data_global _audit_creation_date 2017-05-12 _audit_creation_method SHELXL-2014 data_SS _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H16 S2' _chemical_formula_sum 'C29 H16 S2' _chemical_formula_weight 428.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' _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' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 15.2176(5) _cell_length_b 8.3864(3) _cell_length_c 32.8506(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4192.4(2) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 19727 _cell_measurement_theta_min 3.96 _cell_measurement_theta_max 68.16 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_F_000 1776 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 2.396 _shelx_estimated_absorpt_T_min 0.447 _shelx_estimated_absorpt_T_max 0.954 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_absorpt_correction_T_min 0.553 _exptl_absorpt_correction_T_max 0.953 _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_source 'Rotating anode' _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 35742 _diffrn_reflns_av_unetI/netI 0.0522 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.960 _diffrn_reflns_theta_max 68.236 _diffrn_reflns_theta_full 67.687 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_point_group_measured_fraction_full 0.992 _reflns_number_total 3796 _reflns_number_gt 2177 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; _computing_data_collection 'RAPID AUTO (Rigaku, 2004)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1200P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3796 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.2390 _refine_ls_wR_factor_gt 0.1950 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 -0.07141(7) 1.04818(14) 0.22225(4) 0.0696(4) Uani 1 1 d . . . . . S2 S 0.15928(8) 0.82083(16) 0.03404(4) 0.0720(4) Uani 1 1 d . . . . . C1 C -0.0061(3) 0.7835(5) 0.12685(12) 0.0580(11) Uani 1 1 d . . . . . C2 C -0.1064(3) 0.7798(5) 0.12214(13) 0.0572(11) Uani 1 1 d . . . . . C3 C -0.1568(3) 0.7069(5) 0.09279(13) 0.0645(12) Uani 1 1 d . . . . . H3 H -0.1297 0.6469 0.0717 0.077 Uiso 1 1 calc R U . . . C4 C -0.2480(3) 0.7218(5) 0.09425(15) 0.0717(13) Uani 1 1 d . . . . . H4 H -0.2832 0.6735 0.0738 0.086 Uiso 1 1 calc R U . . . C5 C -0.2872(3) 0.8062(6) 0.12522(15) 0.0747(14) Uani 1 1 d . . . . . H5 H -0.3494 0.8145 0.1260 0.090 Uiso 1 1 calc R U . . . C6 C -0.2371(3) 0.8802(5) 0.15564(15) 0.0681(12) Uani 1 1 d . . . . . H6 H -0.2648 0.9378 0.1770 0.082 Uiso 1 1 calc R U . . . C7 C -0.1473(3) 0.8678(5) 0.15393(13) 0.0603(11) Uani 1 1 d . . . . . C8 C -0.0769(2) 0.9288(5) 0.17911(13) 0.0553(10) Uani 1 1 d . . . . . C9 C 0.0024(3) 0.8839(5) 0.16517(12) 0.0575(11) Uani 1 1 d . . . . . C10 C 0.0749(3) 0.9411(5) 0.18902(13) 0.0580(11) Uani 1 1 d . . . . . C11 C 0.0422(3) 1.0343(5) 0.22192(13) 0.0631(12) Uani 1 1 d . . . . . C12 C 0.1001(3) 1.1114(5) 0.24839(13) 0.0676(12) Uani 1 1 d . . . . . H12 H 0.0785 1.1743 0.2703 0.081 Uiso 1 1 calc R U . . . C13 C 0.1892(3) 1.0942(6) 0.24211(15) 0.0784(14) Uani 1 1 d . . . . . H13 H 0.2292 1.1468 0.2598 0.094 Uiso 1 1 calc R U . . . C14 C 0.2214(3) 1.0019(6) 0.21056(15) 0.0786(14) Uani 1 1 d . . . . . H14 H 0.2831 0.9913 0.2071 0.094 Uiso 1 1 calc R U . . . C15 C 0.1659(3) 0.9254(5) 0.18422(14) 0.0650(12) Uani 