data_ca061220_1_1 _audit_creation_date 2020-12-07 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226) ; _shelx_SHELXL_version_number '2018/3' loop_ _audit_author_name _audit_author_email _audit_author_address 'Balkenhohl, M.' mbalkenhohl@ethz.ch LOC-Carreira _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_acknowledgements ; X-Ray services provided by SMoCC - The Small Molecule Crystallography Center of ETH Zurich. ; _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C20 H22 N2 O3 S, C3 H3' _chemical_formula_sum 'C23 H25 N2 O3 S' _chemical_formula_weight 409.51 _chemical_melting_point ? _chemical_oxdiff_formula C20H22N2O3S 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' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 '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' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' 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 9.68420(10) _cell_length_b 25.2973(2) _cell_length_c 8.78460(10) _cell_angle_alpha 90 _cell_angle_beta 109.0070(10) _cell_angle_gamma 90 _cell_volume 2034.75(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 26881 _cell_measurement_temperature 100.0(1) _cell_measurement_theta_max 79.6150 _cell_measurement_theta_min 3.4980 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 1.634 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.492 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 868 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2 -1 0 0.1062 -2 1 0 0.0963 -1 0 1 0.1399 0 0 -1 0.1092 0 0 1 0.1151 0 -1 0 0.0175 0 1 0 0.0175 1 -16 0 0.0336 2 -15 -2 0.0786 0 -15 -2 0.0483 -2 -16 0 0.0370 4 11 0 0.0825 1 -10 -4 0.0947 1 -1 -6 0.1115 1 8 -5 0.0915 -2 15 0 0.0455 0 10 4 0.0955 3 -13 0 0.0681 1 -13 3 0.0763 -1 -15 2 0.0565 _exptl_crystal_size_max 0.269 _exptl_crystal_size_mid 0.209 _exptl_crystal_size_min 0.035 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 2.0001 -1.0060 0.0003 0.0858 -0.2765 0.1821 -2.0001 1.0060 -0.0003 -0.0858 0.2765 -0.1821 -1.0001 0.0027 1.0001 0.0072 -0.0020 -0.2057 0.0000 0.0004 -1.0005 -0.0199 0.1437 0.1157 -0.0000 -0.0004 1.0005 0.0199 -0.1437 -0.1157 -0.0000 -0.9996 -0.0003 0.0605 0.0067 0.0021 0.0000 0.9996 0.0003 -0.0605 -0.0067 -0.0021 0.7122 -16.2920 -0.4929 0.9848 0.0787 0.1552 2.2678 -14.7337 -2.0444 0.8790 0.0708 0.4714 0.2470 -15.2141 -2.0906 0.8820 0.3668 0.2959 -1.7859 -15.5991 -0.1676 0.9181 0.3811 -0.1088 4.3567 11.3302 -0.1653 -0.6344 -0.6688 0.3876 1.0493 -10.0337 -4.4826 0.5311 0.5622 0.6340 1.0382 -0.7363 -5.6187 -0.0541 0.6649 0.7450 0.5437 8.2699 -4.7943 -0.5888 0.5564 0.5863 -2.3641 15.0906 0.0590 -0.9413 0.2256 -0.2512 0.1680 10.1842 4.1774 -0.5310 -0.6917 -0.4894 3.3694 -13.4276 0.1373 0.8571 -0.4072 0.3155 0.7629 -13.4620 2.7907 0.8794 -0.4190 -0.2260 -1.0547 -15.4181 1.9287 0.9580 -0.0248 -0.2859 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_unetI/netI 0.0228 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 50821 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 79.997 _diffrn_reflns_theta_min 3.494 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.0(1) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 5.8140 _diffrn_detector_type 