# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email daniel.lumpi@tuwien.ac.at _publ_contact_author_name 'Daniel Lumpi' loop_ _publ_author_name 'Daniel Lumpi' 'Berthold Stoeger' 'Christian Hametner' 'Frank Kubel' 'Georg Reider' 'Hans Hagemann' ; A.Karpfen ; 'Johannes Froehlich' data_(I) _database_code_depnum_ccdc_archive 'CCDC 835683' #TrackingRef '6367_web_deposit_cif_file_0_DanielLumpi_1311090705.final.cif' #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C12 H13 N3 S1' _chemical_formula_weight 231.3 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2xab;2ybc;2zac' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x+1/2,-y,z+1/2 3 -x,y+1/2,-z+1/2 4 x+1/2,-y+1/2,-z _cell_length_a 4.8314(2) _cell_length_b 15.4009(6) _cell_length_c 15.6421(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1163.90(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 21812 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 28.9 _cell_measurement_temperature 100 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 1.3197 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 0.253 _exptl_crystal_description rod _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_colour 'clear colourless' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.9415 _exptl_absorpt_correction_T_max 0.9879 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 100 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Bruker CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ? _diffrn_reflns_number 21682 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 30.13 _diffrn_reflns_theta_full 30.13 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ; _reflns_number_total 3390 _reflns_number_gt 2525 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_gt 0.0293 _refine_ls_R_factor_all 0.0429 _refine_ls_wR_factor_ref 0.0301 _refine_ls_goodness_of_fit_ref 1.25 _refine_ls_goodness_of_fit_gt 1.43 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 3390 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(F)+0.0001F^2^) _refine_ls_hydrogen_treatment none _refine_ls_shift/su_max 0.0384 _refine_ls_shift/su_mean 0.0004 _refine_diff_density_max 0.21 _refine_diff_density_min -0.14 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(6) _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.003 0.002 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.125 0.123 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' N 0.006 0.003 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.000 0.000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'Jana2006 (Petricek, Dusek & Palatinus, 2006)' _computing_molecular_graphics ? _computing_publication_material 'Jana2006 (Petricek, Dusek & Palatinus, 2006)' #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.50856(9) 0.30525(2) 0.10155(2) Uani 