1 1 d . . . . . H15 H 0.1890 0.8620 0.1628 0.078 Uiso 1 1 calc R U . . . C16 C 0.0391(3) 0.6193(5) 0.12964(13) 0.0612(11) Uani 1 1 d . . . . . C17 C 0.0234(3) 0.4963(5) 0.15693(14) 0.0696(12) Uani 1 1 d . . . . . H17 H -0.0211 0.5057 0.1771 0.083 Uiso 1 1 calc R U . . . C18 C 0.0748(3) 0.3578(6) 0.15411(16) 0.0772(14) Uani 1 1 d . . . . . H18 H 0.0647 0.2719 0.1724 0.093 Uiso 1 1 calc R U . . . C19 C 0.1405(3) 0.3453(6) 0.12468(17) 0.0818(15) Uani 1 1 d . . . . . H19 H 0.1754 0.2515 0.1234 0.098 Uiso 1 1 calc R U . . . C20 C 0.1554(3) 0.4671(6) 0.09746(15) 0.0710(13) Uani 1 1 d . . . . . H20 H 0.1999 0.4573 0.0773 0.085 Uiso 1 1 calc R U . . . C21 C 0.1047(3) 0.6047(5) 0.09981(13) 0.0634(11) Uani 1 1 d . . . . . C22 C 0.1026(3) 0.7516(5) 0.07593(12) 0.0592(11) Uani 1 1 d . . . . . C23 C 0.0411(3) 0.8534(5) 0.09030(13) 0.0578(11) Uani 1 1 d . . . . . C24 C 0.0370(3) 0.9987(5) 0.06819(13) 0.0602(11) Uani 1 1 d . . . . . C25 C 0.0996(3) 0.9985(5) 0.03604(13) 0.0637(12) Uani 1 1 d . . . . . C26 C 0.1076(3) 1.1292(6) 0.01008(15) 0.0757(14) Uani 1 1 d . . . . . H26 H 0.1499 1.1296 -0.0112 0.091 Uiso 1 1 calc R U . . . C27 C 0.0526(3) 1.2573(7) 0.01598(15) 0.0782(14) Uani 1 1 d . . . . . H27 H 0.0567 1.3465 -0.0018 0.094 Uiso 1 1 calc R U . . . C28 C -0.0084(3) 1.2592(6) 0.04719(14) 0.0736(13) Uani 1 1 d . . . . . H28 H -0.0451 1.3500 0.0505 0.088 Uiso 1 1 calc R U . . . C29 C -0.0173(3) 1.1316(5) 0.07363(14) 0.0657(12) Uani 1 1 d . . . . . H29 H -0.0594 1.1343 0.0950 0.079 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 0.0642(8) 0.0723(8) 0.0723(8) -0.0098(6) 0.0129(5) -0.0030(6) S2 0.0563(8) 0.0936(9) 0.0663(8) -0.0061(6) 0.0052(5) -0.0038(6) C1 0.049(3) 0.065(3) 0.060(2) -0.005(2) 0.0029(19) 0.000(2) C2 0.049(3) 0.061(3) 0.061(3) 0.006(2) 0.010(2) 0.002(2) C3 0.065(3) 0.065(3) 0.064(3) -0.001(2) 0.004(2) -0.004(2) C4 0.055(3) 0.075(3) 0.085(3) 0.004(3) -0.003(2) -0.007(2) C5 0.053(3) 0.076(3) 0.095(4) 0.000(3) 0.007(3) 0.002(2) C6 0.053(3) 0.063(3) 0.088(3) 0.000(2) 0.014(2) 0.003(2) C7 0.053(3) 0.060(3) 0.068(3) 0.007(2) 0.002(2) -0.005(2) C8 0.045(2) 0.057(3) 0.064(3) -0.002(2) 0.0070(19) 0.0006(19) C9 0.056(3) 0.060(3) 0.057(2) -0.002(2) 0.002(2) -0.001(2) C10 0.058(3) 0.056(3) 0.060(3) 0.002(2) 0.002(2) 0.001(2) C11 0.065(3) 0.060(3) 0.064(3) 0.000(2) 0.002(2) 0.003(2) C12 0.070(3) 0.075(3) 0.058(3) -0.003(2) 0.004(2) -0.003(2) C13 0.081(4) 0.080(3) 0.074(3) 0.000(3) -0.015(3) -0.002(3) C14 0.061(3) 0.090(4) 0.085(3) -0.010(3) -0.006(3) 0.006(3) C15 0.059(3) 0.066(3) 0.070(3) -0.010(2) -0.001(2) 0.005(2) C16 0.059(3) 0.062(3) 0.062(3) -0.003(2) -0.003(2) 0.003(2) C17 0.073(3) 0.068(3) 0.068(3) 0.000(2) 0.000(2) -0.001(2) C18 0.087(4) 0.067(3) 0.077(3) -0.005(3) -0.017(3) 0.002(3) C19 0.080(4) 0.070(3) 0.095(4) -0.013(3) -0.025(3) 0.013(3) C20 0.057(3) 0.078(3) 0.078(3) -0.016(3) -0.007(2) 0.005(2) C21 0.054(3) 0.070(3) 0.066(3) -0.010(2) -0.008(2) 0.003(2) C22 0.048(3) 0.070(3) 0.059(2) -0.002(2) -0.0015(19) -0.004(2) C23 0.051(3) 0.065(3) 0.058(2) -0.007(2) 0.0049(19) -0.003(2) C24 0.054(3) 0.066(3) 0.061(3) 0.003(2) -0.004(2) -0.009(2) C25 0.057(3) 0.073(3) 0.062(3) 0.001(2) -0.006(2) -0.009(2) C26 0.060(3) 0.102(4) 0.065(3) 0.008(3) -0.001(2) -0.014(3) C27 0.071(3) 0.088(4) 0.076(3) 0.018(3) -0.010(3) -0.020(3) C28 0.077(3) 0.068(3) 0.075(3) 