236.78 12.40 6 -5 2 240.08 9.10 6 -5 2 223.98 13.70 6 -5 2 230.68 9.50 6 5 3 63.59 4.10 6 5 3 55.89 8.00 6 5 3 63.89 5.70 6 -5 3 55.69 6.10 6 -5 3 60.79 5.50 6 -5 3 60.49 9.30 6 5 4 4.00 2.90 6 5 4 11.30 3.40 6 5 4 1.80 5.30 6 -5 4 -4.10 5.90 6 -5 4 10.50 4.30 6 5 5 511.45 20.40 6 5 5 482.45 15.90 -6 5 -5 503.45 17.70 6 5 5 501.25 15.90 6 -5 5 465.95 17.10 6 -5 5 481.25 18.60 6 -5 5 478.95 21.80 -6 5 -6 106.79 9.10 6 5 6 108.19 10.70 6 5 6 115.59 8.40 6 5 6 126.79 8.50 6 -5 6 99.59 12.30 -6 5 -7 4.30 4.60 6 5 7 10.50 6.30 6 -5 7 8.80 7.70 6 5 8 20.30 6.40 -6 5 -8 26.60 7.00 6 -5 8 31.00 10.10 6 5 9 9.80 6.60 6 5 9 3.50 5.20 6 -5 9 0.90 8.20 -6 5 -10 4.90 5.80 6 5 10 3.30 6.20 6 5 10 -2.70 5.50 6 -5 10 -9.40 8.70 -6 6 11 1.60 6.60 6 6 -11 5.20 6.10 -6 -6 11 -5.60 7.80 6 -6 -11 9.10 4.60 6 -6 -11 6.40 6.80 6 6 -10 48.30 9.50 -6 -6 10 48.90 10.50 6 -6 -10 54.89 7.30 6 -6 -10 56.09 11.10 -6 6 9 2.70 4.00 6 6 -9 9.70 6.60 -6 -6 9 10.90 6.60 6 -6 -9 3.90 6.80 6 -6 -9 10.20 4.10 -6 6 8 -3.40 3.10 6 6 -8 -2.70 5.30 -6 -6 8 0.50 5.70 6 -6 -8 -1.20 2.70 6 6 -7 71.39 10.00 -6 6 7 52.19 5.30 6 -6 -7 84.09 12.30 -6 -6 7 62.29 9.00 6 -6 -7 59.09 5.20 6 6 -6 13.70 4.20 -6 6 6 14.20 3.00 6 6 -6 15.90 6.40 6 -6 -6 21.30 7.40 -6 -6 6 13.70 5.70 6 -6 -6 17.20 3.00 -6 6 5 86.29 4.20 6 6 -5 85.79 7.20 6 6 -5 93.99 9.60 6 -6 -5 93.29 5.20 6 -6 -5 82.39 10.50 -6 -6 5 98.99 7.90 6 6 -4 127.89 10.30 6 6 -4 136.49 7.90 -6 -6 4 146.99 8.40 6 -6 -4 141.69 12.20 6 6 -3 139.79 10.20 6 6 -3 132.79 6.70 6 -6 -3 134.29 11.70 -6 -6 3 126.69 6.80 6 6 -2 0.90 4.20 6 -6 -2 -1.20 5.00 6 6 -1 4.10 4.70 6 -6 -1 6.70 6.10 6 6 0 23.10 5.90 6 -6 0 22.40 1.60 6 -6 0 22.30 1.70 6 -6 0 16.20 6.60 6 6 1 66.19 8.60 6 -6 1 53.69 4.00 6 -6 1 60.19 9.50 6 6 2 177.48 11.30 6 -6 2 178.58 13.40 6 -6 2 190.58 8.10 6 -6 2 187.38 7.70 6 6 3 472.05 18.90 6 6 3 510.45 14.40 6 6 3 508.15 12.80 6 -6 3 489.25 15.90 6 -6 3 473.35 21.50 6 -6 3 474.65 14.90 6 6 4 68.19 5.40 6 6 4 59.39 5.30 6 6 4 58.59 9.20 6 -6 4 55.49 10.10 6 -6 4 73.49 6.50 6 -6 4 67.79 7.40 6 6 5 73.99 9.60 6 6 5 61.99 6.00 -6 6 -5 63.89 6.90 6 -6 5 62.49 6.70 6 -6 5 65.99 8.20 6 -6 5 44.20 9.90 6 6 6 337.37 14.30 6 6 6 354.26 17.80 -6 6 -6 356.16 15.40 6 6 6 411.96 14.90 6 -6 6 347.17 20.10 6 6 7 75.89 8.70 6 6 7 70.09 10.10 -6 6 -7 82.69 8.70 6 -6 7 73.29 12.40 6 6 8 -6.50 5.10 6 6 8 -6.20 3.50 -6 6 -8 4.30 5.20 6 -6 8 2.80 8.00 6 6 9 5.20 5.10 -6 6 -9 6.70 5.80 6 6 9 1.10 6.30 6 -6 9 -8.40 7.90 6 7 -10 18.00 7.70 6 -7 -10 9.50 7.60 6 -7 -10 24.40 4.70 6 7 -9 34.50 8.70 -6 7 9 33.70 5.90 6 -7 -9 44.70 10.40 -6 -7 9 50.09 10.30 6 7 -8 64.09 9.90 -6 -7 8 56.79 9.60 6 -7 -8 47.80 9.70 6 -7 -8 60.09 5.00 -6 7 7 -0.50 2.20 6 7 -7 6.30 6.00 6 -7 -7 2.10 5.60 -6 -7 7 -6.40 5.30 6 -7 -7 9.40 2.30 6 7 -6 48.70 8.80 -6 7 6 35.20 2.50 6 7 -6 43.00 6.60 6 -7 -6 37.20 9.30 -6 -7 6 34.10 8.40 6 7 -5 23.20 5.10 6 7 -5 21.40 6.50 -6 -7 5 11.10 5.20 6 -7 -5 18.10 7.50 6 7 -4 4.20 3.30 6 7 -4 5.50 6.00 -6 -7 4 8.00 4.10 6 -7 -4 6.90 6.40 6 7 -3 48.00 4.90 6 7 -3 48.90 7.70 -6 -7 3 48.80 5.10 6 -7 -3 47.20 9.20 6 7 -2 4.00 4.80 -6 -7 2 7.60 2.60 6 -7 -2 4.00 6.40 6 7 -1 12.50 2.10 6 7 -1 10.10 5.20 -6 -7 1 15.50 3.10 6 -7 -1 7.80 6.80 6 7 0 3.90 4.70 6 -7 0 2.70 6.10 6 7 1 69.99 8.30 6 -7 1 68.89 2.70 6 -7 1 66.89 10.50 6 -7 1 67.59 2.70 6 7 2 55.99 8.30 6 7 2 41.80 2.80 6 7 2 48.10 2.80 6 -7 2 50.09 4.40 6 -7 2 47.60 4.10 6 -7 2 48.40 9.70 6 7 3 466.75 19.10 6 7 3 455.15 12.50 6 -7 3 439.56 13.60 6 -7 3 427.56 21.40 6 -7 3 447.46 14.40 6 7 4 13.40 3.50 6 7 4 9.80 6.30 6 7 4 25.40 3.90 6 -7 4 8.80 7.50 6 -7 4 9.70 3.90 6 -7 4 12.10 4.30 6 7 5 2.80 5.50 6 7 5 -1.80 2.80 6 -7 5 -3.50 7.90 6 -7 5 -2.80 3.60 6 -7 5 -4.50 3.70 -6 7 -6 19.50 4.80 6 7 6 4.30 3.90 6 7 6 11.40 5.90 6 -7 6 19.60 9.00 6 7 7 45.60 14.70 -6 7 -7 54.89 7.80 6 7 7 51.29 7.50 6 -7 7 48.10 11.20 6 7 8 -2.70 6.00 -6 7 -8 2.60 4.60 6 7 8 -4.50 3.90 6 -7 8 5.40 8.70 6 8 -9 -8.70 4.80 -6 8 9 0.40 2.50 6 -8 -9 5.40 6.70 -6 -8 9 -11.60 6.80 -6 8 8 -3.70 2.60 6 8 -8 10.80 6.60 -6 8 8 0.40 2.00 6 -8 -8 11.30 6.80 -6 -8 8 -5.40 6.60 6 8 -7 -1.30 6.60 6 -8 -7 7.20 7.00 -6 -8 7 -3.60 6.10 6 8 -6 36.10 8.40 -6 -8 6 34.50 7.00 6 -8 -6 49.90 10.20 6 8 -5 16.40 6.30 6 8 -5 17.70 4.90 -6 -8 5 20.70 5.50 6 8 -4 40.20 8.50 6 8 -4 41.20 5.80 6 -8 -4 51.19 10.00 -6 -8 4 40.60 5.90 6 8 -3 -10.00 3.90 6 8 -3 -1.00 2.70 6 -8 -3 0.60 5.70 -6 -8 3 5.50 3.00 6 8 -2 2.50 2.60 6 8 -2 0.60 4.80 6 -8 -2 -1.50 5.90 -6 -8 2 4.60 2.60 6 8 -1 24.60 6.40 -6 -8 1 43.20 4.10 6 -8 -1 34.50 9.00 6 8 0 -3.30 4.20 6 8 0 -2.00 1.60 6 -8 0 2.80 6.30 6 8 1 151.28 10.90 6 8 1 150.48 5.20 6 -8 1 161.78 13.90 6 8 2 47.10 3.90 6 8 2 56.89 8.30 6 -8 2 51.09 10.20 6 -8 2 49.90 3.00 6 8 3 16.80 6.00 6 8 3 23.10 3.50 6 -8 3 18.50 3.70 6 -8 3 13.20 3.20 6 -8 3 25.50 9.60 6 8 4 26.60 7.10 6 8 4 24.80 4.20 6 8 4 35.80 4.70 6 -8 4 27.50 5.00 6 -8 4 33.30 9.40 6 -8 4 25.30 4.60 6 8 5 77.59 10.20 6 8 5 105.19 6.80 6 8 5 76.09 6.70 6 -8 5 79.79 12.70 6 -8 5 77.49 7.50 6 -8 5 93.99 9.50 6 8 6 13.20 7.40 6 8 6 25.80 5.60 6 -8 6 23.80 9.40 6 -8 6 25.50 5.90 -6 8 -7 46.60 7.20 6 8 7 30.80 6.30 6 8 7 31.90 7.80 6 -8 7 31.80 10.90 6 9 -8 7.50 6.30 6 -9 -8 13.50 7.00 -6 -9 8 -0.50 6.40 6 9 -7 2.20 6.00 6 -9 -7 4.10 6.80 -6 -9 7 -3.60 5.60 6 9 -6 14.30 6.70 6 -9 -6 41.60 10.20 -6 -9 6 32.30 6.80 6 9 -5 4.70 5.90 6 9 -5 3.50 4.20 -6 -9 5 2.60 4.00 6 -9 -5 0.20 6.10 6 9 -4 40.70 8.10 6 -9 -4 50.09 10.60 -6 -9 4 50.69 6.10 6 9 -3 4.60 5.90 6 9 -3 8.10 3.60 6 -9 -3 25.20 8.30 6 9 -2 39.00 5.00 6 9 -2 32.80 7.60 -6 -9 2 50.89 5.10 6 -9 -2 29.40 8.80 6 9 -1 21.60 3.70 6 9 -1 18.90 6.30 6 -9 -1 28.60 8.40 6 9 0 183.18 12.70 -6 -9 0 242.48 8.30 6 -9 0 186.48 15.40 6 9 1 -1.50 5.00 6 -9 1 -7.20 5.20 6 9 2 2.00 2.10 6 9 2 -5.50 4.90 6 -9 2 3.20 6.80 6 9 3 10.90 5.70 6 9 3 4.00 3.50 6 9 3 15.60 3.30 6 -9 3 22.50 8.50 6 -9 3 15.60 2.70 6 9 4 9.70 6.70 6 9 4 3.80 2.90 6 -9 4 1.90 3.00 6 -9 4 6.80 7.20 6 -9 4 2.60 3.30 6 9 5 5.10 3.50 6 9 5 0.30 4.90 6 -9 5 6.70 4.80 6 -9 5 14.60 8.10 6 9 6 2.70 3.90 6 9 6 -4.90 4.90 6 -9 6 6.00 8.00 6 -9 6 12.10 4.80 6 10 -6 6.10 6.40 -6 -10 6 20.60 5.30 6 -10 -6 7.10 6.40 6 10 -5 8.40 6.80 6 -10 -5 12.50 7.30 -6 -10 5 18.80 4.80 6 -10 -4 46.30 10.60 6 10 -3 107.29 10.50 6 10 -3 89.29 7.80 6 -10 -3 136.49 14.20 6 10 -2 8.80 5.70 6 10 -2 5.90 3.60 6 -10 -2 13.40 8.00 6 10 -1 0.50 3.10 6 10 -1 6.10 6.20 6 -10 -1 12.80 7.70 6 10 0 4.30 5.00 6 10 0 -0.50 2.80 6 -10 0 11.10 8.20 6 10 1 -6.00 4.80 6 10 1 -6.00 4.00 6 -10 1 12.40 7.80 6 10 2 5.10 5.80 6 10 2 2.80 2.40 6 -10 2 22.20 8.20 6 10 3 41.40 8.30 6 10 3 28.70 4.10 6 -10 3 43.00 10.30 6 10 4 8.10 3.40 6 -10 4 -2.00 2.60 6 -10 4 16.70 8.70 6 -11 -1 18.10 7.90 6 11 0 3.20 6.10 6 -11 0 23.70 8.90 -7 0 12 -2.70 6.20 7 0 -12 1.00 5.10 7 0 -11 1.70 5.20 -7 0 11 2.60 6.70 7 0 -10 -0.60 5.50 -7 0 10 2.90 5.50 -7 0 9 -3.70 4.40 7 0 -9 -7.40 4.50 -7 0 8 3.50 5.50 7 0 -8 -3.00 4.60 7 0 -7 3.70 4.70 -7 0 7 15.40 5.60 7 0 -6 806.02 24.30 -7 0 6 849.81 26.00 -7 0 6 792.62 26.10 -7 0 5 -2.10 2.80 -7 0 5 -0.70 3.20 7 0 -5 2.10 3.50 7 0 -5 0.60 3.90 7 0 -4 194.08 10.30 -7 0 4 193.88 10.90 -7 0 4 203.68 10.10 7 0 -4 185.28 9.70 7 0 -3 -0.80 3.10 -7 0 3 1.60 2.80 7 0 -3 1.40 2.90 -7 0 3 -1.80 2.60 -7 0 2 0.70 2.80 -7 0 2 2.80 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3.20 7 -6 -8 10.40 6.40 7 6 -7 49.00 8.90 -7 6 7 33.40 4.60 7 -6 -7 42.80 4.60 7 -6 -7 40.10 9.70 -7 -6 7 40.60 7.80 7 6 -6 81.19 10.30 -7 6 6 74.59 5.20 7 -6 -6 79.59 11.90 7 -6 -6 94.09 5.30 -7 -6 6 95.99 9.00 7 6 -5 69.29 9.20 -7 -6 5 89.79 8.00 -7 -6 5 79.39 7.40 7 -6 -5 65.49 10.70 7 -6 -5 67.39 3.90 7 6 -4 10.90 6.00 -7 -6 4 24.20 4.50 7 -6 -4 18.30 1.40 7 -6 -4 16.10 7.00 -7 -6 4 14.80 4.10 7 6 -3 12.30 5.90 7 -6 -3 14.40 6.80 -7 -6 3 15.10 3.40 -7 -6 3 21.00 3.30 7 6 -2 -0.40 4.50 7 -6 -2 1.10 5.40 7 6 -1 29.40 6.60 7 -6 -1 21.30 7.10 7 6 0 58.59 8.50 7 -6 0 43.80 8.90 7 -6 0 60.99 3.50 7 6 1 23.30 6.20 7 -6 1 26.80 3.50 7 -6 1 19.70 7.20 7 -6 1 25.40 3.60 7 6 2 -4.30 4.80 7 -6 2 -5.10 5.60 7 -6 2 -0.90 2.90 7 -6 2 4.90 2.90 7 6 3 195.08 12.80 7 -6 3 180.48 14.10 7 -6 3 179.78 8.90 7 -6 3 192.68 9.70 7 6 4 16.60 3.30 7 6 4 24.90 4.30 7 6 4 18.40 6.90 7 -6 4 21.50 5.30 7 -6 4 10.80 7.40 7 -6 4 27.00 4.90 7 6 5 38.30 4.90 7 6 5 36.90 8.20 7 -6 5 45.70 10.50 7 -6 5 36.10 7.10 7 6 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7.10 7 -7 3 10.60 3.50 7 -7 3 7.00 3.50 7 7 4 9.40 2.40 7 7 4 10.10 6.10 7 -7 4 12.80 4.10 7 7 5 52.79 5.20 7 7 5 75.19 5.20 7 7 5 52.09 9.20 7 -7 5 54.39 11.10 7 -7 5 56.09 7.20 7 7 6 1.40 3.60 7 7 6 6.50 6.20 7 -7 6 15.00 5.90 7 -7 6 5.60 8.50 7 7 7 1.70 4.00 7 7 7 12.40 7.60 7 -7 7 20.00 6.40 7 -7 7 13.00 10.00 7 7 8 20.50 7.50 7 7 8 9.80 5.40 7 -7 8 -1.00 7.60 7 -7 8 12.30 5.90 7 8 -8 13.00 7.50 -7 -8 8 0.80 6.60 7 -8 -8 16.50 8.10 7 8 -7 9.10 6.50 -7 -8 7 -9.10 5.00 7 -8 -7 2.90 6.60 7 8 -5 15.40 6.70 7 -8 -5 15.50 7.30 7 8 -4 7.90 6.80 7 -8 -4 16.20 7.90 -7 -8 4 19.10 3.80 7 8 -3 30.30 7.60 -7 -8 3 27.50 3.60 7 8 -2 64.19 9.00 7 -8 -2 58.49 10.70 7 8 -1 34.90 7.80 7 -8 -1 46.50 9.60 7 8 0 10.50 5.70 7 -8 0 12.20 7.50 7 8 1 8.80 6.10 7 8 2 4.90 5.70 7 -8 2 1.90 1.90 7 -8 2 6.00 6.70 7 8 3 30.10 7.50 7 -8 3 29.60 4.20 7 -8 3 36.70 9.80 7 -8 3 35.50 4.40 7 8 4 -0.10 5.40 7 -8 4 -1.40 3.30 7 -8 4 2.70 6.90 7 -8 4 -2.90 3.20 7 8 5 63.19 5.10 7 8 5 51.19 4.90 7 8 5 50.39 11.00 7 -8 5 67.99 12.40 7 -8 5 39.50 6.30 7 -8 5 52.89 7.00 7 8 6 6.70 3.80 7 8 6 9.30 6.40 7 -8 6 13.70 8.90 7 -8 6 6.00 5.30 7 8 7 -6.00 3.50 7 8 7 0.50 6.90 7 -8 7 1.00 4.90 7 -8 7 -3.40 7.20 7 9 -7 4.80 6.10 7 -9 -7 10.40 7.30 -7 -9 7 7.90 5.70 7 9 -6 7.60 6.70 -7 -9 6 17.30 5.30 7 -9 -6 18.80 7.50 7 9 -5 59.79 9.90 7 -9 -5 54.49 10.70 -7 -9 5 64.89 6.40 7 9 -4 137.59 13.80 7 -9 -4 144.39 14.60 -7 -9 4 155.08 7.70 7 9 -3 4.90 6.60 7 -9 -3 9.30 6.90 7 9 -2 58.89 9.30 7 -9 -2 50.19 9.90 7 9 -1 24.30 7.30 7 -9 -1 38.20 9.40 7 9 0 101.09 10.90 7 -9 0 138.79 14.10 7 9 1 54.99 8.70 7 -9 1 47.30 10.40 7 9 2 -1.20 5.10 7 -9 2 7.00 7.30 7 9 3 -5.30 4.80 7 -9 3 18.50 8.10 7 9 4 20.60 7.00 7 -9 4 11.20 3.80 7 -9 4 23.90 9.00 7 9 5 168.68 14.00 7 9 5 150.38 6.90 7 -9 5 198.98 18.00 7 10 -5 30.30 8.30 7 -10 -5 46.50 10.60 7 10 -4 140.49 12.50 7 -10 -4 167.88 15.90 7 10 -3 1.50 5.70 7 -10 -3 18.50 7.30 7 10 -2 -1.70 5.30 7 -10 -2 16.70 8.40 7 10 -1 42.70 9.40 7 -10 -1 38.20 10.00 7 -10 0 22.80 8.00 7 10 1 1.50 6.10 7 -10 1 7.10 6.80 7 10 2 0.80 5.40 7 -10 2 8.80 7.50 7 10 3 8.70 6.50 7 -10 3 15.30 8.40 8 0 -12 90.59 12.20 -8 0 12 61.39 12.20 -8 0 11 -4.10 6.10 8 0 -11 2.40 5.50 -8 0 10 3.90 5.90 8 0 -10 -0.50 5.60 8 0 -9 -3.40 4.90 -8 0 9 -0.30 5.10 -8 0 8 46.80 9.20 8 0 -8 45.40 7.80 -8 0 7 4.00 5.10 8 0 -7 3.60 4.90 8 0 -6 495.05 19.60 -8 0 6 481.45 18.70 8 0 -6 502.75 18.40 8 0 -5 -1.90 4.40 -8 0 5 1.20 3.40 8 0 -5 -1.80 3.20 8 0 -4 21.40 5.30 -8 0 4 13.60 4.30 8 0 -4 19.80 5.00 -8 0 4 22.80 5.10 -8 0 3 -0.90 2.70 -8 0 3 2.40 3.40 8 0 -3 -0.30 3.60 8 0 -3 -2.80 2.90 -8 0 2 1482.95 35.10 8 0 -2 1459.75 35.40 8 0 -2 1496.05 36.20 -8 0 2 1416.16 36.30 8 0 -1 -0.90 2.90 -8 0 1 3.70 3.20 8 0 -1 1.50 3.40 -8 0 1 -3.10 2.90 -8 0 0 179.68 9.90 -8 0 0 173.18 8.70 8 0 0 176.88 9.90 8 0 0 180.18 8.90 -8 0 -1 0.30 3.10 8 0 1 -5.70 2.70 -8 0 -1 4.30 3.50 -8 0 -2 67.49 6.20 8 0 2 65.89 6.70 -8 0 -2 76.09 7.50 8 0 2 73.59 7.70 8 0 2 69.59 6.70 -8 0 -3 -0.40 3.60 8 0 3 -4.40 3.50 8 0 3 -1.00 4.20 -8 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1 -4 23.30 5.60 -8 1 4 19.90 4.60 8 1 -4 21.80 4.90 -8 -1 4 28.20 4.90 8 -1 -4 21.00 5.50 8 -1 -4 26.90 5.00 8 1 -3 6.30 4.20 -8 1 3 4.50 3.10 8 1 -3 5.00 3.10 8 -1 -3 4.40 4.00 -8 -1 3 6.50 3.00 -8 -1 3 6.10 3.90 8 -1 -3 4.10 3.50 8 1 -2 36.10 6.10 -8 1 2 33.90 5.20 8 1 -2 36.40 4.80 -8 1 2 33.80 5.50 -8 -1 2 29.50 5.50 8 -1 -2 39.50 6.10 8 -1 -2 27.90 4.80 -8 -1 2 34.60 4.40 8 1 -1 67.89 7.80 8 1 -1 51.59 4.70 -8 1 1 51.39 5.70 -8 1 1 55.89 5.80 -8 -1 1 54.29 4.90 8 -1 -1 55.39 5.90 8 -1 -1 55.19 6.40 -8 -1 1 56.39 6.30 8 1 0 27.10 5.50 -8 1 0 21.30 5.30 8 1 0 26.70 4.00 -8 -1 0 23.10 3.80 8 -1 0 21.30 4.90 8 -1 0 24.90 5.00 -8 -1 0 18.00 4.80 -8 1 -1 23.40 5.30 -8 1 -1 36.10 5.90 8 1 1 32.20 6.20 8 1 1 24.50 4.00 8 -1 1 22.40 4.90 -8 -1 -1 24.40 5.40 -8 -1 -1 26.60 4.00 8 -1 1 18.20 5.00 8 1 2 6.80 4.50 8 1 2 4.20 3.10 -8 1 -2 4.10 4.00 8 -1 2 3.00 3.80 -8 -1 -2 7.00 3.30 8 -1 2 6.70 4.20 8 -1 2 6.40 3.80 8 1 3 47.20 7.70 8 1 3 44.30 5.60 -8 1 -3 45.40 8.00 8 -1 3 53.09 7.70 8 -1 3 47.80 7.30 -8 -1 -3 46.40 5.50 8 1 4 5.20 4.40 8 1 4 -0.20 5.10 -8 1 -4 0.10 4.10 -8 -1 -4 -2.20 3.30 8 -1 4 6.50 5.10 8 1 5 44.20 8.20 8 1 5 45.10 7.00 8 -1 5 35.90 7.80 8 -1 5 45.50 7.90 8 1 6 96.19 9.40 8 1 6 97.49 10.50 8 -1 6 101.79 10.40 8 -1 6 95.19 10.40 -8 -1 -6 105.59 8.90 8 1 7 -5.30 5.40 8 1 7 2.10 5.80 8 -1 7 8.80 6.00 8 -1 7 0.50 6.70 8 1 8 6.30 6.60 8 1 8 -0.90 6.10 8 -1 8 2.40 6.60 8 1 9 11.60 7.60 8 1 9 10.40 7.00 8 -1 9 18.50 8.10 8 -1 9 7.70 7.90 8 1 10 25.10 11.00 8 1 10 13.40 8.50 8 -1 10 2.90 7.70 8 -1 10 24.00 8.90 8 2 -12 3.70 6.20 -8 2 12 11.40 8.10 -8 -2 12 8.60 7.20 8 -2 -12 10.10 6.20 -8 2 11 -3.60 6.10 8 2 -11 3.00 7.40 -8 -2 11 4.10 6.60 8 2 -10 31.00 8.20 -8 2 10 27.80 8.80 8 -2 -10 49.20 8.50 -8 -2 10 43.50 9.20 8 2 -9 -4.50 5.20 -8 2 9 6.10 6.20 8 -2 -9 0.70 5.50 -8 -2 9 -8.00 3.70 8 -2 -9 4.50 4.80 8 2 -8 18.50 7.00 8 -2 -8 31.40 7.90 8 -2 -8 16.10 6.10 -8 -2 8 22.60 6.50 8 -2 -7 1284.87 34.30 -8 -2 7 1278.17 36.60 8 -2 -7 1272.97 39.00 -8 -2 7 1278.97 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283.57 9.40 8 -2 2 280.37 13.70 8 -2 2 268.07 12.10 8 -2 2 262.57 12.60 8 2 3 204.08 12.50 8 2 3 208.28 8.90 -8 2 -3 191.98 11.50 8 -2 3 182.58 10.30 8 -2 3 175.58 10.80 8 -2 3 209.38 12.10 -8 -2 -3 191.08 8.70 8 2 4 3.00 3.90 8 2 4 8.30 5.50 8 -2 4 7.70 5.20 -8 -2 -4 9.20 3.50 8 -2 4 5.20 6.10 8 2 5 90.19 10.10 8 2 5 95.89 8.30 8 -2 5 77.79 9.30 8 -2 5 90.29 10.70 -8 -2 -5 82.69 7.30 8 2 6 -5.70 4.20 8 2 6 1.40 5.60 8 -2 6 -1.70 6.10 -8 -2 -6 0.10 3.80 8 -2 6 -5.20 5.60 8 2 7 1.10 5.60 8 2 7 6.90 6.00 8 -2 7 -7.10 6.60 8 -2 7 1.60 5.30 8 2 8 17.00 6.70 8 2 8 17.40 7.60 8 -2 8 13.20 9.00 8 2 9 63.99 11.20 8 2 9 66.29 10.60 8 -2 9 74.89 11.20 8 -2 9 64.39 12.60 8 2 10 -4.40 6.50 8 2 10 0.10 6.60 8 -2 10 -7.80 9.00 8 -2 10 4.40 6.70 8 3 -12 12.60 7.50 -8 3 12 -0.30 7.70 -8 -3 12 -1.40 7.00 8 -3 -12 2.30 5.40 8 3 -11 7.60 7.00 -8 3 11 15.90 8.10 8 -3 -11 8.90 5.90 -8 -3 11 6.30 6.40 8 3 -10 16.10 7.20 -8 3 10 25.40 8.80 -8 -3 10 13.40 7.00 8 -3 -10 19.40 8.60 8 -3 -10 26.30 6.70 8 -3 -9 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-8 15.90 7.00 -8 -4 8 20.70 6.70 8 -4 -8 4.20 6.30 8 -4 -8 19.90 5.10 -8 4 7 97.19 7.90 8 4 -7 117.89 11.20 8 -4 -7 116.69 11.80 -8 -4 7 110.09 9.50 -8 -4 7 150.08 10.30 8 -4 -7 101.49 9.30 8 4 -6 23.40 6.20 -8 4 6 17.90 4.30 -8 -4 6 22.80 5.40 8 -4 -6 22.10 4.80 8 -4 -6 28.00 7.90 -8 -4 6 37.30 6.20 8 4 -5 47.30 8.20 -8 4 5 52.39 5.70 8 -4 -5 56.49 5.70 8 -4 -5 58.19 9.40 -8 -4 5 54.79 5.80 -8 -4 5 71.39 7.00 -8 4 4 60.09 5.50 8 4 -4 67.89 8.80 8 -4 -4 67.79 9.00 -8 -4 4 59.79 5.30 8 -4 -4 58.99 5.60 -8 -4 4 66.29 5.80 -8 4 3 78.09 5.70 8 4 -3 85.59 8.90 -8 -4 3 80.59 4.20 8 -4 -3 80.09 5.80 8 -4 -3 81.79 9.20 -8 4 2 29.50 4.40 8 4 -2 27.90 6.30 8 -4 -2 37.10 4.60 8 -4 -2 30.60 7.20 8 4 -1 -4.90 4.00 8 -4 -1 2.70 2.90 8 -4 -1 4.10 5.70 8 -4 -1 2.20 2.70 8 4 0 8.00 5.20 8 -4 0 3.10 2.90 8 -4 0 2.60 5.30 8 -4 0 2.70 3.00 8 4 1 82.09 8.80 8 -4 1 82.39 6.80 8 -4 1 86.69 6.30 8 -4 1 69.69 8.80 8 4 2 292.67 15.10 8 -4 2 297.17 15.90 8 -4 2 317.67 12.40 8 -4 2 289.97 12.50 8 4 3 14.00 6.10 8 4 3 7.10 1.50 8 -4 3 8.60 3.70 8 -4 3 9.00 5.50 8 -4 3 7.50 6.10 8 4 4 190.38 13.30 8 4 4 197.68 8.00 8 4 4 223.48 10.60 8 -4 4 188.28 11.30 8 -4 4 196.78 14.10 8 4 5 34.50 7.90 8 4 5 28.00 4.90 8 4 5 37.70 4.80 8 -4 5 33.60 7.40 8 -4 5 40.70 10.10 8 4 6 78.29 11.00 8 4 6 64.19 7.00 8 -4 6 63.89 9.00 8 -4 6 58.19 10.70 8 4 7 -1.70 5.50 8 -4 7 5.60 5.50 8 4 8 18.70 6.30 8 4 8 40.00 9.20 8 -4 8 24.40 9.50 8 4 9 -1.10 5.80 8 4 9 4.90 6.80 8 -4 9 -4.40 8.20 8 -4 9 8.50 6.10 -8 5 11 164.48 17.10 8 5 -11 163.08 14.90 8 -5 -11 165.68 16.00 -8 -5 11 168.68 15.30 8 5 -10 12.60 7.50 -8 -5 10 2.90 6.50 8 -5 -10 26.40 5.60 8 -5 -10 21.60 8.60 8 5 -9 72.09 11.40 -8 -5 9 66.39 9.80 8 -5 -9 92.99 8.00 8 -5 -9 78.69 13.00 8 5 -8 1.10 6.00 -8 5 8 2.10 4.00 8 -5 -8 9.20 6.60 -8 -5 8 2.90 5.20 8 -5 -8 7.40 3.80 -8 5 7 5.10 3.90 8 5 -7 3.20 5.50 -8 -5 7 2.50 4.80 8 -5 -7 8.30 3.70 8 -5 -7 8.90 6.50 8 5 -6 15.80 6.70 -8 5 6 8.20 3.60 8 -5 -6 14.40 4.00 -8 -5 6 10.10 4.70 8 -5 -6 6.30 6.50 -8 -5 6 23.80 4.90 8 5 -5 27.00 7.40 -8 5 5 22.90 3.90 -8 -5 5 43.80 6.20 8 -5 -5 21.30 3.80 -8 -5 5 26.60 5.00 8 -5 -5 19.90 7.30 -8 5 4 1.10 2.40 8 5 -4 0.70 5.20 8 -5 -4 -1.20 2.50 8 -5 -4 -2.30 5.00 -8 -5 4 1.30 2.60 -8 -5 4 -1.30 2.90 -8 5 3 196.08 8.00 8 5 -3 235.48 13.40 8 -5 -3 206.38 7.80 8 -5 -3 213.48 14.50 8 5 -2 13.90 5.90 8 -5 -2 9.20 6.30 8 -5 -2 13.50 3.10 8 -5 -2 12.40 2.90 8 5 -1 98.99 9.70 8 -5 -1 102.29 5.80 8 -5 -1 104.69 5.70 8 -5 -1 95.99 