0.02509(10) 4 1 d . . . N1 N -0.0405(2) 0.53754(7) 0.14349(7) Uani 0.0176(3) 4 1 d . . . N2 N -0.0168(3) 0.57270(7) 0.22291(7) Uani 0.0229(3) 4 1 d . . . N3 N 0.1782(3) 0.52929(8) 0.26225(8) Uani 0.0225(4) 4 1 d . . . C1 C -0.2410(3) 0.57073(9) 0.08507(8) Uani 0.0178(4) 4 1 d . . . C2 C -0.2933(3) 0.52630(11) 0.00940(9) Uani 0.0224(5) 4 1 d . . . C3 C -0.4922(4) 0.55752(9) -0.04646(9) Uani 0.0254(4) 4 1 d . . . C4 C -0.6385(3) 0.63182(11) -0.02708(10) Uani 0.0252(5) 4 1 d . . . C5 C -0.5842(3) 0.67590(10) 0.04819(10) Uani 0.0236(5) 4 1 d . . . C6 C -0.3850(3) 0.64573(10) 0.10456(10) Uani 0.0213(4) 4 1 d . . . C7 C 0.1405(3) 0.47146(10) 0.13353(9) Uani 0.0182(4) 4 1 d . . . C8 C 0.2803(3) 0.46574(10) 0.20938(9) Uani 0.0189(4) 4 1 d . . . C9 C 0.4988(4) 0.40887(9) 0.24093(8) Uani 0.0201(4) 4 1 d . . . C10 C 0.6100(3) 0.33801(10) 0.20537(9) Uani 0.0199(4) 4 1 d . . . C11 C 0.8346(3) 0.28713(11) 0.24805(11) Uani 0.0251(5) 4 1 d . . . C12 C 0.5713(5) 0.19023(12) 0.10079(13) Uani 0.0421(7) 4 1 d . . . H2 H -0.194(3) 0.4776(11) -0.0026(9) Uiso 0.028(4) 4 1 d . . . H3 H -0.530(3) 0.5261(9) -0.0934(9) Uiso 0.030(4) 4 1 d . . . H4 H -0.781(3) 0.6545(10) -0.0638(9) Uiso 0.026(4) 4 1 d . . . H5 H -0.680(3) 0.7255(10) 0.0620(9) Uiso 0.018(4) 4 1 d . . . H6 H -0.347(3) 0.6759(9) 0.1568(9) Uiso 0.018(4) 4 1 d . . . H7 H 0.149(3) 0.4372(9) 0.0819(9) Uiso 0.023(4) 4 1 d . . . H9 H 0.575(3) 0.4262(9) 0.2944(10) Uiso 0.029(4) 4 1 d . . . H111 H 0.884(3) 0.3120(11) 0.3004(11) Uiso 0.039(5) 4 1 d . . . H112 H 0.993(4) 0.2834(9) 0.2118(9) Uiso 0.033(4) 4 1 d . . . H113 H 0.789(3) 0.2245(10) 0.2593(8) Uiso 0.018(4) 4 1 d . . . H121 H 0.483(4) 0.1634(12) 0.1416(12) Uiso 0.055(6) 4 1 d . . . H122 H 0.773(4) 0.1781(12) 0.1069(12) Uiso 0.058(6) 4 1 d . . . H123 H 0.491(4) 0.1742(10) 0.0418(12) Uiso 0.056(5) 4 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 S 0.03124(17) 0.02364(18) 0.02038(17) 0.0039(2) -0.00071(19) -0.00057(15) N1 N 0.0201(6) 0.0182(6) 0.0146(5) -0.0021(5) 0.0026(5) 0.0003(4) N2 N 0.0310(6) 0.0207(6) 0.0171(6) -0.0019(7) -0.0001(6) -0.0027(5) N3 N 0.0278(6) 0.0211(7) 0.0187(6) -0.0015(6) -0.0012(5) -0.0016(5) C1 C 0.0168(6) 0.0195(8) 0.0173(7) -0.0037(6) 0.0027(5) 0.0049(6) C2 C 0.0249(8) 0.0220(9) 0.0204(8) 0.0007(7) 0.0037(6) -0.0014(7) C3 C 0.0273(7) 0.0310(8) 0.0178(7) -0.0033(9) 0.0006(8) 0.0009(6) C4 C 0.0214(7) 0.0302(9) 0.0240(9) -0.0024(7) 0.0001(6) 0.0089(7) C5 C 0.0212(7) 0.0218(9) 0.0279(9) 0.0004(6) 0.0031(6) 0.0026(7) C6 C 0.0216(6) 0.0211(8) 0.0211(8) -0.0024(6) 0.0031(6) 0.0004(7) C7 C 0.0200(7) 0.0169(8) 0.0176(8) -0.0015(6) 0.0030(6) -0.0012(6) C8 C 0.0205(7) 0.0181(8) 0.0180(7) -0.0042(6) 0.0017(6) 0.0003(6) C9 C 0.0212(6) 0.0219(7) 0.0171(7) -0.0058(8) -0.0006(7) 0.0028(5) C10 C 0.0186(6) 0.0221(8) 0.0191(8) -0.0056(6) 0.0013(6) 0.0051(6) C11 C 0.0226(7) 0.0250(10) 0.0277(10) 0.0004(7) -0.0022(7) 0.0028(7) C12 C 0.0713(15) 0.0241(9) 0.0308(10) 0.0082(10) -0.0056(10) -0.0045(9) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 C10 . . 