0.002(3) -0.008(3) -0.004(3) C29 0.062(3) 0.068(3) 0.067(3) -0.001(2) -0.001(2) -0.003(2) _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. ; 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 C11 1.732(5) . ? S1 C8 1.737(4) . ? S2 C22 1.725(4) . ? S2 C25 1.747(5) . ? C1 C23 1.517(5) . ? C1 C9 1.520(5) . ? C1 C2 1.535(6) . ? C1 C16 1.542(6) . ? C2 C3 1.376(6) . ? C2 C7 1.422(5) . ? C3 C4 1.395(6) . ? C3 H3 0.9500 . ? C4 C5 1.375(6) . ? C4 H4 0.9500 . ? C5 C6 1.402(6) . ? C5 H5 0.9500 . ? C6 C7 1.372(5) . ? C6 H6 0.9500 . ? C7 C8 1.447(5) . ? C8 C9 1.344(5) . ? C9 C10 1.436(5) . ? C10 C15 1.400(5) . ? C10 C11 1.424(6) . ? C11 C12 1.396(6) . ? C12 C13 1.380(6) . ? C12 H12 0.9500 . ? C13 C14 1.383(6) . ? C13 H13 0.9500 . ? C14 C15 1.369(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.387(6) . ? C16 C21 1.404(6) . ? C17 C18 1.403(6) . ? C17 H17 0.9500 . ? C18 C19 1.395(7) . ? C18 H18 0.9500 . ? C19 C20 1.377(6) . ? C19 H19 0.9500 . ? C20 C21 1.390(6) . ? C20 H20 0.9500 . ? C21 C22 1.461(6) . ? C22 C23 1.352(5) . ? C23 C24 1.420(5) . ? C24 C29 1.399(5) . ? C24 C25 1.421(6) . ? C25 C26 1.394(6) . ? C26 C27 1.375(7) . ? C26 H26 0.9500 . ? C27 C28 1.384(6) . ? C27 H27 0.9500 . ? C28 C29 1.385(6) . ? C28 H28 0.9500 . ? C29 H29 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 C11 S1 C8 90.2(2) . . ? C22 S2 C25 89.8(2) . . ? C23 C1 C9 113.7(3) . . ? C23 C1 C2 113.5(3) . . ? C9 C1 C2 100.3(3) . . ? C23 C1 C16 100.4(3) . . ? C9 C1 C16 114.1(3) . . ? C2 C1 C16 115.6(3) . . ? C3 C2 C7 120.1(4) . . ? C3 C2 C1 129.4(4) . . ? C7 C2 C1 110.5(4) . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 120.2(5) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 121.3(4) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C7 C6 C5 118.6(4) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C6 C7 C2 120.4(4) . . ? C6 C7 C8 133.4(4) . . ? C2 C7 C8 106.2(4) . . ? C9 C8 C7 111.7(4) . . ? C9 C8 S1 113.3(3) . . ? C7 C8 S1 134.9(3) . . ? C8 C9 C10 114.2(4) . . ? C8 C9 C1 111.2(4) . . ? C10 C9 C1 134.6(4) . . ? C15 C10 C11 118.9(4) . . ? C15 C10 C9 131.9(4) . . ? C11 C10 C9 109.2(4) . . ? C12 C11 C10 120.4(4) . . ? C12 C11 S1 126.5(4) . . ? C10 C11 S1 113.0(3) . . ? C13 C12 C11 118.6(4) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C12 C13 C14 121.2(5) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C15 C14 C13 121.2(4) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C10 119.7(4) . . ? C14 C15 H15 120.2 . . ? C10 C15 H15 120.2 . . ? C17 C16 C21 120.6(4) . . ? C17 C16 C1 128.7(4) . . ? C21 C16 C1 110.7(4) . . ? C16 C17 C18 118.5(4) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C19 C18 C17 120.5(5) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C18 120.9(5) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 119.2(5) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C20 C21 C16 120.4(4) . . ? C20 C21 C22 133.0(4) . . ? C16 C21 C22 106.6(4) . . ? C23 C22 C21 111.1(4) . . ? C23 C22 S2 114.4(3) . . ? C21 C22 S2 134.5(3) . . ? C22 C23 C24 113.2(4) . . ? C22 C23 C1 111.1(4) . . ? C24 C23 C1 135.7(4) . . ? C29 C24 C23 130.1(4) . . ? C29 C24 C25 119.4(4) . . ? C23 C24 C25 110.5(4) . . ? C26 C25 C24 120.8(4) . . ? C26 C25 S2 127.0(4) . . ? C24 C25 S2 112.2(3) . . ? C27 C26 C25 118.3(5) . . ? C27 C26 H26 120.8 . . ? C25 C26 H26 120.8 . . ? C26 C27 C28 121.5(5) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C27 C28 C29 121.4(5) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C28 C29 C24 118.5(4) . . ? C28 C29 H29 120.7 . . ? C24 C29 H29 120.7 . . ? 