10.40 8 5 0 92.99 9.40 8 -5 0 92.69 5.90 8 -5 0 95.39 6.00 8 -5 0 86.19 10.30 8 5 1 23.10 6.40 8 -5 1 24.10 4.00 8 -5 1 14.40 6.60 8 -5 1 19.40 4.30 8 5 2 124.59 11.00 8 -5 2 132.19 7.50 8 -5 2 137.59 8.50 8 -5 2 136.49 12.10 8 5 3 -0.60 4.90 8 -5 3 1.20 2.60 8 -5 3 1.90 6.30 8 -5 3 2.30 3.90 8 5 4 3.90 5.40 8 -5 4 -0.90 6.50 8 -5 4 1.70 4.40 8 -5 4 9.70 4.30 8 5 5 -1.80 4.80 8 5 5 1.10 3.00 8 -5 5 3.10 5.40 8 -5 5 5.80 7.30 8 -5 6 5.90 5.10 8 5 7 0.40 4.30 8 5 7 3.00 6.40 8 -5 7 13.20 6.20 8 -5 7 4.10 7.60 8 5 8 60.29 8.60 8 5 8 84.19 11.80 8 -5 8 60.49 12.00 8 5 9 2.30 5.80 8 5 9 15.60 8.10 8 -5 9 8.80 5.70 8 -5 9 -5.70 8.10 8 6 -10 13.60 7.70 8 -6 -10 19.90 4.50 8 -6 -10 9.00 7.00 -8 -6 10 -0.40 7.00 8 6 -9 29.90 8.50 8 -6 -9 29.60 5.00 8 -6 -9 30.20 9.20 -8 -6 9 20.20 7.30 8 6 -8 47.00 9.60 8 -6 -8 67.49 5.80 8 -6 -8 54.99 11.20 -8 -6 8 55.29 9.10 8 6 -7 17.00 7.20 -8 6 7 -1.00 3.00 8 -6 -7 10.20 3.20 -8 -6 7 -0.50 5.00 8 -6 -7 8.70 7.00 -8 6 6 17.90 3.50 8 6 -6 25.60 7.40 8 -6 -6 17.00 7.80 -8 -6 6 21.30 5.80 8 6 -5 -3.30 5.30 8 -6 -5 1.70 1.90 -8 -6 5 -0.60 3.70 8 -6 -5 5.60 6.50 8 6 -4 11.90 6.30 -8 -6 4 10.50 3.10 8 -6 -4 10.80 6.70 8 6 -3 190.58 12.50 8 -6 -3 166.68 5.00 8 -6 -3 177.68 6.30 8 -6 -3 156.08 13.30 8 6 -2 17.00 6.30 8 -6 -2 17.90 2.80 8 -6 -2 19.40 7.50 8 -6 -2 15.50 1.90 8 6 -1 3.40 5.40 8 -6 -1 -0.40 2.90 8 -6 -1 2.00 6.10 8 -6 -1 9.90 2.00 8 6 0 31.40 7.30 8 -6 0 40.20 3.70 8 -6 0 39.30 8.90 8 -6 0 35.60 3.90 8 6 1 62.49 9.00 8 -6 1 62.69 5.00 8 -6 1 62.89 10.40 8 -6 1 60.59 5.20 8 6 2 -0.80 5.00 8 -6 2 0.10 2.60 8 -6 2 -0.40 6.80 8 -6 2 0.00 3.20 8 6 3 25.30 7.40 8 -6 3 47.80 6.40 8 -6 3 32.70 8.80 8 -6 3 28.90 5.60 8 6 4 -5.80 5.20 8 -6 4 0.80 3.90 8 -6 4 1.80 6.70 8 -6 4 9.30 4.00 8 6 5 7.40 2.90 8 -6 5 10.90 8.70 8 -6 5 8.30 4.80 8 6 6 26.40 7.70 8 -6 6 21.30 6.60 8 -6 6 16.60 8.50 8 6 7 66.39 10.90 8 6 7 62.09 7.20 8 -6 7 74.39 12.70 8 -6 7 83.49 10.90 8 6 8 4.70 6.70 8 -6 8 4.40 8.10 8 -6 8 9.60 7.30 8 7 -9 25.00 8.30 8 -7 -9 33.50 9.70 -8 -7 9 12.60 7.60 8 7 -8 87.19 12.00 -8 7 8 58.09 6.80 8 -7 -8 70.09 12.20 8 -7 -8 95.99 5.50 -8 -7 8 64.49 9.80 8 7 -7 24.80 8.60 8 -7 -7 41.00 3.30 -8 -7 7 17.90 6.60 8 -7 -7 17.90 7.90 8 7 -6 8.40 6.40 8 -7 -6 0.40 6.00 -8 -7 6 -4.50 4.40 8 7 -5 6.10 6.80 -8 -7 5 3.70 3.60 8 -7 -5 11.70 6.90 8 7 -4 24.10 7.50 -8 -7 4 33.30 3.50 8 -7 -4 22.30 8.20 8 7 -3 4.70 5.70 8 -7 -3 6.70 6.40 8 7 -2 28.40 7.20 8 -7 -2 27.70 8.50 8 7 -1 64.29 9.30 8 -7 -1 51.19 9.90 8 7 0 11.40 6.30 8 -7 0 7.50 6.80 8 7 1 75.29 10.00 8 -7 1 75.89 4.30 8 -7 1 71.69 11.50 8 7 2 2.50 5.70 8 -7 2 7.00 2.90 8 -7 2 1.60 3.00 8 -7 2 4.50 6.20 8 7 3 20.40 7.90 8 -7 3 19.90 4.10 8 -7 3 20.50 4.60 8 -7 3 21.70 8.20 8 -7 4 156.58 8.90 8 -7 4 163.68 14.80 8 7 5 7.10 6.50 8 -7 5 12.50 8.60 8 -7 5 10.40 5.10 8 7 6 30.80 8.30 8 -7 6 22.10 6.30 8 -7 6 36.00 10.20 8 7 7 -1.70 6.70 8 -7 7 12.90 8.40 8 -7 7 0.80 5.30 8 8 -8 14.80 7.40 8 -8 -8 18.80 7.40 8 8 -7 13.70 7.20 8 -8 -7 38.20 9.60 -8 -8 7 9.40 5.80 8 8 -6 -6.80 5.30 -8 -8 6 -4.70 3.60 8 -8 -6 -2.50 6.10 8 8 -5 1.90 6.10 -8 -8 5 13.40 3.40 8 -8 -5 9.60 6.70 8 8 -4 80.79 12.50 8 -8 -4 83.09 12.70 -8 -8 4 96.19 4.70 8 8 -3 3.10 5.60 8 -8 -3 16.90 8.20 8 8 -2 2.60 5.60 8 -8 -2 8.40 6.60 8 8 -1 -6.20 5.10 8 -8 -1 7.00 7.30 8 8 0 9.40 6.30 8 -8 0 5.90 6.60 8 8 1 -2.90 6.20 8 -8 1 -4.50 6.20 8 8 2 68.59 10.60 8 -8 2 67.49 4.30 8 -8 2 64.39 11.50 8 8 3 7.80 6.80 8 -8 3 -4.20 2.70 8 -8 3 0.70 3.10 8 -8 3 6.40 6.60 8 8 4 -2.60 5.40 8 -8 4 1.90 7.10 8 -8 4 -5.70 3.50 8 8 5 156.18 13.50 8 -8 5 134.59 9.80 8 -8 5 154.68 15.10 8 8 6 0.00 5.80 8 -8 6 -2.00 4.50 8 -8 6 -2.00 7.00 8 9 -6 16.00 7.90 -8 -9 6 22.00 4.70 8 -9 -6 22.10 8.20 8 9 -5 35.50 8.50 8 -9 -5 36.30 9.40 8 9 -4 9.70 6.70 8 -9 -4 17.30 7.80 8 9 -3 10.80 6.90 8 -9 -3 18.50 7.60 8 9 -2 8.20 6.20 8 -9 -2 15.40 6.90 8 9 -1 -3.10 5.20 8 -9 -1 10.40 7.20 8 9 0 -2.30 5.60 8 -9 0 11.80 7.80 8 9 1 1.70 5.60 8 -9 1 8.00 7.40 8 9 2 1.80 5.70 8 -9 2 7.00 7.00 8 9 3 -1.60 6.20 8 -9 3 6.60 6.70 8 9 4 15.20 7.80 8 -9 4 33.20 9.10 8 -9 4 10.20 4.10 8 10 -3 58.79 10.20 8 10 -2 5.10 6.40 8 -10 -2 44.10 11.00 8 10 -1 1.40 6.00 8 -10 -1 1.30 6.50 8 10 0 8.80 6.50 8 -10 0 24.90 8.90 8 10 1 4.80 6.90 8 -10 1 25.70 9.50 -9 0 12 2.80 7.40 9 0 -12 2.20 6.30 -9 0 11 6.70 6.30 9 0 -11 2.60 5.90 9 0 -10 8.00 7.10 -9 0 10 -2.90 5.40 9 0 -9 -2.10 5.10 -9 0 9 0.00 5.00 9 0 -8 636.74 23.80 -9 0 8 677.93 26.50 9 0 -7 1.80 5.20 9 0 -7 -0.60 4.50 -9 0 7 -0.50 4.50 9 0 -6 95.39 9.10 9 0 -6 84.59 8.70 -9 0 5 2.30 3.60 9 0 -5 -1.40 4.50 9 0 -5 0.30 4.70 9 0 -4 289.47 13.40 -9 0 4 271.67 12.70 9 0 -4 294.27 13.40 -9 0 3 3.60 3.30 9 0 -3 -1.00 3.40 9 0 -3 6.60 4.80 9 0 -2 335.37 14.10 -9 0 2 308.97 15.20 9 0 -2 329.57 13.20 -9 0 2 329.27 12.80 -9 0 1 -3.70 3.10 9 0 -1 -0.30 3.50 9 0 -1 2.60 4.20 -9 0 1 -0.40 3.70 9 0 0 359.06 13.70 -9 0 0 363.56 13.60 9 0 0 366.96 15.10 9 0 1 -3.20 3.90 9 0 1 -3.50 3.40 -9 0 -1 0.60 3.90 -9 0 -2 993.70 27.40 9 0 2 1027.40 30.10 9 0 2 1005.10 27.40 9 0 3 0.50 4.10 -9 0 -3 -0.10 3.80 9 0 3 -3.80 4.40 9 0 4 4.90 4.90 9 0 4 17.30 6.90 -9 0 -4 -0.10 4.30 9 0 5 -1.00 4.90 9 0 5 -6.60 5.50 -9 0 -5 -3.00 4.00 9 0 6 93.99 10.80 9 0 6 80.39 9.90 9 0 7 -4.00 5.90 9 0 8 31.80 8.90 9 0 8 14.60 7.50 9 0 9 4.10 7.20 9 0 9 -8.30 7.10 -9 1 11 17.50 8.30 9 1 -11 33.90 8.50 9 -1 -11 24.10 7.40 -9 -1 11 12.20 7.90 9 1 -10 -3.00 5.50 -9 1 10 5.10 7.30 9 -1 -10 1.30 5.30 -9 -1 10 2.10 5.90 -9 1 9 -1.70 5.70 9 1 -9 2.80 6.20 -9 -1 9 -2.70 4.70 9 -1 -9 5.20 5.40 9 1 -8 11.40 6.40 -9 1 8 7.20 6.00 -9 -1 8 14.20 6.50 9 -1 -8 16.60 6.50 9 -1 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5.70 -9 -4 5 2.50 3.10 9 -4 -5 5.00 5.70 -9 -4 5 5.00 3.20 9 -4 -5 3.80 3.80 9 4 -4 246.18 14.30 -9 4 4 257.17 10.90 9 -4 -4 263.87 10.90 -9 -4 4 276.97 9.60 -9 -4 4 263.17 9.60 9 -4 -4 267.87 15.90 -9 4 3 96.29 6.90 9 4 -3 90.69 9.90 -9 -4 3 97.39 3.80 9 -4 -3 104.89 7.10 -9 -4 3 96.49 3.70 9 -4 -3 105.19 10.60 9 4 -2 65.09 9.10 -9 4 2 77.19 6.20 9 -4 -2 60.89 5.90 9 -4 -2 60.89 9.30 9 4 -1 24.40 7.00 9 -4 -1 26.40 4.60 9 -4 -1 29.30 7.50 9 -4 -1 26.50 4.90 9 4 0 28.30 7.30 9 -4 0 27.00 4.90 9 -4 0 21.10 7.60 9 -4 0 24.60 4.60 9 4 1 13.30 6.30 9 -4 1 24.10 5.10 9 -4 1 10.90 7.20 9 4 2 250.47 14.80 9 -4 2 259.57 11.70 9 -4 2 240.78 14.90 9 4 3 5.20 5.90 9 -4 3 4.90 4.30 9 -4 3 11.10 7.10 9 4 4 105.69 5.20 9 4 4 116.29 11.50 9 -4 4 111.29 10.00 9 -4 4 101.19 11.20 9 4 5 15.50 4.00 9 4 5 21.90 7.90 9 -4 5 8.90 5.20 9 -4 5 21.30 8.30 9 4 6 10.50 4.90 9 4 6 21.30 7.50 9 -4 6 19.60 8.20 9 -4 6 18.50 7.40 9 4 7 37.30 9.40 9 -4 7 44.80 10.20 9 -4 7 47.80 9.30 9 4 8 35.30 9.40 9 4 8 28.50 7.40 9 -4 8 47.00 10.50 9 -4 8 48.20 9.30 9 5 -10 50.19 10.60 9 -5 -10 65.49 7.70 -9 -5 10 37.40 8.90 9 -5 -10 52.59 11.70 9 5 -9 18.80 7.50 -9 -5 9 13.00 6.80 9 -5 -9 18.80 5.10 9 -5 -9 14.20 7.50 9 5 -8 77.29 11.30 -9 -5 8 102.29 9.70 9 -5 -8 103.39 7.80 9 -5 -8 96.79 12.10 9 5 -7 10.10 6.70 -9 5 7 -5.90 3.30 9 -5 -7 5.40 3.50 9 -5 -7 15.40 8.80 9 5 -6 109.99 11.40 -9 5 6 99.69 7.20 9 -5 -6 117.79 7.40 -9 -5 6 122.99 8.50 9 -5 -6 121.29 12.70 9 5 -5 18.90 7.10 -9 5 5 1.40 3.10 9 -5 -5 3.40 5.30 -9 -5 5 4.80 3.60 9 -5 -5 6.10 3.30 -9 5 4 1.60 2.60 9 5 -4 0.70 5.40 9 -5 -4 -4.20 5.20 9 -5 -4 -2.90 2.70 -9 -5 4 -6.70 3.30 -9 -5 4 6.40 2.30 -9 5 3 3.50 2.80 9 5 -3 -0.50 5.30 9 -5 -3 0.10 2.70 9 -5 -3 -7.00 4.50 9 5 -2 82.19 10.10 9 -5 -2 64.09 5.30 9 -5 -2 61.09 9.80 9 -5 -2 73.09 5.30 9 5 -1 47.10 8.40 9 -5 -1 34.80 4.60 9 -5 -1 45.70 4.60 9 -5 -1 42.80 9.10 9 5 0 -1.60 5.30 9 -5 0 5.80 3.00 9 -5 0 1.10 3.10 9 -5 0 -0.50 5.60 9 5 1 161.28 12.10 9 -5 1 138.99 7.80 9 -5 1 135.49 12.40 9 -5 1 115.09 7.80 9 5 2 48.20 8.90 9 -5 2 49.99 5.60 9 -5 2 40.20 6.20 9 -5 2 42.50 8.90 9 5 3 -1.80 5.60 9 -5 3 6.70 3.80 9 -5 3 5.70 6.90 9 -5 3 0.00 4.60 9 5 4 6.60 5.80 9 -5 4 11.20 7.10 9 -5 4 5.20 5.00 9 5 5 -4.80 4.80 9 5 5 0.10 2.30 9 -5 5 2.20 5.30 9 5 6 73.59 11.20 9 5 6 50.49 6.10 9 -5 6 75.39 12.00 9 -5 6 61.89 9.50 9 5 7 1.30 4.70 9 5 7 9.40 7.00 9 -5 7 9.20 6.60 9 -5 7 13.40 8.70 9 5 8 2.80 5.80 9 5 8 17.10 8.30 9 -5 8 20.20 10.00 9 -5 8 24.80 7.80 9 6 -9 3.80 6.70 -9 -6 9 -8.40 6.10 9 -6 -9 7.40 6.80 9 -6 -9 12.70 3.90 -9 6 8 -2.40 3.90 9 6 -8 16.70 7.60 -9 -6 8 8.60 6.20 9 -6 -8 20.50 7.40 9 -6 -8 21.40 4.00 -9 6 7 2.70 3.20 9 6 -7 10.00 6.70 9 -6 -7 14.20 3.20 9 -6 -7 2.90 6.40 -9 6 6 -0.80 2.80 9 6 -6 -5.20 5.60 9 -6 -6 7.90 2.60 -9 -6 6 -1.00 4.10 9 -6 -6 6.40 6.60 -9 6 5 4.70 2.60 -9 -6 5 3.20 3.60 9 -6 -5 5.40 6.50 9 -6 -5 12.70 2.70 9 6 -4 4.80 6.00 9 -6 -4 6.10 6.30 9 -6 -4 5.30 2.20 9 6 -3 252.67 14.90 9 -6 -3 246.88 7.70 9 -6 -3 258.77 16.90 9 6 -2 44.90 8.60 9 -6 -2 49.99 3.90 9 -6 -2 58.09 10.20 9 6 -1 64.49 9.50 9 -6 -1 75.99 4.60 9 -6 -1 54.99 10.20 9 -6 -1 65.99 4.60 9 6 0 14.80 6.40 9 -6 0 13.50 3.00 9 -6 0 7.40 6.10 9 -6 0 7.10 3.10 9 6 1 4.50 6.10 9 -6 1 6.30 3.30 9 -6 1 7.70 6.80 9 6 2 0.10 5.50 9 -6 2 4.90 3.00 9 -6 2 1.80 3.60 9 -6 2 -0.40 6.60 9 6 3 7.40 6.00 9 -6 3 22.00 3.90 9 -6 3 15.30 7.80 9 6 4 51.59 10.10 9 -6 4 39.50 9.60 9 -6 4 53.29 7.50 9 6 5 129.59 12.80 9 -6 5 107.99 9.60 9 -6 5 124.39 13.50 9 6 6 39.70 9.20 9 6 6 30.60 4.20 9 -6 6 40.90 7.80 9 -6 6 31.20 10.70 9 6 7 4.10 6.30 9 -6 7 13.60 9.80 9 -6 7 6.70 5.50 9 7 -8 -1.90 6.40 9 -7 -8 11.20 7.30 -9 7 7 13.80 3.40 9 7 -7 23.70 8.70 9 -7 -7 22.70 8.50 9 7 -6 103.09 11.70 9 -7 -6 110.59 13.00 -9 -7 6 93.79 7.50 9 7 -5 -0.70 5.40 -9 -7 5 7.50 2.70 9 -7 -5 6.90 7.10 9 7 -4 -0.50 6.00 9 -7 -4 27.90 9.30 9 -7 -3 71.49 11.70 9 7 -2 106.79 11.20 9 -7 -2 122.59 15.20 9 7 -1 148.49 12.40 9 7 0 98.39 10.90 9 -7 0 105.39 16.20 9 -7 0 96.49 4.00 9 7 1 81.79 12.00 9 -7 1 103.09 12.20 9 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-9 -1 32.80 9.80 9 9 0 20.50 8.70 9 -9 0 32.90 9.40 9 9 1 -5.50 5.60 9 -9 1 16.10 7.80 9 9 2 103.19 12.90 9 -9 2 119.09 14.10 -10 0 11 4.50 7.20 10 0 -11 0.40 5.30 10 0 -10 5.00 6.10 -10 0 10 6.80 8.20 10 0 -9 -0.30 5.20 -10 0 9 0.70 5.30 -10 0 8 767.82 28.90 10 0 -7 -1.50 5.70 -10 0 7 1.10 5.30 10 0 -7 -5.00 4.60 10 0 -6 1.50 5.20 10 0 -6 2.60 4.90 10 0 -5 -1.00 4.00 10 0 -5 0.80 4.80 -10 0 5 10.20 4.00 10 0 -4 206.38 11.80 -10 0 4 202.68 11.00 10 0 -4 203.68 12.00 -10 0 3 -3.90 3.30 10 0 -3 -1.20 3.90 10 0 -3 0.50 4.70 -10 0 2 238.88 11.60 10 0 -2 241.98 11.60 10 0 -2 231.58 12.70 10 0 -1 -0.40 4.50 10 0 -1 0.50 3.60 -10 0 1 -4.30 4.20 10 0 0 700.23 23.20 10 0 0 698.83 21.20 -10 0 0 656.53 20.70 10 0 1 1.80 4.10 10 0 1 3.00 5.00 -10 0 -1 -0.50 4.20 10 0 2 1099.09 29.80 -10 0 -2 1085.19 29.90 10 0 2 1084.59 32.60 10 0 3 1.40 5.30 10 0 3 -0.20 4.10 -10 0 -3 -3.40 3.40 -10 0 -4 1.70 4.50 10 0 4 -1.10 5.30 10 0 4 9.40 5.10 10 0 5 5.20 6.00 10 0 5 9.50 5.50 10 0 6 6.50 5.60 10 0 6 5.80 7.20 10 0 7 -2.90 6.00 10 0 7 -4.00 5.50 10 0 8 0.70 7.10 10 0 8 21.20 8.00 10 1 -11 15.50 7.80 -10 1 11 6.10 7.40 10 -1 -11 11.10 6.70 -10 -1 11 2.30 6.10 -10 1 10 1.20 6.10 10 1 -10 3.40 5.80 -10 -1 10 9.30 6.80 10 -1 -10 3.10 5.90 -10 1 9 1.40 5.50 10 1 -9 3.00 6.30 -10 -1 9 -5.10 5.30 10 -1 -9 4.70 5.10 10 1 -8 9.10 6.10 10 -1 -8 4.50 5.50 -10 -1 8 5.30 5.50 10 -1 -8 3.40 5.80 10 1 -7 51.59 8.70 -10 -1 7 42.30 8.20 10 -1 -7 34.20 7.70 10 -1 -7 60.69 10.20 10 1 -6 11.30 5.90 -10 -1 6 1.20 4.30 -10 -1 6 17.60 4.40 10 -1 -6 8.70 5.60 10 -1 -6 2.00 4.70 10 1 -5 11.50 4.90 10 1 -5 7.90 6.30 10 -1 -5 2.80 5.10 10 -1 -5 11.20 5.60 -10 -1 5 14.10 4.60 10 1 -4 125.09 10.40 10 1 -4 130.49 9.20 -10 1 4 125.89 9.50 -10 -1 4 123.39 8.40 10 -1 -4 118.49 9.40 10 -1 -4 136.09 10.50 10 1 -3 176.18 11.60 10 1 -3 173.18 9.60 -10 1 3 168.58 10.60 10 -1 -3 175.08 10.70 -10 -1 3 167.28 9.10 -10 1 2 375.96 15.60 10 1 -2 389.86 16.70 10 1 -2 387.66 13.90 10 -1 -2 377.76 16.10 -10 -1 2 376.56 13.50 10 -1 -2 399.06 16.20 10 1 -1 211.48 9.60 10 1 -1 211.18 12.50 -10 1 1 203.88 11.70 -10 -1 1 197.98 9.70 10 -1 -1 199.88 11.60 10 -1 -1 209.48 11.70 10 1 0 8.80 3.50 10 1 0 14.10 5.90 -10 1 0 6.70 5.40 10 -1 0 9.20 4.90 -10 -1 0 -0.60 3.70 10 -1 0 6.90 5.00 -10 1 -1 202.18 11.70 10 1 1 186.88 12.50 10 1 1 226.28 10.10 10 -1 1 200.68 12.50 -10 -1 -1 202.98 9.70 10 -1 1 208.88 11.90 -10 1 -2 27.50 6.40 10 1 2 28.10 7.00 10 1 2 27.30 5.00 -10 -1 -2 25.10 4.90 10 -1 2 20.30 6.90 10 1 3 24.70 5.20 10 1 3 35.20 7.90 -10 1 -3 23.10 6.10 10 -1 3 33.10 7.40 -10 -1 -3 24.10 5.30 10 -1 3 34.30 6.70 10 1 4 14.40 4.90 10 1 4 18.70 6.80 10 -1 4 9.20 5.70 -10 -1 -4 12.70 6.90 10 -1 4 10.00 6.00 10 1 5 3.60 5.40 10 1 5 4.00 5.90 10 -1 5 7.60 5.90 10 -1 5 -1.80 5.20 -10 -1 -5 -1.00 3.80 10 1 6 5.30 5.60 10 1 6 7.10 6.40 10 -1 6 8.20 6.20 10 -1 6 -0.20 5.90 10 1 7 -1.10 5.70 10 1 7 3.50 6.40 10 -1 7 4.40 7.00 10 -1 7 8.50 7.40 10 1 8 4.40 7.00 10 1 8 6.10 6.80 10 -1 8 8.30 8.20 10 -1 8 7.40 6.80 10 2 -11 122.09 13.10 -10 2 11 111.29 14.00 10 -2 -11 117.09 12.10 -10 -2 11 130.89 13.60 -10 2 10 7.60 6.40 10 2 -10 7.10 6.90 10 -2 -10 10.30 6.90 -10 -2 10 1.80 5.80 10 2 -9 95.49 12.10 10 -2 -9 83.79 14.50 -10 -2 9 99.89 11.20 10 -2 -9 95.39 9.90 10 -2 -8 45.80 8.30 -10 -2 8 60.29 9.30 10 -2 -8 46.80 9.60 10 2 -7 274.57 15.80 -10 -2 7 264.57 14.60 10 -2 -7 283.27 14.50 10 -2 -7 295.37 17.50 10 2 -6 18.70 6.90 10 -2 -6 18.40 6.50 -10 -2 6 27.40 7.10 -10 -2 6 29.50 5.60 10 -2 -6 20.40 5.80 10 2 -5 117.59 11.00 -10 -2 5 144.19 8.80 -10 -2 5 126.49 9.00 10 -2 -5 128.59 11.00 10 -2 -5 119.29 9.00 10 2 -4 50.99 8.50 -10 -2 4 73.49 6.20 10 -2 -4 69.19 8.50 -10 -2 4 66.89 6.50 10 -2 -4 70.89 8.10 10 2 -3 8.30 5.80 -10 2 3 4.10 3.80 10 -2 -3 17.00 5.60 -10 -2 3 11.50 3.60 -10 -2 3 7.20 3.30 10 -2 -3 10.60 4.80 -10 2 2 0.60 3.50 10 2 -2 -1.90 2.30 10 2 -2 4.50 5.30 -10 -2 2 -2.30 2.90 10 -2 -2 6.90 5.20 10 -2 -2 -3.40 4.00 10 2 -1 11.30 5.90 -10 2 1 12.00 4.30 -10 2 1 7.40 6.30 10 2 -1 13.30 3.00 10 -2 -1 6.10 5.00 10 -2 -1 15.50 5.10 10 2 0 31.50 3.80 -10 2 0 27.90 8.60 10 2 0 31.30 7.10 10 -2 0 28.60 6.60 10 -2 0 23.90 6.50 10 2 1 913.71 29.50 10 2 1 963.00 22.50 10 -2 1 942.81 28.00 10 -2 1 947.11 29.20 10 2 2 0.20 5.60 10 2 2 10.60 3.40 -10 -2 -2 7.10 2.90 10 -2 2 4.90 4.90 10 -2 2 3.80 5.40 10 2 3 9.30 3.50 10 2 3 5.40 6.20 10 -2 3 2.70 5.60 -10 -2 -3 8.20 3.50 10 -2 3 1.60 5.50 10 2 4 10.70 3.90 10 2 4 10.70 6.80 -10 -2 -4 10.80 3.80 10 -2 4 4.20 5.70 10 -2 4 4.20 5.40 10 2 5 115.19 8.80 10 -2 5 110.79 11.00 10 -2 5 110.99 11.70 -10 -2 -5 121.09 9.40 10 2 6 -5.90 4.10 10 2 6 -3.50 5.90 -10 -2 -6 5.50 4.10 10 -2 6 5.80 6.60 10 -2 6 -2.50 6.30 10 2 7 71.79 9.40 10 2 7 103.89 13.50 10 -2 7 84.69 12.20 10 -2 7 72.89 11.20 10 2 8 -4.10 5.90 10 2 8 -14.10 5.80 10 -2 8 -1.90 6.60 10 -2 8 15.10 7.80 10 3 -10 1.90 6.50 -10 3 10 4.30 6.40 10 -3 -10 -7.60 5.00 -10 -3 10 -3.30 5.30 10 -3 -10 -0.70 5.00 10 3 -9 22.30 7.90 -10 -3 9 20.50 7.00 10 -3 -9 25.90 6.40 10 -3 -9 36.70 9.40 10 3 -8 5.80 6.80 10 -3 -8 3.70 4.80 10 -3 -8 -3.10 6.50 -10 -3 8 2.70 5.40 10 3 -7 41.60 9.60 10 -3 -7 44.50 9.40 10 -3 -7 42.20 7.40 -10 -3 7 75.49 8.50 -10 -3 7 50.29 7.80 10 3 -6 50.19 9.00 10 -3 -6 50.99 9.80 -10 -3 6 50.39 6.70 10 -3 -6 42.70 6.90 -10 3 5 59.29 7.30 10 3 -5 57.79 9.10 10 -3 -5 69.99 10.20 10 -3 -5 61.49 7.30 -10 -3 5 55.09 6.10 -10 -3 5 80.59 6.50 10 3 -4 27.50 7.30 -10 3 4 27.10 5.60 10 -3 -4 28.80 7.50 -10 -3 4 42.10 4.70 -10 -3 4 28.30 4.60 10 -3 -4 25.50 5.70 -10 3 3 31.00 5.60 10 3 -3 32.10 7.70 -10 -3 3 35.20 3.80 10 -3 -3 48.20 9.10 10 -3 -3 42.90 7.20 -10 3 2 -1.00 3.30 10 3 -2 4.90 5.80 10 -3 -2 1.30 4.90 10 -3 -2 -1.10 4.00 -10 -3 2 -0.80 1.40 10 3 -1 16.20 6.60 -10 3 1 11.30 4.20 10 -3 -1 14.70 6.60 10 3 0 33.70 7.70 10 -3 0 55.69 7.50 10 -3 0 59.19 8.90 10 -3 0 46.90 6.10 10 3 1 20.00 6.90 10 -3 1 17.00 6.60 10 -3 1 18.40 5.20 10 3 2 45.20 8.30 10 -3 2 48.50 8.90 10 -3 2 49.80 7.50 10 3 3 79.99 5.50 10 3 3 82.19 7.80 10 3 3 72.69 10.50 10 -3 3 71.79 9.40 10 -3 3 71.79 9.40 10 3 4 2.40 5.70 10 3 4 7.90 3.00 10 -3 4 -0.40 5.40 10 -3 4 11.10 6.90 10 3 5 49.70 5.90 10 3 5 42.30 8.90 10 -3 5 40.70 8.70 10 -3 5 41.00 9.00 10 3 6 31.70 8.70 10 3 6 42.20 6.50 10 -3 6 47.20 9.60 10 -3 6 40.00 8.40 10 3 7 11.90 5.60 10 3 7 11.00 7.70 10 -3 7 16.50 7.40 10 -3 7 15.80 8.00 10 3 8 -3.40 5.90 10 3 8 -5.80 6.10 10 -3 8 -5.00 6.20 10 -3 8 -2.90 6.80 10 4 -10 1.10 6.90 10 -4 -10 8.60 6.50 10 -4 -10 10.60 4.80 -10 -4 10 -3.10 5.10 10 4 -9 13.60 7.30 10 -4 -9 12.50 5.30 -10 -4 9 4.20 5.80 10 -4 -9 11.70 7.60 10 4 -8 3.40 6.30 -10 -4 8 5.80 5.10 10 -4 -8 7.60 4.80 10 -4 -8 14.70 7.80 10 4 -7 5.10 6.20 10 -4 -7 11.50 10.70 -10 -4 7 17.90 6.30 10 -4 -7 14.10 4.90 -10 4 6 7.70 4.30 10 -4 -6 14.30 5.20 -10 -4 6 5.60 3.90 10 -4 -6 11.40 6.60 -10 4 5 70.69 7.20 10 4 -5 78.79 10.60 10 -4 -5 71.09 7.20 10 -4 -5 100.19 11.90 -10 -4 5 82.09 6.30 10 4 -4 84.29 10.00 -10 4 4 79.69 7.60 10 -4 -4 77.49 10.00 -10 -4 4 84.69 5.20 10 -4 -4 77.09 7.30 -10 4 3 4.30 3.60 10 4 -3 2.20 5.40 10 -4 -3 -8.80 4.40 10 -4 -3 4.20 3.80 -10 4 2 20.00 5.00 10 4 -2 18.90 6.70 10 -4 -2 11.70 7.10 10 -4 -2 17.30 4.50 10 4 -1 145.69 12.00 10 -4 -1 146.69 8.70 10 -4 -1 158.28 13.30 10 4 0 35.40 8.20 10 -4 0 57.99 6.80 10 -4 0 55.49 6.40 10 -4 0 43.00 9.30 10 4 1 4.30 