1.7695(14) yes S1 C12 . . 1.7970(18) yes N1 N2 . . 1.3599(15) yes N1 C1 . . 1.4264(17) yes N1 C7 . . 1.3504(18) yes N2 N3 . . 1.3085(18) yes N3 C8 . . 1.3727(19) yes C1 C2 . . 1.390(2) yes C1 C6 . . 1.383(2) yes C2 C3 . . 1.384(2) yes C2 H2 . . 0.909(17) yes C3 C4 . . 1.379(2) yes C3 H3 . . 0.896(14) yes C4 C5 . . 1.384(2) yes C4 H4 . . 0.961(15) yes C5 C6 . . 1.385(2) yes C5 H5 . . 0.916(15) yes C6 H6 . . 0.957(14) yes C7 C8 . . 1.3681(19) yes C7 H7 . . 0.963(14) yes C8 C9 . . 1.458(2) yes C9 C10 . . 1.338(2) yes C9 H9 . . 0.951(15) yes C10 C11 . . 1.495(2) yes C11 H111 . . 0.935(17) yes C11 H112 . . 0.953(17) yes C11 H113 . . 1.006(15) yes C12 H121 . . 0.869(19) yes C12 H122 . . 1.00(2) yes C12 H123 . . 1.029(19) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C10 S1 C12 . . . 103.91(8) yes N2 N1 C1 . . . 119.99(11) yes N2 N1 C7 . . . 110.53(11) yes C1 N1 C7 . . . 129.46(11) yes N1 N2 N3 . . . 106.67(11) yes N2 N3 C8 . . . 109.84(11) yes N1 C1 C2 . . . 119.51(13) yes N1 C1 C6 . . . 119.98(12) yes C2 C1 C6 . . . 120.51(13) yes C1 C2 C3 . . . 119.50(14) yes C1 C2 H2 . . . 119.0(10) yes C3 C2 H2 . . . 121.5(10) yes C2 C3 C4 . . . 120.34(14) yes C2 C3 H3 . . . 118.0(10) yes C4 C3 H3 . . . 121.5(10) yes C3 C4 C5 . . . 119.80(14) yes C3 C4 H4 . . . 122.4(9) yes C5 C4 H4 . . . 117.8(9) yes C4 C5 C6 . . . 120.56(14) yes C4 C5 H5 . . . 120.8(9) yes C6 C5 H5 . . . 118.7(9) yes C1 C6 C5 . . . 119.30(14) yes C1 C6 H6 . . . 119.7(8) yes C5 C6 H6 . . . 121.0(8) yes N1 C7 C8 . . . 105.54(12) yes N1 C7 H7 . . . 122.3(9) yes C8 C7 H7 . . . 132.1(9) yes N3 C8 C7 . . . 107.41(12) yes N3 C8 C9 . . . 118.97(12) yes C7 C8 C9 . . . 133.61(13) yes C8 C9 C10 . . . 129.81(13) yes C8 C9 H9 . . . 114.1(9) yes C10 C9 H9 . . . 116.0(9) yes S1 C10 C9 . . . 120.20(11) yes S1 C10 C11 . . . 117.47(11) yes C9 C10 C11 . . . 122.22(13) yes C10 C11 H111 . . . 111.1(10) yes C10 C11 H112 . . . 110.4(9) yes C10 C11 H113 . . . 115.1(8) yes H111 C11 H112 . . . 110.0(14) yes H111 C11 H113 . . . 107.2(13) yes H112 C11 H113 . . . 102.7(12) yes S1 C12 H121 . . . 112.3(12) yes S1 C12 H122 . . . 110.4(11) yes S1 C12 H123 . . . 100.3(9) yes H121 C12 H122 . . . 108.7(17) yes H121 C12 H123 . . . 110.9(17) yes H122 C12 H123 . . . 114.2(15) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C6 H6 N2 . . . 