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 C23 C1 C2 C3 58.3(6) . . . . ? C9 C1 C2 C3 180.0(4) . . . . ? C16 C1 C2 C3 -56.9(6) . . . . ? C23 C1 C2 C7 -121.4(4) . . . . ? C9 C1 C2 C7 0.2(4) . . . . ? C16 C1 C2 C7 123.3(4) . . . . ? C7 C2 C3 C4 0.8(6) . . . . ? C1 C2 C3 C4 -179.0(4) . . . . ? C2 C3 C4 C5 -1.2(7) . . . . ? C3 C4 C5 C6 0.7(7) . . . . ? C4 C5 C6 C7 0.4(7) . . . . ? C5 C6 C7 C2 -0.8(6) . . . . ? C5 C6 C7 C8 179.2(4) . . . . ? C3 C2 C7 C6 0.2(6) . . . . ? C1 C2 C7 C6 -180.0(4) . . . . ? C3 C2 C7 C8 -179.7(4) . . . . ? C1 C2 C7 C8 0.1(4) . . . . ? C6 C7 C8 C9 179.7(5) . . . . ? C2 C7 C8 C9 -0.3(5) . . . . ? C6 C7 C8 S1 -1.6(8) . . . . ? C2 C7 C8 S1 178.3(4) . . . . ? C11 S1 C8 C9 -0.9(3) . . . . ? C11 S1 C8 C7 -179.6(5) . . . . ? C7 C8 C9 C10 180.0(3) . . . . ? S1 C8 C9 C10 1.0(5) . . . . ? C7 C8 C9 C1 0.5(5) . . . . ? S1 C8 C9 C1 -178.5(3) . . . . ? C23 C1 C9 C8 121.1(4) . . . . ? C2 C1 C9 C8 -0.4(4) . . . . ? C16 C1 C9 C8 -124.5(4) . . . . ? C23 C1 C9 C10 -58.3(6) . . . . ? C2 C1 C9 C10 -179.8(4) . . . . ? C16 C1 C9 C10 56.1(6) . . . . ? C8 C9 C10 C15 -177.8(4) . . . . ? C1 C9 C10 C15 1.5(8) . . . . ? C8 C9 C10 C11 -0.5(5) . . . . ? C1 C9 C10 C11 178.8(4) . . . . ? C15 C10 C11 C12 1.3(6) . . . . ? C9 C10 C11 C12 -176.4(4) . . . . ? C15 C10 C11 S1 177.5(3) . . . . ? C9 C10 C11 S1 -0.2(4) . . . . ? C8 S1 C11 C12 176.5(4) . . . . ? C8 S1 C11 C10 0.6(3) . . . . ? C10 C11 C12 C13 -0.4(6) . . . . ? S1 C11 C12 C13 -176.1(3) . . . . ? C11 C12 C13 C14 -0.5(7) . . . . ? C12 C13 C14 C15 0.6(8) . . . . ? C13 C14 C15 C10 0.3(7) . . . . ? C11 C10 C15 C14 -1.2(7) . . . . ? C9 C10 C15 C14 175.8(4) . . . . ? C23 C1 C16 C17 -178.8(4) . . . . ? C9 C1 C16 C17 59.2(6) . . . . ? C2 C1 C16 C17 -56.2(6) . . . . ? C23 C1 C16 C21 2.3(4) . . . . ? C9 C1 C16 C21 -119.7(4) . . . . ? C2 C1 C16 C21 124.9(4) . . . . ? C21 C16 C17 C18 0.3(7) . . . . ? C1 C16 C17 C18 -178.5(4) . . . . ? C16 C17 C18 C19 0.5(7) . . . . ? C17 C18 C19 C20 -1.0(7) . . . . ? C18 C19 C20 C21 0.7(7) . . . . ? C19 C20 C21 C16 0.1(6) . . . . ? C19 C20 C21 C22 -179.0(4) . . . . ? C17 C16 C21 C20 -0.6(6) . . . . ? C1 C16 C21 C20 178.4(4) . . . . ? C17 C16 C21 C22 178.7(4) . . . . ? C1 C16 C21 C22 -2.3(5) . . . . ? C20 C21 C22 C23 -179.5(4) . . . . ? C16 C21 C22 C23 1.2(5) . . . . ? C20 C21 C22 S2 1.3(8) . . . . ? C16 C21 C22 S2 -177.9(3) . . . . ? C25 S2 C22 C23 1.2(3) . . . . ? C25 S2 C22 C21 -179.7(4) . . . . ? C21 C22 C23 C24 179.6(3) . . . . ? S2 C22 C23 C24 -1.1(5) . . . . ? C21 C22 C23 C1 0.3(5) . . . . ? S2 C22 C23 C1 179.6(3) . . . . ? C9 C1 C23 C22 120.7(4) . . . . ? C2 C1 C23 C22 -125.5(4) . . . . ? C16 C1 C23 C22 -1.6(4) . . . . ? C9 C1 C23 C24 -58.3(6) . . . . ? C2 C1 C23 C24 55.4(6) . . . . ? C16 C1 C23 C24 179.4(5) . . . . ? C22 C23 C24 C29 179.9(4) . . . . ? C1 C23 C24 C29 -1.1(8) . . . . ? C22 C23 C24 C25 0.3(5) . . . . ? C1 C23 C24 C25 179.3(4) . . . . ? C29 C24 C25 C26 0.3(6) . . . . ? C23 C24 C25 C26 179.9(4) . . . . ? C29 C24 C25 S2 -179.0(3) . . . . ? C23 C24 C25 S2 0.6(5) . . . . ? C22 S2 C25 C26 179.8(4) . . . . ? C22 S2 C25 C24 -1.0(3) . . . . ? C24 C25 C26 C27 -0.9(7) . . . . ? S2 C25 