# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a30403a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 I N O2 S' _chemical_formula_weight 413.26 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_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' _cell_length_a 12.460(5) _cell_length_b 7.632(3) _cell_length_c 17.002(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.153(6) _cell_angle_gamma 90.00 _cell_volume 1616.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 957 _cell_measurement_theta_min 2.396 _cell_measurement_theta_max 26.006 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 2.114 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4497 _exptl_absorpt_correction_T_max 0.6772 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.70 _diffrn_reflns_number 6934 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3166 _reflns_number_gt 1945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0934P)^2^+0.5778P] 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 SHELXL _refine_ls_extinction_coef 0.0155(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3166 _refine_ls_number_parameters 194 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1747 _refine_ls_wR_factor_gt 0.1569 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.002 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I -0.07275(4) 1.00659(6) 0.11183(3) 0.0988(3) Uani 1 1 d . . . S1 S 0.24176(15) 1.0838(3) 0.45842(8) 0.0902(6) Uani 1 1 d U . . N1 N 0.1450(5) 0.9391(8) 0.4445(3) 0.0923(16) Uani 1 1 d DU . . O1 O 0.2933(5) 1.0477(8) 0.5318(3) 0.1233(19) Uani 1 1 d . . . O2 O 0.1933(4) 1.2534(7) 0.4455(3) 0.1112(16) Uani 1 1 d . . . C1 C 0.3267(5) 1.0384(7) 0.3812(3) 0.0719(15) Uani 1 1 d . . . C2 C 0.4380(5) 1.0457(8) 0.3898(5) 0.087(2) Uani 1 1 d . . . H2 H 0.4693 1.0760 0.4380 0.105 Uiso 1 1 calc R . . C3 C 0.5000(6) 1.0088(8) 0.3285(5) 0.088(2) Uani 1 1 d . . . H3 H 0.5742 1.0159 0.3347 0.106 Uiso 1 1 calc R . . C4 C 0.4570(5) 0.9609(7) 0.2564(4) 0.0785(17) Uani 1 1 d . . . C5 C 0.3460(5) 0.9521(7) 0.2478(4) 0.0691(15) Uani 1 1 d . . . H5 H 0.3162 0.9185 0.1996 0.083 Uiso 1 1 calc R . . C6 C 0.2776(4) 0.9926(6) 0.3098(3) 0.0607(13) Uani 1 1 d . . . C7 C 0.1602(4) 0.9753(5) 0.3021(3) 0.0586(12) Uani 1 1 d . . . C8 C 0.1077(4) 0.9909(6) 0.2297(3) 0.0607(12) Uani 1 1 d . . . H8 H 0.1465 1.0192 0.1853 0.073 Uiso 1 1 calc R . . C9 C -0.0018(5) 0.9645(6) 0.2231(3) 0.0656(14) Uani 1 1 d . . . C10 C -0.0624(4) 0.9201(8) 0.2868(3) 0.0698(14) Uani 1 1 d . . . C11 C -0.0102(5) 0.9127(8) 0.3594(3) 0.0754(14) Uani 1 1 d . . . H11 H -0.0498 0.8870 0.4037 0.090 Uiso 1 1 calc R . . C12 C 0.0985(5) 0.9421(7) 0.3679(3) 0.0669(13) Uani 1 1 d . . . C13 C 0.5271(6) 0.9133(10) 0.1888(5) 0.105(2) Uani 1 1 d . . . H13A H 0.5491 1.0181 0.1623 0.158 Uiso 1 1 calc R . . H13B H 0.4878 0.8398 0.1527 0.158 Uiso 1 1 calc R . . H13C H 0.5894 0.8518 0.2083 0.158 Uiso 1 1 calc R . . C14 C -0.1824(4) 0.8874(11) 0.2818(4) 0.101(2) Uani 1 1 d . . . H14A H -0.2188 0.9946 0.2686 0.151 Uiso 1 1 calc R . . H14B H -0.2066 0.8457 0.3317 0.151 Uiso 1 1 calc R . . H14C H -0.1976 0.8012 0.2421 0.151 Uiso 1 1 calc R . . C15 C 0.1295(8) 0.7973(13) 0.4992(5) 0.163(4) Uani 1 1 d DU . . H15A H 0.0555 0.7577 0.4996 0.196 Uiso 1 1 calc R . . H15B H 0.1534 0.8272 0.5521 0.196 Uiso 1 1 calc R . . C16 C 0.2002(8) 0.6703(14) 0.4621(5) 0.150(4) Uani 1 1 d DU . . H16A H 0.1815 0.6605 0.4073 0.225 Uiso 1 1 calc R . . H16B H 0.1924 0.5582 0.4870 0.225 Uiso 1 1 calc R . . H16C H 0.2733 0.7088 0.4678 0.225 Uiso 1 1 calc R . . 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 I1 0.0994(5) 0.1126(5) 0.0822(4) -0.0023(2) -0.0496(3) 0.0098(2) S1 0.1029(13) 0.1071(13) 0.0594(8) 0.0017(8) -0.0289(8) -0.0229(11) N1 0.108(4) 0.112(4) 0.056(3) 0.029(3) -0.028(3) -0.033(3) O1 0.133(4) 0.168(5) 0.067(3) 0.004(3) -0.047(3) -0.030(4) O2 0.137(4) 0.103(3) 0.092(3) -0.017(3) -0.019(3) -0.003(3) C1 0.079(4) 0.071(3) 0.065(3) 0.013(2) -0.031(3) -0.012(3) C2 0.078(4) 0.085(4) 0.097(5) 0.022(3) -0.046(4) -0.022(3) C3 0.060(3) 0.096(5) 0.108(6) 0.021(4) -0.029(4) -0.015(3) C4 0.068(4) 0.057(3) 0.110(5) 0.012(3) -0.016(3) -0.003(3) C5 0.065(3) 0.058(3) 0.083(4) 0.004(3) -0.023(3) -0.005(2) C6 0.060(3) 0.060(3) 0.062(3) 0.007(2) -0.023(2) -0.005(2) C7 0.063(3) 0.053(3) 0.059(3) 0.002(2) -0.018(2) -0.002(2) C8 0.059(3) 0.065(3) 0.057(3) -0.002(2) -0.016(2) 0.005(2) C9 0.069(3) 0.065(3) 0.062(3) -0.006(2) -0.027(3) 0.008(2) C10 0.060(3) 0.066(3) 0.083(4) -0.006(3) -0.015(3) 0.001(3) C11 0.070(3) 0.084(4) 0.072(3) 0.004(3) -0.005(3) -0.009(3) C12 0.067(3) 0.074(3) 0.060(3) 0.005(3) -0.015(3) -0.010(3) C13 0.081(4) 0.098(5) 0.138(6) -0.011(5) 0.001(4) 0.005(4) C14 0.057(3) 0.123(6) 0.122(5) -0.001(5) -0.022(3) -0.008(4) C15 0.158(8) 0.198(9) 0.132(7) -0.030(7) -0.028(6) -0.014(7) C16 0.178(9) 0.166(9) 0.104(6) -0.004(6) -0.049(6) -0.004(8) _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 I1 C9 2.096(5) . ? S1 O1 1.418(5) . ? S1 O2 1.443(6) . ? S1 N1 1.649(6) . ? S1 C1 1.738(7) . ? N1 C12 1.415(7) . ? N1 C15 1.442(8) . ? C1 C6 1.392(7) . ? C1 C2 1.393(9) . ? C2 C3 1.339(11) . ? C3 C4 1.377(11) . ? C4 C5 1.389(8) . ? C4 C13 1.503(10) . ? C5 C6 1.404(9) . ? C6 C7 1.472(7) . ? C7 C8 1.387(7) . ? C7 C12 1.394(8) . ? C8 C9 1.382(8) . ? C9 C10 1.375(8) . ? C10 C11 1.384(7) . ? C10 C14 1.516(7) . ? C11 C12 1.378(8) . ? C15 C16 1.461(8) . ? 