0.957(14) 2.476(13) 2.8033(19) 99.9(9) yes #======================================================================= # 11. STRUCTURE-FACTOR LIST loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 2 0 0 2995.55 2770.77 21.73 o 4 0 0 574.75 567.32 15.90 o 1 1 0 65.38 65.41 2.20 o 2 1 0 362.49 380.52 9.60 o 3 1 0 27.95 29.28 4.17 o 4 1 0 378.50 384.06 9.92 o 5 1 0 260.07 257.41 15.74 o 6 1 0 0.59 4.25 14.48 < 0 2 0 1741.24 1251.13 5.12 o 1 2 0 282.23 282.20 2.05 o 2 2 0 1252.92 1257.67 6.77 o 3 2 0 1483.41 1512.55 8.74 o 4 2 0 88.73 97.14 5.67 o 5 2 0 401.80 390.99 10.15 o 6 2 0 1.24 12.83 15.43 < 1 3 0 463.25 504.50 3.07 o 2 3 0 101.09 103.20 2.68 o 3 3 0 3.65 0.71 2.68 < 4 3 0 7.41 7.87 3.07 < 5 3 0 134.36 126.18 5.75 o 6 3 0 9.23 11.89 8.97 < 0 4 0 729.53 649.18 6.38 o 1 4 0 537.10 547.48 3.70 o 2 4 0 448.44 498.75 4.49 o 3 4 0 370.98 350.29 4.96 o 4 4 0 136.84 145.55 5.27 o 5 4 0 43.62 41.01 3.86 o 6 4 0 37.34 29.76 4.96 o 1 5 0 153.18 166.80 3.46 o 2 5 0 226.58 226.00 3.94 o 3 5 0 7.13 6.30 2.44 < 4 5 0 115.59 116.50 5.51 o 5 5 0 15.63 8.97 3.62 < 6 5 0 5.27 6.22 4.72 < 0 6 0 2777.33 2773.45 15.59 o 1 6 0 887.74 878.41 6.53 o 2 6 0 0.85 0.79 1.89 < 3 6 0 384.07 382.17 5.51 o 4 6 0 337.24 326.28 7.56 o 5 6 0 128.70 126.50 5.98 o 6 6 0 9.64 9.37 5.35 < 1 7 0 281.07 311.25 5.35 o 2 7 0 113.25 104.69 3.70 o 3 7 0 46.59 51.09 3.15 o 4 7 0 652.29 620.69 11.02 o 5 7 0 5.83 6.61 4.09 < 6 7 0 12.74 8.19 5.43 < 0 8 0 6481.14 6569.03 27.16 o 1 8 0 466.63 481.91 6.93 o 2 8 0 2120.40 2097.42 13.07 o 3 8 0 306.54 288.50 6.38 o 4 8 0 903.77 883.68 13.54 o 5 8 0 7.66 7.40 4.57 < 6 8 0 24.28 26.13 6.30 o 1 9 0 13.83 15.74 3.23 o 2 9 0 93.86 88.79 4.57 o 3 9 0 31.83 30.23 4.80 o 4 9 0 3.28 -0.24 4.41 < 5 9 0 18.96 26.37 5.27 o 6 9 0 94.91 113.67 10.23 o 0 10 0 4.93 1.42 3.62 < 1 10 0 272.53 270.55 6.69 o 2 10 0 553.31 517.57 9.13 o 3 10 0 9.07 2.13 4.33 < 4 10 0 269.11 283.85 8.58 o 5 10 0 14.60 19.21 6.69 < 6 10 0 90.25 105.56 10.71 o 1 11 0 27.79 30.86 3.86 o 2 11 0 47.30 50.06 4.96 o 3 11 0 109.65 99.66 6.69 o 4 11 0 151.88 142.32 8.74 o 5 11 0 16.73 12.99 6.93 < 0 12 0 585.36 577.63 12.67 o 1 12 0 369.92 364.54 8.19 o 2 12 0 3.76 6.69 4.17 < 3 12 0 212.26 192.78 8.66 o 4 12 0 7.33 7.24 5.98 < 5 12 0 132.26 144.37 10.71 o 1 13 0 394.60 367.22 9.45 o 2 13 0 62.57 54.55 5.51 o 3 13 0 0.01 1.73 5.04 < 4 13 0 80.88 84.78 8.34 o 5 13 0 28.78 34.87 8.42 o 0 14 0 124.25 156.18 14.17 o 1 14 0 30.44 42.51 5.51 o 2 14 0 2.21 5.04 5.67 < 3 14 0 85.83 85.96 8.42 o 4 14 0 0.53 1.18 6.53 < 5 14 0 40.08 43.14 9.21 o 1 15 0 107.82 104.14 8.27 o 2 15 0 153.41 147.36 9.84 o 3 15 0 49.76 54.79 8.11 o 4 15 0 2.17 3.86 6.85 < 0 16 0 28.11 14.96 10.08 < 1 16 0 87.50 92.81 9.21 o 2 16 0 338.17 321.17 20.31 o 3 16 0 388.71 391.22 15.98 o 4 16 0 90.52 119.57 10.78 o 1 17 0 2.35 5.04 7.01 < 2 17 0 20.19 20.15 10.71 < 3 17 0 52.89 47.47 10.94 o 4 17 0 3.27 7.95 11.49 < 0 18 0 1019.67 1082.44 32.75 o 1 18 0 61.26 54.39 10.78 o 2 18 0 44.67 42.90 12.83 o 3 18 0 9.79 11.89 12.20 < 1 19 0 87.92 86.51 15.66 o 2 19 0 14.57 5.75 11.73 < 3 19 0 47.61 39.59 13.78 < 0 20 0 34.64 21.25 12.99 < 1 