C26 C27 178.3(3) . . . . ? C25 C26 C27 C28 1.0(7) . . . . ? C26 C27 C28 C29 -0.5(7) . . . . ? C27 C28 C29 C24 -0.1(6) . . . . ? C23 C24 C29 C28 -179.3(4) . . . . ? C25 C24 C29 C28 0.2(6) . . . . ? _refine_diff_density_max 0.438 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.075 _shelxl_version_number 2014-3 _shelx_res_file ; TITL NakanoLab_170510_1_ CELL 1.54187 15.2176 8.3864 32.8506 90.000 90.000 90.000 ZERR 8.00 0.0005 0.0003 0.0011 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, Z SYMM X, 1/2 - Y, 1/2 + Z SYMM 1/2 - X, - Y, 1/2 + Z SFAC C H S UNIT 232 128 16 MERG 2 FMAP 2 SIZE 0.020 0.200 0.400 ACTA HTAB 2.00000 BOND $H CONF LIST 4 WPDB -2 L.S. 5 TEMP -80.00 WGHT 0.120000 FVAR 0.37612 S1 3 -0.071408 1.048181 0.222246 11.00000 0.06419 0.07225 = 0.07228 -0.00983 0.01290 -0.00304 S2 3 0.159279 0.820830 0.034038 11.00000 0.05627 0.09357 = 0.06629 -0.00613 0.00522 -0.00385 C1 1 -0.006053 0.783474 0.126849 11.00000 0.04939 0.06493 = 0.05965 -0.00457 0.00288 -0.00035 C2 1 -0.106380 0.779786 0.122144 11.00000 0.04938 0.06072 = 0.06138 0.00553 0.01003 0.00207 C3 1 -0.156794 0.706864 0.092794 11.00000 0.06479 0.06491 = 0.06389 -0.00147 0.00389 -0.00366 AFIX 43 H3 2 -0.129714 0.646858 0.071716 11.00000 -1.20000 AFIX 0 C4 1 -0.248037 0.721808 0.094254 11.00000 0.05528 0.07457 = 0.08511 0.00382 -0.00293 -0.00670 AFIX 43 H4 2 -0.283229 0.673536 0.073792 11.00000 -1.20000 AFIX 0 C5 1 -0.287190 0.806185 0.125217 11.00000 0.05300 0.07604 = 0.09496 -0.00032 0.00680 0.00171 AFIX 43 H5 2 -0.349426 0.814491 0.126012 11.00000 -1.20000 AFIX 0 C6 1 -0.237084 0.880213 0.155639 11.00000 0.05319 0.06267 = 0.08843 -0.00042 0.01353 0.00271 AFIX 43 H6 2 -0.264759 0.937752 0.176998 11.00000 -1.20000 AFIX 0 C7 1 -0.147280 0.867848 0.153930 11.00000 0.05256 0.06006 = 0.06828 0.00666 0.00209 -0.00453 C8 1 -0.076905 0.928776 0.179113 11.00000 0.04521 0.05692 = 0.06376 -0.00208 0.00704 0.00060 C9 1 0.002350 0.883853 0.165174 11.00000 0.05588 0.05980 = 0.05690 -0.00211 0.00209 -0.00119 C10 1 0.074868 0.941082 0.189017 11.00000 0.05843 0.05600 = 0.05969 0.00245 0.00166 0.00065 C11 1 0.042172 1.034330 0.221921 11.00000 0.06507 0.06040 = 0.06389 0.00013 0.00187 0.00282 C12 1 0.100074 1.111350 0.248390 11.00000 0.06975 0.07549 = 0.05751 -0.00320 0.00422 -0.00345 AFIX 43 H12 2 0.078534 1.174257 0.270273 11.00000 -1.20000 AFIX 0 C13 1 0.189206 1.094203 0.242108 11.00000 0.08106 0.07986 = 0.07420 -0.00050 -0.01455 -0.00200 AFIX 43 H13 2 0.229243 1.146784 0.259775 11.00000 -1.20000 AFIX 0 C14 1 0.221353 1.001876 0.210563 11.00000 0.06143 0.08971 = 0.08479 -0.00974 -0.00577 0.00586 AFIX 43 H14 2 0.283065 0.991347 0.207120 11.00000 -1.20000 AFIX 0 C15 1 0.165876 0.925403 0.184218 11.00000 0.05922 0.06625 = 0.06951 -0.00978 -0.00140 0.00520 AFIX 43 H15 2 0.189004 0.862001 0.162781 11.00000 -1.20000 AFIX 0 C16 1 0.039135 0.619277 0.129638 11.00000 0.05904 0.06233 = 0.06217 -0.00274 -0.00263 0.00314 C17 1 0.023439 0.496299 0.156930 11.00000 0.07257 0.06808 = 0.06810 0.00050 -0.00008 -0.00122 AFIX 43 H17 2 -0.021062 0.505669 0.177070 11.00000 -1.20000 AFIX 0 C18 1 0.074783 0.357759 0.154115 11.00000 0.08739 0.06726 = 0.07681 -0.00455 -0.01690 0.00167 AFIX 43 H18 2 0.064725 0.271862 0.172383 11.00000 -1.20000 AFIX 0 C19 1 0.140485 0.345279 0.124681 11.00000 0.07981 0.07028 = 0.09533 -0.01314 -0.02460 0.01280 AFIX 43 H19 2 0.175386 0.251490 0.123403 11.00000 -1.20000 AFIX 0 C20 1 0.155414 0.467123 0.097458 11.00000 0.05656 0.07828 = 0.07827 -0.01562 -0.00739 0.00540 AFIX 43 H20 2 0.199860 0.457320 0.077305 11.00000 -1.20000 AFIX 0 C21 1 0.104674 0.604680 0.099808 11.00000 0.05403 0.07016 = 0.06607 -0.01044 -0.00839 0.00324 C22 1 0.102582 0.751593 0.075928 11.00000 0.04841 0.07039 = 0.05892 -0.00194 -0.00150 -0.00442 C23 1 0.041108 0.853376 0.090302 11.00000 0.05078 0.06499 = 0.05774 -0.00739 0.00487 -0.00305 C24 1 0.037036 0.998733 0.068188 11.00000 0.05435 0.06552 = 0.06078 0.00347 -0.00366 -0.00853 C25 1 0.099562 0.998548 0.036041 11.00000 0.05673 0.07274 = 0.06153 0.00124 -0.00612 -0.00887 C26 1 0.107551 1.129151 0.010076 11.00000 0.05989 0.10183 = 0.06544 0.00762 -0.00094 -0.01396 AFIX 43 H26 2 0.149886 1.129648 -0.011177 11.00000 -1.20000 AFIX 0 C27 1 0.052626 1.257295 0.015983 11.00000 0.07063 0.08818 = 0.07572 0.01844 -0.00974 -0.01980 AFIX 43 H27 2 0.056698 1.346469 -0.001750 11.00000 -1.20000 AFIX 0 C28 1 -0.008438 1.259203 0.047188 11.00000 0.07742 0.06780 = 0.07548 0.00177 -0.00831 -0.00427 AFIX 43 H28 2 -0.045060 1.349996 0.050544 11.00000 -1.20000 AFIX 0 C29 1 -0.017319 1.131641 0.073625 11.00000 0.06241 0.06790 = 0.06665 -0.00106 -0.00124 -0.00264 AFIX 43 H29 2 -0.059381 1.134279 0.094984 11.00000 -1.20000 AFIX 0 HKLF 4 REM NakanoLab_170510_1_ REM R1 = 0.0779 for 2177 Fo > 4sig(Fo) and 0.1155 for all 3796 data REM 280 parameters refined using 0 restraints END WGHT 0.1467 0.0000 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.438, deepest hole -0.509, 1-sigma level 0.075 Q1 1 0.1737 0.6304 0.0598 11.00000 0.05 0.44 Q2 1 0.2591 1.0471 0.2773 11.00000 0.05 0.33 Q3 1 0.2221 0.8200 0.0695 11.00000 0.05 0.26 Q4 1 -0.1425 1.0273 0.2512 11.00000 0.05 0.24 Q5 1 0.2525 0.8292 0.0344 11.00000 0.05 0.24 Q6 1 0.0935 0.4510 0.1888 11.00000 0.05 0.24 Q7 1 0.2273 0.8173 -0.0034 11.00000 0.05 0.23 Q8 1 0.0927 0.8225 0.0014 11.00000 0.05 0.23 Q9 1 -0.3499 0.8287 0.0891 11.00000 0.05 0.22 Q10 1 -0.0648 0.8650 0.2217 11.00000 0.05 0.22 Q11 1 -0.3435 0.6858 0.1000 11.00000 0.05 0.22 Q12 1 0.3816 1.0371 0.2222 11.00000 0.05 0.22 Q13 1 0.1598 0.9096 -0.0177 11.00000 0.05 0.22 Q14 1 -0.0331 0.6097 0.0618 11.00000 0.05 0.22 Q15 1 0.0566 0.8246 0.0341 11.00000 0.05 0.21 Q16 1 0.1990 1.1988 0.0055 11.00000 0.05 0.21 Q17 1 -0.0978 1.2175 0.2169 11.00000 0.05 0.21 Q18 1 -0.2940 0.5854 0.1273 11.00000 0.05 0.21 Q19 1 0.0810 0.9437 0.2552 11.00000 0.05 0.21 Q20 1 0.1393 0.1992 0.0901 11.00000 0.05 0.21 ; _shelx_res_checksum 50755 _shelx_hkl_file ; 0 0 -3 2.23 3.43 0 0 3 2.10 6.79 0 0 -3 2.15 4.31 0 0 -3 1.09 4.00 0 0 3 3.60 4.14 0 0 3 2.79 3.72 0 0 -3 0.14 3.43 0 0 3 2.21 2.69 0 0 -4 2534.24 149.52 0 0 4 2630.73 126.12 0 0 -4 2796.82 161.91 0 0 -4 2783.25 137.48 0 0 4 2312.86 117.24 0 0 -4 2599.22 113.03 0 0 4 2686.32 134.29 0 0 4 2494.07 129.07 0 0 5 3.76 7.97 0 0 -5 0.40 4.51 0 0 5 -0.47 10.02 0 0 5 1.33 2.90 0 0 -5 -0.92 5.91 0 0 -5 1.34 4.50 0 0 -5 1.07 5.21 0 0 5 -1.65 4.71 0 0 -6 458.26 26.08 0 0 6 465.79 33.93 0 0 -6 465.94 35.64 0 0 6 448.07 25.27 0 0 -6 506.91 67.13 0 0 6 468.88 40.70 0 0 6 462.96 36.44 0 0 -7 0.88 6.46 0 0 7 -0.79 6.86 0 0 -7 1.13 10.83 0 0 7 3.90 5.24 0 0 -7 0.65 3.80 0 0 7 -2.38 10.38 0 0 7 0.35 6.27 0 0 8 360.06 21.73 0 0 8 364.06 33.34 