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 O1 S1 O2 119.3(3) . . ? O1 S1 N1 108.2(3) . . ? O2 S1 N1 106.0(3) . . ? O1 S1 C1 110.8(4) . . ? O2 S1 C1 108.8(3) . . ? N1 S1 C1 102.3(3) . . ? C12 N1 C15 123.2(6) . . ? C12 N1 S1 113.9(4) . . ? C15 N1 S1 121.2(5) . . ? C6 C1 C2 121.4(6) . . ? C6 C1 S1 116.4(5) . . ? C2 C1 S1 122.2(5) . . ? C3 C2 C1 119.9(6) . . ? C2 C3 C4 121.9(6) . . ? C3 C4 C5 118.4(7) . . ? C3 C4 C13 121.5(6) . . ? C5 C4 C13 120.1(6) . . ? C4 C5 C6 121.9(6) . . ? C1 C6 C5 116.6(5) . . ? C1 C6 C7 121.3(5) . . ? C5 C6 C7 122.0(5) . . ? C8 C7 C12 118.0(5) . . ? C8 C7 C6 121.5(5) . . ? C12 C7 C6 120.5(5) . . ? C9 C8 C7 120.5(5) . . ? C10 C9 C8 121.9(5) . . ? C10 C9 I1 121.4(4) . . ? C8 C9 I1 116.7(4) . . ? C9 C10 C11 117.2(5) . . ? C9 C10 C14 123.5(5) . . ? C11 C10 C14 119.2(6) . . ? C12 C11 C10 122.0(5) . . ? C11 C12 C7 120.2(5) . . ? C11 C12 N1 118.5(5) . . ? C7 C12 N1 121.3(5) . . ? N1 C15 C16 97.5(8) . . ? 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 O1 S1 N1 C12 -170.2(5) . . . . ? O2 S1 N1 C12 60.8(6) . . . . ? C1 S1 N1 C12 -53.2(6) . . . . ? O1 S1 N1 C15 -4.6(8) . . . . ? O2 S1 N1 C15 -133.7(7) . . . . ? C1 S1 N1 C15 112.4(7) . . . . ? O1 S1 C1 C6 152.5(4) . . . . ? O2 S1 C1 C6 -74.5(5) . . . . ? N1 S1 C1 C6 37.4(5) . . . . ? O1 S1 C1 C2 -27.0(6) . . . . ? O2 S1 C1 C2 106.0(5) . . . . ? N1 S1 C1 C2 -142.1(5) . . . . ? C6 C1 C2 C3 0.3(9) . . . . ? S1 C1 C2 C3 179.7(5) . . . . ? C1 C2 C3 C4 -1.0(9) . . . . ? C2 C3 C4 C5 0.4(9) . . . . ? C2 C3 C4 C13 -177.7(6) . . . . ? C3 C4 C5 C6 0.8(8) . . . . ? C13 C4 C5 C6 179.0(5) . . . . ? C2 C1 C6 C5 0.8(7) . . . . ? S1 C1 C6 C5 -178.6(4) . . . . ? C2 C1 C6 C7 176.5(5) . . . . ? S1 C1 C6 C7 -3.0(6) . . . . ? C4 C5 C6 C1 -1.4(7) . . . . ? C4 C5 C6 C7 -177.0(5) . . . . ? C1 C6 C7 C8 157.1(5) . . . . ? C5 C6 C7 C8 -27.4(7) . . . . ? C1 C6 C7 C12 -23.1(7) . . . . ? C5 C6 C7 C12 152.4(5) . . . . ? C12 C7 C8 C9 -3.4(7) . . . . ? C6 C7 C8 C9 176.4(4) . . . . ? C7 C8 C9 C10 -0.9(7) . . . . ? C7 C8 C9 I1 176.5(3) . . . . ? C8 C9 C10 C11 3.7(8) . . . . ? I1 C9 C10 C11 -173.5(4) . . . . ? C8 C9 C10 C14 -179.1(6) . . . . ? I1 C9 C10 C14 3.7(8) . . . . ? C9 C10 C11 C12 -2.3(9) . . . . ? C14 C10 C11 C12 -179.6(6) . . . . ? C10 C11 C12 C7 -2.0(10) . . . . ? C10 C11 C12 N1 177.4(6) . . . . ? C8 C7 C12 C11 4.8(8) . . . . ? C6 C7 C12 C11 -175.0(5) . . . . ? C8 C7 C12 N1 -174.6(5) . . . . ? C6 C7 C12 N1 5.6(8) . . . . ? C15 N1 C12 C11 51.3(11) . . . . ? S1 N1 C12 C11 -143.5(5) . . . . ? C15 N1 C12 C7 -129.3(8) . . . . ? S1 N1 C12 C7 36.0(8) . . . . ? C12 N1 C15 C16 74.7(9) . . . . ? S1 N1 C15 C16 -89.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.890 _refine_diff_density_min -1.040 _refine_diff_density_rms 0.111 _database_code_depnum_ccdc_archive 'CCDC 951230' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a30403b _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H17 N O2 S' _chemical_formula_weight 287.36 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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' _cell_length_a 9.396(4) _cell_length_b 17.340(6) _cell_length_c 9.934(4) _cell_angle_alpha 90 _cell_angle_beta 114.283(4) _cell_angle_gamma 90 _cell_volume 1475.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 997 _cell_measurement_theta_min 2.538 _cell_measurement_theta_max 24.768 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_F_000 608 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_min 0.150 _exptl_absorpt_coefficient_mu 0.220 _shelx_estimated_absorpt_T_min 0.915 _shelx_estimated_absorpt_T_max 0.968 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6517 _diffrn_reflns_av_unetI/netI 0.0797 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.349 _diffrn_reflns_theta_max 26.008 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 2901 _reflns_number_gt 2309 _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 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0940P)^2^+0.3772P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.075(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2901 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.1882 _refine_ls_wR_factor_gt 0.1731 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.006 _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 0.77604(7) 0.06327(4) 0.06424(6) 0.0527(3) Uani 1 1 d . . . . . O1 O 0.7566(2) -0.01789(11) 0.0413(2) 0.0690(6) Uani 1 1 d . . . . . O2 O 0.7069(2) 0.11308(12) -0.06014(18) 0.0667(6) Uani 1 1 d . . . . . N1 N 0.9626(2) 0.08170(12) 0.1409(2) 0.0503(5) Uani 1 1 d . . . . . C1 C 0.7141(3) 0.09281(15) 0.2001(3) 0.0517(6) Uani 1 1 d . . . . . C2 C 0.5978(3) 0.05282(18) 0.2216(3) 0.0651(7) Uani 1 1 d . . . . . H2 H 0.5545 0.0085 0.1674 0.078 Uiso 1 1 calc R U . . . C3 C 0.5476(3) 0.0797(2) 0.3244(4) 