20 0 63.34 63.37 14.96 o 2 20 0 216.39 225.92 21.73 o 1 21 0 5.37 6.22 12.52 < 1 0 1 213.45 173.57 2.36 o 2 0 1 50.64 55.10 3.46 o 3 0 1 486.78 444.67 7.32 o 4 0 1 4.80 6.53 4.57 < 5 0 1 5.23 0.55 8.34 < 6 0 1 0.21 -1.57 13.93 < -6 1 1 187.22 215.29 27.16 o -5 1 1 39.67 33.69 10.23 o -4 1 1 393.49 384.77 9.84 o -3 1 1 87.59 81.55 4.49 o -2 1 1 1367.42 1277.42 8.58 o -1 1 1 1432.78 1402.74 4.33 o 0 1 1 2.73 1.26 0.31 o 1 1 1 1442.68 1392.35 3.70 o 2 1 1 1346.21 1307.02 9.60 o 3 1 1 91.18 83.44 4.64 o 4 1 1 401.47 380.36 7.01 o 5 1 1 38.20 33.38 5.59 o -6 2 1 61.16 81.24 20.15 o -5 2 1 23.85 25.50 5.43 o -4 2 1 92.72 89.66 3.86 o -3 2 1 355.95 340.22 5.20 o -2 2 1 110.25 115.71 3.31 o -1 2 1 5266.53 4999.33 7.48 o 0 2 1 381.28 301.72 2.13 o 1 2 1 5249.45 5272.40 7.87 o 2 2 1 113.13 121.22 3.23 o 3 2 1 360.29 360.13 7.32 o 4 2 1 89.27 95.25 5.98 o 5 2 1 21.69 21.25 5.51 o 6 2 1 61.30 81.24 19.99 o -6 3 1 17.80 24.32 6.93 o -5 3 1 37.72 37.39 5.04 o -4 3 1 449.22 453.57 6.45 o -3 3 1 63.57 61.16 2.44 o -2 3 1 516.41 523.00 4.17 o -1 3 1 5111.50 5173.61 8.89 o 0 3 1 7296.01 6927.20 12.83 o 1 3 1 5162.73 5229.66 7.79 o 2 3 1 519.58 521.42 4.09 o 3 3 1 66.95 66.91 3.07 o 4 3 1 446.20 435.46 6.38 o 5 3 1 41.27 37.55 4.33 o 6 3 1 17.54 27.31 7.01 o -6 4 1 46.47 42.74 5.27 o -5 4 1 94.77 97.85 5.35 o -4 4 1 149.06 147.52 4.96 o -3 4 1 118.40 114.06 3.62 o -2 4 1 459.98 449.71 4.01 o -1 4 1 3201.52 3273.06 7.95 o 0 4 1 2290.20 2207.23 6.85 o 1 4 1 3212.58 3309.59 7.64 o 2 4 1 451.84 443.34 4.25 o 3 4 1 116.58 116.97 3.38 o 4 4 1 153.36 156.25 5.20 o 5 4 1 95.22 92.10 5.67 o 6 4 1 46.91 49.28 7.95 o -6 5 1 2.40 1.57 4.80 < -5 5 1 272.49 264.02 7.56 o -4 5 1 636.63 616.67 7.87 o -3 5 1 322.20 320.14 5.43 o -2 5 1 205.45 199.86 4.01 o -1 5 1 669.16 675.79 4.88 o 0 5 1 264.18 272.05 4.33 o 1 5 1 652.07 657.92 5.20 o 2 5 1 203.69 197.03 3.70 o 3 5 1 315.92 316.29 4.96 o 4 5 1 633.30 618.09 8.27 o 5 5 1 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10.00 o -2 15 1 54.67 56.52 8.50 o -1 15 1 243.28 253.78 11.81 o 0 15 1 67.39 67.46 8.34 o 1 15 1 244.65 249.22 10.78 o 2 15 1 51.68 48.65 7.56 o 3 15 1 133.15 130.12 9.92 o 4 15 1 32.74 30.70 7.87 o -4 16 1 41.35 46.99 9.68 o -3 16 1 4.75 5.12 8.58 < -2 16 1 75.80 64.08 12.75 o -1 16 1 89.29 87.38 9.13 o 0 16 1 3.63 6.69 6.77 < 1 16 1 92.88 81.94 8.19 o 2 16 1 72.97 72.34 10.78 o 3 16 1 4.97 0.87 7.32 < 4 16 1 42.74 53.92 8.97 o -4 17 1 37.78 52.11 14.09 o -3 17 1 1.61 0.47 10.86 < -2 17 1 298.97 329.83 20.78 o -1 17 1 14.29 10.47 7.16 < 0 17 1 51.46 57.07 8.90 o 1 17 1 15.40 8.74 6.45 < 2 17 1 302.15 327.39 17.40 o 3 17 1 1.54 0.63 8.66 < 4 17 1 37.61 54.55 14.17 o -3 18 1 156.98 176.48 19.05 o -2 18 1 36.62 23.30 12.04 < -1 18 1 33.37 37.23 9.92 o 0 18 1 141.48 132.95 11.49 o 1 18 1 34.04 41.17 10.08 o 2 18 1 36.81 38.02 