6.00 10 -4 1 7.40 6.00 10 -4 1 10.50 4.20 10 -4 1 8.20 4.60 10 4 2 23.00 7.10 10 -4 2 22.70 5.80 10 -4 2 12.10 7.10 10 4 3 2.20 6.30 10 -4 3 12.90 5.20 10 -4 3 11.30 7.10 10 4 4 2.50 5.90 10 -4 4 7.30 6.40 10 -4 4 9.10 5.80 10 4 5 2.90 6.10 10 4 5 5.80 2.80 10 -4 5 3.90 6.10 10 -4 5 -3.90 5.70 10 4 6 18.40 7.70 10 4 6 12.00 4.20 10 -4 6 3.80 7.00 10 -4 6 6.00 6.10 10 4 7 33.10 7.00 10 4 7 50.49 10.10 10 -4 7 41.70 8.70 10 -4 7 39.30 10.30 10 5 -9 2.60 6.50 10 -5 -9 12.40 4.10 10 -5 -9 7.00 7.90 -10 -5 9 8.40 6.40 10 5 -8 118.89 12.90 10 -5 -8 146.09 9.20 -10 -5 8 93.19 9.70 10 -5 -8 144.89 15.00 10 5 -7 20.60 7.80 -10 5 7 23.30 5.20 10 -5 -7 22.10 4.80 10 -5 -7 14.70 7.90 -10 -5 7 15.90 5.80 -10 5 6 15.60 6.90 10 5 -6 17.20 7.20 10 -5 -6 17.40 8.70 -10 -5 6 12.80 4.30 10 -5 -6 21.40 4.60 10 5 -5 29.20 9.70 -10 5 5 28.50 4.80 10 -5 -5 34.40 9.00 -10 -5 5 29.80 4.50 10 -5 -5 31.80 5.00 10 5 -4 7.20 6.00 -10 5 4 5.60 3.30 10 -5 -4 9.50 6.60 10 -5 -4 1.30 3.00 10 5 -3 7.40 6.40 -10 5 3 12.10 3.50 10 -5 -3 5.20 3.30 10 -5 -3 9.80 7.40 10 5 -2 32.70 7.70 10 -5 -2 35.70 9.10 10 -5 -2 30.90 4.30 10 -5 -2 25.30 4.40 10 5 -1 164.48 12.80 10 -5 -1 149.88 13.30 10 -5 -1 157.58 8.40 10 -5 -1 180.98 8.60 10 5 0 0.70 5.80 10 -5 0 10.80 3.30 10 -5 0 2.90 3.80 10 -5 0 2.90 5.80 10 5 1 77.19 10.70 10 -5 1 74.79 7.20 10 -5 1 81.99 6.90 10 -5 1 75.29 11.30 10 5 2 0.40 5.90 10 -5 2 5.70 6.30 10 -5 2 1.80 4.50 10 -5 2 10.70 3.60 10 5 3 61.39 10.00 10 -5 3 54.09 7.50 10 -5 3 63.69 10.60 10 5 4 1.20 5.90 10 -5 4 -0.10 4.80 10 5 5 63.19 11.30 10 -5 5 51.19 11.00 10 -5 5 47.60 7.90 10 5 6 4.20 2.50 10 5 6 -1.80 6.30 10 -5 6 -3.00 5.40 10 -5 6 9.80 8.00 10 5 7 -6.40 6.30 10 -5 7 -4.20 5.20 10 -5 7 15.00 8.20 10 6 -8 -0.20 6.80 -10 -6 8 -11.40 4.60 10 -6 -8 16.20 7.40 10 6 -7 24.20 7.90 -10 6 7 14.30 4.10 -10 -6 7 14.10 5.60 10 -6 -7 29.20 8.30 10 6 -6 6.40 6.60 -10 6 6 3.80 3.00 -10 -6 6 -7.50 3.60 10 -6 -6 12.50 2.90 10 -6 -6 8.80 6.90 10 6 -5 20.30 7.50 -10 6 5 21.20 3.60 10 -6 -5 22.80 3.40 10 -6 -5 37.90 9.20 10 6 -4 14.50 6.80 10 -6 -4 14.30 3.00 10 -6 -4 11.10 7.20 10 6 -3 38.40 9.50 10 -6 -3 49.99 4.30 10 -6 -3 67.59 4.50 10 -6 -2 12.70 6.80 10 -6 -2 16.40 2.90 10 -6 -1 58.89 5.00 10 -6 -1 71.79 11.60 10 -6 -1 76.79 5.20 10 -6 0 12.30 7.40 10 -6 0 14.30 3.10 10 6 1 2.90 6.20 10 -6 1 17.90 3.30 10 -6 1 7.50 7.60 10 -6 1 7.40 3.80 10 6 2 61.79 10.00 10 -6 2 72.89 12.40 10 -6 2 62.39 6.80 10 6 3 -0.80 5.90 10 -6 3 18.40 7.80 10 -6 3 1.50 4.40 10 6 4 14.80 7.40 10 -6 4 3.00 5.20 10 -6 4 14.80 8.10 10 6 5 -4.00 6.00 10 -6 5 -5.40 4.40 10 -6 5 -1.60 7.40 10 6 6 115.89 13.40 10 -6 6 136.39 11.60 10 -6 6 154.48 15.30 10 7 -7 1.40 6.40 10 -7 -7 12.20 7.10 10 7 -6 36.10 8.90 -10 -7 6 27.10 4.20 10 -7 -6 48.80 10.60 10 7 -5 -2.80 5.50 10 -7 -5 -1.80 6.00 10 7 -4 66.59 10.70 10 -7 -4 78.59 12.20 10 7 -3 9.30 6.60 10 -7 -3 11.80 7.40 10 7 -2 2.10 6.10 10 -7 -2 2.60 6.00 10 7 -1 7.70 6.70 10 -7 -1 13.00 7.50 10 7 0 -7.90 5.50 10 -7 0 -3.90 2.00 10 -7 0 3.50 6.80 10 -7 0 8.20 3.40 10 7 1 103.09 12.80 10 -7 1 93.19 6.00 10 -7 1 129.09 13.50 10 -7 1 114.49 6.20 10 7 2 -10.50 5.40 10 -7 2 7.40 7.20 10 -7 2 -7.50 2.80 10 7 3 7.70 7.10 10 -7 3 21.00 6.90 10 -7 3 18.50 7.90 10 7 4 -8.40 5.70 10 -7 4 -10.30 3.80 10 -7 4 3.20 6.80 10 7 5 90.39 13.20 10 -7 5 102.69 10.10 10 -7 5 126.49 15.40 10 8 -5 15.80 7.80 10 -8 -5 34.80 9.90 10 8 -4 4.80 6.80 10 -8 -4 -0.20 5.90 10 8 -3 62.09 10.60 10 -8 -3 71.69 12.00 10 8 -2 3.80 6.20 10 -8 -2 0.30 6.10 10 8 -1 -1.20 6.90 10 -8 -1 8.60 7.50 10 8 0 14.20 7.30 10 -8 0 17.40 7.50 10 8 1 1.60 6.30 10 -8 1 13.60 7.50 10 8 2 14.30 7.70 10 -8 2 8.20 3.30 10 -8 2 20.60 9.20 10 8 3 44.60 9.90 10 -8 3 26.00 4.90 10 -8 3 54.19 11.50 11 0 -10 10.10 6.50 -11 0 10 7.80 7.50 11 0 -9 13.50 7.50 -11 0 9 -3.10 5.80 11 0 -8 155.88 12.60 -11 0 8 187.78 14.00 -11 0 7 -1.10 4.90 11 0 -7 0.30 5.10 11 0 -7 4.70 5.60 11 0 -6 34.60 7.50 11 0 -6 46.50 8.20 11 0 -5 1.00 4.50 11 0 -5 -5.80 4.80 -11 0 4 16.80 4.80 11 0 -4 9.50 4.70 11 0 -4 12.80 6.40 11 0 -3 -2.60 4.00 -11 0 3 -4.40 3.80 11 0 -3 -3.20 4.80 11 0 -2 3.10 4.00 -11 0 2 -9.50 6.40 11 0 -2 -5.20 4.20 11 0 -1 0.70 5.10 11 0 -1 -0.60 3.50 -11 0 1 -6.50 4.30 -11 0 0 823.62 24.80 11 0 0 880.21 25.20 11 0 0 830.22 27.30 11 0 1 -6.90 3.70 11 0 1 -3.70 4.90 -11 0 -1 -5.90 4.10 11 0 2 161.38 10.10 11 0 2 150.38 11.90 -11 0 -2 134.49 9.40 11 0 3 2.30 5.80 11 0 3 -1.80 6.40 11 0 4 21.30 7.20 11 0 4 29.70 6.30 11 0 5 9.10 5.20 11 0 5 5.30 6.20 11 0 6 77.69 9.70 11 0 6 52.39 10.30 11 0 7 2.30 6.10 11 0 7 -6.60 5.10 -11 1 10 5.10 6.40 11 1 -10 9.40 6.90 -11 -1 10 -0.10 6.20 11 -1 -10 7.00 6.00 11 1 -9 3.20 6.20 -11 -1 9 7.00 6.10 11 1 -8 4.40 5.60 11 -1 -8 4.60 6.50 -11 -1 8 6.30 5.70 11 -1 -8 11.30 5.70 11 1 -7 8.40 6.00 -11 -1 7 16.50 6.20 11 -1 -7 2.10 5.40 11 -1 -7 15.20 7.10 11 1 -6 5.20 5.60 11 -1 -6 6.90 5.20 11 -1 -6 8.40 5.30 -11 -1 6 -0.40 4.10 11 1 -5 17.70 6.80 11 -1 -5 27.00 6.90 11 -1 -5 19.20 6.40 -11 -1 5 24.20 4.90 11 1 -4 25.20 5.80 11 1 -4 30.00 7.30 11 -1 -4 28.10 6.50 11 -1 -4 20.00 6.30 -11 -1 4 29.80 6.20 11 1 -3 55.39 9.10 11 1 -3 50.99 6.30 -11 -1 3 49.90 6.60 11 -1 -3 44.60 7.40 11 -1 -3 53.89 8.20 11 1 -2 217.48 13.30 -11 1 2 203.58 12.00 11 1 -2 224.98 10.60 -11 -1 2 201.98 10.30 11 -1 -2 226.98 12.80 11 -1 -2 204.88 12.10 -11 1 1 28.30 7.20 11 1 -1 46.50 6.00 11 1 -1 37.90 7.90 -11 -1 1 40.50 6.20 11 -1 -1 37.30 7.00 11 -1 -1 46.60 7.50 11 1 0 277.07 11.30 11 1 0 274.57 15.00 -11 1 0 231.48 13.10 11 -1 0 264.37 14.00 -11 -1 0 244.08 11.00 11 -1 0 285.67 14.50 11 1 1 5.20 3.50 -11 1 -1 -3.90 4.90 11 1 1 3.10 5.60 -11 -1 -1 0.20 3.30 11 -1 1 5.80 4.70 11 -1 1 -4.70 4.40 11 1 2 45.40 5.80 11 1 2 30.80 7.80 11 -1 2 44.20 7.90 11 -1 2 41.90 7.30 -11 -1 -2 34.00 5.60 11 1 3 5.10 6.00 11 1 3 14.00 4.60 -11 -1 -3 11.30 4.40 11 -1 3 17.30 5.90 11 -1 3 12.50 6.40 11 1 4 29.20 9.20 11 1 4 28.10 5.70 11 -1 4 25.20 7.50 11 -1 4 21.30 6.60 -11 -1 -4 26.40 5.50 11 1 5 1.10 4.50 11 1 5 2.90 6.60 -11 -1 -5 -5.60 4.20 11 -1 5 -0.60 5.10 11 1 6 -14.90 5.50 11 1 6 1.80 5.10 11 -1 6 -1.00 6.00 11 -1 6 9.10 6.60 11 1 7 8.20 7.50 11 1 7 2.90 5.90 11 -1 7 13.30 7.60 11 -1 7 10.00 7.10 11 2 -10 8.80 7.00 -11 2 10 1.70 6.60 -11 -2 10 2.00 6.70 11 -2 -10 7.60 6.00 11 2 -9 100.39 11.70 11 -2 -9 105.49 12.10 11 -2 -9 108.89 11.00 -11 -2 9 92.79 11.10 11 2 -8 37.80 8.40 11 -2 -8 47.80 10.50 -11 -2 8 42.60 8.30 11 -2 -8 41.20 7.90 11 2 -7 22.50 7.30 -11 -2 7 16.80 5.80 11 -2 -7 17.40 5.90 11 -2 -7 27.20 8.50 11 2 -6 10.40 6.70 11 -2 -6 4.90 5.50 11 -2 -6 3.00 5.20 -11 -2 6 7.50 4.50 11 2 -5 5.30 6.00 11 -2 -5 4.60 4.40 -11 -2 5 14.10 4.10 11 -2 -5 -1.90 5.00 -11 -2 5 1.80 3.80 11 2 -4 25.30 7.60 -11 -2 4 24.00 4.50 11 -2 -4 16.20 5.60 -11 -2 4 13.60 4.00 11 -2 -4 13.80 6.40 11 2 -3 9.00 6.10 11 -2 -3 14.10 5.80 -11 -2 3 15.50 4.20 -11 -2 3 14.70 3.80 11 -2 -3 10.60 5.90 11 2 -2 54.39 5.30 11 2 -2 56.69 9.10 11 -2 -2 45.50 7.40 11 -2 -2 63.89 9.30 -11 -2 2 40.60 5.40 11 2 -1 31.60 7.60 11 2 -1 35.30 4.30 11 -2 -1 41.10 7.80 11 -2 -1 40.20 6.80 -11 -2 1 33.60 4.70 11 2 0 60.39 4.80 11 2 0 57.29 9.20 11 -2 0 58.29 8.30 11 -2 0 68.89 9.10 11 2 1 208.28 8.20 11 2 1 209.08 14.00 -11 -2 -1 209.48 11.30 11 -2 1 228.28 12.70 11 -2 1 209.58 13.00 11 2 2 105.49 6.40 11 2 2 50.89 9.30 -11 -2 -2 80.39 5.70 11 -2 2 86.39 9.10 11 -2 2 83.79 9.70 11 2 3 100.39 6.80 11 2 3 76.49 10.70 -11 -2 -3 72.49 6.10 11 -2 3 80.39 9.10 11 -2 3 66.69 9.20 11 2 4 8.50 5.90 11 2 4 18.50 4.20 -11 -2 -4 6.90 3.80 11 -2 4 16.70 6.00 11 -2 4 12.00 7.00 11 2 5 36.60 8.80 11 2 5 52.69 6.60 11 -2 5 53.49 10.10 11 -2 5 32.70 8.20 11 2 6 3.60 4.50 11 2 6 -6.70 5.70 -11 -2 -6 -4.00 4.90 11 -2 6 0.00 6.10 11 -2 6 0.00 5.80 11 2 7 4.40 7.10 11 2 7 2.30 4.80 11 -2 7 -0.10 5.90 11 -2 7 7.10 6.70 -11 -3 10 21.80 8.00 11 3 -9 103.29 13.60 -11 -3 9 91.09 10.70 11 -3 -9 128.19 11.00 11 -3 -9 103.49 12.60 11 3 -8 54.19 10.30 11 -3 -8 69.09 9.20 -11 -3 8 44.90 8.20 11 -3 -8 69.59 11.10 11 3 -7 15.00 7.00 -11 -3 7 22.50 6.00 11 -3 -7 22.50 6.30 11 -3 -7 28.60 8.30 11 3 -6 34.60 8.40 -11 -3 6 32.00 6.00 11 -3 -6 39.50 6.80 11 -3 -6 30.90 8.20 11 3 -5 22.20 7.40 11 -3 -5 22.90 5.90 11 -3 -5 16.10 7.20 -11 -3 5 15.10 4.20 11 3 -4 15.00 6.70 11 -3 -4 5.10 4.50 11 -3 -4 6.50 5.90 -11 -3 4 9.50 3.20 -11 -3 4 6.60 3.00 11 3 -3 5.10 5.90 11 -3 -3 16.30 5.30 -11 -3 3 14.40 2.80 11 -3 -3 25.50 7.40 11 3 -2 0.10 5.70 11 -3 -2 9.60 5.10 11 -3 -2 10.50 6.30 11 3 -1 9.50 6.40 11 -3 -1 6.20 5.90 11 -3 -1 7.40 5.00 11 3 0 36.70 8.20 11 -3 0 31.20 6.70 11 -3 0 31.00 7.50 11 3 1 6.10 6.00 11 -3 1 13.60 5.70 11 -3 1 17.10 6.80 11 3 2 77.89 10.60 11 -3 2 92.49 9.70 11 -3 2 88.69 10.80 11 3 3 3.60 6.10 11 -3 3 1.30 4.90 11 -3 3 11.40 7.00 11 3 4 1.70 6.30 11 -3 4 17.20 7.10 11 -3 4 10.80 6.40 11 3 5 42.80 5.10 11 3 5 11.20 7.10 11 -3 5 28.40 8.30 11 -3 5 11.70 6.10 11 3 6 36.90 5.80 11 3 6 31.00 9.10 11 -3 6 38.20 8.60 11 -3 6 35.20 9.10 11 3 7 2.80 4.40 11 3 7 -3.70 6.10 11 -3 7 -9.30 7.00 11 -3 7 12.10 7.20 11 4 -9 6.80 7.40 11 -4 -9 17.70 8.00 -11 -4 9 9.40 6.00 11 -4 -9 13.70 5.60 11 4 -8 208.18 15.50 11 -4 -8 200.98 12.00 11 -4 -8 200.78 16.40 -11 -4 8 193.18 12.40 11 4 -7 72.69 11.10 11 -4 -7 63.59 8.00 11 -4 -7 73.39 11.70 11 4 -6 5.00 6.50 -11 -4 6 12.50 4.30 11 -4 -6 16.80 11.40 11 -4 -6 16.90 5.40 11 4 -5 -0.20 6.00 11 -4 -5 6.20 6.10 -11 -4 5 15.00 3.10 11 -4 -5 3.40 4.40 -11 -4 5 -0.50 3.00 -11 4 4 33.10 5.70 11 -4 -4 33.60 9.10 -11 -4 4 34.40 3.30 11 -4 -4 33.60 5.80 11 4 -3 81.89 10.80 -11 4 3 76.89 7.50 11 -4 -3 68.19 7.30 11 -4 -3 92.99 10.80 -11 4 2 5.60 3.60 11 4 -2 5.30 6.00 11 -4 -2 0.50 4.20 11 -4 -2 -5.40 4.40 11 4 -1 12.20 6.40 11 -4 -1 6.60 6.60 11 -4 -1 8.00 4.60 11 -4 -1 14.50 4.30 11 4 0 10.10 6.80 11 -4 0 9.00 4.70 11 -4 0 22.40 7.90 11 -4 1 129.79 12.10 11 -4 1 120.59 9.40 11 4 2 11.40 6.70 11 -4 2 0.90 5.50 11 -4 2 3.10 5.00 11 4 3 -8.50 5.30 11 -4 3 1.90 5.70 11 -4 3 3.70 5.40 11 4 4 302.07 18.30 11 -4 4 308.77 18.60 11 -4 4 298.97 16.00 11 4 5 67.59 4.80 11 4 5 55.69 10.60 11 -4 5 53.19 10.60 11 -4 5 53.89 9.40 11 4 6 90.99 5.90 11 4 6 59.39 11.20 11 -4 6 49.70 10.10 11 -4 6 70.59 10.50 11 5 -8 66.69 11.30 11 -5 -8 67.79 12.40 11 -5 -8 74.89 7.50 -11 -5 8 59.59 8.30 11 5 -7 16.40 7.60 11 -5 -7 19.50 4.80 11 -5 -7 22.10 8.10 -11 -5 7 3.90 4.50 11 5 -6 -8.60 5.50 -11 5 6 -7.70 3.20 -11 -5 6 -7.90 3.10 11 -5 -6 3.20 3.60 11 -5 -6 10.50 6.90 -11 5 5 -3.70 3.20 11 5 -5 8.80 6.80 11 -5 -5 6.20 4.10 11 -5 -5 -1.00 5.80 11 5 -4 2.80 6.00 11 -5 -4 0.40 3.30 11 5 -3 22.30 7.90 11 -5 -3 24.10 4.70 11 -5 -3 35.90 8.40 11 5 -2 0.50 5.80 11 -5 -2 0.10 3.60 11 -5 -2 11.50 7.10 11 5 -1 8.80 6.70 11 -5 -1 7.60 6.80 11 -5 -1 7.10 4.10 11 5 0 -1.00 6.00 11 -5 0 6.00 7.10 11 5 1 9.30 6.60 11 -5 1 16.40 4.80 11 -5 1 17.70 7.90 11 5 2 74.69 10.90 11 -5 2 82.09 8.20 11 5 3 -7.10 5.60 11 -5 3 -0.40 4.80 11 -5 3 2.60 6.10 11 5 4 34.30 8.60 11 -5 4 38.80 7.50 11 -5 4 44.20 9.60 11 5 5 30.40 9.00 11 -5 5 20.10 7.30 11 -5 5 11.60 7.60 11 6 -7 28.90 8.70 -11 -6 7 17.50 5.50 11 -6 -7 33.80 9.80 11 6 -6 5.40 6.60 11 -6 -6 10.20 3.20 11 -6 -6 29.40 9.20 -11 -6 6 -1.70 3.10 -11 6 5 9.60 3.10 11 6 -5 -0.50 6.50 11 -6 -5 -1.20 5.80 11 -6 -5 7.70 2.90 11 6 -4 66.69 10.60 11 -6 -4 66.49 5.20 11 -6 -4 94.09 5.70 11 -6 -4 61.89 11.10 11 6 -3 30.40 8.20 11 -6 -3 42.80 9.60 11 -6 -3 36.40 4.40 11 6 -2 1.30 6.00 11 -6 -2 12.90 3.00 11 -6 -2 4.10 6.40 11 -6 -2 -3.10 2.50 11 6 -1 49.20 9.40 11 -6 -1 56.79 10.70 11 -6 -1 39.70 5.00 11 6 0 13.20 7.10 11 -6 0 0.90 3.60 11 -6 0 6.20 6.80 11 6 1 -1.30 6.40 11 -6 1 -6.50 5.30 11 -6 1 3.00 5.90 11 6 2 19.40 8.10 11 -6 2 6.00 4.70 11 -6 2 24.20 8.40 11 6 3 7.90 7.10 11 -6 3 17.80 8.20 11 -6 3 2.90 4.80 11 6 4 10.60 7.50 11 -6 4 10.00 5.90 11 -6 4 15.90 7.50 11 7 -6 -4.00 6.50 11 -7 -6 20.30 7.60 11 7 -5 21.20 8.20 11 -7 -5 30.10 8.80 11 7 -4 1.70 6.80 11 -7 -4 1.60 5.90 11 7 -3 4.50 6.90 11 -7 -3 20.90 8.40 11 7 -2 -7.30 5.50 11 -7 -2 4.80 6.30 11 7 -1 -5.70 5.20 11 -7 -1 -3.30 1.90 11 -7 -1 1.80 6.50 11 7 0 83.09 11.90 11 -7 0 52.59 4.90 11 -7 0 83.29 13.00 11 7 1 -1.30 6.30 11 -7 1 -7.60 3.00 11 -7 1 7.70 7.20 11 7 2 130.29 13.40 11 -7 2 123.59 12.10 11 -7 2 141.89 14.60 11 7 3 31.60 9.10 11 -7 3 26.90 6.00 11 -7 3 35.50 10.00 11 8 -3 -1.00 6.70 11 -8 -3 22.30 8.10 11 8 -2 -0.30 6.40 11 -8 -2 6.90 7.60 11 8 -1 38.10 9.60 11 -8 -1 47.50 10.20 11 8 0 14.00 8.30 11 -8 0 37.60 9.70 12 0 -9 -6.80 5.60 12 0 -8 42.50 8.60 -12 0 8 57.59 9.80 -12 0 7 2.40 4.90 12 0 -6 15.00 7.30 12 0 -6 22.30 6.10 12 0 -5 3.70 4.70 12 0 -5 -6.90 5.70 12 0 -4 78.19 10.50 12 0 -4 108.39 9.50 -12 0 3 -1.20 4.40 12 0 -3 1.70 5.40 12 0 -3 5.50 4.60 12 0 -2 3.60 5.50 12 0 -2 3.60 3.70 -12 0 2 -5.30 4.40 12 0 -1 -0.10 3.80 12 0 -1 -3.30 5.10 -12 0 0 292.17 14.20 12 0 0 348.37 14.70 12 0 0 336.77 16.80 -12 0 -1 -8.70 4.10 12 0 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13 -1 -2 2.80 5.30 13 1 -1 50.79 9.40 13 1 -1 81.59 6.80 -13 -1 1 58.29 7.40 13 -1 -1 80.29 8.90 13 -1 -1 59.49 9.30 13 1 0 10.20 3.40 13 1 0 -0.20 6.00 13 -1 0 -2.80 6.30 13 -1 0 8.60 4.60 -13 -1 0 -6.90 3.90 13 1 1 2.40 6.20 13 1 1 10.40 3.50 -13 -1 -1 -2.40 4.00 13 -1 1 -0.30 5.10 13 -1 1 13.60 5.70 13 1 2 15.80 4.00 13 1 2 8.10 6.60 13 -1 2 -3.20 6.20 13 -1 2 16.80 5.70 13 1 3 12.70 7.50 13 -1 3 38.90 7.20 -13 -1 -3 14.30 8.00 13 1 4 -3.90 5.90 13 -1 4 -10.10 5.30 13 -1 4 16.50 6.00 13 1 5 -14.50 6.10 13 -1 5 16.90 5.30 13 -1 5 -5.20 7.00 -13 -2 8 67.39 10.00 13 2 -7 -9.20 5.60 13 -2 -7 8.30 6.50 -13 -2 7 -1.20 4.40 13 -2 -7 1.80 6.00 13 2 -6 -9.60 6.00 13 -2 -6 0.00 5.70 13 -2 -6 0.40 5.10 -13 -2 6 0.50 4.00 13 2 -5 17.00 7.70 13 -2 -5 24.20 7.30 -13 -2 5 30.40 5.70 -13 -2 5 32.10 6.10 13 -2 -5 14.50 5.90 13 2 -4 29.60 8.80 -13 -2 4 19.30 4.40 -13 -2 4 14.10 5.10 13 -2 -4 22.60 7.10 13 -2 -4 20.40 6.60 13 2 -3 0.60 6.70 13 -2 -3 1.70 5.70 -13 -2 3 -0.60 2.60 13 -2 -3 8.10 5.90 13 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64.39 10.90 13 -3 1 106.09 11.40 13 -3 1 64.69 9.30 13 3 2 3.30 6.30 13 -3 2 11.70 6.60 13 -3 2 4.80 6.00 13 3 3 0.70 6.70 13 -3 3 8.90 6.20 13 3 4 7.30 7.60 13 -3 4 1.50 6.10 13 -3 4 14.70 6.70 13 4 -6 54.49 11.20 13 -4 -6 34.30 6.70 -13 -4 6 21.20 4.70 13 -4 -6 53.29 10.30 13 4 -5 6.40 7.80 13 -4 -5 11.70 5.70 13 -4 -5 6.60 5.60 13 4 -4 -8.10 6.20 13 -4 -4 -1.10 4.70 13 -4 -4 3.10 6.00 13 4 -3 -3.90 5.90 13 -4 -3 -3.80 4.90 13 -4 -3 8.00 6.50 13 4 -2 8.90 6.90 13 -4 -2 -5.70 5.00 13 4 -1 32.10 9.00 13 -4 -1 29.70 6.90 13 4 0 32.20 9.10 13 -4 0 31.80 7.10 13 4 1 39.50 9.50 13 -4 1 43.90 8.90 13 -4 1 25.80 6.80 13 4 2 2.50 7.10 13 -4 2 15.40 7.40 13 -4 2 3.20 6.00 13 4 3 10.30 7.80 13 -4 3 4.90 6.20 13 -4 3 29.50 7.70 13 5 -5 -4.00 6.40 13 -5 -5 15.00 6.90 13 -5 -5 -4.00 4.00 13 5 -4 16.60 7.90 13 -5 -4 38.30 9.30 13 -5 -4 11.30 5.00 13 5 -3 -2.20 6.20 13 -5 -3 4.40 4.70 13 -5 -3 18.50 8.10 13 5 -2 9.40 7.70 13 -5 -2 27.80 8.20 13 -5 -2 -0.50 4.50 13 5 -1 16.70 8.50 13 -5 -1 53.49 10.20 13 -5 -1 30.60 6.40 13 5 0 105.49 13.70 13 -5 0 141.69 14.10 13 -5 0 121.09 9.60 13 5 1 40.80 9.80 13 -5 1 46.10 9.50 13 -5 1 23.30 6.70 13 5 2 17.90 8.10 13 -5 2 13.50 6.40 13 -5 2 29.80 8.80 14 0 -6 108.39 11.80 14 0 -6 122.29 10.60 14 0 -5 -1.40 5.80 14 0 -5 6.10 4.20 14 0 -4 62.59 7.70 14 0 -4 15.60 7.20 14 0 -3 -0.90 5.70 14 0 -2 69.69 7.60 14 0 -2 33.10 8.70 14 0 -1 -6.70 5.60 14 0 0 155.68 13.20 14 0 0 177.18 10.60 14 0 1 -9.50 6.50 14 0 2 245.28 12.40 14 0 2 181.68 14.80 14 0 3 -6.80 6.20 14 1 -6 26.60 7.70 -14 -1 6 37.50 7.20 14 -1 -6 44.00 9.40 14 1 -5 38.10 9.00 14 -1 -5 42.30 8.80 14 -1 -5 42.10 8.20 -14 -1 5 47.20 7.70 14 1 -4 48.80 10.40 14 1 -4 95.39 8.10 14 -1 -4 87.49 9.30 14 1 -3 77.79 7.20 14 1 -3 57.79 9.90 14 -1 -3 60.09 9.80 14 -1 -3 56.29 8.60 14 1 -2 20.80 4.30 14 1 -2 0.10 6.50 14 -1 -2 14.80 5.40 14 -1 -2 0.90 6.00 14 1 -1 89.99 6.70 14 1 -1 69.29 10.90 14 -1 -1 56.29 10.20 14 -1 -1 68.59 8.50 14 1 0 297.77 11.80 14 1 0 239.58 16.40 14 -1 0 289.07 15.00 14 -1 0 253.67 16.50 14 1 1 12.70 7.70 14 -1 1 11.10 7.70 14 1 2 81.89 12.20 14 -1 2 84.99 11.60 14 2 -6 1.70 7.20 -14 -2 6 -0.90 4.40 14 -2 -6 -5.30 4.80 14 2 -5 15.50 8.70 14 -2 -5 41.00 7.70 -14 -2 5 25.40 5.80 14 2 -4 10.40 7.00 -14 -2 4 8.20 3.90 14 -2 -4 12.40 6.90 14 -2 -4 13.90 5.90 14 2 -3 -3.90 6.30 -14 -2 3 -0.90 2.80 14 -2 -3 -5.80 5.50 14 -2 -3 14.00 6.10 14 2 -2 12.40 7.50 14 -2 -2 24.10 6.60 14 -2 -2 -2.30 5.70 -14 -2 2 9.50 2.90 14 2 -1 22.10 9.00 14 -2 -1 27.80 6.30 14 -2 -1 12.20 8.20 14 2 0 108.49 12.60 14 -2 0 106.99 12.60 14 -2 0 150.78 11.70 14 2 1 1.60 7.70 14 -2 1 2.60 6.00 14 2 2 -5.70 6.10 14 -2 2 -7.00 6.00 14 3 -5 28.10 9.30 -14 -3 5 20.20 4.50 14 -3 -5 35.20 8.10 14 -3 -5 29.00 7.70 14 3 -4 7.70 8.20 14 -3 -4 20.20 7.20 14 -3 -4 -4.40 5.00 14 -3 -3 -8.70 5.10 14 3 -2 23.90 9.20 14 -3 -2 39.00 8.60 14 -3 -2 15.60 6.60 14 3 -1 59.29 10.90 14 -3 -1 100.49 10.80 14 -3 -1 73.39 9.70 14 3 0 -9.90 6.20 14 -3 0 16.10 5.70 14 -3 0 -12.80 5.30 14 3 1 1.30 7.30 14 -3 1 5.80 6.80 14 4 -3 -8.80 6.00 14 -4 -3 6.90 6.10 14 -4 -3 -6.70 4.50 14 4 -2 42.60 10.40 14 -4 -2 53.69 9.90 14 -4 -2 29.10 7.30 14 4 -1 45.60 10.70 14 -4 -1 50.29 9.40 14 -4 -1 24.70 7.