0.0736(9) Uani 1 1 d . . . . . H3 H 0.4680 0.0538 0.3381 0.088 Uiso 1 1 calc R U . . . C4 C 0.6126(3) 0.1446(2) 0.4083(3) 0.0660(8) Uani 1 1 d . . . . . C5 C 0.7314(3) 0.18286(17) 0.3866(3) 0.0577(7) Uani 1 1 d . . . . . H5 H 0.7761 0.2263 0.4430 0.069 Uiso 1 1 calc R U . . . C6 C 0.7851(3) 0.15784(14) 0.2825(3) 0.0489(6) Uani 1 1 d . . . . . C7 C 0.9140(3) 0.19726(14) 0.2615(2) 0.0467(6) Uani 1 1 d . . . . . C8 C 1.0013(3) 0.15853(14) 0.1962(2) 0.0472(6) Uani 1 1 d . . . . . C9 C 1.1282(3) 0.19406(15) 0.1843(3) 0.0558(6) Uani 1 1 d . . . . . H9 H 1.1855 0.1672 0.1422 0.067 Uiso 1 1 calc R U . . . C10 C 1.1708(3) 0.26829(17) 0.2336(3) 0.0641(7) Uani 1 1 d . . . . . C11 C 1.0830(3) 0.30737(16) 0.2954(3) 0.0657(8) Uani 1 1 d . . . . . H11 H 1.1090 0.3578 0.3283 0.079 Uiso 1 1 calc R U . . . C12 C 0.9585(3) 0.27244(15) 0.3085(3) 0.0579(7) Uani 1 1 d . . . . . H12 H 0.9018 0.3000 0.3503 0.070 Uiso 1 1 calc R U . . . C13 C 1.0747(3) 0.01982(16) 0.2121(3) 0.0645(8) Uani 1 1 d . . . . . H13A H 1.1750 0.0335 0.2127 0.077 Uiso 1 1 calc R U . . . H13B H 1.0394 -0.0271 0.1548 0.077 Uiso 1 1 calc R U . . . C14 C 1.0945(6) 0.0049(2) 0.3668(4) 0.1124(15) Uani 1 1 d . . . . . H14A H 1.1402 0.0493 0.4267 0.169 Uiso 1 1 calc R U . . . H14B H 1.1616 -0.0389 0.4056 0.169 Uiso 1 1 calc R U . . . H14C H 0.9945 -0.0054 0.3677 0.169 Uiso 1 1 calc R U . . . C15 C 0.5582(4) 0.1719(3) 0.5228(4) 0.0944(12) Uani 1 1 d . . . . . H15A H 0.6100 0.1429 0.6121 0.142 Uiso 1 1 calc R U . . . H15B H 0.4474 0.1646 0.4870 0.142 Uiso 1 1 calc R U . . . H15C H 0.5825 0.2256 0.5423 0.142 Uiso 1 1 calc R U . . . C16 C 1.3045(5) 0.3082(2) 0.2144(5) 0.0969(12) Uani 1 1 d . . . . . H16A H 1.3647 0.2708 0.1890 0.145 Uiso 1 1 calc R U . . . H16B H 1.3699 0.3333 0.3050 0.145 Uiso 1 1 calc R U . . . H16C H 1.2638 0.3459 0.1371 0.145 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 0.0464(4) 0.0628(5) 0.0425(4) -0.0076(3) 0.0117(3) -0.0031(2) O1 0.0633(13) 0.0673(13) 0.0681(12) -0.0204(10) 0.0187(10) -0.0126(9) O2 0.0624(12) 0.0838(14) 0.0430(10) 0.0018(9) 0.0108(9) 0.0046(9) N1 0.0465(12) 0.0560(12) 0.0472(11) -0.0056(9) 0.0180(9) 0.0002(8) C1 0.0369(12) 0.0658(15) 0.0468(13) -0.0006(12) 0.0117(10) -0.0012(10) C2 0.0428(14) 0.086(2) 0.0599(16) -0.0034(14) 0.0148(13) -0.0126(12) C3 0.0395(14) 0.115(3) 0.0664(18) 0.0032(18) 0.0217(14) -0.0124(14) C4 0.0443(14) 0.102(2) 0.0533(15) 0.0051(15) 0.0223(13) 0.0051(14) C5 0.0506(14) 0.0733(17) 0.0500(14) -0.0015(13) 0.0216(12) 0.0019(12) C6 0.0421(13) 0.0612(15) 0.0423(12) 0.0025(11) 0.0164(10) 0.0043(10) C7 0.0449(13) 0.0535(14) 0.0396(11) -0.0006(10) 0.0154(10) 0.0003(10) C8 0.0466(13) 0.0559(14) 0.0381(11) 0.0004(10) 0.0164(10) -0.0017(10) C9 0.0529(15) 0.0669(16) 0.0522(14) 0.0033(12) 0.0261(12) -0.0022(11) C10 0.0592(16) 0.0683(17) 0.0645(16) 0.0108(14) 0.0252(14) -0.0097(13) C11 0.0742(19) 0.0535(15) 0.0676(17) -0.0006(13) 0.0274(16) -0.0102(13) C12 0.0610(16) 0.0571(15) 0.0562(15) -0.0037(12) 0.0245(13) 0.0019(12) C13 0.0514(15) 0.0606(17) 0.0721(18) -0.0084(13) 0.0160(14) 0.0070(11) C14 0.145(4) 0.092(3) 0.065(2) 0.014(2) 0.007(2) 0.029(3) C15 0.071(2) 0.149(3) 0.079(2) -0.005(2) 0.0479(19) 0.004(2) C16 0.092(3) 0.089(2) 0.128(3) 0.013(2) 0.064(3) -0.0225(19) _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 O1 1.425(2) . ? S1 O2 1.426(2) . ? S1 N1 1.630(2) . ? S1 C1 1.751(3) . ? N1 C8 1.430(3) . ? N1 C13 1.466(3) . ? C1 C2 1.383(4) . ? C1 C6 1.392(4) . ? C2 C3 1.371(4) . ? C3 C4 1.382(4) . ? C4 C5 1.389(4) . ? C4 C15 1.502(4) . ? C5 C6 1.394(3) . ? C6 C7 1.479(3) . ? C7 C12 1.390(3) . ? C7 C8 1.408(3) . ? C8 C9 1.390(3) . ? C9 C10 1.377(4) . ? C10 C11 1.391(4) . ? C10 C16 1.513(4) . ? C11 C12 1.370(4) . ? C13 C14 1.493(5) . ? 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 O1 S1 O2 118.48(12) . . ? O1 S1 N1 108.12(11) . . ? O2 S1 N1 107.76(11) . . ? O1 S1 C1 110.50(12) . . ? O2 S1 C1 108.24(12) . . ? N1 S1 C1 102.53(11) . . ? C8 N1 C13 118.6(2) . . ? C8 N1 S1 114.65(16) . . ? C13 N1 S1 120.20(18) . . ? C2 C1 C6 122.2(2) . . ? C2 C1 S1 120.4(2) . . ? C6 C1 S1 117.39(18) . . ? C3 C2 C1 118.7(3) . . ? C2 C3 C4 121.6(3) . . ? C3 C4 C5 118.6(2) . . ? C3 C4 C15 120.6(3) . . ? C5 C4 C15 120.7(3) . . ? C4 C5 C6 121.7(3) . . ? C1 C6 C5 117.2(2) . . ? C1 C6 C7 120.9(2) . . ? C5 C6 C7 121.9(2) . . ? C12 C7 C8 116.8(2) . . ? C12 C7 C6 122.5(2) . . ? C8 C7 C6 120.7(2) . . ? C9 C8 C7 120.7(2) . . ? C9 C8 N1 118.2(2) . . ? C7 C8 N1 121.1(2) . . ? C10 C9 C8 121.2(2) . . ? C9 C10 C11 118.3(2) . . ? C9 C10 C16 121.2(3) . . ? C11 C10 C16 120.5(3) . . ? C12 C11 C10 120.8(3) . . ? C11 C12 C7 122.2(2) . . ? N1 C13 C14 112.6(3) . . ? 