10.55 o 3 18 1 160.14 159.95 18.58 o -3 19 1 11.10 18.10 12.75 < -2 19 1 48.95 56.20 14.64 o -1 19 1 15.28 8.19 12.20 < 0 19 1 187.03 211.67 13.70 o 1 19 1 14.42 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709.32 3.23 o 1 2 2 5720.88 5599.47 7.64 o 2 2 2 483.23 483.32 3.94 o 3 2 2 45.24 45.58 2.60 o 4 2 2 80.68 74.15 3.54 o 5 2 2 53.46 47.23 5.27 o 6 2 2 32.59 36.45 6.06 o -6 3 2 25.13 29.05 7.01 o -5 3 2 28.67 28.73 4.41 o -4 3 2 95.56 93.36 3.86 o -3 3 2 2.16 2.13 1.81 < -2 3 2 1119.94 1163.21 5.35 o -1 3 2 6483.08 6714.98 10.31 o 0 3 2 278.44 268.43 3.07 o 1 3 2 6413.21 6652.08 9.68 o 2 3 2 1109.51 1143.68 5.43 o 3 3 2 1.76 1.65 2.13 < 4 3 2 90.18 88.16 3.94 o 5 3 2 31.17 30.54 4.96 o 6 3 2 23.90 19.52 7.01 < -6 4 2 1.84 6.61 4.80 < -5 4 2 744.25 722.31 10.00 o -4 4 2 113.78 112.25 4.33 o -3 4 2 207.37 202.15 3.94 o -2 4 2 609.09 652.09 4.88 o -1 4 2 3319.80 3391.85 8.27 o 0 4 2 470.40 451.44 3.94 o 1 4 2 3305.15 3353.51 8.03 o 2 4 2 613.76 651.23 4.96 o 3 4 2 206.34 206.95 3.78 o 4 4 2 116.24 116.97 4.57 o 5 4 2 745.82 750.18 11.10 o 6 4 2 1.68 0.08 4.33 < -6 5 2 87.15 96.98 6.85 o -5 5 2 7.83 4.88 4.01 < -4 5 2 195.02 190.73 5.59 o -3 5 2 167.93 183.96 4.33 o -2 5 2 990.15 959.56 5.90 o -1 5 2 268.53 261.73 3.70 o 0 5 2 1990.40 1977.38 7.71 o 1 5 2 265.97 259.14 3.78 o 2 5 2 984.30 959.56 6.30 o 3 5 2 168.96 188.37 4.17 o 4 5 2 204.67 204.74 5.59 o 5 5 2 7.51 9.76 4.01 < 6 5 2 87.64 89.03 6.61 o -6 6 2 23.33 26.06 5.83 o -5 6 2 56.09 47.15 5.12 o -4 6 2 100.28 101.70 5.35 o -3 6 2 159.21 158.46 4.72 o -2 6 2 1114.22 1171.71 7.32 o -1 6 2 20.78 22.59 2.05 o 0 6 2 905.84 853.69 6.77 o 1 6 2 19.48 22.83 2.20 o 2 6 2 1116.23 1132.58 6.61 o 3 6 2 155.09 151.85 4.09 o 4 6 2 99.71 97.14 5.12 o 5 6 2 55.33 45.34 5.12 o 6 6 2 22.51 25.43 5.75 o -6 7 2 36.15 38.57 6.53 o -5 7 2 170.42 177.43 7.79 o -4 7 2 474.90 442.78 8.90 o -3 7 2 908.86 894.62 8.19 o -2 7 2 88.77 66.75 3.23 o -1 7 2 1553.70 1555.85 9.68 o 0 7 2 358.20 346.83 5.51 o 1 7 2 1560.34 1591.43 9.76 o 2 7 2 92.74 80.92 3.07 o 3 7 2 908.15 879.19 7.95 o 4 7 2 473.54 461.05 8.66 o 5 7 2 169.53 159.09 7.71 o 6 7 2 37.47 37.31 6.38 o -6 8 2 9.21 5.43 5.90 < -5 8 2 76.06 82.65 6.53 o -4 8 2 110.17 100.52 6.06 o -3 8 2 641.05 629.34 8.58 o -2 8 2 162.17 159.01 5.43 o -1 8 2 404.95 431.69 6.22 o 0 8 2 0.50 1.18 2.44 < 1 8 2 405.35 434.99 6.85 o 2 8 2 158.20 158.14 4.57 o 3 8 2 635.63 621.55 8.90 o 4 8 2 108.71 92.41 6.06 o 5 8 2 75.71 87.69 6.77 o 6 8 2 9.28 6.53 5.90 < -6 9 2 27.42 17.32 9.60 < -5 9 2 67.73 83.60 7.01 o -4 9 2 48.58 53.76 5.59 o -3 9 2 220.39 218.60 7.16 o -2 9 2 9.49 8.97 3.46 < -1 9 2 1265.20 1213.66 10.39 o 0 9 2 303.27 334.71 6.22 o 1 9 2 1270.72 1222.48 11.02 o 2 9 2 9.42 7.40 2.99 < 3 9 2 209.35 206.16 7.32 o 4 9 2 48.40 49.43 5.59 o 5 9 2 65.73 75.80 7.71 o 6 9 2 27.16 19.13 