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 2861 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_xv559 _database_code_depnum_ccdc_archive 'CCDC 2044221' loop_ _audit_author_name _audit_author_address 'Peter Mayer' ;LMU Muenchen Germany ; _audit_update_record ; 2020-11-13 deposited with the CCDC. 2021-02-09 downloaded from the CCDC. ; _chemical_name_common RNH378 _chemical_compound_source ? _chemical_absolute_configuration syn _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.100 #?# in millimeters _exptl_crystal_size_mid 0.040 #?# in millimeters _exptl_crystal_size_min 0.020 #?# in millimeters _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_special_details ; ; _audit_creation_date ? #?# style: 18-Aug-1998 _diffrn_ambient_temperature 103.(2) #?# in K _diffrn_source_type 'Bruker TXS' _diffrn_source_power 2.5 #?# in kW _diffrn_source_voltage 50 #?# in kV _diffrn_source_current 50 #?# in mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode (TXS)' _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_collimation ? _diffrn_measurement_device 'fixed-chi three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture TXS' _diffrn_measurement_method 'mix of phi and omega scans' _diffrn_measurement_details ? _diffrn_detector_area_resol_mean 7.3910 _diffrn_special_details ? _diffrn_orient_matrix_type ? _diffrn_orient_matrix_UB_11 ? _diffrn_orient_matrix_UB_12 ? _diffrn_orient_matrix_UB_13 ? _diffrn_orient_matrix_UB_21 ? _diffrn_orient_matrix_UB_22 ? _diffrn_orient_matrix_UB_23 ? _diffrn_orient_matrix_UB_31 ? _diffrn_orient_matrix_UB_32 ? _diffrn_orient_matrix_UB_33 ? _cell_length_a 21.9099(11) _cell_length_b 6.5137(4) _cell_length_c 14.4743(8) _cell_angle_alpha 90 _cell_angle_beta 115.663(2) _cell_angle_gamma 90 _cell_volume 1861.93(18) _cell_measurement_temperature 103.(2) #?# in K _cell_measurement_reflns_used 5076 _cell_measurement_theta_min 2.9029 _cell_measurement_theta_max 26.3594 _cell_special_details ? _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 1.00 _shelx_estimated_absorpt_T_min 0.992 _shelx_estimated_absorpt_T_max 0.998 _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _diffrn_reflns_number 10760 #xl _diffrn_reflns_av_R_equivalents 0.0360 #xl _diffrn_reflns_av_unetI/netI 0.0431 #xl _diffrn_reflns_limit_h_min -27 #xl _diffrn_reflns_limit_h_max 27 #xl _diffrn_reflns_limit_k_min -8 #xl _diffrn_reflns_limit_k_max 8 #xl _diffrn_reflns_limit_l_min -18 #xl _diffrn_reflns_limit_l_max 17 #xl _diffrn_reflns_theta_min 3.080 #xl _diffrn_reflns_theta_max 26.370 #xl _diffrn_measured_fraction_theta_max 0.997 #xl _diffrn_reflns_theta_full 25.242 #xl _diffrn_measured_fraction_theta_full 0.996 #xl _diffrn_reflns_Laue_measured_fraction_max 0.997 #xl _diffrn_reflns_Laue_measured_fraction_full 0.996 #xl _diffrn_reflns_point_group_measured_fraction_max 0.992 #xl _diffrn_reflns_point_group_measured_fraction_full 0.995 #xl _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'C 1 2 1' _space_group_name_Hall 'C 2y' _space_group_IT_number 5 _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' 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' N N 0.0061 0.0033 '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' _reflns_number_total 3790 #xl _reflns_number_gt 3410 #xl _reflns_threshold_expression 'I > 2\s(I)' #xl _reflns_Friedel_coverage 0.823 #xl _reflns_Friedel_fraction_max 0.986 #xl _reflns_Friedel_fraction_full 0.994 #xl _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. ; _refine_ls_structure_factor_coef Fsqd #xl _refine_ls_matrix_type full #xl _refine_ls_weighting_scheme calc #xl _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+1.4361P] where P=(Fo^2^+2Fc^2^)/3' #xl _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr #?# _refine_ls_extinction_method none #xl _refine_ls_extinction_coef . #xl _refine_ls_abs_structure_details ; Flack x determined using 1338 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.2(6) #xl _refine_ls_number_reflns 3790 #xl _refine_ls_number_parameters 246 #xl _refine_ls_number_restraints 1 #xl _refine_ls_R_factor_all 0.0489 #xl _refine_ls_R_factor_gt 0.0423 #xl _refine_ls_wR_factor_ref 0.1041 #xl _refine_ls_wR_factor_gt 0.1005 #xl _refine_ls_goodness_of_fit_ref 1.070 #xl _refine_ls_restrained_S_all 1.069 #xl _refine_ls_shift/su_max 0.000 #xl _refine_ls_shift/su_mean 0.000 #xl _refine_diff_density_max 0.177 #xl _refine_diff_density_min -0.185 #xl _refine_diff_density_rms 0.044 #xl _refine_special_details ; ; _computing_data_collection 'APEX3 v2016.5-0, Bruker AXS (2016)' _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 924)' _computing_publication_material ? 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 C1 C -0.04928(15) 0.3140(5) 0.0656(2) 0.0244(7) Uani 1 1 d . . . . . C2 C -0.00876(15) 0.1579(5) 0.1359(2) 0.0221(7) Uani 1 1 d . . . . . C3 C -0.01132(15) -0.0441(5) 0.1034(2) 0.0235(7) Uani 1 1 d . . . . . H3 H -0.044759 -0.084406 0.037886 0.028 Uiso 1 1 calc R U . . . C4 C 0.03479(15) -0.1863(5) 0.1663(2) 0.0224(7) Uani 1 1 d . . . . . H4 H 0.033241 -0.323342 0.142933 0.027 Uiso 1 1 calc R U . . . C5 C 0.08356(14) -0.1321(5) 0.2637(2) 0.0196(6) Uani 1 1 d . . . . . C6 C 0.08229(15) 0.0679(5) 0.2983(2) 0.0225(7) Uani 1 1 d . . . . . H6 H 0.112828 0.105003 0.366234 0.027 Uiso 1 1 calc R U . . . C7 C 0.03733(15) 0.2119(5) 0.2353(2) 0.0246(7) Uani 1 1 d . . . . . H7 H 0.037704 0.347789 0.259379 0.030 Uiso 1 1 calc R U . . . C8 C 0.13642(14) -0.2785(5) 0.3304(2) 0.0203(6) Uani 1 1 d . . . . . H8 H 0.133604 -0.317125 0.395271 0.024 Uiso 1 1 calc R U . . . C9 C 0.16439(15) -0.4418(5) 0.2864(2) 0.0232(7) Uani 1 1 d . . . . . H9A H 0.146182 -0.450392 0.210846 0.028 Uiso 1 1 calc R U . . . H9AB H 0.176479 -0.575468 0.322422 0.028 Uiso 1 1 calc R U . . . C10 C 0.20800(14) -0.2561(5) 0.3395(2) 0.0173(6) Uani 1 1 d . . . . . C11 C 0.26426(15) -0.2981(5) 0.4411(2) 0.0204(6) Uani 1 1 d . . . . . C12 C 0.31002(14) -0.0961(5) 0.3554(2) 0.0182(6) Uani 1 1 d . . . . . H12 H 0.331420 -0.171696 0.316912 0.022 Uiso 1 1 calc R U . . . C13 C 0.34304(14) 0.1121(5) 0.3871(2) 0.0211(6) Uani 1 1 d . . . . . H13 H 0.311188 0.226005 0.382172 0.025 Uiso 1 1 calc R U . . . C14 C 0.40268(16) 0.1759(5) 0.3724(2) 0.0251(7) Uani 1 1 d . . . . . C15 C 0.40670(18) 0.4001(6) 0.3491(3) 0.0308(8) Uani 1 1 d . . . . . H15A H 0.454591 0.439882 0.371085 0.037 Uiso 1 1 calc R U . . . H15B H 0.387964 0.485097 0.387417 0.037 Uiso 1 1 calc R U . . . C16 C 0.36610(18) 0.4384(5) 0.2327(3) 0.0323(8) Uani 1 1 d . . . . . H16A H 0.363008 0.587938 0.219077 0.039 Uiso 1 1 calc R U . . . H16B H 0.390079 0.374895 0.195603 0.039 Uiso 1 1 calc R U . . . C17 C 0.29632(18) 0.3501(5) 0.1941(3) 0.0278(7) Uani 1 1 d . . . . . H17 H 0.266133 0.419103 0.214921 0.033 Uiso 1 1 calc R U . . . C18 C 0.27139(16) 0.1868(5) 0.1343(2) 0.0246(7) Uani 1 1 d . . . . . C19 C 0.20401(15) 0.0971(5) 0.1176(2) 0.0254(7) Uani 1 1 d . . . . . H19A H 0.176809 0.075506 0.043138 0.030 Uiso 1 1 calc R U . . . H19B H 0.179788 0.198844 0.140319 0.030 Uiso 1 1 calc R U . . . C20 C 0.20742(15) -0.1065(5) 0.1730(2) 0.0224(6) Uani 1 1 d . . . . . H20A H 0.238162 -0.200808 0.159754 0.027 Uiso 1 1 calc R U . . . H20B H 0.161792 -0.169440 0.143109 0.027 Uiso 1 1 calc R U . . . C21 C 0.23189(14) -0.0884(5) 0.2897(2) 0.0178(6) Uani 1 1 d . . . . . H21 H 0.215340 0.045841 0.303653 0.021 Uiso 1 1 calc R U . . . C22 C 0.44088(16) 0.0309(6) 0.3360(3) 0.0312(8) Uani 1 1 d . . . . . H22A H 0.488733 0.070614 0.365673 0.047 Uiso 1 1 calc R U . . . H22B H 0.422048 0.036535 0.261039 0.047 Uiso 1 1 calc R U . . . H22C H 0.436818 -0.109100 0.357457 0.047 Uiso 1 1 calc R U . . . C23 C 0.30605(18) 0.0768(6) 0.0794(3) 0.0346(8) Uani 1 1 d . . . . . H23A H 0.275843 0.071416 0.005983 0.052 Uiso 1 1 calc R U . . . H23B H 0.317350 -0.063131 0.106344 0.052 Uiso 1 1 calc R U . . . H23C H 0.347629 0.150196 0.090117 0.052 Uiso 1 1 calc R U . . . N1 N -0.07844(14) 0.4416(5) 0.0080(2) 0.0303(7) Uani 1 1 d . . . . . O1 O 0.32154(10) -0.2090(3) 0.44857(15) 0.0218(5) Uani 1 1 d . . . . . O2 O 0.26356(11) -0.3988(4) 0.51046(16) 0.0289(5) Uani 1 1 d . . . . . O3 O 0.40846(11) 0.1257(4) 0.47372(16) 0.0284(5) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0180(15) 0.0270(17) 0.0275(16) -0.0055(15) 0.0092(13) -0.0036(14) C2 0.0169(14) 0.0255(17) 0.0256(16) -0.0010(13) 0.0108(12) -0.0007(12) C3 0.0214(15) 0.0272(18) 0.0214(15) -0.0044(14) 0.0088(13) -0.0034(13) C4 0.0236(15) 0.0228(16) 0.0208(14) -0.0049(13) 0.0095(12) -0.0025(13) C5 0.0158(14) 0.0248(17) 0.0203(14) -0.0020(12) 0.0098(12) -0.0032(12) C6 0.0191(14) 0.0272(17) 0.0196(15) -0.0043(13) 0.0070(12) -0.0013(13) C7 0.0191(14) 0.0252(17) 0.0302(17) -0.0072(14) 0.0113(13) -0.0002(13) C8 0.0205(14) 0.0222(16) 0.0199(14) 0.0000(13) 0.0102(12) -0.0046(13) C9 0.0237(15) 0.0190(16) 0.0239(16) -0.0006(13) 0.0076(13) -0.0034(13) C10 0.0172(13) 0.0177(15) 0.0163(13) 0.0016(12) 0.0066(11) -0.0003(11) C11 0.0216(15) 0.0171(15) 0.0220(15) 0.0006(13) 0.0090(12) 0.0027(12) C12 0.0216(14) 0.0187(15) 0.0156(13) 0.0030(12) 0.0095(11) 0.0010(13) C13 0.0208(14) 0.0224(16) 0.0187(14) -0.0007(13) 0.0071(11) 0.0008(13) C14 0.0241(15) 0.0294(18) 0.0232(15) -0.0067(14) 0.0115(12) -0.0066(14) C15 0.0333(18) 0.0272(18) 0.0392(19) -0.0096(16) 0.0225(15) -0.0080(15) C16 0.044(2) 0.0214(17) 0.042(2) -0.0015(16) 0.0284(17) -0.0060(16) C17 0.0392(19) 0.0214(17) 0.0297(16) 0.0085(14) 0.0216(15) 0.0079(14) C18 0.0335(17) 0.0234(17) 0.0201(15) 0.0072(13) 0.0148(13) 0.0043(14) C19 0.0281(16) 0.0292(18) 0.0176(14) 0.0055(14) 0.0089(12) 0.0053(15) C20 0.0233(15) 0.0266(17) 0.0162(14) 0.0010(13) 0.0075(12) -0.0008(13) C21 0.0201(14) 0.0163(14) 0.0175(14) 0.0014(12) 0.0086(11) 0.0018(12) C22 0.0231(16) 0.034(2) 0.039(2) -0.0074(16) 0.0154(15) -0.0035(14) C23 0.042(2) 0.038(2) 0.0311(18) -0.0061(17) 0.0231(16) -0.0056(18) N1 0.0245(14) 0.0310(16) 0.0301(15) -0.0010(14) 0.0068(12) 0.0030(13) O1 0.0189(10) 0.0262(12) 0.0176(10) 0.0065(9) 0.0055(8) 0.0018(9) O2 0.0304(12) 0.0345(14) 0.0211(11) 0.0111(11) 0.0104(9) 0.0004(11) O3 0.0233(11) 0.0371(14) 0.0222(11) -0.0044(10) 0.0076(9) -0.0070(10) 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 C1 N1 1.154(4) . ? C1 C2 1.440(5) . ? C2 C3 1.390(4) . ? C2 C7 1.398(4) . ? C3 C4 1.383(4) . ? C3 H3 0.9500 . ? C4 C5 1.396(4) . ? C4 H4 0.9500 . ? C5 C6 1.400(5) . ? C5 C8 1.488(4) . ? C6 C7 1.380(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.500(4) . ? C8 C10 1.523(4) . ? C8 H8 1.0000 . ? C9 C10 1.527(4) . ? C9 H9A 0.9900 . ? C9 H9AB 0.9900 . ? C10 C11 1.479(4) . ? C10 C21 1.520(4) . ? C11 O2 1.204(4) . ? C11 O1 1.344(4) . ? C12 O1 1.458(3) . ? C12 C13 1.512(4) . ? C12 C21 1.558(4) . ? C12 H12 1.0000 . ? C13 O3 1.442(3) . ? C13 C14 1.472(4) . ? C13 H13 1.0000 . ? C14 O3 1.454(4) . ? C14 C22 1.501(5) . ? C14 C15 1.510(5) . ? C15 C16 1.547(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.497(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.330(5) . ? C17 H17 0.9500 . ? C18 C23 1.498(4) . ? C18 C19 1.507(5) . ? C19 C20 1.535(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.540(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? 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 N1 C1 C2 175.8(3) . . ? C3 C2 C7 119.5(3) . . ? C3 C2 C1 120.5(3) . . ? C7 C2 C1 119.9(3) . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 121.1(3) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C6 118.2(3) . . ? C4 C5 C8 122.2(3) . . ? C6 C5 C8 119.6(3) . . ? C7 C6 C5 121.0(3) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C2 120.0(3) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? C5 C8 C9 121.7(3) . . ? C5 C8 C10 118.5(2) . . ? C9 C8 C10 60.67(19) . . ? C5 C8 H8 115.0 . . ? C9 C8 H8 115.0 . . ? C10 C8 H8 115.0 . . ? C8 C9 C10 60.41(19) . . ? C8 C9 H9A 117.7 . . ? C10 C9 H9A 117.7 . . ? C8 C9 H9AB 117.7 . . ? C10 C9 H9AB 117.7 . . ? H9A C9 H9AB 114.9 . . ? C11 C10 C21 107.1(2) . . ? C11 C10 C8 116.8(2) . . ? C21 C10 C8 125.5(2) . . ? C11 C10 C9 115.1(2) . . ? C21 C10 C9 126.9(2) . . ? C8 C10 C9 58.92(19) . . ? O2 C11 O1 121.1(3) . . ? O2 C11 C10 128.6(3) . . ? O1 C11 C10 110.3(2) . . ? O1 C12 C13 107.7(2) . . ? O1 C12 C21 106.6(2) . . ? C13 C12 C21 114.3(2) . . ? O1 C12 H12 109.4 . . ? C13 C12 H12 109.4 . . ? C21 C12 H12 109.4 . . ? O3 C13 C14 59.88(19) . . ? O3 C13 C12 118.9(3) . . ? C14 C13 C12 123.2(3) . . ? O3 C13 H13 114.6 . . ? C14 C13 H13 114.6 . . ? C12 C13 H13 114.6 . . ? O3 C14 C13 59.03(18) . . ? O3 C14 C22 113.2(3) . . ? C13 C14 C22 122.5(3) . . ? O3 C14 C15 117.0(3) . . ? C13 C14 C15 116.5(3) . . ? C22 C14 C15 115.8(3) . . ? C14 C15 C16 109.7(3) . . ? C14 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? C14 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C17 C16 C15 110.9(3) . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.0 . . ? C18 C17 C16 128.0(3) . . ? C18 C17 H17 116.0 . . ? C16 C17 H17 116.0 . . ? C17 C18 C23 124.6(3) . . ? C17 C18 C19 120.8(3) . . ? C23 C18 C19 114.6(3) . . ? C18 C19 C20 115.4(3) . . ? C18 C19 H19A 108.4 . . ? C20 C19 H19A 108.4 . . ? C18 C19 H19B 108.4 . . ? C20 C19 H19B 108.4 . . ? H19A C19 H19B 107.5 . . ? C19 C20 C21 115.0(3) . . ? C19 C20 H20A 108.5 . . ? C21 C20 H20A 108.5 . . ? C19 C20 H20B 108.5 . . ? C21 C20 H20B 108.5 . . ? H20A C20 H20B 107.5 . . ? C10 C21 C20 115.9(2) . . ? C10 C21 C12 101.6(2) . . ? C20 C21 C12 115.8(2) . . ? C10 C21 H21 107.7 . . ? C20 C21 H21 107.7 . . ? C12 C21 H21 107.7 . . ? C14 C22 H22A 109.5 . . ? C14 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C14 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C11 O1 C12 111.2(2) . . ? C13 O3 C14 61.09(19) . . ? 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 C7 C2 C3 C4 -4.8(4) . . . . ? C1 C2 C3 C4 170.4(3) . . . . ? C2 C3 C4 C5 1.3(4) . . . . ? C3 C4 C5 C6 3.4(4) . . . . ? C3 C4 C5 C8 -176.1(3) . . . . ? C4 C5 C6 C7 -4.7(4) . . . . ? C8 C5 C6 C7 174.9(3) . . . . ? C5 C6 C7 C2 1.3(5) . . . . ? C3 C2 C7 C6 3.5(5) . . . . ? C1 C2 C7 C6 -171.7(3) . . . . ? C4 C5 C8 C9 31.6(4) . . . . ? C6 C5 C8 C9 -148.0(3) . . . . ? C4 C5 C8 C10 103.0(3) . . . . ? C6 C5 C8 C10 -76.6(4) . . . . ? C5 C8 C9 C10 107.3(3) . . . . ? C5 C8 C10 C11 143.1(3) . . . . ? C9 C8 C10 C11 -104.5(3) . . . . ? C5 C8 C10 C21 3.1(4) . . . . ? C9 C8 C10 C21 115.5(3) . . . . ? C5 C8 C10 C9 -112.4(3) . . . . ? C8 C9 C10 C11 107.4(3) . . . . ? C8 C9 C10 C21 -113.3(3) . . . . ? C21 C10 C11 O2 169.0(3) . . . . ? C8 C10 C11 O2 22.2(5) . . . . ? C9 C10 C11 O2 -44.1(4) . . . . ? C21 C10 C11 O1 -12.4(3) . . . . ? C8 C10 C11 O1 -159.3(3) . . . . ? C9 C10 C11 O1 134.4(3) . . . . ? O1 C12 C13 O3 41.0(3) . . . . ? C21 C12 C13 O3 159.2(2) . . . . ? O1 C12 C13 C14 112.1(3) . . . . ? C21 C12 C13 C14 -129.7(3) . . . . ? C12 C13 C14 O3 -106.8(3) . . . . ? O3 C13 C14 C22 99.4(3) . . . . ? C12 C13 C14 C22 -7.4(5) . . . . ? O3 C13 C14 C15 -107.0(3) . . . . ? C12 C13 C14 C15 146.2(3) . . . . ? O3 C14 C15 C16 -151.8(3) . . . . ? C13 C14 C15 C16 -84.9(3) . . . . ? C22 C14 C15 C16 70.5(4) . . . . ? C14 C15 C16 C17 50.6(4) . . . . ? C15 C16 C17 C18 -109.1(4) . . . . ? C16 C17 C18 C23 -10.3(5) . . . . ? C16 C17 C18 C19 169.3(3) . . . . ? C17 C18 C19 C20 -106.3(4) . . . . ? C23 C18 C19 C20 73.3(3) . . . . ? C18 C19 C20 C21 73.1(3) . . . . ? C11 C10 C21 C20 143.7(3) . . . . ? C8 C10 C21 C20 -73.2(4) . . . . ? C9 C10 C21 C20 1.9(4) . . . . ? C11 C10 C21 C12 17.3(3) . . . . ? C8 C10 C21 C12 160.4(3) . . . . ? C9 C10 C21 C12 -124.5(3) . . . . ? C19 C20 C21 C10 154.3(3) . . . . ? C19 C20 C21 C12 -86.8(3) . . . . ? O1 C12 C21 C10 -16.6(3) . . . . ? C13 C12 C21 C10 -135.5(2) . . . . ? O1 C12 C21 C20 -143.1(3) . . . . ? C13 C12 C21 C20 98.1(3) . . . . ? O2 C11 O1 C12 179.9(3) . . . . ? C10 C11 O1 C12 1.2(3) . . . . ? C13 C12 O1 C11 133.3(2) . . . . ? C21 C12 O1 C11 10.3(3) . . . . ? C12 C13 O3 C14 113.8(3) . . . . ? C22 C14 O3 C13 -115.2(3) . . . . ? C15 C14 O3 C13 106.2(3) . . . . ? _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. ; _audit_block_code C23H25NO3_xv559_ofial _audit_creation_method 'APEX3 v2018.7-2' _shelxl_version_number ? _chemical_name_systematic ? _chemical_formula_moiety 'C23 H25 N O3' _chemical_formula_sum 'C23 H25 N O3' _chemical_formula_weight 363.44 #?# (Cohen, 1996) _chemical_melting_point ? #?# in K! _cell_formula_units_Z 4 #?# adjust to _chemical_formula_[] _exptl_crystal_density_diffrn 1.297 _exptl_crystal_F_000 776 #?