0 0 -8 389.60 36.64 0 0 -8 356.75 38.85 0 0 8 366.87 50.26 0 0 8 368.00 38.45 0 0 -8 370.17 34.67 0 0 9 25.72 18.71 0 0 -9 22.77 16.92 0 0 9 15.45 8.70 0 0 9 14.74 7.64 0 0 -9 0.74 5.73 0 0 9 -3.85 8.42 0 0 10 137.47 11.80 0 0 -10 158.20 23.29 0 0 10 131.84 17.93 0 0 10 145.34 34.90 0 0 -10 136.71 21.73 0 0 -10 141.74 24.21 0 0 10 138.65 24.39 0 0 11 0.84 4.88 0 0 -11 0.21 10.64 0 0 -11 1.76 3.40 0 0 11 3.18 7.93 0 0 11 -0.36 5.03 0 0 11 -0.45 6.65 0 0 11 2.44 5.16 0 0 -11 0.49 5.99 0 0 -12 75.63 16.86 0 0 12 78.42 14.42 0 0 12 74.20 14.30 0 0 12 69.58 32.30 0 0 -12 96.60 16.80 0 0 12 83.54 13.19 0 0 -12 82.80 16.71 0 0 12 76.54 8.00 0 0 -13 0.03 1.95 0 0 13 3.16 3.11 0 0 13 -1.54 5.33 0 0 13 0.14 2.81 0 0 -13 -2.47 3.70 0 0 -13 -0.86 6.31 0 0 13 4.64 7.38 0 0 13 -1.31 2.76 0 0 -14 152.50 19.98 0 0 -14 132.31 18.08 0 0 14 142.87 16.49 0 0 -14 150.26 33.83 0 0 14 158.14 22.50 0 0 14 152.88 24.85 0 0 14 139.07 9.02 0 0 -15 -0.37 2.00 0 0 15 0.99 4.54 0 0 -15 -0.77 3.92 0 0 -15 -0.29 4.03 0 0 15 -0.16 3.27 0 0 15 -0.59 2.63 0 0 15 0.65 2.79 0 0 -16 1787.70 128.95 0 0 -16 1788.04 94.20 0 0 16 1799.84 77.32 0 0 16 1786.31 114.11 0 0 -16 1820.15 97.60 0 0 16 1865.24 91.32 0 0 16 1766.25 133.02 0 0 -17 10.54 8.61 0 0 17 0.75 3.95 0 0 17 1.48 5.74 0 0 17 1.88 5.65 0 0 -17 10.61 5.11 0 0 -17 -1.15 2.35 0 0 17 2.05 3.01 0 0 -18 12.60 6.43 0 0 -18 24.85 8.44 0 0 18 20.24 5.41 0 0 18 20.67 9.49 0 0 -18 17.28 8.31 0 0 18 13.98 2.96 0 0 18 14.19 6.52 0 0 19 1.46 6.06 0 0 -19 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33.81 2 -3 2 90.52 30.16 -2 3 2 85.71 10.36 2 3 -2 84.81 13.17 -2 -3 -2 87.76 10.95 2 -3 2 87.90 9.70 -2 -3 -2 92.66 8.16 2 3 -2 101.71 17.53 2 -3 2 81.78 5.51 -2 3 2 57.84 32.50 2 3 -2 82.70 23.09 2 3 -2 96.32 17.29 2 3 -2 86.80 8.59 -2 -3 -2 84.01 13.51 -2 3 2 90.11 14.12 -2 3 -3 22.55 9.70 2 3 3 21.25 8.69 2 3 3 22.58 9.34 2 3 3 18.74 10.42 -2 3 -3 17.41 15.55 -2 -3 3 19.02 7.15 -2 -3 3 -0.39 10.52 2 3 3 18.35 13.87 2 -3 -3 18.92 10.37 2 -3 -3 27.09 12.32 -2 3 -3 22.52 4.43 2 3 3 22.38 6.40 -2 -3 3 18.23 6.90 -2 -3 3 19.00 6.79 -2 3 3 14.62 12.38 2 -3 3 22.27 10.92 2 -3 3 16.63 7.27 -2 3 3 14.85 11.49 2 3 -3 17.17 14.98 2 3 -3 20.31 8.05 2 3 -3 16.60 5.54 -2 3 3 20.39 8.75 2 -3 3 27.43 4.10 2 3 -3 21.30 18.77 -2 -3 -3 17.01 11.54 -2 -3 -3 22.08 4.60 -2 3 -4 172.90 8.03 -2 3 -4 179.66 30.16 -2 3 -4 175.03 21.75 2 -3 -4 169.32 37.64 -2 -3 4 184.46 27.09 2 3 4 174.20 17.60 2 -3 -4 186.96 43.89 -2 -3 4 177.39 16.38 2 3 4 169.61 8.69 2 3 4 174.52 29.15 2 3 4 179.49 22.49 -2 -3 4 173.82 22.15 -2 -3 4 170.20 23.32 2 3 4 179.13 19.25 -2 -3 -4 182.04 19.44 2 3 -4 169.65 22.95 2 3 -4 170.71 30.74 -2 3 4 175.81 18.42 -2 3 4 182.58 17.21 2 -3 4 167.96 11.33 2 -3 4 181.93 23.19 -2 -3 -4 181.48 23.29 2 3 -4 181.91 28.49 2 -3 4 174.42 18.41 2 3 -4 171.45 13.24 -2 -3 -4 173.44 16.94 -2 3 4 174.56 23.51 2 -3 -5 1863.30 101.79 2 3 5 1836.76 112.77 -2 3 -5 1879.70 133.04 2 3 5 1846.13 103.11 2 3 5 1808.13 80.07 -2 -3 5 1953.08 96.15 -2 -3 5 1844.05 85.02 -2 -3 5 1915.00 102.58 2 3 5 1895.99 121.06 -2 3 -5 1829.51 90.73 2 3 5 1914.65 92.96 -2 -3 5 1857.00 90.17 2 -3 -5 1939.93 113.87 -2 3 -5 1522.18 52.44 2 3 -5 1825.88 107.90 2 -3 5 1949.35 86.55 -2 -3 -5 1881.31 103.11 2 3 -5 1835.25 96.79 -2 3 5 1980.63 141.46 2 3 -5 1831.71 101.65 -2 3 5 1864.07 94.21 2 3 -5 1849.44 