7.95 < -6 10 2 17.09 20.62 10.23 < -5 10 2 37.13 34.40 7.87 o -4 10 2 0.86 1.73 5.83 < -3 10 2 307.48 288.89 8.27 o -2 10 2 2.34 6.61 3.62 < -1 10 2 160.52 158.69 5.75 o 0 10 2 0.16 4.01 2.99 < 1 10 2 160.75 159.87 5.90 o 2 10 2 1.98 1.02 3.07 < 3 10 2 309.72 286.22 8.11 o 4 10 2 0.65 4.17 5.27 < 5 10 2 36.28 38.81 7.32 o 6 10 2 16.41 21.25 10.47 < -5 11 2 41.39 43.29 7.40 o -4 11 2 93.53 94.15 8.74 o 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1.26 5.27 < 1 14 2 232.77 223.32 8.66 o 2 14 2 119.88 122.72 9.13 o 3 14 2 14.62 17.55 6.69 < 4 14 2 3.29 3.07 6.69 < 5 14 2 35.15 41.17 9.21 o -4 15 2 174.84 201.28 13.22 o -3 15 2 57.32 64.71 9.13 o -2 15 2 59.27 64.31 10.00 o -1 15 2 348.89 395.87 13.85 o 0 15 2 4.04 9.76 5.90 < 1 15 2 354.49 367.14 12.20 o 2 15 2 62.27 65.49 8.90 o 3 15 2 54.71 62.66 8.34 o 4 15 2 177.10 193.09 11.89 o -4 16 2 18.98 22.51 8.97 < -3 16 2 7.10 9.45 10.47 < -2 16 2 57.11 42.66 11.65 o -1 16 2 42.48 45.66 8.03 o 0 16 2 658.42 646.98 15.59 o 1 16 2 41.43 42.82 7.16 o 2 16 2 55.65 57.94 10.31 o 3 16 2 7.60 7.87 7.79 < 4 16 2 18.33 20.07 8.90 < -4 17 2 22.27 22.28 12.28 < -3 17 2 91.90 82.02 14.80 o -2 17 2 67.14 65.18 13.38 o -1 17 2 242.99 250.79 12.99 o 0 17 2 272.99 260.95 13.30 o 1 17 2 234.18 233.16 11.57 o 2 17 2 67.96 87.53 12.12 o 3 17 2 92.94 76.43 12.04 o 4 17 2 23.30 13.78 12.04 < -3 18 2 19.50 24.24 12.36 < -2 18 2 3.38 10.71 11.34 < -1 18 2 11.34 15.66 8.90 < 0 18 2 0.53 -1.81 7.16 < 1 18 2 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1189.73 9.29 o 2 4 10 44.78 41.41 3.70 o 3 4 10 244.66 242.29 8.27 o 4 4 10 157.44 157.43 7.56 o 5 4 10 101.60 102.02 8.11 o -5 5 10 8.46 6.06 6.30 < -4 5 10 12.59 11.57 5.83 < -3 5 10 259.18 229.85 7.95 o -2 5 10 86.89 94.54 4.41 o -1 5 10 3.73 3.62 2.60 < 0 5 10 62.10 57.54 3.38 o 1 5 10 3.58 5.98 2.83 < 2 5 10 87.44 93.04 4.96 o 3 5 10 256.40 234.89 7.64 o 4 5 10 13.03 17.40 5.20 o 5 5 10 7.90 10.94 6.06 < -5 6 10 77.54 82.97 8.58 o -4 6 10 40.39 42.51 6.85 o -3 6 10 155.27 163.10 8.11 o -2 6 10 430.87 419.33 7.08 o -1 6 10 554.85 575.90 7.40 o 0 6 10 642.56 589.83 7.79 o 1 6 10 546.08 567.39 8.03 o 2 6 10 438.10 442.55 8.11 o 3 6 10 159.57 172.55 8.19 o 4 6 10 40.96 40.62 6.53 o 5 6 10 76.95 90.13 8.19 o -5 7 10 54.94 51.64 7.79 o -4 7 10 2.99 2.20 5.90 < -3 7 10 165.19 151.53 8.11 o -2 7 10 163.02 159.56 6.06 o -1 7 10 143.86 142.48 5.51 o 0 7 10 29.26 28.50 3.62 o 1 7 10 144.87 150.11 5.59 o 2 7 10 161.27 159.95 6.69 o 3 7 10 166.81 146.57 8.19 o 4 7 10 2.95 3.46 6.06 < 5 7 10 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5.83 < -3 2 12 174.56 172.94 8.34 o -2 2 12 290.07 279.53 6.61 o -1 2 12 86.56 84.15 4.49 o 0 2 12 39.61 38.18 3.78 o 1 2 12 86.90 81.39 5.20 o 2 2 12 293.99 291.33 7.16 o 3 2 12 174.94 169.87 8.03 o 4 2 12 4.61 -0.71 5.35 < 5 2 12 43.64 38.10 