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 O1 S1 N1 C8 -168.75(17) . . . . ? O2 S1 N1 C8 62.08(19) . . . . ? C1 S1 N1 C8 -52.00(19) . . . . ? O1 S1 N1 C13 -17.6(2) . . . . ? O2 S1 N1 C13 -146.8(2) . . . . ? C1 S1 N1 C13 99.1(2) . . . . ? O1 S1 C1 C2 -29.1(3) . . . . ? O2 S1 C1 C2 102.1(2) . . . . ? N1 S1 C1 C2 -144.2(2) . . . . ? O1 S1 C1 C6 151.60(19) . . . . ? O2 S1 C1 C6 -77.2(2) . . . . ? N1 S1 C1 C6 36.6(2) . . . . ? C6 C1 C2 C3 2.1(4) . . . . ? S1 C1 C2 C3 -177.1(2) . . . . ? C1 C2 C3 C4 -1.3(5) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C2 C3 C4 C15 -178.6(3) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C15 C4 C5 C6 179.1(3) . . . . ? C2 C1 C6 C5 -1.6(4) . . . . ? S1 C1 C6 C5 177.63(18) . . . . ? C2 C1 C6 C7 177.2(2) . . . . ? S1 C1 C6 C7 -3.5(3) . . . . ? C4 C5 C6 C1 0.3(4) . . . . ? C4 C5 C6 C7 -178.5(2) . . . . ? C1 C6 C7 C12 161.6(2) . . . . ? C5 C6 C7 C12 -19.6(4) . . . . ? C1 C6 C7 C8 -20.5(4) . . . . ? C5 C6 C7 C8 158.3(2) . . . . ? C12 C7 C8 C9 1.8(3) . . . . ? C6 C7 C8 C9 -176.2(2) . . . . ? C12 C7 C8 N1 -178.5(2) . . . . ? C6 C7 C8 N1 3.5(3) . . . . ? C13 N1 C8 C9 64.7(3) . . . . ? S1 N1 C8 C9 -143.7(2) . . . . ? C13 N1 C8 C7 -115.1(3) . . . . ? S1 N1 C8 C7 36.5(3) . . . . ? C7 C8 C9 C10 -1.1(4) . . . . ? N1 C8 C9 C10 179.2(2) . . . . ? C8 C9 C10 C11 -0.3(4) . . . . ? C8 C9 C10 C16 -177.3(3) . . . . ? C9 C10 C11 C12 0.8(4) . . . . ? C16 C10 C11 C12 177.8(3) . . . . ? C10 C11 C12 C7 0.0(4) . . . . ? C8 C7 C12 C11 -1.3(4) . . . . ? C6 C7 C12 C11 176.7(2) . . . . ? C8 N1 C13 C14 66.6(3) . . . . ? S1 N1 C13 C14 -83.4(3) . . . . ? _refine_diff_density_max 0.573 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.080 _shelxl_version_number 2013-2 _shelx_res_file ; TITL a30403b in P2(1)/c CELL 0.71073 9.3959 17.3404 9.9341 90.000 114.283 90.000 ZERR 4.00 0.0035 0.0063 0.0037 0.000 0.004 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 64 68 4 8 4 OMIT -2.00 52.02 L.S. 5 ACTA BOND FMAP 2 PLAN 1 CONF SIZE 0.41 0.26 0.15 TEMP 20 WGHT 0.094000 0.377200 EXTI 0.074549 FVAR 0.45376 MOLE 1 S1 5 0.776042 0.063270 0.064240 11.00000 0.04638 0.06276 = 0.04251 -0.00762 0.01173 -0.00310 O1 4 0.756560 -0.017893 0.041347 11.00000 0.06328 0.06730 = 0.06808 -0.02042 0.01871 -0.01262 O2 4 0.706912 0.113083 -0.060137 11.00000 0.06241 0.08383 = 0.04297 0.00179 0.01079 0.00455 N1 3 0.962606 0.081701 0.140880 11.00000 0.04649 0.05600 = 0.04723 -0.00562 0.01802 0.00017 C1 1 0.714150 0.092811 0.200060 11.00000 0.03688 0.06584 = 0.04682 -0.00060 0.01173 -0.00119 C2 1 0.597814 0.052819 0.221596 11.00000 0.04278 0.08644 = 0.05990 -0.00341 0.01478 -0.01258 AFIX 43 H2 2 0.554493 0.008541 0.167388 11.00000 -1.20000 AFIX 0 C3 1 0.547627 0.079749 0.324447 11.00000 0.03948 0.11479 = 0.06643 0.00320 0.02170 -0.01236 AFIX 43 H3 2 0.467982 0.053780 0.338129 11.00000 -1.20000 AFIX 0 C4 1 0.612557 0.144558 0.408272 11.00000 0.04434 0.10248 = 0.05331 0.00512 0.02230 0.00507 C5 1 0.731350 0.182855 0.386613 11.00000 0.05061 0.07330 = 0.04998 -0.00155 0.02162 0.00193 AFIX 43 H5 2 0.776149 0.226302 0.443037 11.00000 -1.20000 AFIX 0 C6 1 0.785087 0.157837 0.282517 11.00000 0.04214 0.06124 = 0.04230 0.00253 0.01637 0.00433 C7 1 0.914032 0.197262 0.261515 11.00000 0.04490 0.05354 = 0.03956 -0.00059 0.01536 0.00029 C8 1 1.001338 0.158532 0.196179 11.00000 0.04659 0.05590 = 0.03807 0.00040 0.01638 -0.00170 C9 1 1.128236 0.194065 0.184269 11.00000 0.05288 0.06691 = 0.05218 0.00332 0.02609 -0.00217 AFIX 43 H9 2 1.185457 0.167210 0.142236 11.00000 -1.20000 AFIX 0 C10 1 1.170788 0.268293 0.233554 11.00000 0.05925 0.06832 = 0.06454 0.01078 0.02522 -0.00968 C11 1 1.082956 0.307368 0.295442 11.00000 0.07415 0.05352 = 0.06764 -0.00061 0.02737 -0.01020 AFIX 43 H11 2 1.109034 0.357779 0.328291 11.00000 -1.20000 AFIX 0 C12 1 0.958497 0.272437 0.308548 11.00000 0.06103 0.05708 = 0.05617 -0.00368 0.02453 0.00192 AFIX 43 H12 2 0.901849 0.299953 0.350326 11.00000 -1.20000 AFIX 0 C13 1 1.074659 0.019816 0.212068 11.00000 0.05142 0.06064 = 0.07211 -0.00841 0.01603 0.00705 AFIX 23 H13A 2 1.175000 0.033548 0.212677 11.00000 -1.20000 H13B 2 1.039391 -0.027109 0.154753 11.00000 -1.20000 AFIX 0 C14 1 1.094476 0.004889 0.366817 11.00000 0.14465 0.09220 = 0.06452 0.01356 0.00683 0.02859 AFIX 137 H14A 2 1.140152 0.049323 0.426679 11.00000 -1.50000 H14B 2 1.161559 -0.038866 0.405583 11.00000 -1.50000 H14C 2 0.994460 -0.005388 0.367682 11.00000 -1.50000 AFIX 0 C15 1 0.558186 0.171900 0.522761 11.00000 0.07149 0.14944 = 0.07903 -0.00464 0.04791 0.00426 AFIX 137 H15A 2 0.609967 0.142898 0.612060 11.00000 -1.50000 H15B 2 0.447394 0.164638 0.487034 11.00000 -1.50000 H15C 2 0.582455 0.225636 0.542343 11.00000 -1.50000 AFIX 0 C16 1 1.304496 0.308196 0.214427 11.00000 0.09233 0.08913 = 0.12793 0.01311 0.06430 -0.02252 AFIX 137 H16A 2 1.364699 0.270789 0.189046 11.00000 -1.50000 H16B 2 1.369857 0.333261 0.305035 11.00000 -1.50000 H16C 2 1.263763 0.345854 0.137065 11.00000 -1.50000 AFIX 0 HKLF 4 REM a30403b in P2(1)/c REM R1 = 0.0687 for 2309 Fo > 4sig(Fo) and 0.0804 for all 2901 data REM 185 parameters refined using 0 restraints END WGHT 0.0938 0.3802 REM Highest difference peak 0.573, deepest hole -0.554, 1-sigma level 0.080 Q1 1 0.7427 0.0694 0.1399 11.00000 0.05 0.57 ; _shelx_res_checksum 7874 _shelx_hkl_file ; 4 -8 -12 2.28 0.93 4 -7 -12 1.09 0.77 3 -6 -12 1.01 0.73 4 -6 -12 0.09 0.51 5 -6 -12 13.40 2.78 3 -5 -12 0.29 0.55 4 -5 -12 16.25 3.17 5 -5 -12 5.75 1.47 3 -4 -12 0.20 0.49 4 -4 -12 6.46 1.58 5 -4 -12 0.56 0.56 6 -4 -12 0.62 0.57 3 -3 -12 3.05 