# check! _shelx_res_file ; TITL xv559_0m_a.res in C2 xv559_0m_a.res created by SHELXL-2018/3 at 11:04:15 on 30-Aug-2019 REM Old TITL xv559_0m in C2 REM SHELXT solution in C2 REM R1 0.095, Rweak 0.035, Alpha 0.004, Orientation as input REM Flack x = -0.553 ( 0.569 ) from Parsons' quotients REM Formula found by SHELXT: C23 N O3 CELL 0.71073 21.9099 6.5137 14.4743 90.000 115.663 90.000 ZERR 4.000 0.0011 0.0004 0.0008 0.000 0.002 0.000 LATT -7 SYMM -X, Y, -Z SFAC C H N O UNIT 92 100 4 12 TEMP -170 SIZE 0.02 0.04 0.10 L.S. 10 BOND $H LIST 4 CONF ACTA SHEL 9.0 0.80 FMAP 2 PLAN -20 WGHT 0.043800 1.436100 FVAR 0.59342 C1 1 -0.049279 0.313978 0.065613 11.00000 0.01798 0.02697 = 0.02747 -0.00545 0.00924 -0.00356 C2 1 -0.008764 0.157885 0.135856 11.00000 0.01691 0.02551 = 0.02560 -0.00097 0.01083 -0.00066 C3 1 -0.011324 -0.044083 0.103364 11.00000 0.02141 0.02721 = 0.02141 -0.00438 0.00881 -0.00341 AFIX 43 H3 2 -0.044759 -0.084406 0.037886 11.00000 -1.20000 AFIX 0 C4 1 0.034787 -0.186323 0.166334 11.00000 0.02359 0.02277 = 0.02085 -0.00489 0.00950 -0.00253 AFIX 43 H4 2 0.033241 -0.323342 0.142933 11.00000 -1.20000 AFIX 0 C5 1 0.083556 -0.132053 0.263670 11.00000 0.01581 0.02480 = 0.02026 -0.00202 0.00983 -0.00321 C6 1 0.082292 0.067933 0.298324 11.00000 0.01913 0.02721 = 0.01960 -0.00431 0.00702 -0.00134 AFIX 43 H6 2 0.112828 0.105003 0.366234 11.00000 -1.20000 AFIX 0 C7 1 0.037335 0.211939 0.235261 11.00000 0.01910 0.02517 = 0.03024 -0.00715 0.01130 -0.00019 AFIX 43 H7 2 0.037704 0.347789 0.259379 11.00000 -1.20000 AFIX 0 C8 1 0.136422 -0.278528 0.330360 11.00000 0.02046 0.02218 = 0.01987 0.00002 0.01017 -0.00457 AFIX 13 H8 2 0.133604 -0.317125 0.395271 11.00000 -1.20000 AFIX 0 C9 1 0.164388 -0.441840 0.286392 11.00000 0.02373 0.01896 = 0.02392 -0.00060 0.00761 -0.00344 AFIX 23 H9A 2 0.146182 -0.450392 0.210846 11.00000 -1.20000 H9AB 2 0.176479 -0.575468 0.322422 11.00000 -1.20000 AFIX 0 C10 1 0.207999 -0.256087 0.339464 11.00000 0.01721 0.01773 = 0.01628 0.00157 0.00664 -0.00028 C11 1 0.264257 -0.298093 0.441138 11.00000 0.02164 0.01711 = 0.02197 0.00062 0.00895 0.00265 C12 1 0.310019 -0.096100 0.355449 11.00000 0.02161 0.01874 = 0.01563 0.00298 0.00946 0.00103 AFIX 13 H12 2 0.331420 -0.171696 0.316912 11.00000 -1.20000 AFIX 0 C13 1 0.343043 0.112089 0.387053 11.00000 0.02079 0.02236 = 0.01871 -0.00074 0.00707 0.00085 AFIX 13 H13 2 0.311188 0.226005 0.382172 11.00000 -1.20000 AFIX 0 C14 1 0.402682 0.175924 0.372351 11.00000 0.02410 0.02936 = 0.02322 -0.00668 0.01153 -0.00657 C15 1 0.406701 0.400104 0.349087 11.00000 0.03328 0.02719 = 0.03918 -0.00964 0.02250 -0.00802 AFIX 23 H15A 2 0.454591 0.439882 0.371085 11.00000 -1.20000 H15B 2 0.387964 0.485097 0.387417 11.00000 -1.20000 AFIX 0 C16 1 0.366099 0.438445 0.232701 11.00000 0.04435 0.02139 = 0.04155 -0.00150 0.02840 -0.00599 AFIX 23 H16A 2 0.363008 0.587938 0.219077 11.00000 -1.20000 H16B 2 0.390079 0.374895 0.195603 11.00000 -1.20000 AFIX 0 C17 1 0.296318 0.350090 0.194126 11.00000 0.03924 0.02145 = 0.02967 0.00851 0.02156 0.00793 AFIX 43 H17 2 0.266133 0.419103 0.214921 11.00000 -1.20000 AFIX 0 C18 1 0.271390 0.186823 0.134311 11.00000 0.03352 0.02344 = 0.02008 0.00717 0.01476 0.00430 C19 1 0.204013 0.097133 0.117591 11.00000 0.02814 0.02924 = 0.01757 0.00550 0.00886 0.00532 AFIX 23 H19A 2 0.176809 0.075506 0.043138 11.00000 -1.20000 H19B 2 0.179788 0.198844 0.140319 11.00000 -1.20000 AFIX 0 C20 1 0.207423 -0.106504 0.173040 11.00000 0.02334 0.02659 = 0.01622 0.00105 0.00752 -0.00075 AFIX 23 H20A 2 0.238162 -0.200808 0.159754 11.00000 -1.20000 H20B 2 0.161792 -0.169440 0.143109 11.00000 -1.20000 AFIX 0 C21 1 0.231892 -0.088406 0.289738 11.00000 0.02010 0.01635 = 0.01754 0.00144 0.00860 0.00179 AFIX 13 H21 2 0.215340 0.045841 0.303653 11.00000 -1.20000 AFIX 0 C22 1 0.440883 0.030918 0.335975 11.00000 0.02307 0.03361 = 0.03901 -0.00743 0.01542 -0.00350 AFIX 137 H22A 2 0.488733 0.070614 0.365673 11.00000 -1.50000 H22B 2 0.422048 0.036535 0.261039 11.00000 -1.50000 H22C 2 0.436818 -0.109100 0.357457 11.00000 -1.50000 AFIX 0 C23 1 0.306048 0.076821 0.079448 11.00000 0.04218 0.03840 = 0.03111 -0.00610 0.02314 -0.00561 AFIX 137 H23A 2 0.275843 0.071416 0.005983 11.00000 -1.50000 H23B 2 0.317350 -0.063131 0.106344 11.00000 -1.50000 H23C 2 0.347629 0.150196 0.090117 11.00000 -1.50000 AFIX 0 N1 3 -0.078437 0.441561 0.008015 11.00000 0.02446 0.03105 = 0.03010 -0.00103 0.00677 0.00303 O1 4 0.321544 -0.209005 0.448575 11.00000 0.01894 0.02618 = 0.01759 0.00649 0.00548 0.00183 O2 4 0.263564 -0.398771 0.510460 11.00000 0.03040 0.03452 = 0.02108 0.01112 0.01037 0.00038 O3 4 0.408459 0.125692 0.473718 11.00000 0.02332 0.03712 = 0.02218 -0.00445 0.00758 -0.00702 HKLF 4 REM xv559_0m_a.res in C2 REM wR2 = 0.104050, GooF = S = 1.06952, Restrained GooF = 1.06937 for all data REM R1 = 0.042282 for 3410 Fo > 4sig(Fo) and 0.048876 for all 3790 data REM 246 parameters refined using 1 restraints END WGHT 0.0438 1.4363 REM Highest difference peak 0.177, deepest hole -0.185, 1-sigma level 0.044 Q1 1 0.0758 -0.1182 0.2027 11.00000 0.05 0.17 Q2 1 0.0596 0.3644 0.2480 11.00000 0.05 0.16 Q3 1 0.2886 0.4255 0.2643 11.00000 0.05 0.16 Q4 1 0.4392 -0.2471 0.5159 11.00000 0.05 0.16 Q5 1 0.1630 -0.3794 0.4690 11.00000 0.05 0.16 Q6 1 0.3604 0.1445 0.3527 11.00000 0.05 0.16 Q7 1 0.4492 -0.3357 0.4391 11.00000 0.05 0.15 Q8 1 0.1331 0.2877 0.4180 11.00000 0.05 0.15 Q9 1 0.2080 -0.1678 0.3018 11.00000 0.05 0.15 Q10 1 0.1407 -0.5405 0.1385 11.00000 0.05 0.15 Q11 1 0.1459 -0.0982 0.1420 11.00000 0.05 0.15 Q12 1 0.4896 0.4102 0.2915 11.00000 0.05 0.14 Q13 1 0.3509 -0.2247 0.2402 11.00000 0.05 0.14 Q14 1 0.3678 0.0639 0.1002 11.00000 0.05 0.14 Q15 1 0.3999 -0.0369 0.2181 11.00000 0.05 0.14 Q16 1 0.2113 -0.3695 0.2978 11.00000 0.05 0.14 Q17 1 0.3060 -0.0435 -0.0515 11.00000 0.05 0.14 Q18 1 0.1726 -0.0986 0.3681 11.00000 0.05 0.14 Q19 1 0.4285 -0.1432 0.4094 11.00000 0.05 0.14 Q20 1 0.2206 -0.0912 0.2324 11.00000 0.05 0.14 ; _shelx_res_checksum 55658 _shelx_hkl_file ; -4 0 0 464.55 13.10 4 0 0 472.05 13.40 4 0 0 467.95 12.20 -4 0 0 480.95 12.10 6 0 0 611.34 15.90 -6 0 0 622.24 15.60 6 0 0 605.34 17.60 -6 0 0 562.04 17.10 -8 0 0 1054.99 26.40 -8 0 0 961.80 27.60 8 0 0 1025.10 28.50 -8 0 0 1050.59 25.60 10 0 0 389.26 15.20 -10 0 0 355.46 15.60 -10 0 0 378.76 12.60 -10 0 0 380.96 11.70 -12 0 0 165.58 7.10 12 0 0 176.78 10.70 -12 0 0 187.98 10.20 -12 0 0 181.48 8.50 14 0 0 21.60 5.90 -14 0 0 30.00 3.70 -14 0 0 27.40 4.40 -14 0 0 22.00 5.20 16 0 0 145.99 11.60 -16 0 0 129.99 6.60 -16 0 0 135.09 10.40 -16 0 0 134.09 8.00 -18 0 0 129.89 6.70 18 0 0 107.99 11.50 -18 0 0 128.49 7.70 -18 0 0 144.59 11.60 -20 0 0 22.10 4.20 -20 0 0 20.40 3.40 22 0 0 168.18 15.30 -22 0 0 173.88 7.30 -22 0 0 190.08 8.50 24 0 0 52.49 11.30 1 -1 0 763.92 18.50 1 -1 0 699.73 18.50 -1 -1 0 636.94 18.70 1 1 0 715.73 19.00 -1 1 0 768.22 18.40 -1 1 0 733.33 18.70 1 1 0 749.13 19.50 3 -1 0 2099.29 49.40 3 -1 0 2150.48 49.90 -3 -1 0 2138.49 51.89 -3 -1 0 2178.48 51.79 -3 -1 0 2213.78 51.79 -3 1 0 2209.28 50.09 3 1 0 2234.68 52.09 3 1 0 2083.19 51.69 -3 1 0 2119.79 49.50 -5 -1 0 998.00 25.90 5 -1 0 925.81 24.10 5 -1 0 973.70 22.10 -5 -1 0 967.80 26.30 -5 -1 0 966.10 26.30 -5 1 0 966.20 22.50 -5 1 0 865.11 24.10 5 1 0 971.30 26.60 7 -1 0 86.39 3.20 7 -1 0 95.49 5.70 -7 -1 0 93.19 6.70 -7 -1 0 90.49 7.00 -7 -1 0 87.09 6.30 7 1 0 97.99 7.80 -7 1 0 88.59 3.30 -7 1 0 89.29 5.50 -9 -1 0 3436.66 79.79 9 -1 0 3256.17 74.69 -9 -1 0 3397.16 81.29 -9 -1 0 3309.27 80.49 9 -1 0 3339.67 79.29 -9 1 0 3363.26 74.59 -9 1 0 3185.58 78.79 9 1 0 3345.27 82.29 -11 -1 0 283.87 11.90 -11 -1 0 281.27 13.10 -11 -1 0 297.27 12.90 11 -1 0 275.77 12.30 11 1 0 289.37 14.60 -11 1 0 275.67 7.70 -11 1 0 271.47 11.90 -11 1 0 298.07 8.20 -13 -1 0 89.49 6.90 13 -1 0 98.69 8.10 -13 -1 0 94.69 7.70 -13 -1 0 92.99 8.10 -13 1 0 86.99 3.80 -13 1 0 99.09 7.60 13 1 0 71.99 8.40 -13 1 0 86.69 3.40 15 -1 0 6.60 4.00 -15 -1 0 7.30 3.30 -15 -1 0 4.40 3.90 -15 -1 0 2.50 4.00 -15 1 0 2.50 3.90 15 1 0 13.50 5.00 17 -1 0 559.34 22.90 -17 -1 0 565.24 21.60 -17 -1 0 550.44 22.90 -17 -1 0 582.44 21.50 17 1 0 545.95 25.10 -17 1 0 560.94 21.90 -19 -1 0 119.39 9.60 -19 -1 0 96.19 7.60 19 -1 0 112.49 10.90 -19 1 0 112.99 10.00 19 1 0 99.29 21.20 21 -1 0 26.10 7.80 -21 -1 0 4.30 3.70 -21 -1 0 13.30 5.00 21 1 0 18.80 8.00 23 -1 0 1.30 5.40 -23 -1 0 2.30 3.50 -23 -1 0 12.00 5.10 23 1 0 6.60 7.30 0 -2 0 172.18 8.30 0 -2 0 178.18 8.90 0 2 0 176.08 8.40 0 2 0 181.08 9.20 2 -2 0 292.67 10.50 2 -2 0 311.47 11.50 2 -2 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0 -15 59.79 9.70 10 0 -15 68.19 9.30 10 0 -15 65.69 10.80 -10 0 15 52.19 9.70 8 0 -15 3.00 4.20 8 0 -15 -0.60 4.30 8 0 -15 0.60 4.80 6 0 -15 -1.30 4.10 6 0 -15 7.30 5.40 6 0 -15 8.70 5.40 4 0 -15 168.08 14.30 4 0 -15 148.99 11.00 4 0 -15 168.48 12.50 2 0 -15 1.50 4.90 2 0 -15 2.20 3.90 0 0 -15 24.50 6.10 0 0 -15 26.50 6.20 0 0 -15 21.40 7.00 -2 0 -15 2.10 5.30 -2 0 -15 1.40 4.00 -2 0 -15 3.20 7.10 23 -1 -15 66.79 10.00 23 -1 -15 62.79 11.10 23 1 -15 56.49 10.70 21 -1 -15 97.49 10.40 21 -1 -15 107.89 14.10 21 1 -15 117.19 13.70 21 1 -15 123.69 13.10 19 -1 -15 70.59 10.50 19 -1 -15 96.89 13.70 19 1 -15 74.99 11.90 19 1 -15 81.39 11.60 17 -1 -15 85.99 10.20 17 -1 -15 68.69 10.90 17 1 -15 73.19 10.80 17 1 -15 78.29 12.20 15 -1 -15 18.70 7.20 15 -1 -15 23.30 7.10 15 1 -15 36.50 8.60 15 1 -15 38.40 8.10 13 -1 -15 38.40 8.00 -13 -1 15 24.70 7.40 13 -1 -15 48.70 9.40 13 1 -15 41.60 9.70 13 1 -15 42.30 8.40 11 -1 -15 75.49 10.90 -11 -1 15 82.09 10.80 11 -1 -15 79.89 10.70 11 1 -15 94.99 13.50 11 1 -15 83.69 9.00 -9 -1 15 15.10 5.80 9 -1 -15 14.90 7.30 9 -1 -15 19.30 7.30 9 1 -15 3.40 4.30 9 1 -15 11.10 5.90 7 -1 -15 14.00 7.30 7 -1 -15 8.90 5.20 7 -1 -15 5.20 6.10 7 1 -15 11.80 6.50 7 1 -15 11.50 5.20 7 1 -15 14.40 4.90 5 -1 -15 74.09 10.40 5 -1 -15 58.89 9.70 5 -1 -15 42.20 8.70 5 1 -15 57.19 7.30 5 1 -15 52.69 7.70 5 1 -15 46.60 10.00 3 -1 -15 116.39 12.80 3 -1 -15 105.39 10.30 3 -1 -15 107.19 12.00 3 1 -15 106.49 14.50 3 1 -15 110.39 9.10 3 1 -15 95.39 7.60 1 -1 -15 43.10 8.30 1 -1 -15 46.30 8.20 1 -1 -15 31.90 8.30 1 1 -15 46.40 6.40 1 1 -15 69.39 12.00 -1 -1 -15 76.19 10.10 -1 -1 -15 68.69 9.60 -1 -1 -15 84.69 12.50 -1 1 -15 110.89 12.80 -1 1 -15 69.09 6.00 -3 -1 -15 55.39 9.00 -3 -1 -15 59.49 12.70 -3 -1 -15 68.89 12.60 -3 1 -15 54.69 11.10 -3 1 -15 57.19 5.90 -3 1 -15 41.30 5.00 22 -2 -15 16.00 5.60 22 -2 -15 12.00 7.80 22 2 -15 28.60 7.90 22 2 -15 37.40 9.40 20 -2 -15 -1.30 5.20 20 -2 -15 19.50 5.70 20 2 -15 11.70 7.20 20 2 -15 7.70 6.10 18 -2 -15 0.60 4.80 18 -2 -15 1.90 4.60 18 2 -15 -3.20 5.00 18 2 -15 -2.90 5.40 16 -2 -15 19.10 7.00 16 -2 -15 30.70 7.30 16 2 -15 24.40 8.40 16 2 -15 15.20 5.80 14 -2 -15 146.09 13.80 -14 -2 15 124.49 12.10 14 -2 -15 133.29 12.50 14 2 -15 118.69 13.70 14 2 -15 146.19 12.00 12 -2 -15 93.89 12.90 12 -2 -15 100.29 10.50 -12 -2 15 74.99 10.20 12 2 -15 109.89 13.10 12 2 -15 95.79 9.80 10 -2 -15 3.00 4.90 -10 -2 15 1.70 3.60 10 -2 -15 -1.20 4.40 10 2 -15 3.40 4.10 10 2 -15 5.30 5.60 8 -2 -15 29.00 7.20 8 -2 -15 26.00 7.30 8 2 -15 26.40 5.40 8 2 -15 30.60 5.80 8 2 -15 17.10 7.60 6 -2 -15 125.99 12.60 6 -2 -15 108.89 11.80 6 2 -15 109.49 9.30 6 2 -15 122.09 9.10 6 2 -15 137.39 14.10 4 -2 -15 33.60 7.40 4 -2 -15 45.60 9.40 4 2 -15 41.10 10.00 4 2 -15 34.80 4.60 4 2 -15 37.70 5.30 2 -2 -15 5.90 5.60 2 -2 -15 0.60 5.00 2 2 -15 14.80 7.90 0 -2 -15 52.09 9.40 0 -2 -15 61.49 12.30 0 2 -15 70.39 12.20 -2 -2 -15 79.39 12.00 -2 -2 -15 100.89 11.70 -2 2 -15 95.49 14.70 19 -3 -15 38.80 7.70 19 -3 -15 34.90 9.50 19 3 -15 49.80 10.10 19 3 -15 41.50 9.90 17 -3 -15 -2.00 5.30 17 -3 -15 1.80 4.40 17 3 -15 5.00 7.10 17 3 -15 6.70 5.60 15 -3 -15 115.59 11.40 15 -3 -15 144.29 14.00 15 3 -15 112.69 18.40 15 3 -15 128.29 14.60 13 -3 -15 8.90 5.80 -13 -3 15 2.90 5.40 13 -3 -15 1.60 5.50 13 3 -15 7.50 4.90 13 3 -15 8.70 6.80 11 -3 -15 163.88 14.90 -11 -3 15 140.39 11.30 11 -3 -15 140.59 13.30 11 3 -15 149.49 11.00 11 3 -15 152.88 15.80 -9 -3 15 53.09 7.50 9 -3 -15 42.00 8.70 9 -3 -15 43.80 10.00 9 3 -15 26.40 8.80 9 3 -15 45.90 6.30 7 -3 -15 0.60 5.50 7 -3 -15 15.00 5.90 7 3 -15 9.60 6.70 7 3 -15 13.00 3.50 5 -3 -15 168.18 15.00 5 -3 -15 149.69 14.30 5 3 -15 155.38 15.60 3 -3 -15 4.80 5.40 3 -3 -15 -6.40 5.70 3 3 -15 17.10 7.10 1 -3 -15 43.60 9.50 1 -3 -15 36.30 9.10 1 3 -15 46.40 12.00 16 -4 -15 67.39 12.20 16 -4 -15 77.79 11.00 16 4 -15 82.59 11.10 16 4 -15 86.09 14.40 14 -4 -15 2.50 4.80 14 -4 -15 -0.30 6.10 -14 -4 15 -3.10 5.20 14 4 -15 1.40 7.30 14 4 -15 3.60 5.10 12 -4 -15 5.00 12.10 -12 -4 15 11.80 5.40 12 -4 -15 27.30 7.40 12 4 -15 17.70 5.80 12 4 -15 24.80 9.20 10 -4 -15 63.89 10.50 10 -4 -15 95.19 14.40 -10 -4 15 70.09 7.90 10 4 -15 69.49 20.30 10 4 -15 87.99 8.40 8 -4 -15 34.40 9.20 8 -4 -15 20.40 7.50 8 4 -15 43.70 15.70 8 4 -15 36.20 4.70 6 -4 -15 5.10 6.30 6 4 -15 19.10 8.70 4 -4 -15 8.00 5.90 4 -4 -15 3.90 6.70 4 4 -15 13.50 7.90 22 0 -16 7.50 5.30 22 0 -16 -20.10 8.20 20 0 -16 7.10 6.40 20 0 -16 3.10 5.50 18 0 -16 -2.40 5.50 18 0 -16 0.10 4.40 16 0 -16 175.98 15.50 16 0 -16 148.59 13.40 14 0 -16 33.30 8.10 14 0 -16 30.50 8.10 12 0 -16 33.80 8.80 12 0 -16 13.20 5.60 10 0 -16 13.80 6.40 10 0 -16 13.20 5.80 8 0 -16 1.30 4.20 8 0 -16 5.10 5.60 8 0 -16 4.90 5.10 6 0 -16 496.85 23.20 6 0 -16 454.45 20.20 6 0 -16 498.45 25.50 4 0 -16 127.29 13.40 4 0 -16 110.29 10.20 2 0 -16 58.89 10.80 2 0 -16 83.29 9.80 2 0 -16 78.09 9.00 0 0 -16 7.60 4.50 0 0 -16 20.80 7.90 0 0 -16 12.70 6.50 21 -1 -16 72.59 10.70 21 -1 -16 47.40 15.90 21 1 -16 72.69 12.60 21 1 -16 46.30 10.00 19 -1 -16 29.10 7.90 19 -1 -16 47.90 10.40 19 1 -16 35.00 8.90 19 1 -16 46.10 10.60 17 -1 -16 32.20 7.70 17 -1 -16 12.80 6.60 17 1 -16 41.80 10.00 17 1 -16 9.40 6.20 15 -1 -16 27.20 7.40 15 -1 -16 34.80 8.90 15 1 -16 42.10 9.60 15 1 -16 38.30 8.00 13 -1 -16 10.90 6.30 13 -1 -16 3.80 5.60 13 1 -16 16.10 6.90 13 1 -16 12.80 6.90 11 -1 -16 14.50 6.30 -11 -1 16 17.70 6.40 11 -1 -16 26.00 7.40 11 1 -16 28.70 9.30 11 1 -16 16.40 5.60 9 -1 -16 3.00 4.70 9 -1 -16 0.90 5.10 9 1 -16 -0.90 4.00 9 1 -16 4.50 5.90 7 -1 -16 -2.80 4.20 7 -1 -16 -1.50 5.10 7 1 -16 -1.80 4.70 7 1 -16 2.10 4.20 7 1 -16 -6.20 3.70 5 -1 -16 19.80 7.10 5 1 -16 27.00 6.20 5 1 -16 17.30 4.80 5 1 -16 18.50 7.50 3 -1 -16 50.59 10.50 3 1 -16 67.69 6.80 3 1 -16 76.59 8.60 3 1 -16 85.89 13.60 1 -1 -16 27.90 8.60 1 1 -16 30.50 6.10 20 -2 -16 17.30 7.60 20 -2 -16 22.20 6.30 20 2 -16 18.10 7.40 20 2 -16 29.40 8.90 18 -2 -16 21.30 7.30 18 -2 -16 11.60 6.60 18 2 -16 31.50 9.60 18 2 -16 38.90 8.70 16 -2 -16 66.69 10.30 16 -2 -16 70.49 11.40 16 2 -16 77.39 13.80 16 2 -16 67.99 10.10 14 -2 -16 101.89 11.50 14 -2 -16 85.19 12.10 14 2 -16 89.89 13.00 14 2 -16 112.49 13.50 12 -2 -16 -5.90 4.10 12 -2 -16 4.40 5.80 -12 -2 16 -9.50 4.60 12 2 -16 3.20 4.40 12 2 -16 2.40 6.60 -10 -2 16 39.90 7.90 10 -2 -16 57.29 10.00 10 -2 -16 50.69 10.00 10 2 -16 50.99 7.70 10 2 -16 63.99 11.80 8 -2 -16 70.39 11.40 8 -2 -16 83.79 12.20 8 2 -16 78.69 7.50 8 2 -16 74.69 8.50 8 2 -16 85.09 13.80 6 -2 -16 12.50 6.50 6 -2 -16 9.50 6.40 6 2 -16 11.50 6.40 6 2 -16 16.50 4.90 6 2 -16 11.10 3.90 4 -2 -16 44.80 9.30 4 2 -16 28.20 9.00 4 2 -16 37.10 4.50 4 2 -16 43.20 5.50 2 -2 -16 56.49 10.00 2 -2 -16 65.59 10.10 2 2 -16 58.39 13.90 17 -3 -16 36.80 9.90 17 -3 -16 45.10 9.30 17 3 -16 33.80 10.30 17 3 -16 48.00 9.00 15 -3 -16 204.68 28.90 15 -3 -16 164.48 14.20 15 3 -16 160.48 13.20 13 -3 -16 21.50 7.20 -13 -3 16 13.40 6.40 13 -3 -16 15.20 7.40 13 3 -16 27.90 6.50 -11 -3 16 33.40 7.00 11 -3 -16 36.60 8.70 11 -3 -16 37.90 10.10 11 3 -16 42.70 7.00 9 -3 -16 4.80 4.90 9 -3 -16 -3.90 5.40 9 3 -16 13.20 5.00 9 3 -16 9.60 4.10 7 -3 -16 78.19 12.40 7 3 -16 85.59 9.10 7 3 -16 75.29 15.70 7 3 -16 80.39 6.30 5 -3 -16 78.59 12.60 5 -3 -16 75.99 12.20 5 3 -16 120.19 14.60 18 0 -17 29.50 7.80 18 0 -17 25.20 8.10 16 0 -17 73.39 10.80 16 0 -17 102.99 14.50 14 0 -17 17.90 7.40 14 0 -17 4.50 5.90 12 0 -17 106.09 12.40 12 0 -17 79.19 11.20 10 0 -17 -2.30 4.20 10 0 -17 -3.40 4.80 8 0 -17 -4.80 4.30 8 0 -17 5.60 5.30 6 0 -17 100.89 10.00 6 0 -17 111.99 12.20 6 0 -17 86.69 20.70 4 0 -17 19.90 7.30 4 0 -17 34.50 8.10 4 0 -17 30.00 6.80 19 -1 -17 0.70 10.70 19 -1 -17 15.80 6.60 19 1 -17 4.70 6.40 19 1 -17 0.90 5.80 17 -1 -17 60.19 11.20 17 -1 -17 101.29 11.40 17 1 -17 71.19 11.10 17 1 -17 104.59 12.70 15 -1 -17 54.19 10.60 15 -1 -17 52.59 10.20 15 1 -17 87.89 11.70 15 1 -17 78.39 13.30 13 -1 -17 47.30 9.20 13 -1 -17 31.20 8.30 13 1 -17 50.19 9.10 13 1 -17 47.50 10.60 11 -1 -17 62.09 11.40 11 -1 -17 58.19 9.40 11 1 -17 44.60 10.50 11 1 -17 49.20 8.30 11 1 -17 53.99 11.30 9 -1 -17 63.99 10.30 9 -1 -17 59.89 11.00 9 1 -17 52.29 8.10 9 1 -17 60.49 12.70 9 1 -17 44.20 8.50 7 -1 -17 8.00 6.20 7 1 -17 22.80 6.70 7 1 -17 7.40 4.80 5 -1 -17 15.10 6.30 5 -1 -17 15.20 6.90 5 1 -17 14.50 7.30 5 1 -17 2.70 4.50 5 1 -17 8.50 6.40 16 -2 -17 57.39 11.20 16 -2 -17 39.10 9.00 16 2 -17 49.70 13.80 16 2 -17 53.19 8.80 14 -2 -17 42.50 9.80 14 -2 -17 35.20 9.00 14 2 -17 28.50 6.70 14 2 -17 27.50 10.60 12 -2 -17 14.30 7.00 -12 -2 17 0.20 5.60 12 -2 -17 19.00 6.90 12 2 -17 19.10 8.70 12 2 -17 8.50 5.20 10 -2 -17 169.78 24.80 10 -2 -17 116.59 13.60 10 2 -17 166.18 11.40 10 2 -17 163.68 15.80 10 2 -17 144.79 13.30 8 -2 -17 29.70 8.30 8 -2 -17 20.70 8.40 8 2 -17 18.90 8.50 8 2 -17 26.80 5.40 8 2 -17 17.30 6.20 6 -2 -17 8.00 5.80 6 -2 -17 5.20 6.70 6 2 -17 11.80 8.10 6 2 -17 9.80 6.50 6 2 -17 -0.80 5.70 14 0 -18 29.00 9.20 14 0 -18 13.70 7.20 12 0 -18 0.30 5.50 12 0 -18 4.00 5.50 10 0 -18 44.30 10.20 10 0 -18 41.80 8.