85.09 -2 3 5 1909.17 120.38 -2 -3 -5 1859.99 97.23 -2 -3 -5 1916.83 90.86 -2 3 5 1769.04 60.71 2 -3 5 1864.69 104.85 2 -3 5 1865.36 74.72 2 3 6 4.82 8.79 -2 -3 6 6.32 10.71 -2 -3 6 2.35 4.96 2 -3 -6 6.48 6.60 -2 3 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3.08 2.85 2 9 13 1.14 2.56 2 9 13 -1.96 5.46 2 9 -13 1.17 4.91 -2 9 13 -3.65 7.77 2 9 14 1.55 2.97 2 9 14 -1.97 3.16 -2 9 -14 5.81 4.29 -2 9 -14 8.24 3.01 2 9 -14 9.10 9.13 -2 9 14 -0.06 8.47 -2 9 -15 -0.80 5.43 -2 9 15 3.46 3.59 2 9 -15 -1.87 4.05 -2 9 -16 4.11 3.83 2 9 -16 -6.98 7.06 -2 9 16 4.19 3.94 -2 9 -17 -1.57 4.71 -2 9 17 2.51 4.06 -2 10 0 13.19 8.58 2 10 0 15.20 7.18 2 10 1 -0.11 7.92 -2 10 -1 7.00 5.45 -2 10 1 -10.72 9.73 2 10 -1 -9.12 4.78 -2 10 -2 10.71 8.93 2 10 -2 2.07 4.76 -2 10 2 -4.07 9.63 -2 10 3 -1.60 6.57 2 10 -3 -17.67 11.83 -3 0 0 1.04 4.68 3 0 0 2.59 5.32 3 0 0 2.80 10.17 3 0 0 2.60 5.25 -3 0 0 1.59 4.37 -3 0 0 3.44 4.30 -3 0 0 1.41 9.41 3 0 0 1.72 3.47 3 0 -1 4.31 6.89 -3 0 1 0.40 5.68 -3 0 -1 4.92 6.33 -3 0 1 2.14 4.45 -3 0 -1 1.42 4.36 3 0 -1 2.83 7.65 -3 0 -1 0.52 9.13 3 0 1 3.92 4.58 -3 0 1 2.12 6.63 3 0 1 1.37 5.84 -3 0 -1 3.52 4.53 -3 0 1 2.47 6.13 3 0 -1 3.65 5.43 3 0 1 2.67 6.04 3 0 -1 5.49 6.09 3 0 1 2.94 5.42 -3 0 2 6005.42 335.33 3 0 2 5896.04 330.39 -3 0 2 6152.07 336.51 -3 0 -2 6091.04 345.09 -3 0 -2 5925.95 324.32 -3 0 2 5547.65 341.03 3 0 -2 5452.25 336.62 3 0 -2 5912.03 400.73 3 0 -2 6067.05 370.56 3 0 2 6144.76 382.90 -3 0 -2 6274.50 341.98 3 0 2 6091.28 350.73 3 0 -2 6181.03 389.73 3 0 2 5891.45 339.86 -3 0 2 5997.89 400.12 -3 0 -2 5910.98 321.65 -3 0 3 1.38 5.70 3 0 -3 -0.63 6.79 -3 0 -3 -0.69 5.80 -3 0 -3 2.63 3.07 3 0 -3 1.07 6.06 3 0 3 -0.40 9.86 -3 0 3 1.79 8.13 -3 0 -3 0.23 4.80 3 0 3 0.97 4.24 -3 0 3 0.29 6.89 3 0 3 0.89 2.62 -3 0 -3 1.12 4.15 3 0 -3 0.76 4.55 3 0 -3 1.16 8.57 3 0 3 0.78 3.96 3 0 -4 3395.85 194.49 -3 0 -4 3414.36 186.88 -3 0 -4 3704.73 159.86 3 0 4 3658.46 163.45 3 0 4 3685.43 199.68 -3 0 -4 3553.41 175.85 -3 0 4 3331.03 202.06 -3 0 4 3539.96 247.88 -3 0 4 3495.17 227.29 3 0 -4 3391.83 203.90 3 0 4 3407.54 179.71 3 0 -4 3590.48 189.39 3 0 -4 3505.73 182.85 -3 0 -4 3452.45 187.00 3 0 4 3517.86 202.93 3 0 -5 1.76 7.89 -3 0 5 -1.40 5.52 3 0 -5 3.99 11.42 3 0 -5 1.88 8.58 -3 0 -5 0.56 0.75 -3 0 5 -1.59 8.65 3 0 5 1.57 5.06 -3 0 -5 3.08 8.52 3 0 5 -0.58 3.21 -3 0 5 -0.86 6.36 3 0 -5 -3.53 10.26 3 0 5 0.15 0.82 -3 0 -5 3.18 5.23 3 0 5 -0.74 4.67 -3 0 -6 1162.88 101.48 3 0 -6 1172.41 64.58 3 0 -6 1183.93 69.55 3 0 6 1193.26 105.19 -3 0 6 1165.16 68.22 -3 0 6 1216.79 80.60 -3 0 6 1222.09 75.54 3 0 -6 1148.86 118.39 3 0 6 1167.70 55.95 3 0 -6 1187.31 114.13 -3 0 7 12.11 15.06 3 0 -7 7.28 8.90 -3 0 -7 1.98 4.21 -3 0 -7 3.79 13.63 -3 0 7 4.93 6.22 3 0 7 2.26 7.70 3 0 -7 8.71 8.62 3 0 -7 24.40 13.94 -3 0 7 1.74 7.99 -3 0 7 4.16 7.45 3 0 7 1.84 4.49 -3 0 -7 4.55 7.48 3 0 -8 2036.76 156.94 -3 0 8 2082.41 155.23 3 0 -8 2026.39 119.24 3 0 8 2013.13 95.48 -3 0 8 2019.02 113.09 -3 0 8 1974.20 152.29 3 0 -8 1994.54 119.63 -3 0 8 2025.72 106.68 3 0 8 2057.97 117.01 -3 0 -8 2105.98 118.52 -3 0 -8 2056.98 116.20 -3 0 -8 2033.62 157.30 -3 0 9 -1.26 5.23 3 0 -9 -0.25 5.32 3 0 -9 0.13 5.36 -3 0 -9 1.11 5.57 3 0 9 0.16 2.95 -3 0 -9 0.19 5.17 -3 0 9 -1.35 4.37 3 0 -9 -3.76 5.58 -3 0 9 0.74 4.66 -3 0 9 0.46 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