0.90 4 -3 -12 3.91 1.09 5 -3 -12 10.40 2.13 6 -3 -12 5.72 1.38 3 -2 -12 1.90 1.32 4 -2 -12 2.32 0.79 5 -2 -12 6.88 1.54 6 -2 -12 8.88 1.90 4 -1 -12 0.18 0.43 5 -1 -12 3.92 0.91 6 -1 -12 0.19 0.50 4 0 -12 23.60 5.52 5 0 -12 5.58 1.33 6 0 -12 18.30 3.33 7 0 -12 4.69 1.14 5 1 -12 5.41 1.27 6 1 -12 1.00 0.56 7 1 -12 0.77 0.55 5 2 -12 7.25 2.06 6 2 -12 7.39 1.49 6 3 -12 9.22 2.33 5 -11 -11 3.18 1.00 4 -10 -11 0.57 0.65 5 -10 -11 8.82 1.95 4 -9 -11 0.39 0.60 5 -9 -11 1.34 0.78 6 -9 -11 1.16 0.67 3 -8 -11 1.60 0.78 5 -8 -11 5.13 1.32 6 -8 -11 -0.40 0.49 7 -8 -11 -0.40 0.56 3 -7 -11 5.82 1.39 4 -7 -11 24.44 4.32 5 -7 -11 0.98 0.71 6 -7 -11 8.49 1.79 7 -7 -11 -0.24 0.48 3 -6 -11 -0.63 0.47 4 -6 -11 0.22 0.48 5 -6 -11 0.22 0.52 6 -6 -11 4.15 1.02 7 -6 -11 2.46 0.84 8 -6 -11 -0.53 0.50 2 -5 -11 0.79 0.62 3 -5 -11 3.60 1.01 4 -5 -11 3.78 1.02 5 -5 -11 1.33 0.70 6 -5 -11 4.18 1.16 7 -5 -11 0.62 0.56 8 -5 -11 1.04 0.63 2 -4 -11 13.17 2.37 3 -4 -11 2.24 0.77 4 -4 -11 22.24 3.85 5 -4 -11 70.81 12.40 6 -4 -11 8.45 1.75 7 -4 -11 1.46 0.65 8 -4 -11 2.43 0.82 3 -3 -11 4.70 1.10 4 -3 -11 0.58 0.55 5 -3 -11 2.21 0.78 6 -3 -11 1.91 0.71 7 -3 -11 1.09 0.66 8 -3 -11 0.64 0.52 9 -3 -11 6.41 1.56 2 -2 -11 1.12 0.59 3 -2 -11 4.27 1.02 4 -2 -11 -0.28 0.48 5 -2 -11 4.03 0.99 6 -2 -11 3.18 0.89 7 -2 -11 14.81 2.53 8 -2 -11 0.51 0.55 9 -2 -11 19.39 3.60 3 -1 -11 1.63 0.62 4 -1 -11 16.14 2.69 5 -1 -11 0.81 0.53 6 -1 -11 26.11 4.42 7 -1 -11 1.76 0.75 8 -1 -11 12.28 2.31 9 -1 -11 1.76 0.79 3 0 -11 -0.41 0.70 4 0 -11 0.13 0.40 5 0 -11 -0.56 0.41 6 0 -11 -0.24 0.43 7 0 -11 0.28 0.48 8 0 -11 1.26 0.68 9 0 -11 0.29 0.52 4 1 -11 15.06 2.44 5 1 -11 0.40 0.40 6 1 -11 24.53 4.17 7 1 -11 0.83 0.55 8 1 -11 15.15 2.62 9 1 -11 1.04 0.65 4 2 -11 0.93 0.60 5 2 -11 3.82 0.88 6 2 -11 3.10 0.81 7 2 -11 14.79 2.39 8 2 -11 -0.43 0.45 9 2 -11 18.63 2.41 5 3 -11 2.15 1.06 6 3 -11 1.53 0.63 7 3 -11 0.03 0.39 8 3 -11 0.18 0.38 9 3 -11 6.28 1.10 6 4 -11 10.84 2.32 7 4 -11 1.10 0.50 8 4 -11 0.66 0.45 9 4 -11 4.00 0.75 7 5 -11 1.13 0.77 8 5 -11 0.69 0.46 9 5 -11 0.03 0.35 8 6 -11 0.58 0.53 9 6 -11 4.91 1.05 5 -14 -10 -0.37 0.51 5 -13 -10 1.21 0.75 4 -12 -10 -0.51 0.53 5 -12 -10 3.02 0.91 6 -12 -10 0.51 0.53 4 -11 -10 1.14 0.70 5 -11 -10 13.68 2.59 6 -11 -10 2.26 0.77 7 -11 -10 3.26 0.85 3 -10 -10 3.09 0.91 5 -10 -10 4.72 1.17 6 -10 -10 3.65 1.00 7 -10 -10 -0.37 0.45 3 -9 -10 0.06 0.48 4 -9 -10 3.75 0.99 5 -9 -10 0.10 0.47 6 -9 -10 1.97 0.78 7 -9 -10 2.48 0.79 8 -9 -10 0.02 0.46 3 -8 -10 20.62 3.63 4 -8 -10 0.74 0.53 5 -8 -10 -0.56 0.47 6 -8 -10 9.49 1.83 7 -8 -10 2.76 0.77 8 -8 -10 2.79 0.82 2 -7 -10 0.30 0.42 3 -7 -10 2.26 0.72 4 -7 -10 12.57 2.27 5 -7 -10 0.09 0.43 6 -7 -10 -0.39 0.47 7 -7 -10 0.95 0.59 8 -7 -10 0.16 0.44 9 -7 -10 0.27 0.43 2 -6 -10 2.79 0.74 3 -6 -10 3.05 0.79 4 -6 -10 33.26 5.80 5 -6 -10 24.65 4.17 6 -6 -10 0.33 0.44 7 -6 -10 0.46 0.46 8 -6 -10 6.66 1.47 9 -6 -10 1.32 0.70 2 -5 -10 9.51 1.72 3 -5 -10 6.39 1.29 4 -5 -10 -0.21 0.47 5 -5 -10 4.88 1.11 6 -5 -10 2.14 0.67 7 -5 -10 9.81 1.84 8 -5 -10 1.32 0.67 9 -5 -10 2.84 0.88 1 -4 -10 1.98 0.61 2 -4 -10 -0.20 0.42 3 -4 -10 1.97 0.67 4 -4 -10 -0.11 0.42 5 -4 -10 4.64 1.13 6 -4 -10 1.57 0.62 7 -4 -10 1.08 0.60 8 -4 -10 2.29 0.78 9 -4 -10 0.34 0.49 10 -4 -10 7.14 1.63 1 -3 -10 13.67 2.30 2 -3 -10 6.05 1.15 3 -3 -10 24.74 3.92 4 -3 -10 4.44 0.99 5 -3 -10 48.37 7.70 6 -3 -10 20.17 3.32 7 -3 -10 1.38 0.66 8 -3 -10 0.31 0.47 9 -3 -10 9.93 1.93 10 -3 -10 6.04 1.43 2 -2 -10 5.48 1.12 3 -2 -10 3.09 0.77 4 -2 -10 24.87 3.94 5 -2 -10 3.23 0.82 6 -2 -10 5.37 1.05 7 -2 -10 0.40 0.50 8 -2 -10 12.59 2.23 9 -2 -10 1.23 0.66 10 -2 -10 9.99 1.98 2 -1 -10 0.34 0.40 3 -1 -10 0.89 0.47 4 -1 -10 5.95 1.15 5 -1 -10 0.04 0.39 6 -1 -10 6.40 1.30 7 -1 -10 9.73 1.87 8 -1 -10 0.25 0.46 9 -1 -10 1.19 0.64 10 -1 -10 7.55 1.64 3 0 -10 16.01 2.42 4 0 -10 18.87 2.93 5 0 -10 0.80 0.46 6 0 -10 29.00 4.68 7 0 -10 7.68 1.47 8 0 -10 10.65 1.36 9 0 -10 20.24 3.63 10 0 -10 2.76 0.92 3 1 -10 1.42 0.54 4 1 -10 5.80 1.09 5 1 -10 0.15 0.38 6 1 -10 6.51 1.25 7 1 -10 8.86 1.64 8 1 -10 -0.17 0.31 9 1 -10 1.20 0.44 10 1 -10 6.76 1.48 4 2 -10 23.90 3.58 5 2 -10 3.01 0.71 6 2 -10 4.10 0.95 7 2 -10 -0.38 0.41 8 2 -10 13.93 1.67 9 2 -10 0.99 0.42 10 2 -10 10.05 1.46 4 3 -10 6.33 1.55 5 3 -10 37.04 5.66 6 3 -10 13.49 2.07 7 3 -10 1.82 0.62 8 3 -10 0.11 0.33 9 3 -10 9.92 1.34 10 3 -10 5.93 1.01 5 4 -10 5.55 1.37 6 4 -10 2.41 0.63 7 4 -10 0.88 0.33 8 4 -10 1.43 0.43 9 4 -10 0.50 0.37 10 4 -10 6.36 1.56 6 5 -10 2.04 0.77 7 5 -10 9.91 1.20 8 5 -10 1.85 0.44 9 5 -10 3.70 0.66 10 5 -10 0.56 0.62 7 6 -10 0.66 0.35 8 6 -10 7.19 1.01 9 6 -10 1.88 0.48 7 7 -10 0.54 0.50 8 7 -10 0.22 0.45 9 7 -10 0.32 0.50 7 8 -10 2.91 0.85 8 8 -10 2.80 0.87 7 9 -10 2.14 0.78 8 9 -10 0.09 0.48 7 10 -10 -0.07 0.57 1 -15 -9 -1.21 0.62 5 -15 -9 -0.51 0.57 0 -14 -9 -1.13 0.68 1 -14 -9 1.87 0.92 4 -14 -9 -0.06 0.54 5 -14 -9 7.99 1.78 6 -14 -9 -0.53 0.58 -1 -13 -9 0.77 0.80 0 -13 -9 -0.06 0.64 1 -13 -9 -0.20 0.65 4 -13 -9 1.98 0.74 5 -13 -9 19.17 3.41 6 -13 -9 3.56 1.00 7 -13 -9 -0.80 0.49 -1 -12 -9 2.95 1.12 0 -12 -9 2.73 0.87 1 -12 -9 6.24 1.59 4 -12 -9 3.88 0.95 5 -12 -9 10.48 1.96 6 -12 -9 5.97 1.35 7 -12 -9 3.67 1.02 -2 -11 -9 -1.33 0.64 -1 -11 -9 0.89 0.78 0 -11 -9 -0.03 0.61 1 -11 -9 -0.84 0.65 3 -11 -9 -0.03 0.47 4 -11 -9 3.57 0.89 5 -11 -9 2.42 0.77 6 -11 -9 -0.12 0.57 7 -11 -9 0.37 0.50 8 -11 -9 -0.75 0.56 -2 -10 -9 5.27 1.51 -1 -10 -9 12.47 2.73 0 -10 -9 0.03 0.57 3 -10 -9 20.68 3.39 4 -10 -9 1.95 0.69 5 -10 -9 8.82 1.54 6 -10 -9 13.51 2.37 7 -10 -9 -0.35 0.51 8 -10 -9 3.83 0.99 -2 -9 -9 4.53 1.30 -1 -9 -9 14.39 2.86 0 -9 -9 6.30 1.61 2 -9 -9 26.81 4.27 3 -9 -9 1.54 0.61 4 -9 -9 35.07 5.70 5 -9 -9 -0.40 0.43 6 -9 -9 18.96 3.06 7 -9 -9 13.49 2.33 8 -9 -9 3.14 0.92 9 -9 -9 4.75 1.16 -3 -8 -9 2.50 1.10 -2 -8 -9 3.51 1.24 -1 -8 -9 6.31 1.51 0 -8 -9 16.72 3.08 2 -8 -9 18.49 2.97 3 -8 -9 10.71 1.77 4 -8 -9 0.26 0.42 5 -8 -9 7.19 1.42 6 -8 -9 0.15 0.37 7 -8 -9 -0.12 0.41 8 -8 -9 -0.81 0.51 9 -8 -9 0.59 0.58 -2 -7 -9 9.21 1.94 -1 -7 -9 13.31 2.39 0 -7 -9 4.64 1.09 2 -7 -9 1.82 0.61 3 -7 -9 13.99 2.20 4 -7 -9 18.83 3.02 5 -7 -9 -0.18 0.44 6 -7 -9 0.52 0.44 7 -7 -9 2.14 0.62 8 -7 -9 7.42 1.55 9 -7 -9 7.29 1.54 10 -7 -9 -1.00 0.50 -1 -6 -9 2.04 0.80 0 -6 -9 -0.32 0.48 1 -6 -9 -0.30 0.39 2 -6 -9 0.46 0.43 3 -6 -9 23.67 3.65 4 -6 -9 1.16 0.52 5 -6 -9 24.70 3.85 6 -6 -9 5.58 1.17 7 -6 -9 0.00 0.38 8 -6 -9 7.11 1.42 9 -6 -9 2.66 0.82 10 -6 -9 1.31 0.69 0 -5 -9 -0.49 0.51 1 -5 -9 7.82 1.35 2 -5 -9 7.83 1.36 3 -5 -9 6.05 1.24 4 -5 -9 2.90 0.74 5 -5 -9 6.43 1.24 6 -5 -9 2.05 0.61 7 -5 -9 -0.12 0.48 8 -5 -9 0.55 0.49 9 -5 -9 -0.13 0.43 10 -5 -9 2.33 0.79 1 -4 -9 4.54 0.87 2 -4 -9 1.84 0.58 3 -4 -9 38.72 5.77 4 -4 -9 0.38 0.41 5 -4 -9 15.76 2.38 6 -4 -9 3.58 0.81 7 -4 -9 15.54 2.42 8 -4 -9 16.91 2.79 9 -4 -9 0.33 0.49 10 -4 -9 17.08 3.02 11 -4 -9 0.07 0.51 1 -3 -9 -0.17 0.36 2 -3 -9 10.72 1.70 3 -3 -9 0.32 0.41 4 -3 -9 0.68 0.48 5 -3 -9 11.61 1.87 6 -3 -9 1.21 0.52 7 -3 -9 5.28 1.10 8 -3 -9 0.92 0.52 9 -3 -9 0.97 0.57 10 -3 -9 4.59 1.20 11 -3 -9 1.33 0.75 1 -2 -9 24.69 3.48 2 -2 -9 0.97 0.47 3 -2 -9 46.65 6.65 4 -2 -9 3.34 0.76 5 -2 -9 66.28 10.08 6 -2 -9 15.83 2.36 7 -2 -9 0.50 0.44 8 -2 -9 0.63 0.48 9 -2 -9 2.51 0.79 10 -2 -9 3.71 1.04 11 -2 -9 3.30 1.01 2 -1 -9 52.19 7.46 3 -1 -9 0.46 0.43 4 -1 -9 92.18 13.12 5 -1 -9 3.84 0.79 6 -1 -9 4.30 0.94 7 -1 -9 4.54 0.69 8 -1 -9 14.36 1.56 9 -1 -9 16.41 2.65 10 -1 -9 0.60 0.56 2 0 -9 2.03 0.58 3 0 -9 -0.18 0.38 4 0 -9 -0.12 0.41 5 0 -9 0.30 0.32 6 0 -9 0.09 0.36 7 0 -9 0.24 0.27 8 0 -9 -0.14 0.25 9 0 -9 0.33 0.31 10 0 -9 0.47 0.54 2 1 -9 50.91 7.35 3 1 -9 1.06 0.46 4 1 -9 88.30 12.61 5 1 -9 4.14 0.78 6 1 -9 3.52 0.80 7 1 -9 4.91 0.67 8 1 -9 14.68 1.62 9 1 -9 17.55 2.05 10 1 -9 1.58 0.47 3 2 -9 43.85 6.00 4 2 -9 2.27 0.59 5 2 -9 64.93 9.40 6 2 -9 15.12 2.16 7 2 -9 -0.16 0.25 8 2 -9 0.36 0.27 9 2 -9 2.56 0.53 10 2 -9 4.58 0.77 11 2 -9 2.16 0.69 4 3 -9 0.44 0.37 5 3 -9 9.80 1.49 6 3 -9 1.56 0.36 7 3 -9 4.83 0.65 8 3 -9 1.15 0.37 9 3 -9 1.21 0.41 11 3 -9 0.18 0.41 4 4 -9 -0.73 0.49 5 4 -9 10.11 1.52 6 4 -9 2.52 0.41 7 4 -9 14.52 1.53 8 4 -9 16.79 1.83 9 4 -9 0.11 0.32 10 4 -9 18.78 3.38 11 4 -9 0.05 0.43 5 5 -9 4.03 1.14 6 5 -9 1.28 0.34 7 5 -9 0.64 0.27 8 5 -9 -0.28 0.28 9 5 -9 0.14 0.28 10 5 -9 3.80 1.06 6 6 -9 6.75 0.93 7 6 -9 0.07 0.23 8 6 -9 8.13 1.04 9 6 -9 4.13 1.07 10 6 -9 1.84 0.78 6 7 -9 0.82 0.49 7 7 -9 2.36 0.67 8 7 -9 10.21 1.47 9 7 -9 6.57 1.50 10 7 -9 1.42 0.71 6 8 -9 0.97 0.54 7 8 -9 -0.65 0.39 8 8 -9 -0.52 0.46 9 8 -9 0.03 0.50 6 9 -9 24.29 4.28 7 9 -9 14.39 2.54 8 9 -9 4.94 1.23 9 9 -9 4.90 1.31 6 10 -9 14.36 2.59 7 10 -9 0.19 0.35 8 10 -9 3.68 1.04 6 11 -9 1.60 0.66 7 11 -9 0.39 0.48 8 11 -9 -0.23 0.45 6 12 -9 7.30 1.58 7 12 -9 5.33 1.25 2 -17 -8 4.05 0.96 3 -17 -8 3.85 1.04 5 -17 -8 -1.32 0.51 0 -16 -8 -0.47 0.68 1 -16 -8 0.39 0.52 2 -16 -8 9.02 1.68 3 -16 -8 10.77 2.20 5 -16 -8 0.46 0.53 6 -16 -8 2.83 0.78 0 -15 -8 -0.47 0.62 1 -15 -8 -0.38 0.58 2 -15 -8 -0.94 0.46 3 -15 -8 2.67 0.90 4 -15 -8 -0.93 0.49 5 -15 -8 7.05 1.49 6 -15 -8 2.51 0.73 -1 -14 -8 1.09 0.86 0 -14 -8 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17.60 -2 -4 0 26.43 1.77 -1 -4 0 719.87 35.97 0 -4 0 20.81 1.29 1 -4 0 760.01 55.46 2 -4 0 29.84 1.44 3 -4 0 211.05 12.63 4 -4 0 67.75 4.55 5 -4 0 1.50 0.23 6 -4 0 18.12 1.63 7 -4 0 34.35 3.20 8 -4 0 0.53 0.35 9 -4 0 0.07 0.37 10 -4 0 5.07 1.22 -5 -3 0 52.80 5.50 -4 -3 0 72.47 7.03 -3 -3 0 115.99 9.35 -2 -3 0 112.84 7.42 -1 -3 0 1326.57 120.10 0 -3 0 0.28 0.09 1 -3 0 1124.27 74.96 2 -3 0 124.83 6.14 3 -3 0 125.52 7.39 4 -3 0 69.04 4.61 5 -3 0 58.50 4.42 6 -3 0 3.33 0.47 7 -3 0 0.37 0.18 8 -3 0 0.42 0.35 9 -3 0 0.34 0.40 10 -3 0 9.84 2.00 11 -3 0 7.47 1.82 -4 -2 0 232.34 20.54 -3 -2 0 9.41 0.87 -2 -2 0 124.38 7.83 -1 -2 0 112.48 6.52 0 -2 0 26.43 1.11 1 -2 0 89.41 6.79 2 -2 0 147.41 7.29 3 -2 0 9.21 0.54 4 -2 0 248.05 16.03 5 -2 0 57.45 6.68 6 -2 0 97.55 7.97 7 -2 0 34.34 4.66 8 -2 0 1.51 0.55 9 -2 0 6.35 1.29 10 -2 0 1.14 0.67 -2 -1 0 466.62 34.28 -1 -1 0 653.53 44.68 1 -1 0 643.17 31.65 2 -1 0 366.50 18.37 3 -1 0 5.40 0.87 4 -1 0 1.48 0.22 5 -1 0 555.61 39.18 6 -1 0 46.24 3.85 7 -1 0 2.42 0.56 8 -1 0 -0.31 0.34 9 -1 0 -0.01 0.44 10 -1 0 0.98 0.68 1 0 