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 7610 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_vv592 _database_code_depnum_ccdc_archive 'CCDC 2044220' loop_ _audit_author_name _audit_author_address 'Peter Mayer' ;LMU Muenchen Germany ; _audit_update_record ; 2020-11-13 deposited with the CCDC. 2021-02-09 downloaded from the CCDC. ; _chemical_name_common RM445-4-8 _chemical_compound_source ? _chemical_absolute_configuration ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.080 #?# in millimeters _exptl_crystal_size_mid 0.060 #?# in millimeters _exptl_crystal_size_min 0.030 #?# in millimeters _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_special_details ; ; _audit_creation_date ? #?# style: 18-Aug-1998 _diffrn_ambient_temperature 103.(2) #?# in K _diffrn_source_type 'Bruker TXS' _diffrn_source_power 2.5 #?# in kW _diffrn_source_voltage 50 #?# in kV _diffrn_source_current 50 #?# in mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode (TXS)' _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_collimation ? _diffrn_measurement_device 'fixed-chi three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture TXS' _diffrn_measurement_method 'mix of phi and omega scans' _diffrn_measurement_details ? _diffrn_detector_area_resol_mean 7.4074 _diffrn_special_details ? _diffrn_orient_matrix_type ? _diffrn_orient_matrix_UB_11 ? _diffrn_orient_matrix_UB_12 ? _diffrn_orient_matrix_UB_13 ? _diffrn_orient_matrix_UB_21 ? _diffrn_orient_matrix_UB_22 ? _diffrn_orient_matrix_UB_23 ? _diffrn_orient_matrix_UB_31 ? _diffrn_orient_matrix_UB_32 ? _diffrn_orient_matrix_UB_33 ? _cell_length_a 7.3211(2) _cell_length_b 7.9973(2) _cell_length_c 8.7918(3) _cell_angle_alpha 69.1780(10) _cell_angle_beta 74.1170(10) _cell_angle_gamma 83.7140(10) _cell_volume 462.72(2) _cell_measurement_temperature 103.(2) #?# in K _cell_measurement_reflns_used 7233 _cell_measurement_theta_min 2.8930 _cell_measurement_theta_max 27.1291 _cell_special_details ? _exptl_absorpt_coefficient_mu 0.291 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.9226 _exptl_absorpt_correction_T_max 0.9705 _shelx_estimated_absorpt_T_min 0.977 _shelx_estimated_absorpt_T_max 0.991 _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _diffrn_reflns_number 8722 #xl _diffrn_reflns_av_R_equivalents 0.0244 #xl _diffrn_reflns_av_unetI/netI 0.0205 #xl _diffrn_reflns_limit_h_min -9 #xl _diffrn_reflns_limit_h_max 9 #xl _diffrn_reflns_limit_k_min -10 #xl _diffrn_reflns_limit_k_max 10 #xl _diffrn_reflns_limit_l_min -11 #xl _diffrn_reflns_limit_l_max 11 #xl _diffrn_reflns_theta_min 3.345 #xl _diffrn_reflns_theta_max 27.099 #xl _diffrn_measured_fraction_theta_max 0.994 #xl _diffrn_reflns_theta_full 25.242 #xl _diffrn_measured_fraction_theta_full 0.994 #xl _diffrn_reflns_Laue_measured_fraction_max 0.994 #xl _diffrn_reflns_Laue_measured_fraction_full 0.994 #xl _diffrn_reflns_point_group_measured_fraction_max 0.994 #xl _diffrn_reflns_point_group_measured_fraction_full 0.994 #xl _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _space_group_IT_number 2 _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _reflns_number_total 2031 #xl _reflns_number_gt 1867 #xl _reflns_threshold_expression 'I > 2\s(I)' #xl _reflns_Friedel_coverage 0.000 #xl _reflns_Friedel_fraction_max . #xl _reflns_Friedel_fraction_full . #xl _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. ; _refine_ls_structure_factor_coef Fsqd #xl _refine_ls_matrix_type full #xl _refine_ls_weighting_scheme calc #xl _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+0.2230P] where P=(Fo^2^+2Fc^2^)/3' #xl _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr #?# _refine_ls_extinction_method none #xl _refine_ls_extinction_coef . #xl _refine_ls_abs_structure_details ? #xl _refine_ls_abs_structure_Flack ? #xl _refine_ls_number_reflns 2031 #xl _refine_ls_number_parameters 111 #xl _refine_ls_number_restraints 0 #xl _refine_ls_R_factor_all 0.0299 #xl _refine_ls_R_factor_gt 0.0266 #xl _refine_ls_wR_factor_ref 0.0704 #xl _refine_ls_wR_factor_gt 0.0679 #xl _refine_ls_goodness_of_fit_ref 1.065 #xl _refine_ls_restrained_S_all 1.065 #xl _refine_ls_shift/su_max 0.000 #xl _refine_ls_shift/su_mean 0.000 #xl _refine_diff_density_max 0.295 #xl _refine_diff_density_min -0.192 #xl _refine_diff_density_rms 0.042 #xl _refine_special_details ; ; _computing_data_collection 'APEX3 v2016.5-0, Bruker AXS (2016)' _computing_cell_refinement 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_data_reduction 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_structure_solution 'XT, VERSION 2014/5' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 807)' _computing_publication_material ? 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 S1 S 0.71638(4) 0.87135(4) -0.01904(4) 0.01966(10) Uani 1 1 d . . . . . N1 N 1.04059(16) 0.16649(14) 0.57166(15) 0.0251(2) Uani 1 1 d . . . . . C1 C 0.60882(17) 0.77742(16) 0.20614(15) 0.0183(2) Uani 1 1 d . . . . . H1A H 0.6740 0.8254 0.2665 0.022 Uiso 1 1 calc R U . . . H1B H 0.4740 0.8163 0.2293 0.022 Uiso 1 1 calc R U . . . C2 C 0.61912(16) 0.57617(15) 0.27329(14) 0.0156(2) Uani 1 1 d . . . . . C3 C 0.49254(16) 0.46928(16) 0.25347(14) 0.0165(2) Uani 1 1 d . . . . . C4 C 0.51368(17) 0.28376(16) 0.31422(15) 0.0182(2) Uani 1 1 d . . . . . H4 H 0.4290 0.2117 0.3002 0.022 Uiso 1 1 calc R U . . . C5 C 0.65491(17) 0.20136(16) 0.39462(15) 0.0174(2) Uani 1 1 d . . . . . H5 H 0.6677 0.0747 0.4344 0.021 Uiso 1 1 calc R U . . . C6 C 0.77811(16) 0.30805(15) 0.41601(14) 0.0159(2) Uani 1 1 d . . . . . C7 C 0.75967(16) 0.49433(15) 0.35551(14) 0.0163(2) Uani 1 1 d . . . . . H7 H 0.8440 0.5658 0.3707 0.020 Uiso 1 1 calc R U . . . C8 C 0.33383(17) 0.55203(17) 0.17074(16) 0.0212(3) Uani 1 1 d . . . . . H8A H 0.2722 0.4591 0.1545 0.032 Uiso 1 1 calc R U . . . H8B H 0.3855 0.6431 0.0615 0.032 Uiso 1 1 calc R U . . . H8C H 0.2405 0.6077 0.2425 0.032 Uiso 1 1 calc R U . . . C9 C 0.92439(17) 0.22752(15) 0.50200(15) 0.0178(2) Uani 1 1 d . . . . . C10 C 0.95868(18) 0.79601(17) -0.02550(17) 0.0246(3) Uani 1 1 d . . . . . H10A H 1.0394 0.8538 -0.1384 0.037 Uiso 1 1 calc R U . . . H10B H 0.9661 0.6659 0.0017 0.037 Uiso 1 1 calc R U . . . H10C H 1.0024 0.8273 0.0567 0.037 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.02072(16) 0.01741(16) 0.01801(16) -0.00175(11) -0.00643(11) 0.00048(11) N1 0.0271(6) 0.0199(5) 0.0318(6) -0.0080(5) -0.0151(5) 0.0027(4) C1 0.0193(6) 0.0172(6) 0.0177(6) -0.0054(5) -0.0052(4) 0.0024(4) C2 0.0161(5) 0.0164(5) 0.0124(5) -0.0045(4) -0.0015(4) 0.0009(4) C3 0.0138(5) 0.0216(6) 0.0127(5) -0.0051(4) -0.0023(4) 0.0007(4) C4 0.0163(6) 0.0208(6) 0.0173(6) -0.0061(5) -0.0031(4) -0.0035(4) C5 0.0178(6) 0.0154(5) 0.0167(5) -0.0036(4) -0.0028(4) -0.0010(4) C6 0.0149(5) 0.0174(6) 0.0140(5) -0.0043(4) -0.0033(4) 0.0008(4) C7 0.0161(5) 0.0176(6) 0.0154(5) -0.0059(4) -0.0035(4) -0.0011(4) C8 0.0176(6) 0.0243(6) 0.0220(6) -0.0069(5) -0.0077(5) 0.0017(5) C9 0.0198(6) 0.0141(5) 0.0195(6) -0.0055(4) -0.0048(5) -0.0007(4) C10 0.0199(6) 0.0222(6) 0.0265(7) -0.0056(5) -0.0020(5) 0.0014(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 S1 C10 1.8023(13) . ? S1 C1 1.8228(12) . ? N1 C9 1.1484(16) . ? C1 C2 1.5056(16) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.3903(16) . ? C2 C3 1.4098(17) . ? C3 C4 1.3936(17) . ? C3 C8 1.5063(16) . ? C4 C5 1.3866(16) . ? C4 H4 0.9500 . ? C5 C6 1.3973(16) . ? C5 H5 0.9500 . ? C6 C7 1.3973(16) . ? C6 C9 1.4419(16) . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 C10 S1 C1 100.28(6) . . ? C2 C1 S1 113.04(8) . . ? C2 C1 H1A 109.0 . . ? S1 C1 H1A 109.0 . . ? C2 C1 H1B 109.0 . . ? S1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C7 C2 C3 119.37(11) . . ? C7 C2 C1 118.58(10) . . ? C3 C2 C1 122.05(11) . . ? C4 C3 C2 119.07(11) . . ? C4 C3 C8 119.75(11) . . ? C2 C3 C8 121.17(11) . . ? C5 C4 C3 121.83(11) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 118.78(11) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C7 C6 C5 120.26(11) . . ? C7 C6 C9 119.22(10) . . ? C5 C6 C9 120.52(10) . . ? C2 C7 C6 120.67(11) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C6 178.51(13) . . ? S1 C10 H10A 109.5 . . ? S1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? S1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? 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 C10 S1 C1 C2 -62.52(10) . . . . ? S1 C1 C2 C7 100.06(11) . . . . ? S1 C1 C2 C3 -79.17(13) . . . . ? C7 C2 C3 C4 -1.17(17) . . . . ? C1 C2 C3 C4 178.06(10) . . . . ? C7 C2 C3 C8 177.79(10) . . . . ? C1 C2 C3 C8 -2.98(17) . . . . ? C2 C3 C4 C5 0.45(17) . . . . ? C8 C3 C4 C5 -178.53(11) . . . . ? C3 C4 C5 C6 0.48(18) . . . . ? C4 C5 C6 C7 -0.68(17) . . . . ? C4 C5 C6 C9 178.72(11) . . . . ? C3 C2 C7 C6 0.98(17) . . . . ? C1 C2 C7 C6 -178.27(10) . . . . ? C5 C6 C7 C2 -0.05(17) . . . . ? C9 C6 C7 C2 -179.46(11) . . . . ? _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. ; _audit_block_code C10H11NS_vv592_mayr _audit_creation_method 'APEX3 v2016.9-0' _shelxl_version_number ? _chemical_name_systematic ? _chemical_formula_moiety 'C10 H11 N S' _chemical_formula_sum 'C10 H11 N S' _chemical_formula_weight 177.26 #?# (Cohen, 1996) _chemical_melting_point ? #?# in K! _cell_formula_units_Z 2 #?# adjust to _chemical_formula_[] _exptl_crystal_density_diffrn 1.272 _exptl_crystal_F_000 188 #?# check! _shelx_res_file ; vv592_0m_a.res created by SHELXL-2014/7 TITL vv592_0m_a.res in P-1 REM Old TITL vv592_0m in P-1 REM SHELXT solution in P-1 REM R1 0.080, Rweak 0.006, Alpha 0.036, Orientation as input REM Formula found by SHELXT: C10 N S CELL 0.71073 7.3211 7.9973 8.7918 69.178 74.117 83.714 ZERR 2.000 0.0002 0.0002 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H N S UNIT 20 22 2 2 TEMP -170.150 SIZE 0.03 0.06 0.08 L.S. 10 BOND $H LIST 4 CONF ACTA OMIT -3 0 6 OMIT 0 4 0 OMIT 0 6 6 OMIT 3 0 3 SHEL 6.5 0.78 FMAP 2 PLAN -20 WGHT 0.027400 0.223000 FVAR 1.60264 S1 4 0.716384 0.871350 -0.019037 11.00000 0.02072 0.01741 = 0.01801 -0.00175 -0.00643 0.00048 N1 3 1.040588 0.166494 0.571664 11.00000 0.02706 0.01986 = 0.03180 -0.00795 -0.01514 0.00270 C1 1 0.608815 0.777418 0.206143 11.00000 0.01926 0.01725 = 0.01769 -0.00545 -0.00521 0.00240 AFIX 23 H1A 2 0.673970 0.825432 0.266502 11.00000 -1.20000 H1B 2 0.473997 0.816290 0.229282 11.00000 -1.20000 AFIX 0 C2 1 0.619120 0.576173 0.273289 11.00000 0.01611 0.01638 = 0.01236 -0.00448 -0.00149 0.00094 C3 1 0.492544 0.469282 0.253466 11.00000 0.01381 0.02164 = 0.01269 -0.00515 -0.00233 0.00071 C4 1 0.513677 0.283757 0.314215 11.00000 0.01633 0.02080 = 0.01728 -0.00610 -0.00309 -0.00350 AFIX 43 H4 2 0.428964 0.211737 0.300151 11.00000 -1.20000 AFIX 0 C5 1 0.654913 0.201357 0.394618 11.00000 0.01776 0.01536 = 0.01673 -0.00357 -0.00282 -0.00103 AFIX 43 H5 2 0.667679 0.074690 0.434428 11.00000 -1.20000 AFIX 0 C6 1 0.778109 0.308049 0.416009 11.00000 0.01494 0.01742 = 0.01400 -0.00427 -0.00332 0.00082 C7 1 0.759665 0.494326 0.355512 11.00000 0.01609 0.01759 = 0.01536 -0.00588 -0.00348 -0.00106 AFIX 43 H7 2 0.844016 0.565776 0.370716 11.00000 -1.20000 AFIX 0 C8 1 0.333827 0.552034 0.170743 11.00000 0.01758 0.02435 = 0.02203 -0.00690 -0.00770 0.00170 AFIX 137 H8A 2 0.272217 0.459124 0.154459 11.00000 -1.50000 H8B 2 0.385477 0.643071 0.061450 11.00000 -1.50000 H8C 2 0.240529 0.607744 0.242503 11.00000 -1.50000 AFIX 0 C9 1 0.924391 0.227524 0.501996 11.00000 0.01978 0.01415 = 0.01947 -0.00553 -0.00483 -0.00068 C10 1 0.958684 0.796007 -0.025500 11.00000 0.01988 0.02218 = 0.02654 -0.00560 -0.00197 0.00139 AFIX 137 H10A 2 1.039362 0.853784 -0.138398 11.00000 -1.50000 H10B 2 0.966085 0.665919 0.001668 11.00000 -1.50000 H10C 2 1.002357 0.827349 0.056717 11.00000 -1.50000 AFIX 0 HKLF 4 REM vv592_0m_a.res in P-1 REM R1 = 0.0266 for 1867 Fo > 4sig(Fo) and 0.0299 for all 2031 data REM 111 parameters refined using 0 restraints END WGHT 0.0274 0.2230 REM Highest difference peak 0.295, deepest hole -0.192, 1-sigma level 0.042 Q1 1 0.6185 0.6725 0.2373 11.00000 0.05 0.29 Q2 1 0.7213 0.2562 0.3942 11.00000 0.05 0.29 Q3 1 0.4224 0.5073 0.2195 11.00000 0.05 0.28 Q4 1 0.7702 0.3946 0.3746 11.00000 0.05 0.28 Q5 1 0.5571 0.5209 0.2566 11.00000 0.05 0.27 Q6 1 0.5803 0.2481 0.3608 11.00000 0.05 0.26 Q7 1 0.5068 0.3820 0.2849 11.00000 0.05 0.26 Q8 1 0.6616 0.5331 0.3327 11.00000 0.05 0.25 Q9 1 0.6690 0.8446 -0.0959 11.00000 0.05 0.22 Q10 1 0.8438 0.2773 0.4491 11.00000 0.05 0.21 Q11 1 0.6609 0.7962 0.1016 11.00000 0.05 0.19 Q12 1 0.8525 0.8468 -0.0320 11.00000 0.05 0.18 Q13 1 0.7237 0.9846 -0.0809 11.00000 0.05 0.17 Q14 1 0.4795 0.8370 0.1780 11.00000 0.05 0.16 Q15 1 0.2168 0.4858 0.2201 11.00000 0.05 0.14 Q16 1 0.9939 0.2622 0.5223 11.00000 0.05 0.14 Q17 1 0.9172 0.1527 0.5766 11.00000 0.05 0.14 Q18 1 0.9752 0.1360 0.5180 11.00000 0.05 0.14 Q19 1 1.0201 0.8601 -0.0094 11.00000 0.05 0.13 Q20 1 0.7787 0.5215 0.3827 11.00000 0.05 0.12 ; _shelx_res_checksum 33498 _shelx_hkl_file ; -1 0 0 457.35 11.20 -2 0 0 50.39 2.30 -2 0 0 51.89 2.80 -2 0 0 47.90 2.70 2 0 0 49.80 2.80 2 0 0 48.30 2.70 2 0 0 50.89 2.30 -3 0 0 2145.99 52.19 -3 0 0 2284.47 52.29 -3 0 0 2256.17 51.29 3 0 0 2150.88 52.29 3 0 0 2183.28 52.19 3 0 0 2291.87 51.29 -4 0 0 882.11 24.00 -4 0 0 904.51 22.80 -4 0 0 875.61 24.00 4 0 0 911.01 24.10 4 0 0 919.71 22.80 4 0 0 902.81 24.20 -5 0 0 314.77 11.50 -5 0 0 304.47 10.00 -5 0 0 315.07 12.90 5 0 0 288.37 11.20 5 0 0 295.87 9.80 5 0 0 299.27 11.40 -6 0 0 0.10 1.80 -6 0 0 -0.50 1.90 -6 0 0 1.60 2.30 6 0 0 3.10 2.60 6 0 0 -1.00 1.70 6 0 0 1.10 1.60 -7 0 0 111.39 7.70 -7 0 0 107.59 6.40 -7 0 0 101.39 7.50 7 0 0 102.39 7.70 7 0 0 108.69 7.80 7 0 0 97.89 6.00 -8 0 0 49.70 5.10 -8 0 0 59.99 6.60 -8 0 0 54.89 6.70 8 0 0 38.80 5.50 8 0 0 46.70 6.20 8 0 0 40.70 4.60 -9 0 0 197.68 12.10 -9 0 0 225.48 10.50 9 0 0 229.68 13.10 8 -1 0 274.67 10.60 8 -1 0 290.37 13.70 -8 1 0 290.17 15.50 -8 1 0 281.27 10.90 -8 1 0 294.57 13.90 7 -1 0 295.47 12.90 7 -1 0 279.17 10.30 7 -1 0 284.77 13.00 -7 1 0 313.17 13.30 -7 1 0 318.57 10.80 -7 1 0 306.17 13.20 6 -1 0 93.19 4.80 6 -1 0 92.39 6.60 6 -1 0 92.89 6.50 -6 1 0 96.79 5.20 -6 1 0 89.19 6.50 -6 1 0 91.49 6.60 5 -1 0 4.50 2.20 5 -1 0 0.60 1.10 5 -1 0 -1.00 1.50 -5 1 0 -0.40 1.60 -5 1 0 -0.40 1.70 4 -1 0 424.66 11.40 4 -1 0 421.46 16.70 4 -1 0 420.56 13.20 -4 1 0 411.46 13.10 -4 1 0 396.06 13.10 -4 1 0 437.36 11.60 3 -1 0 891.91 23.10 3 -1 0 902.01 23.20 3 -1 0 917.41 21.60 -3 1 0 899.31 23.20 -3 1 0 895.81 23.20 -3 1 0 916.61 21.60 2 -1 0 268.67 8.10 2 -1 0 271.27 8.00 2 -1 0 282.87 7.00 -2 1 0 263.97 8.00 -2 1 0 285.97 7.00 -2 1 0 271.87 8.10 1 -1 0 2695.83 69.79 -1 1 0 2682.33 69.69 -1 -1 0 591.64 14.30 -1 -1 0 585.04 14.20 -1 -1 0 608.04 14.50 1 1 0 603.44 14.50 1 1 0 573.14 14.20 -2 -1 0 153.28 5.20 -2 -1 0 147.99 5.30 -2 -1 0 159.38 5.30 2 1 0 158.78 5.40 2 1 0 155.58 5.30 2 1 0 155.38 5.20 -3 -1 0 582.24 15.50 -3 -1 0 580.34 15.80 -3 -1 0 563.34 15.80 3 1 0 577.94 15.40 3 1 0 559.04 15.90 3 1 0 593.44 16.00 -4 -1 0 154.08 6.40 -4 -1 0 154.38 6.90 -4 -1 0 151.78 6.80 4 1 0 154.68 7.80 4 1 0 155.48 6.90 4 1 0 152.28 6.30 -5 -1 0 497.95 15.80 -5 -1 0 494.15 15.70 -5 -1 0 486.15 14.80 5 1 0 482.25 15.70 5 1 0 482.85 14.70 5 1 0 491.75 16.00 -6 -1 0 4.70 2.20 -6 -1 0 2.80 2.30 -6 -1 0 3.80 2.20 6 1 0 3.00 1.90 6 1 0 4.40 2.40 6 1 0 7.20 2.70 -7 -1 0 480.05 16.00 -7 -1 0 471.35 17.20 7 1 0 462.85 17.40 7 1 0 473.85 17.80 7 1 0 463.45 15.70 -8 -1 0 1421.96 37.90 -8 -1 0 1480.15 40.20 8 1 0 1420.36 40.80 8 1 0 1242.18 45.80 8 -2 0 344.77 11.50 8 -2 0 357.16 16.10 -8 2 0 358.86 11.90 -8 2 0 372.16 15.80 7 -2 0 85.39 6.90 7 -2 0 85.99 4.60 -7 2 0 77.79 4.70 -7 2 0 97.19 9.50 6 -2 0 62.49 5.60 6 -2 0 65.39 5.80 6 -2 0 63.29 3.60 -6 2 0 69.69 5.90 -6 2 0 70.79 6.00 5 -2 0 311.17 11.50 5 -2 0 314.47 9.10 5 -2 0 322.27 11.80 -5 2 0 310.57 9.20 -5 2 0 305.27 11.60 -5 2 0 319.97 11.80 4 -2 0 574.84 16.80 4 -2 0 589.14 16.80 4 -2 0 593.74 14.40 -4 2 0 574.14 16.90 -4 2 0 581.64 14.50 -4 2 0 553.44 16.80 3 -2 0 1517.25 34.60 3 -2 0 1520.75 37.20 3 -2 0 1510.15 36.80 -3 2 0 1509.75 36.90 -3 2 0 1529.55 34.70 2 -2 0 1186.38 26.30 2 -2 0 1158.58 27.80 2 -2 0 1168.68 27.90 -2 2 0 1130.59 27.90 -2 2 0 1166.28 26.40 1 -2 0 559.84 13.30 1 -2 0 569.54 13.20 1 -2 0 560.44 13.60 1 -2 0 551.24 13.50 -1 2 0 569.84 13.70 0 -2 0 1702.03 43.60 0 2 0 1709.63 43.90 -1 -2 0 5640.04 134.59 1 2 0 5412.46 134.19 -2 -2 0 713.03 18.90 -2 -2 0 753.52 19.40 -2 -2 0 803.92 19.40 2 2 0 753.32 19.10 2 2 0 773.52 19.50 -3 -2 0 237.68 8.50 -3 -2 0 228.08 7.90 -3 -2 0 243.48 8.30 3 2 0 232.18 8.10 3 2 0 225.58 8.00 3 2 0 220.08 8.10 -4 -2 0 346.27 11.50 -4 -2 0 356.56 11.70 -4 -2 0 375.26 11.90 4 2 0 360.96 11.90 4 2 0 346.87 11.50 4 2 0 357.46 12.00 -5 -2 0 645.84 18.90 -5 -2 0 633.44 19.10 -5 -2 0 621.54 19.10 5 2 0 640.94 19.40 5 2 0 672.43 19.90 5 2 0 627.64 18.60 -6 -2 0 243.08 10.10 -6 -2 0 235.58 10.40 -6 -2 0 242.48 10.70 6 2 0 254.47 11.30 6 2 0 228.18 9.90 6 2 0 245.98 10.90 -7 -2 0 -0.20 1.90 -7 -2 0 -1.50 2.10 -7 -2 0 -2.20 1.90 7 2 0 -3.30 1.90 7 2 0 -0.40 2.40 -8 -2 0 55.29 6.20 -8 -2 0 