7.01 o -5 3 12 81.87 86.75 8.34 o -4 3 12 111.48 107.69 8.66 o -3 3 12 538.97 527.09 11.89 o -2 3 12 625.52 619.03 8.58 o -1 3 12 897.86 915.64 9.52 o 0 3 12 271.67 291.57 6.06 o 1 3 12 892.05 923.20 10.08 o 2 3 12 623.17 623.91 10.47 o 3 3 12 541.32 540.16 11.57 o 4 3 12 109.43 113.83 8.34 o 5 3 12 81.50 94.70 9.60 o -5 4 12 4.17 12.12 6.77 < -4 4 12 44.17 41.64 7.08 o -3 4 12 84.21 78.17 6.77 o -2 4 12 30.02 21.65 4.17 o -1 4 12 53.07 46.29 4.01 o 0 4 12 49.86 50.06 3.78 o 1 4 12 51.26 46.92 4.25 o 2 4 12 29.45 23.69 4.64 o 3 4 12 82.46 75.17 6.45 o 4 4 12 42.80 42.11 6.85 o 5 4 12 4.45 5.12 6.69 < -5 5 12 31.73 29.91 7.40 o -4 5 12 270.31 267.17 11.57 o -3 5 12 215.45 203.64 10.39 o -2 5 12 330.89 317.39 7.95 o -1 5 12 279.39 260.24 6.77 o 0 5 12 579.61 562.59 8.11 o 1 5 12 278.35 262.36 7.16 o 2 5 12 329.00 317.07 8.66 o 3 5 12 215.75 217.73 9.29 o 4 5 12 266.53 275.12 10.86 o 5 5 12 32.15 30.07 7.40 o -5 6 12 7.78 3.15 7.56 < -4 6 12 16.64 26.92 7.01 o -3 6 12 156.19 144.76 9.45 o -2 6 12 32.74 27.55 4.41 o -1 6 12 66.45 63.60 4.88 o 0 6 12 120.82 111.07 5.35 o 1 6 12 65.03 61.01 5.12 o 2 6 12 31.95 25.50 5.27 o 3 6 12 155.48 149.72 9.52 o 4 6 12 16.08 23.85 7.08 o 5 6 12 7.30 6.22 7.16 < -5 7 12 18.66 26.21 8.42 o -4 7 12 29.84 37.94 7.56 o -3 7 12 64.57 63.21 7.71 o -2 7 12 145.93 143.58 6.61 o -1 7 12 394.11 369.97 8.19 o 0 7 12 0.08 3.78 3.86 < 1 7 12 388.34 376.35 9.84 o 2 7 12 137.76 132.09 8.11 o 3 7 12 67.77 56.60 7.79 o 4 7 12 29.54 38.81 7.79 o 5 7 12 18.66 18.73 8.11 < -5 8 12 27.88 33.38 9.05 o -4 8 12 5.29 12.83 7.08 < -3 8 12 29.90 32.90 7.16 o -2 8 12 257.10 241.03 8.27 o -1 8 12 3.07 -1.89 4.09 < 0 8 12 0.29 -2.05 4.72 < 1 8 12 3.24 3.70 4.96 < 2 8 12 260.35 241.50 10.00 o 3 8 12 30.67 34.79 7.24 o 4 8 12 4.97 5.27 6.85 < 5 8 12 28.23 26.37 8.74 o -4 9 12 15.19 19.21 7.64 < -3 9 12 275.87 302.51 12.83 o -2 9 12 58.71 55.97 6.22 o -1 9 12 360.24 367.29 9.68 o 0 9 12 1.08 0.08 5.04 < 1 9 12 358.63 367.29 11.34 o 2 9 12 58.84 53.21 8.42 o 3 9 12 269.87 272.91 12.36 o 4 9 12 14.97 15.11 7.40 < -4 10 12 22.88 28.42 8.03 o -3 10 12 15.46 5.27 7.48 < -2 10 12 176.16 156.65 9.05 o -1 10 12 5.97 1.10 5.20 < 0 10 12 332.35 334.47 10.78 o 1 10 12 5.76 1.89 5.59 < 2 10 12 174.81 154.29 11.49 o 3 10 12 15.04 14.25 7.87 < 4 10 12 23.75 23.46 7.95 < -4 11 12 85.63 77.38 10.78 o -3 11 12 65.78 79.98 10.55 o -2 11 12 37.73 42.04 7.16 o -1 11 12 432.79 449.00 12.28 o 0 11 12 39.35 34.87 6.22 o 1 11 12 428.77 465.14 15.74 o 2 11 12 40.19 37.55 9.60 o 3 11 12 67.84 66.36 9.92 o 4 11 12 81.95 73.84 12.20 o -4 12 12 59.26 79.19 12.83 o -3 12 12 2.44 -1.26 8.66 < -2 12 12 8.67 7.40 7.01 < -1 12 12 37.92 36.21 7.01 o 0 12 12 3.77 2.68 6.45 < 1 12 12 37.96 36.60 7.32 o 2 12 12 9.06 13.15 8.74 < 3 12 12 2.21 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