0 912.28 72.82 2 0 0 390.18 19.21 3 0 0 27.26 1.48 4 0 0 639.24 41.27 5 0 0 19.81 1.41 6 0 0 379.09 27.60 7 0 0 4.54 0.85 8 0 0 0.54 0.36 9 0 0 6.89 1.43 10 0 0 2.46 0.88 1 1 0 635.07 44.07 2 1 0 472.60 24.28 3 1 0 13.64 0.80 4 1 0 1.30 0.17 5 1 0 539.39 35.41 6 1 0 41.39 5.46 7 1 0 2.60 0.63 8 1 0 0.07 0.34 9 1 0 0.19 0.42 10 1 0 -0.94 0.56 1 2 0 90.94 5.40 2 2 0 136.28 10.08 3 2 0 9.57 0.40 4 2 0 242.55 12.54 5 2 0 55.44 3.42 6 2 0 91.84 12.52 7 2 0 38.68 5.89 8 2 0 1.61 0.59 9 2 0 6.29 1.41 10 2 0 0.07 0.60 0 3 0 0.60 0.06 1 3 0 1060.49 95.45 2 3 0 126.35 9.91 3 3 0 124.43 11.55 4 3 0 64.86 2.87 5 3 0 56.54 6.90 6 3 0 3.79 0.65 7 3 0 0.51 0.38 8 3 0 0.83 0.42 9 3 0 -0.04 0.51 10 3 0 11.42 2.52 0 4 0 19.02 0.83 1 4 0 489.41 37.72 2 4 0 29.83 2.47 3 4 0 207.90 19.64 4 4 0 71.11 7.74 5 4 0 1.47 0.34 6 4 0 13.85 1.92 7 4 0 39.34 6.09 8 4 0 0.63 0.47 9 4 0 -0.06 0.53 10 4 0 5.40 1.62 0 5 0 0.24 0.06 1 5 0 0.35 0.10 2 5 0 12.15 1.06 3 5 0 0.65 0.21 4 5 0 -0.02 0.17 5 5 0 75.00 9.25 6 5 0 36.70 5.10 7 5 0 0.28 0.30 8 5 0 3.58 0.91 9 5 0 2.47 0.88 10 5 0 20.81 4.65 0 6 0 143.59 8.58 1 6 0 75.28 5.74 2 6 0 31.89 2.98 3 6 0 1.97 0.39 4 6 0 61.65 6.96 5 6 0 24.41 3.08 6 6 0 10.72 1.55 7 6 0 -1.22 0.39 8 6 0 8.29 1.65 9 6 0 -0.16 0.58 10 6 0 2.54 1.06 0 7 0 0.10 0.09 1 7 0 88.06 6.97 2 7 0 14.94 1.34 3 7 0 2.26 0.40 4 7 0 312.38 34.36 5 7 0 5.47 0.87 6 7 0 41.83 5.99 7 7 0 6.83 1.30 8 7 0 8.25 1.74 9 7 0 1.68 0.81 10 7 0 0.76 0.67 0 8 0 608.02 43.81 1 8 0 9.16 0.78 2 8 0 10.97 1.03 3 8 0 46.99 5.20 4 8 0 20.80 2.45 5 8 0 13.79 1.84 6 8 0 47.69 7.07 7 8 0 10.62 1.85 8 8 0 1.86 0.73 9 8 0 28.41 5.72 0 9 0 0.28 0.16 1 9 0 167.49 14.89 3 9 0 32.06 3.55 4 9 0 -0.28 0.27 5 9 0 143.41 19.39 6 9 0 0.54 0.42 7 9 0 -0.21 0.40 8 9 0 4.02 1.01 9 9 0 0.00 0.54 0 10 0 34.33 2.69 1 10 0 49.51 4.36 2 10 0 4.85 0.60 3 10 0 32.02 3.56 4 10 0 16.55 1.96 5 10 0 373.54 49.09 6 10 0 4.76 1.02 7 10 0 17.48 3.06 8 10 0 7.17 1.68 9 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40.34 4.79 -3 -14 1 105.56 12.31 -2 -14 1 5.74 0.81 -1 -14 1 20.36 2.46 0 -14 1 1.47 0.41 1 -14 1 43.04 5.63 2 -14 1 1.62 0.43 3 -14 1 1.62 0.48 4 -14 1 0.45 0.32 5 -14 1 -0.39 0.32 6 -14 1 7.89 1.39 7 -14 1 0.60 0.46 -7 -13 1 4.68 1.09 -6 -13 1 0.41 0.51 -5 -13 1 16.99 2.23 -4 -13 1 125.05 14.18 -3 -13 1 18.03 1.89 -2 -13 1 1.07 0.24 -1 -13 1 -0.14 0.17 0 -13 1 1.57 0.32 1 -13 1 25.79 3.11 2 -13 1 0.45 0.28 3 -13 1 8.92 1.24 4 -13 1 1.95 0.54 5 -13 1 0.56 0.35 6 -13 1 0.74 0.41 7 -13 1 0.23 0.38 8 -13 1 0.93 0.60 -7 -12 1 18.01 3.02 -6 -12 1 11.00 1.86 -5 -12 1 158.20 20.31 -4 -12 1 0.05 0.31 -3 -12 1 21.37 2.22 -2 -12 1 6.24 0.51 -1 -12 1 17.65 1.91 0 -12 1 2.10 0.23 1 -12 1 159.04 17.36 2 -12 1 75.94 8.97 3 -12 1 56.02 7.14 4 -12 1 57.59 7.88 5 -12 1 0.35 0.31 6 -12 1 20.40 2.98 7 -12 1 1.04 0.51 8 -12 1 16.71 3.05 -7 -11 1 2.54 0.81 -6 -11 1 13.44 2.23 -5 -11 1 61.22 7.69 -4 -11 1 151.77 18.51 -3 -11 1 8.64 0.91 -2 -11 1 5.41 0.44 -1 -11 1 0.35 0.20 0 -11 1 1.31 0.31 1 -11 1 1.75 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2 36.73 6.01 7 0 2 26.62 4.82 8 0 2 0.57 0.59 9 0 2 11.23 2.59 0 1 2 20.11 1.38 1 1 2 133.26 10.66 2 1 2 13.80 1.33 3 1 2 0.14 0.21 4 1 2 28.85 2.17 5 1 2 68.99 9.68 6 1 2 48.90 7.90 7 1 2 1.25 0.76 8 1 2 -0.76 0.55 9 1 2 3.79 1.34 -1 2 2 69.34 3.47 0 2 2 919.39 76.33 1 2 2 1509.35 131.59 2 2 2 125.66 12.09 3 2 2 216.19 23.29 4 2 2 71.38 5.21 5 2 2 85.99 12.52 6 2 2 19.55 3.31 7 2 2 60.28 11.00 8 2 2 4.31 1.08 9 2 2 25.60 5.98 -1 3 2 544.46 36.69 0 3 2 290.04 19.91 1 3 2 550.11 45.10 2 3 2 67.63 6.51 3 3 2 151.74 17.42 4 3 2 34.95 4.46 5 3 2 4.21 0.88 6 3 2 124.85 21.55 7 3 2 9.45 1.96 8 3 2 28.04 5.53 9 3 2 -0.13 0.78 -1 4 2 334.75 20.52 0 4 2 136.16 9.14 1 4 2 80.24 6.49 2 4 2 257.51 23.92 3 4 2 28.12 3.23 4 4 2 42.01 5.51 5 4 2 11.94 2.07 6 4 2 2.80 0.85 7 4 2 5.89 1.38 8 4 2 2.03 0.97 9 4 2 4.47 1.54 -1 5 2 10.15 0.39 0 5 2 348.19 23.65 2 5 2 1122.98 130.11 3 5 2 153.77 18.01 4 5 2 108.07 15.28 5 5 2 29.77 4.76 6 5 2 130.67 21.52 7 5 2 23.08 4.31 8 5 2 51.59 10.70 9 5 2 -0.67 0.66 0 6 2 40.68 2.84 1 6 2 838.13 74.00 2 6 2 7.54 0.91 3 6 2 83.00 10.72 4 6 2 8.60 1.28 5 6 2 22.90 3.48 6 6 2 18.73 3.05 7 6 2 70.90 13.16 8 6 2 3.74 1.21 9 6 2 21.65 4.88 0 7 2 12.19 0.86 1 7 2 0.63 0.21 2 7 2 0.74 0.30 3 7 2 35.20 4.27 4 7 2 13.79 1.78 5 7 2 0.74 0.45 6 7 2 12.09 2.15 7 7 2 1.78 0.82 8 7 2 -0.13 0.65 9 7 2 1.05 0.81 0 8 2 81.93 5.83 1 8 2 50.91 4.53 2 8 2 11.17 1.17 3 8 2 102.07 12.17 4 8 2 14.84 2.07 5 8 2 130.90 19.93 6 8 2 74.00 12.52 7 8 2 17.39 3.31 8 8 2 2.16 0.95 0 9 2 139.41 11.22 1 9 2 4.74 0.53 2 9 2 12.61 1.28 3 9 2 81.08 9.69 4 9 2 24.11 3.29 5 9 2 2.66 0.72 6 9 2 8.31 1.66 7 9 2 3.12 0.93 8 9 2 9.03 2.15 0 10 2 37.10 2.78 1 10 2 77.85 7.27 2 10 2 0.24 0.22 3 10 2 57.95 6.98 4 10 2 26.95 3.70 5 10 2 17.77 2.67 6 10 2 13.07 2.26 7 10 2 16.19 3.13 8 10 2 7.63 1.84 2 11 2 42.92 4.74 3 11 2 44.21 5.39 4 11 2 107.84 14.31 5 11 2 -0.30 0.36 6 11 2 24.65 4.18 7 11 2 0.51 0.58 8 11 2 9.63 2.24 3 12 2 0.70 0.21 4 12 2 0.54 0.36 5 12 2 0.11 0.35 6 12 2 4.96 1.16 7 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0.27 