58.79 5.70 8 2 0 46.40 6.10 8 2 0 53.89 6.50 8 -3 0 0.90 2.40 -8 3 0 -5.50 3.20 -8 3 0 -1.10 1.50 -8 3 0 -1.60 2.50 7 -3 0 60.29 5.90 -7 3 0 61.99 6.20 -7 3 0 62.89 3.50 6 -3 0 108.29 6.90 6 -3 0 104.49 4.00 6 -3 0 117.09 9.70 -6 3 0 90.69 7.70 -6 3 0 111.09 4.30 5 -3 0 493.05 20.10 5 -3 0 535.65 16.60 5 -3 0 519.55 12.80 -5 3 0 528.85 13.00 -5 3 0 497.95 16.50 -5 3 0 529.55 16.80 4 -3 0 18.90 1.20 4 -3 0 15.20 2.40 -4 3 0 12.70 2.40 -4 3 0 18.70 2.90 -4 3 0 17.50 1.30 3 -3 0 1978.20 47.40 3 -3 0 2044.30 47.50 3 -3 0 2000.50 44.80 -3 3 0 1969.90 44.80 -3 3 0 2000.50 47.70 2 -3 0 4.10 0.80 2 -3 0 5.00 0.90 2 -3 0 5.90 1.40 2 -3 0 4.60 1.20 -2 3 0 3.80 1.30 1 -3 0 604.54 14.30 1 -3 0 604.24 14.30 1 -3 0 608.04 14.60 1 -3 0 602.94 14.70 -1 3 0 537.05 14.70 -1 3 0 608.14 14.60 0 -3 0 6793.52 162.58 0 3 0 7119.89 163.38 -1 -3 0 833.52 19.10 -1 -3 0 799.32 19.10 -1 -3 0 775.02 20.40 1 3 0 796.22 20.50 1 3 0 834.52 19.40 1 3 0 808.32 19.60 -2 -3 0 27.60 2.40 -2 -3 0 29.20 3.10 -2 -3 0 32.50 2.40 2 3 0 34.80 2.80 2 3 0 28.20 2.50 2 3 0 26.70 2.80 -3 -3 0 658.63 18.30 -3 -3 0 635.04 17.30 -3 -3 0 635.44 17.50 3 3 0 660.63 17.90 3 3 0 655.43 18.20 -4 -3 0 405.56 12.90 -4 -3 0 396.16 13.20 -4 -3 0 385.36 12.60 4 3 0 421.86 13.30 4 3 0 412.66 13.10 4 3 0 409.26 13.30 -5 -3 0 40.10 4.10 -5 -3 0 44.70 4.20 -5 -3 0 42.70 4.60 5 3 0 42.50 4.50 5 3 0 37.30 4.10 -6 -3 0 152.28 8.30 -6 -3 0 159.18 8.40 -6 -3 0 166.78 8.50 6 3 0 160.08 8.70 6 3 0 162.98 9.00 -7 -3 0 1.90 2.50 -7 -3 0 1.90 2.00 7 3 0 2.90 2.40 7 3 0 3.50 2.70 -8 -3 0 -1.10 2.60 -8 -3 0 0.40 2.20 8 3 0 -0.40 3.00 8 3 0 0.10 2.00 8 -4 0 6.70 3.80 7 -4 0 415.46 15.90 -7 4 0 402.06 15.80 -7 4 0 415.46 16.20 6 -4 0 51.09 4.90 -6 4 0 47.00 5.00 -6 4 0 48.90 5.20 5 -4 0 23.20 3.20 5 -4 0 18.70 2.90 4 -4 0 2.50 1.60 4 -4 0 -1.00 1.90 -4 4 0 1.00 1.50 -4 4 0 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9 44.20 6.30 -3 -5 -9 102.39 7.90 -3 -5 -9 123.69 8.60 -3 -5 -9 110.49 7.80 3 5 9 111.89 8.10 3 5 9 114.19 8.40 -4 -5 -9 19.70 4.00 -4 -5 -9 15.50 3.50 -4 -5 -9 26.00 5.20 4 5 9 24.20 5.20 4 5 9 23.10 4.80 -5 -5 -9 20.80 4.10 -5 -5 -9 9.10 3.20 -5 -5 -9 17.00 4.70 5 5 9 20.10 4.60 -6 -5 -9 252.17 13.20 -6 -5 -9 243.28 12.90 -6 -5 -9 233.68 12.70 6 5 9 248.28 13.10 -7 -5 -9 126.09 9.70 7 5 9 137.39 10.20 2 -6 -9 28.70 4.70 2 -6 -9 47.60 5.70 -2 6 9 33.50 4.50 1 -6 -9 3.80 2.50 1 -6 -9 8.10 2.90 -1 6 9 10.80 3.70 -1 6 9 8.30 4.30 -1 6 9 9.10 3.50 0 -6 -9 168.68 9.90 0 -6 -9 165.48 12.20 0 -6 -9 162.58 9.00 0 6 9 170.88 10.60 0 6 9 161.28 10.20 -1 -6 -9 -1.00 2.40 -1 -6 -9 -3.40 2.50 -1 -6 -9 -1.10 1.80 1 6 9 -3.60 3.30 1 6 9 5.60 3.30 -2 -6 -9 149.39 9.20 -2 -6 -9 167.38 9.60 -2 -6 -9 150.48 9.40 2 6 9 156.78 10.00 2 6 9 158.98 14.20 -3 -6 -9 -2.20 2.40 -3 -6 -9 -0.30 2.40 -3 -6 -9 5.00 3.00 3 6 9 1.40 2.70 3 6 9 2.80 3.10 -4 -6 -9 34.10 5.70 -4 -6 -9 32.90 5.60 -4 -6 -9 22.50 4.30 4 6 9 26.40 4.80 4 6 9 27.40 5.30 -5 -6 -9 169.68 10.20 -5 -6 -9 152.28 13.40 5 6 9 159.28 10.50 5 6 9 166.18 10.60 -6 -6 -9 152.48 10.50 -6 -6 -9 145.49 9.90 6 6 9 149.69 10.40 1 -7 -9 84.99 7.60 -1 7 9 73.29 6.20 -1 7 9 87.19 8.40 -1 7 9 84.89 9.20 0 -7 -9 29.70 4.50 0 -7 -9 19.90 3.90 0 7 9 19.80 5.90 0 7 9 30.70 5.80 -1 -7 -9 26.70 4.20 1 7 9 38.10 5.70 1 7 9 19.60 4.00 -2 -7 -9 120.59 8.20 -2 -7 -9 109.39 7.80 2 7 9 116.49 9.10 2 7 9 87.59 8.00 -3 -7 -9 243.58 11.90 -3 -7 -9 208.28 11.30 3 7 9 227.88 12.60 3 7 9 232.18 12.20 -4 -7 -9 10.60 3.80 4 7 9 8.60 3.70 -5 -7 -9 209.98 11.70 5 7 9 206.28 12.20 5 7 9 209.28 12.30 0 -8 -9 261.77 13.30 0 -8 -9 282.37 11.70 0 8 9 274.37 14.10 -1 -8 -9 146.19 8.50 -1 -8 -9 111.89 8.60 1 8 9 138.89 10.30 1 8 9 131.49 9.80 -2 -8 -9 -1.10 2.50 -2 -8 -9 1.30 2.90 2 8 9 0.30 3.90 2 8 9 3.20 3.10 -3 -8 -9 96.99 7.90 -3 -8 -9 114.79 8.30 3 8 9 106.29 9.10 3 8 9 115.29 9.90 -4 -8 -9 13.40 4.90 -4 -8 -9 8.20 3.50 4 8 9 12.80 5.90 4 8 9 17.60 5.10 -2 1 -10 143.49 8.80 -2 1 -10 150.28 11.10 2 -1 10 120.29 6.70 -3 1 -10 65.99 6.60 3 -1 10 63.19 5.30 0 0 -10 63.19 7.50 0 0 -10 67.49 6.30 0 0 -10 71.79 7.50 -1 0 -10 96.89 7.40 -1 0 -10 99.09 7.10 -1 0 -10 96.09 8.60 1 0 10 96.59 6.40 -2 0 -10 8.90 3.80 -2 0 -10 5.60 2.40 -2 0 -10 5.60 2.60 2 0 10 7.70 2.60 -3 0 -10 221.98 12.40 -3 0 -10 193.68 10.00 -3 0 -10 240.38 11.20 3 0 10 202.38 9.50 -4 0 -10 180.58 10.20 -4 0 -10 160.18 10.30 -4 0 -10 149.99 8.70 4 0 10 160.78 8.60 -5 0 -10 20.50 4.00 -5 0 -10 25.90 5.10 1 -1 -10 21.10 4.10 1 -1 -10 25.80 5.10 0 -1 -10 7.30 3.50 0 -1 -10 2.50 2.80 0 1 10 7.50 2.60 -1 -1 -10 82.69 6.80 -1 -1 -10 91.59 7.20 -1 -1 -10 98.79 9.10 1 1 10 84.89 6.50 -2 -1 -10 147.19 14.20 -2 -1 -10 147.29 8.70 2 1 10 152.48 8.50 -3 -1 -10 124.59 13.10 -3 -1 -10 110.59 9.80 -3 -1 -10 115.69 7.60 3 1 10 121.99 7.60 -4 -1 -10 90.49 7.50 -4 -1 -10 97.39 8.60 -4 -1 -10 86.69 8.90 4 1 10 83.29 6.50 -5 -1 -10 1.00 3.10 -5 -1 -10 5.40 3.60 -5 -1 -10 0.10 2.10 5 1 10 2.50 2.70 1 -2 -10 109.19 9.50 1 -2 -10 82.09 7.20 -1 2 10 104.79 7.80 0 -2 -10 396.06 16.40 0 -2 -10 364.96 16.20 0 -2 -10 398.46 15.80 0 2 10 412.16 15.90 -1 -2 -10 -1.10 2.10 -1 -2 -10 -0.30 2.60 -1 -2 -10 5.80 3.40 1 2 10 0.90 2.20 -2 -2 -10 112.79 7.80 -2 -2 -10 124.79 8.30 -2 -2 -10 112.79 8.80 2 2 10 105.79 8.80 -3 -2 -10 -1.50 2.40 -3 -2 -10 2.50 2.80 -3 -2 -10 3.40 2.10 3 2 10 7.70 3.40 -4 -2 -10 29.40 4.50 -4 -2 -10 33.60 5.70 4 2 10 47.90 6.80 -5 -2 -10 65.79 7.80 -5 -2 -10 65.09 7.00 -5 -2 -10 56.19 6.10 5 2 10 51.19 6.10 -6 -2 -10 15.70 3.70 -6 -2 -10 26.10 5.60 1 -3 -10 -6.70 2.90 1 -3 -10 -1.50 2.00 1 -3 -10 -0.50 2.60 -1 3 10 3.40 2.40 0 -3 -10 59.09 6.20 0 -3 -10 62.19 8.40 0 -3 -10 53.49 6.00 0 3 10 64.69 6.50 -1 -3 -10 128.99 8.70 -1 -3 -10 105.09 7.80 -1 -3 -10 125.59 8.80 1 3 10 116.09 8.30 -2 -3 -10 66.09 6.50 -2 -3 -10 60.59 6.20 -2 -3 -10 90.59 7.80 2 3 10 71.79 6.60 -3 -3 -10 917.81 28.70 -3 -3 -10 865.41 27.20 -3 -3 -10 852.71 27.70 3 3 10 879.81 27.50 -4 -3 -10 88.89 7.20 -4 -3 -10 95.19 7.80 -4 -3 -10 89.39 8.90 4 3 10 93.99 7.60 -5 -3 -10 39.90 5.70 -5 -3 -10 52.39 6.30 5 3 10 56.99 6.20 -6 -3 -10 -2.90 2.30 -6 -3 -10 -3.10 3.40 6 3 10 -1.40 2.40 1 -4 -10 91.19 7.90 1 -4 -10 114.19 9.40 1 -4 -10 85.39 7.10 -1 4 10 92.09 8.10 0 -4 -10 5.80 3.40 0 -4 -10 5.10 3.00 0 -4 -10 2.40 2.30 -1 -4 -10 197.68 10.70 -1 -4 -10 179.58 10.70 -1 -4 -10 183.28 10.60 1 4 10 183.28 10.60 -2 -4 -10 1.70 2.10 -2 -4 -10 6.10 2.80 -2 -4 -10 6.40 3.10 2 4 10 5.40 2.90 -3 -4 -10 4.00 3.30 -3 -4 -10 3.70 2.50 -3 -4 -10 -2.40 2.60 3 4 10 7.10 3.20 -4 -4 -10 260.27 14.80 -4 -4 -10 282.97 13.60 -4 -4 -10 280.37 13.20 4 4 10 295.07 13.70 -5 -4 -10 62.69 7.40 -5 -4 -10 39.40 6.10 -5 -4 -10 51.69 6.30 5 4 10 53.79 6.30 -6 -4 -10 99.29 8.60 -6 -4 -10 139.69 17.30 -6 -4 -10 113.49 8.90 6 4 10 96.89 8.60 1 -5 -10 36.20 6.30 1 -5 -10 32.50 5.80 1 -5 -10 31.10 4.80 -1 5 10 32.10 5.60 0 -5 -10 55.29 6.40 0 -5 -10 52.39 8.00 0 -5 -10 40.10 5.60 0 5 10 40.60 6.50 -1 -5 -10 2.10 2.70 -1 -5 -10 0.40 2.00 -1 -5 -10 -0.80 3.00 1 5 10 9.70 4.00 -2 -5 -10 73.59 6.80 -2 -5 -10 67.79 6.80 -2 -5 -10 66.49 7.00 2 5 10 78.79 7.20 -3 -5 -10 26.40 4.90 -3 -5 -10 15.50 3.70 -3 -5 -10 32.00 5.20 3 5 10 35.30 5.80 -4 -5 -10 156.78 9.90 -4 -5 -10 159.88 10.30 4 5 10 168.78 10.50 -5 -5 -10 3.70 2.80 -5 -5 -10 7.00 3.90 -5 -5 -10 9.90 6.10 5 5 10 6.60 3.70 -6 -5 -10 448.86 22.30 -6 -5 -10 385.46 17.40 6 5 10 459.65 18.80 0 -6 -10 106.79 7.50 0 6 10 98.39 8.80 -1 -6 -10 15.90 3.90 1 6 10 15.10 4.60 -2 -6 -10 221.18 12.60 -2 -6 -10 199.18 11.30 -2 -6 -10 208.98 11.40 2 6 10 211.28 12.00 -3 -6 -10 84.79 7.80 -3 -6 -10 69.89 7.90 -3 -6 -10 88.39 7.70 3 6 10 82.29 7.90 -4 -6 -10 125.39 10.70 4 6 10 133.49 9.80 -5 -6 -10 44.20 6.60 -5 -6 -10 41.40 6.20 5 6 10 37.70 6.50 -1 -7 -10 13.60 4.30 -1 -7 -10 6.60 3.00 1 7 10 12.40 4.40 -2 -7 -10 3.00 3.00 -2 -7 -10 1.60 2.40 2 7 10 -1.00 3.30 -3 -7 -10 0.20 2.90 -3 -7 -10 3.00 3.40 3 7 10 0.90 3.10 -4 -7 -10 161.38 10.30 -4 -7 -10 144.49 10.10 4 7 10 171.88 11.30 -2 -2 -11 154.58 10.50 -2 -2 -11 136.79 9.00 -3 -2 -11 11.30 3.50 -1 -3 -11 123.39 9.40 -1 -3 -11 122.29 9.80 1 3 11 117.29 12.10 -2 -3 -11 437.36 18.50 -2 -3 -11 448.46 17.70 2 3 11 436.46 18.40 -3 -3 -11 83.09 7.20 -3 -3 -11 82.39 8.40 3 3 11 84.99 7.60 -4 -3 -11 1.40 3.30 -1 -4 -11 243.78 12.60 -1 -4 -11 215.58 12.20 1 4 11 236.98 12.70 -2 -4 -11 257.27 13.40 -2 -4 -11 247.68 12.80 2 4 11 260.47 13.20 -3 -4 -11 40.70 5.80 -3 -4 -11 59.09 6.80 3 4 11 63.19 6.90 -4 -4 -11 124.49 9.10 4 4 11 141.79 9.70 -2 -5 -11 56.49 6.60 -2 -5 -11 75.29 7.60 2 5 11 78.09 7.90 -3 -5 -11 265.97 20.30 -3 -5 -11 227.78 12.50 -3 -5 -11 249.78 12.90 3 5 11 223.78 12.70 -4 -5 -11 84.69 9.40 -4 -5 -11 76.09 7.50 4 5 11 88.89 9.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 11060 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_vv629 _database_code_depnum_ccdc_archive 'CCDC 2044218' loop_ _audit_author_name _audit_author_address 'Peter Mayer' ;LMU Muenchen Germany ; _audit_update_record ; 2020-11-13 deposited with the CCDC. 2021-02-09 downloaded from the CCDC. ; _chemical_name_common RM444 _chemical_compound_source ? _chemical_absolute_configuration ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.100 #?# in millimeters _exptl_crystal_size_mid 0.080 #?# in millimeters _exptl_crystal_size_min 0.050 #?# in millimeters _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_special_details ; ; _audit_creation_date ? #?# style: 18-Aug-1998 _diffrn_ambient_temperature 103.(2) #?# in K _diffrn_source_type 'Bruker TXS' _diffrn_source_power 2.5 #?# in kW _diffrn_source_voltage 50 #?# in kV _diffrn_source_current 50 #?# in mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode (TXS)' _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_collimation ? _diffrn_measurement_device 'fixed-chi three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture TXS' _diffrn_measurement_method 'mix of phi and omega scans' _diffrn_measurement_details ? _diffrn_detector_area_resol_mean 7.4074 _diffrn_special_details ? _diffrn_orient_matrix_type ? _diffrn_orient_matrix_UB_11 ? _diffrn_orient_matrix_UB_12 ? _diffrn_orient_matrix_UB_13 ? _diffrn_orient_matrix_UB_21 ? _diffrn_orient_matrix_UB_22 ? _diffrn_orient_matrix_UB_23 ? _diffrn_orient_matrix_UB_31 ? _diffrn_orient_matrix_UB_32 ? _diffrn_orient_matrix_UB_33 ? _cell_length_a 12.1957(10) _cell_length_b 7.1469(5) _cell_length_c 12.4085(11) _cell_angle_alpha 90 _cell_angle_beta 105.197(3) _cell_angle_gamma 90 _cell_volume 1043.72(15) _cell_measurement_temperature 103.(2) #?# in K _cell_measurement_reflns_used 6941 _cell_measurement_theta_min 3.3349 _cell_measurement_theta_max 26.4637 _cell_special_details ? _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.99 _shelx_estimated_absorpt_T_min 0.991 _shelx_estimated_absorpt_T_max 0.995 _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _diffrn_reflns_number 14056 #xl _diffrn_reflns_av_R_equivalents 0.0402 #xl _diffrn_reflns_av_unetI/netI 0.0254 #xl _diffrn_reflns_limit_h_min -15 #xl _diffrn_reflns_limit_h_max 15 #xl _diffrn_reflns_limit_k_min -8 #xl _diffrn_reflns_limit_k_max 8 #xl _diffrn_reflns_limit_l_min -15 #xl _diffrn_reflns_limit_l_max 15 #xl _diffrn_reflns_theta_min 3.320 #xl _diffrn_reflns_theta_max 26.371 #xl _diffrn_measured_fraction_theta_max 0.996 #xl _diffrn_reflns_theta_full 25.242 #xl _diffrn_measured_fraction_theta_full 0.996 #xl _diffrn_reflns_Laue_measured_fraction_max 0.996 #xl _diffrn_reflns_Laue_measured_fraction_full 0.996 #xl _diffrn_reflns_point_group_measured_fraction_max 0.996 #xl _diffrn_reflns_point_group_measured_fraction_full 0.996 #xl _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' _space_group_IT_number 14 _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. ; 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_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' N N 0.0061 0.0033 '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' _reflns_number_total 2124 #xl _reflns_number_gt 1670 #xl _reflns_threshold_expression 'I > 2\s(I)' #xl _reflns_Friedel_coverage 0.000 #xl _reflns_Friedel_fraction_max . #xl _reflns_Friedel_fraction_full . #xl _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. ; _refine_ls_structure_factor_coef Fsqd #xl _refine_ls_matrix_type full #xl _refine_ls_weighting_scheme calc #xl _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.9886P] where P=(Fo^2^+2Fc^2^)/3' #xl _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr #?# _refine_ls_extinction_method none #xl _refine_ls_extinction_coef . #xl _refine_ls_abs_structure_details ? #xl _refine_ls_abs_structure_Flack ? #xl _refine_ls_number_reflns 2124 #xl _refine_ls_number_parameters 145 #xl _refine_ls_number_restraints 0 #xl _refine_ls_R_factor_all 0.0615 #xl _refine_ls_R_factor_gt 0.0431 #xl _refine_ls_wR_factor_ref 0.1092 #xl _refine_ls_wR_factor_gt 0.0969 #xl _refine_ls_goodness_of_fit_ref 1.054 #xl _refine_ls_restrained_S_all 1.054 #xl _refine_ls_shift/su_max 0.000 #xl _refine_ls_shift/su_mean 0.000 #xl _refine_diff_density_max 0.181 #xl _refine_diff_density_min -0.261 #xl _refine_diff_density_rms 0.049 #xl _refine_special_details ; ; _computing_data_collection 'APEX3 v2016.5-0, Bruker AXS (2016)' _computing_cell_refinement 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_data_reduction 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_structure_solution 'XT, VERSION 2014/5' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 807)' _computing_publication_material ? 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 0.66549(11) 0.94043(18) 0.14363(11) 0.0261(3) Uani 1 1 d . . . . . O2 O 0.49941(11) 1.08961(18) 0.12096(11) 0.0276(3) Uani 1 1 d . . . . . N1 N 0.37415(14) 0.0737(2) 0.58560(14) 0.0327(4) Uani 1 1 d . . . . . C1 C 0.55252(15) 0.9453(3) 0.13700(14) 0.0224(4) Uani 1 1 d . . . . . C2 C 0.51151(15) 0.7531(2) 0.15136(15) 0.0210(4) Uani 1 1 d . . . . . C3 C 0.61629(15) 0.6311(3) 0.18826(16) 0.0237(4) Uani 1 1 d . . . . . H3A H 0.6046 0.5076 0.1509 0.028 Uiso 1 1 calc R U . . . H3B H 0.6382 0.6128 0.2702 0.028 Uiso 1 1 calc R U . . . C4 C 0.70495(17) 0.7470(3) 0.15033(19) 0.0311(5) Uani 1 1 d . . . . . H4A H 0.7802 0.7356 0.2047 0.037 Uiso 1 1 calc R U . . . H4B H 0.7115 0.7035 0.0765 0.037 Uiso 1 1 calc R U . . . C5 C 0.40050(15) 0.6939(3) 0.07218(15) 0.0247(4) Uani 1 1 d . . . . . H5A H 0.3619 0.7843 0.0141 0.030 Uiso 1 1 calc R U . . . H5B H 0.3924 0.5612 0.0486 0.030 Uiso 1 1 calc R U . . . C6 C 0.40317(15) 0.7375(3) 0.19173(15) 0.0223(4) Uani 1 1 d . . . . . H6 H 0.3682 0.8603 0.2026 0.027 Uiso 1 1 calc R U . . . C7 C 0.39355(14) 0.5907(2) 0.27372(14) 0.0211(4) Uani 1 1 d . . . . . C8 C 0.42330(15) 0.4043(3) 0.26196(15) 0.0242(4) Uani 1 1 d . . . . . H8 H 0.4474 0.3682 0.1981 0.029 Uiso 1 1 calc R U . . . C9 C 0.41819(15) 0.2710(3) 0.34193(15) 0.0243(4) Uani 1 1 d . . . . . H9 H 0.4397 0.1452 0.3333 0.029 Uiso 1 1 calc R U . . . C10 C 0.38124(14) 0.3230(3) 0.43507(15) 0.0222(4) Uani 1 1 d . . . . . C11 C 0.34879(15) 0.5073(3) 0.44727(15) 0.0240(4) Uani 1 1 d . . . . . H11 H 0.3223 0.5421 0.5099 0.029 Uiso 1 1 calc R U . . . C12 C 0.35546(14) 0.6393(3) 0.36751(15) 0.0225(4) Uani 1 1 d . . . . . H12 H 0.3339 0.7649 0.3764 0.027 Uiso 1 1 calc R U . . . C13 C 0.37737(15) 0.1842(3) 0.51880(16) 0.0249(4) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0239(7) 0.0234(7) 0.0320(7) 0.0000(5) 0.0094(5) -0.0011(5) O2 0.0344(7) 0.0221(7) 0.0288(7) 0.0007(5) 0.0127(6) 0.0041(6) N1 0.0321(9) 0.0319(9) 0.0348(9) 0.0053(8) 0.0101(7) -0.0008(7) C1 0.0270(9) 0.0231(9) 0.0183(8) -0.0028(7) 0.0081(7) -0.0007(7) C2 0.0214(9) 0.0195(9) 0.0232(9) -0.0002(7) 0.0076(7) 0.0004(7) C3 0.0230(9) 0.0216(9) 0.0279(9) -0.0005(7) 0.0089(7) 0.0020(7) C4 0.0259(10) 0.0238(10) 0.0456(12) 0.0020(9) 0.0128(9) 0.0017(8) C5 0.0257(9) 0.0255(9) 0.0233(9) 0.0000(7) 0.0070(7) -0.0024(8) C6 0.0225(9) 0.0221(9) 0.0237(9) 0.0002(7) 0.0087(7) 0.0000(7) C7 0.0162(8) 0.0230(9) 0.0234(9) -0.0001(7) 0.0041(7) -0.0010(7) C8 0.0259(9) 0.0237(9) 0.0247(9) -0.0029(7) 0.0095(7) -0.0007(7) C9 0.0245(9) 0.0197(9) 0.0291(9) -0.0025(7) 0.0078(7) -0.0007(7) C10 0.0182(8) 0.0229(9) 0.0252(9) 0.0014(7) 0.0051(7) -0.0021(7) C11 0.0225(9) 0.0266(10) 0.0246(9) -0.0019(7) 0.0092(7) -0.0015(7) C12 0.0212(9) 0.0220(9) 0.0254(9) -0.0013(7) 0.0080(7) 0.0017(7) C13 0.0222(9) 0.0243(9) 0.0283(10) -0.0002(8) 0.0069(7) -0.0008(7) 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 1.359(2) . ? O1 C4 1.459(2) . ? O2 C1 1.207(2) . ? N1 C13 1.153(2) . ? C1 C2 1.488(2) . ? C2 C5 1.510(2) . ? C2 C3 1.515(2) . ? C2 C6 1.535(2) . ? C3 C4 1.531(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.508(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.488(2) . ? C6 H6 1.0000 . ? C7 C8 1.398(3) . ? C7 C12 1.405(2) . ? C8 C9 1.389(3) . ? C8 H8 0.9500 . ? C9 C10 1.397(3) . ? C9 H9 0.9500 . ? C10 C11 1.395(3) . ? C10 C13 1.446(3) . ? C11 C12 1.385(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 C4 109.97(14) . . ? O2 C1 O1 121.57(17) . . ? O2 C1 C2 128.76(17) . . ? O1 C1 C2 109.67(15) . . ? C1 C2 C5 116.93(15) . . ? C1 C2 C3 106.49(15) . . ? C5 C2 C3 125.22(16) . . ? C1 C2 C6 116.81(15) . . ? C5 C2 C6 59.36(11) . . ? C3 C2 C6 126.13(15) . . ? C2 C3 C4 101.76(15) . . ? C2 C3 H3A 111.4 . . ? C4 C3 H3A 111.4 . . ? C2 C3 H3B 111.4 . . ? C4 C3 H3B 111.4 . . ? H3A C3 H3B 109.3 . . ? O1 C4 C3 106.32(14) . . ? O1 C4 H4A 110.5 . . ? C3 C4 H4A 110.5 . . ? O1 C4 H4B 110.5 . . ? C3 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? C6 C5 C2 61.14(12) . . ? C6 C5 H5A 117.7 . . ? C2 C5 H5A 117.7 . . ? C6 C5 H5B 117.7 . . ? C2 C5 H5B 117.7 . . ? H5A C5 H5B 114.8 . . ? C7 C6 C5 122.80(16) . . ? C7 C6 C2 120.22(15) . . ? C5 C6 C2 59.50(11) . . ? C7 C6 H6 114.5 . . ? C5 C6 H6 114.5 . . ? C2 C6 H6 114.5 . . ? C8 C7 C12 118.25(17) . . ? C8 C7 C6 122.11(16) . . ? C12 C7 C6 119.63(16) . . ? C9 C8 C7 121.17(17) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.55(17) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 120.25(17) . . ? C11 C10 C13 120.41(17) . . ? C9 C10 C13 119.34(17) . . ? C12 C11 C10 119.61(17) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C7 121.16(17) . . ? C11 C12 H12 119.4 . . ? C7 C12 H12 119.4 . . ? N1 C13 C10 179.9(2) . . ? 