5 -14 4 4.04 0.95 -1 -13 4 33.67 4.58 0 -13 4 105.34 12.66 1 -13 4 8.52 1.16 2 -13 4 44.42 7.24 3 -13 4 2.25 0.69 4 -13 4 13.34 2.38 5 -13 4 0.25 0.33 6 -13 4 5.85 1.34 -1 -12 4 17.86 2.21 0 -12 4 6.61 0.93 1 -12 4 1.62 0.42 2 -12 4 21.75 2.55 3 -12 4 4.87 0.65 4 -12 4 -0.17 0.43 5 -12 4 2.47 0.61 6 -12 4 0.54 0.53 7 -12 4 0.59 0.59 -1 -11 4 -0.11 0.30 0 -11 4 156.88 18.07 1 -11 4 6.76 0.87 2 -11 4 129.06 14.69 3 -11 4 6.52 0.75 4 -11 4 37.10 3.75 5 -11 4 0.19 0.36 6 -11 4 10.96 2.06 7 -11 4 7.22 1.78 -1 -10 4 68.27 7.72 0 -10 4 -0.59 0.23 1 -10 4 50.28 5.39 2 -10 4 13.59 1.56 3 -10 4 55.23 6.64 4 -10 4 -0.25 0.23 5 -10 4 33.41 3.69 6 -10 4 7.26 1.48 7 -10 4 1.80 0.87 -4 -9 4 0.09 0.17 -1 -9 4 1.25 0.33 0 -9 4 63.95 6.67 1 -9 4 0.08 0.17 2 -9 4 0.95 0.31 3 -9 4 10.38 1.36 4 -9 4 8.07 0.95 5 -9 4 11.48 1.33 6 -9 4 7.05 0.95 7 -9 4 2.81 0.94 -4 -8 4 1.16 0.22 -1 -8 4 205.69 20.31 0 -8 4 0.22 0.18 1 -8 4 103.94 10.10 2 -8 4 30.41 3.34 3 -8 4 54.62 6.76 4 -8 4 95.44 9.61 5 -8 4 1.33 0.35 6 -8 4 0.43 0.27 7 -8 4 4.32 1.05 8 -8 4 12.78 2.50 -4 -7 4 20.51 1.55 -1 -7 4 26.11 2.47 0 -7 4 5.96 0.64 1 -7 4 1.52 0.28 2 -7 4 97.31 10.60 3 -7 4 41.95 5.17 4 -7 4 28.18 2.82 5 -7 4 0.06 0.24 6 -7 4 3.43 0.53 8 -7 4 2.35 0.88 -4 -6 4 4.37 0.39 -1 -6 4 3.39 0.40 0 -6 4 18.45 1.62 1 -6 4 21.98 2.10 2 -6 4 9.93 1.20 3 -6 4 0.92 0.35 4 -6 4 94.58 12.90 5 -6 4 0.04 0.25 6 -6 4 19.85 2.13 7 -6 4 1.13 0.59 8 -6 4 5.44 1.44 -4 -5 4 249.84 15.52 -1 -5 4 2.32 0.31 0 -5 4 115.86 10.36 1 -5 4 27.43 2.75 2 -5 4 21.96 2.46 3 -5 4 0.13 0.26 4 -5 4 28.16 3.66 5 -5 4 37.82 3.96 6 -5 4 1.14 0.52 7 -5 4 0.82 0.54 8 -5 4 0.21 0.55 -4 -4 4 304.56 18.12 -1 -4 4 311.17 27.79 0 -4 4 40.46 3.67 1 -4 4 227.27 21.75 2 -4 4 0.13 0.20 3 -4 4 2.33 0.47 4 -4 4 35.61 4.67 5 -4 4 12.69 1.40 6 -4 4 1.94 0.63 7 -4 4 -0.63 0.45 8 -4 4 7.18 1.91 -1 -3 4 0.66 0.18 0 -3 4 11.23 1.05 1 -3 4 45.54 4.63 2 -3 4 30.30 3.29 3 -3 4 126.85 15.61 4 -3 4 52.40 7.28 5 -3 4 85.89 8.85 6 -3 4 -0.04 0.40 7 -3 4 18.87 3.48 -1 -2 4 347.50 27.82 0 -2 4 135.97 11.82 1 -2 4 5.90 0.68 2 -2 4 17.75 1.97 3 -2 4 46.16 6.30 4 -2 4 11.03 1.69 5 -2 4 43.94 6.65 6 -2 4 4.93 1.13 7 -2 4 3.24 0.96 8 -2 4 11.89 2.87 -1 -1 4 6.63 0.55 0 -1 4 27.90 2.37 1 -1 4 54.65 5.90 2 -1 4 12.47 1.45 3 -1 4 82.62 9.96 4 -1 4 14.10 2.00 5 -1 4 4.73 0.97 6 -1 4 14.21 2.47 7 -1 4 33.82 6.44 8 -1 4 2.43 1.10 -2 0 4 852.85 70.40 -1 0 4 463.20 36.77 0 0 4 107.78 9.84 1 0 4 255.22 24.47 2 0 4 189.86 21.11 3 0 4 124.81 15.69 4 0 4 197.29 27.56 5 0 4 73.27 11.50 6 0 4 30.52 5.50 7 0 4 5.44 1.39 8 0 4 106.22 22.75 -2 1 4 117.54 8.02 -1 1 4 7.36 0.66 0 1 4 32.40 2.99 1 1 4 55.14 5.81 2 1 4 17.59 2.18 3 1 4 96.74 12.65 4 1 4 14.74 2.00 5 1 4 4.20 0.90 6 1 4 12.96 2.28 7 1 4 37.75 7.88 8 1 4 0.81 0.97 -2 2 4 116.91 9.02 -1 2 4 393.49 30.76 0 2 4 172.27 16.67 1 2 4 6.23 0.76 2 2 4 16.14 1.76 3 2 4 38.40 5.04 4 2 4 10.07 1.57 5 2 4 47.22 7.82 6 2 4 5.72 1.25 7 2 4 4.18 1.27 8 2 4 13.56 3.63 -2 3 4 203.99 14.56 -1 3 4 0.55 0.15 0 3 4 11.46 1.05 1 3 4 57.12 6.32 2 3 4 36.90 4.56 3 3 4 113.14 14.66 4 3 4 55.26 8.33 5 3 4 115.33 18.71 6 3 4 1.60 0.77 7 3 4 22.72 4.89 8 3 4 0.91 0.86 -2 4 4 1.58 0.26 -1 4 4 351.59 28.40 0 4 4 50.34 4.75 1 4 4 253.15 23.96 2 4 4 0.30 0.25 3 4 4 2.55 0.58 4 4 4 39.11 5.96 5 4 4 12.89 2.25 6 4 4 3.20 1.00 7 4 4 1.21 0.95 8 4 4 8.32 2.21 -3 5 4 45.66 2.83 -2 5 4 236.33 16.13 -1 5 4 3.49 0.38 0 5 4 62.54 6.22 1 5 4 32.83 3.52 2 5 4 23.20 2.71 3 5 4 -0.46 0.34 4 5 4 37.22 5.78 5 5 4 45.74 8.19 6 5 4 1.46 0.79 7 5 4 0.59 0.83 8 5 4 -0.18 0.69 -3 6 4 22.49 1.32 -2 6 4 116.49 8.15 -1 6 4 4.17 0.38 0 6 4 24.84 2.36 1 6 4 27.68 2.94 2 6 4 9.74 1.29 3 6 4 0.53 0.39 4 6 4 101.02 15.16 5 6 4 0.58 0.52 6 6 4 29.07 6.34 7 6 4 1.24 0.81 8 6 4 8.07 2.22 -2 7 4 64.92 4.20 -1 7 4 31.02 2.48 0 7 4 7.03 0.70 1 7 4 0.42 0.14 2 7 4 108.31 13.22 3 7 4 47.00 6.61 4 7 4 35.09 5.65 5 7 4 -0.27 0.59 6 7 4 5.04 1.38 7 7 4 4.83 1.46 -1 8 4 217.46 16.34 0 8 4 1.29 0.26 1 8 4 129.85 13.94 2 8 4 36.82 4.60 3 8 4 59.88 8.53 4 8 4 127.88 21.55 5 8 4 0.48 0.53 6 8 4 1.04 0.73 7 8 4 4.59 1.37 0 9 4 70.91 6.69 1 9 4 0.02 0.23 2 9 4 1.34 0.41 3 9 4 14.09 2.26 4 9 4 8.46 1.57 5 9 4 13.72 2.53 6 9 4 9.36 2.12 7 9 4 4.74 1.46 2 10 4 9.99 1.29 3 10 4 69.01 10.02 4 10 4 -0.08 0.44 5 10 4 40.82 7.40 6 10 4 11.69 2.60 7 10 4 2.10 0.93 3 11 4 6.82 1.18 4 11 4 48.40 7.92 5 11 4 0.69 0.63 6 11 4 16.55 3.36 7 11 4 7.80 1.99 5 12 4 5.03 1.28 6 12 4 0.74 0.65 7 12 4 1.49 0.82 -1 -20 5 5.75 2.04 0 -20 5 5.59 1.87 -1 -19 5 0.26 0.61 0 -19 5 1.10 0.87 1 -19 5 -0.74 0.73 -2 -18 5 0.33 0.62 0 -18 5 -0.02 0.64 1 -18 5 1.51 0.84 2 -18 5 0.30 0.64 0 -17 5 3.67 1.15 1 -17 5 3.25 1.06 2 -17 5 10.55 2.38 -3 -16 5 14.28 2.71 1 -16 5 1.59 0.75 2 -16 5 1.07 0.69 3 -16 5 3.62 1.12 -2 -15 5 2.79 0.83 -1 -15 5 28.32 4.38 2 -15 5 2.80 0.95 3 -15 5 6.16 1.35 4 -15 5 5.57 1.37 -2 -14 5 22.96 3.52 -1 -14 5 1.49 0.63 0 -14 5 35.81 5.27 2 -14 5 -0.16 0.48 3 -14 5 3.17 0.83 4 -14 5 3.83 1.07 5 -14 5 3.10 0.78 -2 -13 5 9.97 1.80 -1 -13 5 20.19 2.94 0 -13 5 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