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 C4 O1 C1 O2 -173.45(17) . . . . ? C4 O1 C1 C2 6.13(19) . . . . ? O2 C1 C2 C5 43.8(3) . . . . ? O1 C1 C2 C5 -135.78(16) . . . . ? O2 C1 C2 C3 -170.67(18) . . . . ? O1 C1 C2 C3 9.80(19) . . . . ? O2 C1 C2 C6 -23.7(3) . . . . ? O1 C1 C2 C6 156.79(14) . . . . ? C1 C2 C3 C4 -20.30(18) . . . . ? C5 C2 C3 C4 121.61(18) . . . . ? C6 C2 C3 C4 -163.29(17) . . . . ? C1 O1 C4 C3 -19.5(2) . . . . ? C2 C3 C4 O1 23.89(19) . . . . ? C1 C2 C5 C6 -106.69(17) . . . . ? C3 C2 C5 C6 114.88(19) . . . . ? C2 C5 C6 C7 -108.38(18) . . . . ? C1 C2 C6 C7 -140.51(17) . . . . ? C5 C2 C6 C7 112.61(19) . . . . ? C3 C2 C6 C7 -0.8(3) . . . . ? C1 C2 C6 C5 106.88(18) . . . . ? C3 C2 C6 C5 -113.4(2) . . . . ? C5 C6 C7 C8 24.4(3) . . . . ? C2 C6 C7 C8 -46.7(2) . . . . ? C5 C6 C7 C12 -156.80(16) . . . . ? C2 C6 C7 C12 132.07(17) . . . . ? C12 C7 C8 C9 -1.6(3) . . . . ? C6 C7 C8 C9 177.27(16) . . . . ? C7 C8 C9 C10 0.9(3) . . . . ? C8 C9 C10 C11 0.5(3) . . . . ? C8 C9 C10 C13 -179.26(16) . . . . ? C9 C10 C11 C12 -1.2(3) . . . . ? C13 C10 C11 C12 178.56(16) . . . . ? C10 C11 C12 C7 0.5(3) . . . . ? C8 C7 C12 C11 0.8(3) . . . . ? C6 C7 C12 C11 -178.01(16) . . . . ? _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. ; _audit_block_code C13H11NO2_vv629_mayr _audit_creation_method 'APEX3 v2016.9-0' _shelxl_version_number ? _chemical_name_systematic ? _chemical_formula_moiety 'C13 H11 N O2' _chemical_formula_sum 'C13 H11 N O2' _chemical_formula_weight 213.23 #?# (Cohen, 1996) _chemical_melting_point ? #?# in K! _cell_formula_units_Z 4 #?# adjust to _chemical_formula_[] _exptl_crystal_density_diffrn 1.357 _exptl_crystal_F_000 448 #?# check! _shelx_res_file ; vv629_0m_a.res created by SHELXL-2014/7 TITL vv629_0m_a.res in P2(1)/n REM Old TITL vv629_0m in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.116, Rweak 0.002, Alpha 0.018, Orientation as input REM Formula found by SHELXT: C13 N O2 CELL 0.71073 12.1957 7.1469 12.4085 90.000 105.197 90.000 ZERR 4.000 0.0010 0.0005 0.0011 0.000 0.003 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O UNIT 52 44 4 8 TEMP -170.150 SIZE 0.05 0.08 0.10 L.S. 10 BOND $H LIST 4 CONF OMIT 9 0 3 OMIT 0 3 6 OMIT 6 0 0 OMIT -6 0 6 OMIT 12 0 0 ACTA SHEL 6.5 0.8 FMAP 2 PLAN -20 WGHT 0.034200 0.988600 FVAR 0.81348 O1 4 0.665490 0.940429 0.143626 11.00000 0.02391 0.02344 = 0.03204 0.00003 0.00940 -0.00114 O2 4 0.499414 1.089615 0.120961 11.00000 0.03442 0.02210 = 0.02879 0.00071 0.01274 0.00414 N1 3 0.374148 0.073729 0.585596 11.00000 0.03210 0.03186 = 0.03480 0.00527 0.01009 -0.00076 C1 1 0.552522 0.945258 0.137001 11.00000 0.02696 0.02308 = 0.01832 -0.00278 0.00814 -0.00073 C2 1 0.511510 0.753081 0.151364 11.00000 0.02142 0.01948 = 0.02319 -0.00021 0.00760 0.00045 C3 1 0.616294 0.631115 0.188257 11.00000 0.02297 0.02157 = 0.02792 -0.00050 0.00892 0.00200 AFIX 23 H3A 2 0.604608 0.507562 0.150917 11.00000 -1.20000 H3B 2 0.638181 0.612843 0.270210 11.00000 -1.20000 AFIX 0 C4 1 0.704950 0.746952 0.150333 11.00000 0.02593 0.02378 = 0.04560 0.00202 0.01282 0.00169 AFIX 23 H4A 2 0.780229 0.735588 0.204722 11.00000 -1.20000 H4B 2 0.711486 0.703524 0.076509 11.00000 -1.20000 AFIX 0 C5 1 0.400496 0.693863 0.072175 11.00000 0.02574 0.02546 = 0.02333 -0.00001 0.00704 -0.00239 AFIX 23 H5A 2 0.361941 0.784330 0.014146 11.00000 -1.20000 H5B 2 0.392385 0.561150 0.048557 11.00000 -1.20000 AFIX 0 C6 1 0.403166 0.737503 0.191728 11.00000 0.02253 0.02215 = 0.02372 0.00018 0.00874 -0.00001 AFIX 13 H6 2 0.368220 0.860289 0.202592 11.00000 -1.20000 AFIX 0 C7 1 0.393551 0.590662 0.273724 11.00000 0.01622 0.02298 = 0.02340 -0.00007 0.00414 -0.00102 C8 1 0.423300 0.404266 0.261963 11.00000 0.02586 0.02366 = 0.02470 -0.00292 0.00948 -0.00073 AFIX 43 H8 2 0.447432 0.368183 0.198140 11.00000 -1.20000 AFIX 0 C9 1 0.418192 0.270968 0.341932 11.00000 0.02448 0.01971 = 0.02906 -0.00250 0.00781 -0.00070 AFIX 43 H9 2 0.439688 0.145215 0.333337 11.00000 -1.20000 AFIX 0 C10 1 0.381240 0.323036 0.435069 11.00000 0.01821 0.02286 = 0.02524 0.00144 0.00512 -0.00210 C11 1 0.348786 0.507304 0.447268 11.00000 0.02255 0.02662 = 0.02458 -0.00186 0.00916 -0.00149 AFIX 43 H11 2 0.322262 0.542070 0.509915 11.00000 -1.20000 AFIX 0 C12 1 0.355456 0.639306 0.367506 11.00000 0.02116 0.02197 = 0.02540 -0.00125 0.00804 0.00167 AFIX 43 H12 2 0.333897 0.764936 0.376360 11.00000 -1.20000 AFIX 0 C13 1 0.377371 0.184203 0.518804 11.00000 0.02219 0.02428 = 0.02826 -0.00018 0.00686 -0.00082 HKLF 4 REM vv629_0m_a.res in P2(1)/n REM R1 = 0.0431 for 1670 Fo > 4sig(Fo) and 0.0615 for all 2124 data REM 145 parameters refined using 0 restraints END WGHT 0.0343 0.9872 REM Highest difference peak 0.181, deepest hole -0.261, 1-sigma level 0.049 Q1 1 0.4664 0.7540 0.1804 11.00000 0.05 0.18 Q2 1 0.3774 0.6198 0.3181 11.00000 0.05 0.18 Q3 1 0.4502 0.3575 0.3154 11.00000 0.05 0.17 Q4 1 0.3616 -0.0421 0.6783 11.00000 0.05 0.16 Q5 1 0.5548 0.6809 0.1646 11.00000 0.05 0.16 Q6 1 0.5235 0.8366 0.1360 11.00000 0.05 0.16 Q7 1 0.4005 0.6669 0.2413 11.00000 0.05 0.16 Q8 1 0.4340 0.5085 0.2816 11.00000 0.05 0.16 Q9 1 0.5710 1.1921 0.0827 11.00000 0.05 0.16 Q10 1 0.4340 1.2217 0.1115 11.00000 0.05 0.16 Q11 1 0.4779 0.0835 0.5642 11.00000 0.05 0.16 Q12 1 0.6603 0.6847 0.1762 11.00000 0.05 0.16 Q13 1 0.6803 0.5955 0.3676 11.00000 0.05 0.15 Q14 1 0.3819 0.2996 0.3831 11.00000 0.05 0.15 Q15 1 0.6212 0.4870 0.1977 11.00000 0.05 0.15 Q16 1 0.6753 0.7252 0.0313 11.00000 0.05 0.15 Q17 1 0.3945 0.4158 0.4493 11.00000 0.05 0.14 Q18 1 0.3742 0.7972 0.4234 11.00000 0.05 0.14 Q19 1 0.3417 0.1861 0.5643 11.00000 0.05 0.14 Q20 1 0.4363 -0.0125 0.3345 11.00000 0.05 0.14 ; _shelx_res_checksum 26028 _shelx_hkl_file ; -2 0 0 2649.93 78.39 2 0 0 2606.14 77.79 3 0 0 2.50 1.50 3 0 0 1.30 1.40 3 0 0 2.30 1.50 -3 0 0 1.40 1.40 -3 0 0 0.80 1.70 -3 0 0 1.80 1.30 -4 0 0 8397.36 231.88 5 0 0 14.80 2.40 -5 0 0 15.40 2.40 -5 0 0 10.50 2.30 5 0 0 16.10 2.70 5 0 0 13.80 2.30 5 0 0 14.70 2.60 -6 0 0 57.99 4.70 6 0 0 49.00 4.50 6 0 0 55.09 4.90 -6 0 0 50.29 4.50 6 0 0 52.39 4.40 6 0 0 54.29 4.90 7 0 0 14.20 3.00 7 0 0 14.40 3.10 7 0 0 12.00 2.50 -7 0 0 16.10 2.70 7 0 0 10.80 2.80 -7 0 0 15.50 4.20 -8 0 0 859.61 23.20 8 0 0 859.71 23.60 -8 0 0 839.22 23.00 8 0 0 865.91 23.70 8 0 0 865.11 23.20 8 0 0 851.71 23.20 9 0 0 8.50 3.20 9 0 0 7.50 3.50 -9 0 0 6.70 3.10 9 0 0 12.00 3.30 -9 0 0 14.10 3.30 9 0 0 9.90 3.10 -10 0 0 272.17 10.50 10 0 0 288.77 10.90 -10 0 0 282.47 11.00 10 0 0 282.37 11.30 10 0 0 294.37 11.40 11 0 0 22.10 4.40 -11 0 0 28.50 6.10 11 0 0 25.50 4.80 11 0 0 23.00 6.80 -11 0 0 21.60 4.40 12 0 0 19.80 4.80 12 0 0 33.20 5.40 -12 0 0 28.30 4.60 12 0 0 22.70 4.70 13 0 0 26.50 5.10 13 0 0 20.70 5.40 -13 0 0 18.50 5.40 14 0 0 10.00 8.80 -14 0 0 7.10 5.50 14 0 0 10.30 5.60 0 1 0 -0.10 0.30 1 -1 0 7.90 0.80 -1 -1 0 9.80 1.10 1 -1 0 7.30 0.80 1 -1 0 8.60 0.60 1 -1 0 6.10 0.80 1 1 0 9.20 1.00 1 1 0 9.70 1.20 -1 1 0 7.20 0.80 1 1 0 9.50 1.20 -2 -1 0 1208.08 30.70 -2 -1 0 1257.57 30.70 -2 -1 0 1267.27 30.70 2 -1 0 1271.17 30.30 2 -1 0 1272.37 30.30 2 -1 0 1283.87 30.30 -2 1 0 1276.77 30.30 -2 1 0 1181.08 30.80 2 1 0 1259.27 30.70 -2 1 0 1273.07 30.20 2 1 0 1292.77 30.80 2 1 0 1276.07 30.70 2 1 0 1249.07 30.60 3 -1 0 775.12 21.20 -3 -1 0 860.31 21.60 3 -1 0 884.41 21.30 3 -1 0 874.31 21.30 -3 -1 0 859.51 21.80 3 -1 0 876.41 21.40 -3 -1 0 867.41 21.70 3 1 0 854.11 21.70 3 1 0 843.02 21.60 3 1 0 884.61 21.80 3 1 0 877.41 21.80 -3 1 0 874.61 21.30 -3 1 0 865.01 21.30 -3 1 0 868.81 21.20 4 -1 0 14.70 2.00 -4 -1 0 12.40 2.10 -4 -1 0 13.10 2.10 4 -1 0 12.20 1.70 4 -1 0 10.50 2.00 4 1 0 11.70 2.20 4 1 0 12.10 2.00 -4 1 0 12.20 1.80 4 1 0 11.90 1.90 4 1 0 11.70 2.30 -4 1 0 14.10 2.20 -4 1 0 12.30 1.70 5 -1 0 1528.55 37.10 5 -1 0 1488.25 36.90 -5 -1 0 1486.05 37.30 -5 -1 0 1451.15 37.20 5 1 0 1455.85 37.20 -5 1 0 1497.45 36.90 -5 1 0 1511.65 36.80 5 1 0 1506.15 37.60 5 1 0 1513.05 37.50 5 1 0 1498.65 37.30 6 -1 0 97.39 6.40 6 -1 0 86.09 5.30 -6 -1 0 88.39 5.50 6 -1 0 92.19 5.40 -6 -1 0 81.79 5.20 6 1 0 86.69 5.10 6 1 0 88.19 5.80 6 1 0 88.39 5.70 -6 1 0 83.29 4.90 6 1 0 84.19 5.20 7 -1 0 113.59 5.50 -7 -1 0 114.79 6.10 -7 -1 0 111.69 5.90 7 -1 0 111.99 6.00 7 -1 0 108.59 5.50 -7 1 0 117.59 5.40 -7 1 0 112.39 5.60 7 1 0 106.89 5.90 7 1 0 111.29 10.70 7 1 0 111.89 6.30 7 1 0 112.19 5.70 8 -1 0 4.00 2.70 8 -1 0 4.50 2.60 8 -1 0 4.30 2.60 8 -1 0 3.30 1.80 -8 -1 0 2.90 2.60 -8 1 0 3.30 2.60 8 1 0 -0.70 2.70 8 1 0 3.00 3.10 -8 1 0 0.80 2.20 8 1 0 2.00 2.40 8 1 0 1.80 2.90 9 -1 0 45.10 5.10 -9 -1 0 51.89 5.60 9 -1 0 43.80 5.50 9 -1 0 52.69 5.10 9 -1 0 47.60 5.00 -9 -1 0 49.50 5.50 9 1 0 49.10 5.50 -9 1 0 47.20 5.40 9 1 0 51.59 5.50 -9 1 0 46.60 4.80 9 1 0 43.80 6.00 10 -1 0 41.20 4.70 -10 -1 0 47.70 5.70 10 -1 0 40.60 5.70 10 -1 0 50.29 5.50 -10 -1 0 41.90 8.30 10 1 0 44.00 6.00 10 1 0 39.80 4.90 10 1 0 42.70 5.30 -10 1 0 42.30 6.10 -10 1 0 41.40 5.80 -11 -1 0 1.30 3.70 11 -1 0 -1.20 3.40 -11 -1 0 4.40 3.90 11 -1 0 -2.70 3.50 11 -1 0 -2.40 3.40 -11 1 0 0.90 3.50 11 1 0 4.20 4.10 -11 1 0 -0.90 2.90 11 1 0 5.30 3.80 11 1 0 0.40 3.90 -12 -1 0 2.20 3.80 12 -1 0 2.20 3.70 12 -1 0 0.30 3.80 -12 -1 0 3.10 3.90 -12 1 0 -1.20 3.80 12 1 0 -0.70 5.60 12 1 0 0.70 4.40 12 1 0 -3.50 4.30 -13 -1 0 4.40 4.40 13 -1 0 -0.10 4.60 13 -1 0 1.30 4.30 13 1 0 4.20 4.40 -13 1 0 -2.00 3.90 13 1 0 -1.20 4.20 14 -1 0 37.30 7.00 -14 -1 0 40.00 6.10 14 -1 0 58.59 7.20 -14 1 0 62.79 8.60 14 1 0 46.20 6.70 14 1 0 66.59 8.80 0 -2 0 443.36 10.90 0 -2 0 432.16 10.90 0 2 0 448.56 10.90 0 2 0 440.26 10.90 -1 -2 0 786.42 19.60 -1 -2 0 796.92 19.60 1 2 0 800.22 19.60 1 2 0 797.82 19.70 2 -2 0 17.40 1.40 2 -2 0 17.10 1.40 -2 -2 0 21.50 2.50 2 -2 0 18.90 1.20 2 2 0 23.30 2.10 2 2 0 19.20 2.20 2 2 0 18.90 2.40 2 2 0 20.90 2.00 -3 -2 0 150.08 5.60 3 -2 0 148.19 4.60 -3 -2 0 160.58 5.60 3 -2 0 158.98 4.70 3 -2 0 158.98 4.70 3 2 0 164.38 5.60 3 2 0 162.18 5.80 3 2 0 161.08 5.80 -3 2 0 152.08 4.40 -3 2 0 152.78 4.50 3 2 0 153.08 5.40 -4 -2 0 2.20 2.20 4 -2 0 3.30 1.70 4 -2 0 1.20 1.80 -4 -2 0 1.70 2.30 4 -2 0 1.70 1.90 4 -2 0 0.40 1.70 4 2 0 -0.50 2.30 -4 2 0 2.00 1.40 -4 2 0 4.40 1.60 4 2 0 1.70 2.50 4 2 0 1.30 2.00 4 2 0 1.50 2.20 5 -2 0 407.76 11.30 -5 -2 0 388.86 11.80 5 -2 0 386.56 11.00 -5 -2 0 399.26 15.50 5 -2 0 405.76 11.30 5 2 0 396.56 12.20 5 2 0 383.16 11.70 5 2 0 414.46 13.20 5 2 0 397.76 11.90 -5 2 0 400.16 11.00 6 -2 0 501.35 13.80 6 -2 0 510.85 13.90 6 -2 0 511.35 14.10 -6 -2 0 517.25 14.70 6 -2 0 501.05 14.10 -6 -2 0 501.35 14.70 6 2 0 498.85 15.00 -6 2 0 511.25 13.70 6 2 0 500.65 14.50 6 2 0 522.15 14.80 -6 2 0 510.45 13.90 6 2 0 504.65 15.10 7 -2 0 13.10 2.50 -7 -2 0 15.10 2.90 7 -2 0 10.30 2.40 7 -2 0 10.70 2.60 -7 -2 0 8.70 2.80 7 -2 0 12.00 2.50 7 2 0 13.10 2.90 7 2 0 7.00 3.00 -7 2 0 9.20 2.10 7 2 0 9.40 3.00 -7 2 0 13.40 2.50 7 2 0 16.80 3.00 8 -2 0 34.00 4.60 8 -2 0 36.10 4.30 8 -2 0 33.70 4.70 -8 -2 0 41.80 5.10 -8 -2 0 37.00 4.30 8 2 0 30.60 4.70 8 2 0 38.70 5.10 8 2 0 43.70 5.00 -8 2 0 36.20 4.00 8 2 0 44.80 5.10 -8 2 0 36.70 4.60 9 -2 0 70.69 5.30 9 -2 0 71.59 9.60 -9 -2 0 69.99 6.40 9 -2 0 75.69 5.80 -9 -2 0 69.59 7.60 9 2 0 71.99 7.10 9 2 0 74.19 8.00 -9 2 0 71.89 5.80 9 2 0 64.39 6.60 -9 2 0 79.59 5.40 -10 -2 0 461.25 15.70 10 -2 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81.59 4.00 4 -4 4 0.60 2.00 -4 -4 -4 2.80 2.80 4 -4 4 2.40 2.40 -4 -4 -4 1.30 2.80 -4 4 -4 0.70 2.20 4 4 4 0.60 3.10 4 4 4 5.50 2.90 -4 4 -4 3.30 1.80 -4 4 -4 0.50 2.00 5 -4 4 5.40 3.70 -5 -4 -4 6.60 3.90 -5 -4 -4 9.80 3.50 -5 -4 -4 6.60 3.20 5 4 4 3.10 3.50 -5 4 -4 9.30 2.50 5 4 4 7.30 3.50 -5 4 -4 3.50 3.10 -6 -4 -4 492.05 15.50 -6 -4 -4 502.45 16.20 6 -4 4 482.45 14.20 -6 -4 -4 484.15 15.90 6 -4 4 512.65 14.50 6 4 4 479.45 15.70 -6 4 -4 540.05 14.70 6 4 4 473.85 15.90 -6 4 -4 482.85 14.40 7 -4 4 22.00 3.70 -7 -4 -4 18.20 4.10 7 -4 4 14.60 3.00 -7 -4 -4 12.90 5.10 7 4 4 14.30 5.90 -7 4 -4 19.70 4.90 -7 4 -4 11.60 3.40 7 4 4 15.70 4.60 7 4 4 8.50 4.00 -8 -4 -4 39.00 6.20 -8 -4 -4 36.90 5.10 8 -4 4 51.89 5.10 -8 -4 -4 32.70 5.10 8 -4 4 55.79 5.60 8 4 4 34.70 5.60 -8 4 -4 44.40 5.70 8 4 4 50.29 7.00 8 4 4 57.29 6.70 9 -4 4 13.90 3.50 9 -4 4 17.80 4.20 -9 -4 -4 9.00 7.10 -9 -4 -4 7.30 3.80 -9 -4 -4 18.00 8.10 -9 4 -4 17.00 4.70 9 4 4 11.80 4.10 9 4 4 4.50 4.80 9 4 4 17.80 4.60 -9 4 -4 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24.70 4.50 9 -2 -10 29.10 5.20 9 -2 -10 30.20 5.40 -9 2 10 30.40 5.20 9 2 -10 25.40 5.00 9 2 -10 23.00 5.90 -9 2 10 24.70 4.80 -8 -2 10 33.30 5.40 8 -2 -10 19.90 4.60 8 -2 -10 23.70 5.00 -8 -2 10 28.60 4.70 8 2 -10 23.70 5.20 -8 2 10 31.90 5.40 -8 2 10 23.90 4.60 8 2 -10 23.20 5.20 7 -2 -10 65.99 6.90 -7 -2 10 59.09 6.60 -7 -2 10 54.99 7.20 7 -2 -10 61.39 7.30 7 2 -10 59.79 7.70 7 2 -10 62.39 7.60 -7 2 10 52.69 6.90 -7 2 10 62.69 7.20 -6 -2 10 0.20 3.70 6 -2 -10 2.50 3.70 -6 -2 10 6.50 4.60 6 -2 -10 0.80 4.20 6 2 -10 -1.50 3.90 -6 2 10 -2.10 3.80 6 2 -10 -2.50 4.20 -6 2 10 7.40 4.00 5 -2 -10 325.47 12.50 5 -2 -10 309.67 12.30 -5 -2 10 334.07 13.20 -5 -2 10 345.47 12.50 5 2 -10 346.37 13.00 -5 2 10 331.67 12.10 -5 2 10 325.07 12.80 5 2 -10 343.87 13.10 4 -2 -10 199.78 9.60 4 -2 -10 199.18 9.70 -4 -2 10 211.58 9.60 -4 -2 10 191.98 10.20 4 2 -10 212.28 10.20 -4 2 10 200.18 9.30 4 2 -10 204.58 10.00 -4 2 10 201.58 10.20 3 -2 -10 300.47 11.60 -3 -2 10 292.77 12.20 -3 -2 10 307.67 11.50 3 -2 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4.30 -7 -3 -10 1.70 5.90 7 -3 10 2.70 4.40 7 3 10 -4.30 5.40 -7 3 -10 0.90 4.80 7 3 10 2.40 4.80 -7 3 -10 11.30 5.60 -11 -4 10 78.79 10.40 11 -4 -10 63.19 8.30 11 -4 -10 86.69 8.20 -11 -4 10 51.79 7.00 -11 4 10 53.79 6.00 11 4 -10 81.09 9.40 -10 -4 10 0.20 4.30 10 -4 -10 -1.60 4.00 -10 -4 10 -2.90 5.10 10 -4 -10 3.60 4.20 -10 4 10 -0.50 4.20 10 4 -10 2.40 5.00 -10 4 10 -6.60 3.50 9 -4 -10 24.10 4.50 9 -4 -10 18.50 4.60 -9 -4 10 21.80 4.60 -9 4 10 18.50 4.80 9 4 -10 21.00 5.40 -9 4 10 13.70 3.80 8 -4 -10 19.50 4.30 -8 -4 10 25.50 4.40 8 -4 -10 16.40 4.50 8 4 -10 24.10 5.10 -8 4 10 26.50 4.80 -8 4 10 18.90 3.80 7 -4 -10 8.00 3.80 7 -4 -10 6.60 4.30 -7 -4 10 11.70 4.10 -7 4 10 5.30 4.00 7 4 -10 6.80 4.40 -7 4 10 12.30 3.50 6 -4 -10 28.50 4.10 6 -4 -10 42.70 5.00 -6 -4 10 57.59 6.70 -6 4 10 45.60 6.30 -6 4 10 44.50 5.80 6 4 -10 41.10 5.70 -5 -4 10 7.80 4.00 5 -4 -10 8.40 4.10 5 4 -10 6.50 4.20 -5 4 10 12.60 3.90 -5 4 10 4.90 4.10 -4 -4 10 7.10 3.60 4 -4 -10 8.30 4.00 -4 4 10 5.20 3.70 4 4 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7.30 -2 -5 10 109.49 7.80 -2 5 10 98.79 7.90 -2 5 10 103.69 7.20 2 5 -10 108.79 7.70 -1 -5 10 -2.10 3.60 1 -5 -10 3.90 3.90 1 -5 -10 -7.30 2.80 1 5 -10 2.40 3.70 -1 5 10 -2.70 4.20 -1 5 10 0.40 3.90 0 -5 -10 62.59 6.70 0 -5 10 81.29 7.00 0 -5 -10 79.49 9.50 0 5 -10 71.29 6.80 0 5 10 71.19 7.00 0 5 10 75.79 7.50 1 -5 10 0.70 3.20 -1 -5 -10 -2.70 5.00 1 5 10 7.20 4.70 -1 5 -10 8.10 3.70 1 5 10 -1.60 3.80 -2 -5 -10 140.99 9.10 2 -5 10 149.39 9.50 2 5 10 150.08 12.60 2 5 10 104.49 13.30 -3 -5 -10 30.00 5.50 3 -5 10 19.00 4.20 3 5 10 16.20 4.90 -3 5 -10 19.70 4.50 3 5 10 26.80 5.50 -4 -5 -10 50.69 7.60 4 -5 10 73.89 7.40 -4 -5 -10 63.89 8.50 -4 5 -10 82.69 7.50 4 5 10 51.89 7.30 4 5 10 80.79 8.10 -5 -5 -10 6.60 6.20 5 5 10 -0.30 5.00 5 5 10 -1.20 6.80 7 -6 -10 -3.70 3.90 -7 -6 10 -2.90 4.00 7 -6 -10 -0.50 4.30 -7 6 10 1.80 3.60 7 6 -10 0.00 4.50 6 -6 -10 21.90 4.20 6 -6 -10 21.80 4.50 -6 -6 10 19.50 4.60 -6 6 10 23.80 4.40 6 6 -10 20.40 5.30 -6 6 10 18.10 4.00 5 -6 -10 -0.50 3.70 5 -6 -10 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-5 2 15 -14.20 5.60 5 2 -15 -2.20 5.50 4 -2 -15 9.60 6.10 -4 -2 15 7.90 5.10 4 -2 -15 -8.90 6.40 4 2 -15 12.50 6.10 -4 2 15 10.40 5.70 -4 2 15 7.90 5.80 3 -2 -15 0.40 6.40 3 -2 -15 0.00 6.30 -3 -2 15 7.50 5.00 3 2 -15 4.60 5.40 -3 2 15 7.10 6.00 -3 2 15 0.50 6.30 -2 -2 15 4.10 4.80 -2 2 15 -0.30 5.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 68329