'Pilatus 300K' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -54.00 -29.00 0.50 0.12 -- 14.00 157.00 55.43 50 2 \w -23.00 2.00 0.50 0.12 -- 14.00 104.00-151.62 50 3 \w -103.00 -35.00 0.50 0.12 -- -34.00 162.00-178.79 136 4 \w 16.00 42.00 0.50 0.12 -- 46.00 92.00-161.41 52 5 \w 17.00 42.00 0.50 0.12 -- 46.00 89.00 93.08 50 6 \w -6.00 21.00 0.50 0.12 -- -48.37 19.00 -30.00 54 7 \w -111.00 -37.00 0.50 0.12 -- -48.37 -32.00 34.54 148 8 \w -90.00 -64.00 0.50 0.12 -- -48.37 -77.00-180.00 52 9 \w -58.00 -25.00 0.50 0.12 -- -48.37 -77.00-180.00 66 10 \w 89.00 116.00 0.50 0.12 -- 48.37 64.00-145.89 54 11 \w 38.00 108.00 0.50 0.12 -- 48.37 57.00 -90.00 140 12 \w 97.00 123.00 0.50 0.12 -- 48.37 19.00 150.00 52 13 \w 48.00 75.00 0.50 0.12 -- 48.37 19.00 150.00 54 14 \w 30.00 79.00 0.50 0.12 -- 48.37 64.00-145.89 98 15 \w 25.00 57.00 0.50 0.12 -- 48.37 77.00 -30.00 64 16 \w 61.00 118.00 0.50 0.12 -- 48.37-178.00 -60.00 114 17 \w 33.00 70.00 0.50 0.12 -- 58.00 80.00 179.87 74 18 \w 34.00 72.00 0.50 0.12 -- 58.00 79.00-121.84 76 19 \w 95.00 120.00 0.50 0.12 -- 58.00 80.00 -13.04 50 20 \w 33.00 75.00 0.50 0.12 -- 58.00 80.00 -13.04 84 21 \w 39.00 67.00 0.50 0.12 -- 62.00 76.00 16.07 56 22 \w 100.00 125.00 0.50 0.12 -- 62.00 76.00 16.07 50 23 \w 37.00 72.00 0.50 0.12 -- 62.00 80.00 70.42 70 24 \w -63.00 -37.00 0.50 0.37 -- -62.00 -79.00 119.42 52 25 \w 91.00 117.00 0.50 0.12 -- 62.00 78.00 62.66 52 26 \w 38.00 64.00 0.50 0.12 -- 62.00 78.00 62.66 52 27 \w -71.00 -46.00 0.50 0.37 -- -70.00 -78.00 116.46 50 28 \w -87.00 -48.00 0.50 0.37 -- -70.00 -73.00 2.78 78 29 \w 101.00 136.00 0.50 0.12 -- 70.00 77.00-108.83 70 30 \w -76.00 -13.00 0.50 0.37 -- -70.00 125.00 0.00 126 31 \w -77.00 -47.00 0.50 0.37 -- -70.00 -74.00 151.89 60 32 \w 45.00 72.00 0.50 0.12 -- 70.00 80.00 78.85 54 33 \w 45.00 71.00 0.50 0.12 -- 70.00 80.00 -79.06 52 34 \w 46.00 84.00 0.50 0.12 -- 70.00 77.00-108.83 76 35 \w 51.00 77.00 0.50 0.12 -- 74.00 78.00-133.04 52 36 \w 55.00 96.00 0.50 0.12 -- 74.00 66.00 -29.08 82 37 \w 115.00 140.00 0.50 0.12 -- 74.00 80.00-164.42 50 38 \w 49.00 76.00 0.50 0.12 -- 74.00 80.00-164.42 54 39 \w 103.00 129.00 0.50 0.12 -- 78.00 78.00-132.81 52 40 \w 56.00 83.00 0.50 0.12 -- 78.00 78.00-132.81 54 41 \w 54.00 79.00 0.50 0.12 -- 78.00 79.00 -74.45 50 42 \w 55.00 88.00 0.50 0.12 -- 78.00 75.00 -2.67 66 43 \w 67.00 95.00 0.50 0.37 -- 82.00 56.00 133.72 56 44 \w 63.00 89.00 0.50 0.37 -- 82.00 67.00 61.98 52 45 \w 63.00 94.00 0.50 0.37 -- 86.00 80.00 72.36 62 46 \w 67.00 114.00 0.50 0.37 -- 86.00 71.00 141.56 94 47 \w 68.00 154.00 0.50 0.37 -- 86.00 70.00 -96.23 172 48 \w 116.00 157.00 0.50 0.37 -- 90.00 71.00 117.29 82 49 \w 70.00 112.00 0.50 0.37 -- 90.00 71.00 117.29 84 50 \w 67.00 103.00 0.50 0.37 -- 90.00 75.00 -16.98 72 51 \w 118.00 157.00 0.50 0.37 -- 90.00 70.00 -69.37 78 52 \w 69.00 105.00 0.50 0.37 -- 90.00 70.00 -69.37 72 53 \w 84.00 167.00 0.50 0.37 -- 94.00 51.00 52.71 166 54 \w 92.00 123.00 0.50 0.37 -- 110.00 68.00 147.71 62 55 \w 38.00 67.00 0.50 0.37 -- 110.00 -57.00-120.00 58 56 \w 78.00 112.00 0.50 0.37 -- 110.00-125.00 150.00 68 57 \w 41.00 72.00 0.50 0.37 -- 110.00-125.00 150.00 62 58 \w 143.00 170.00 0.50 0.37 -- 110.00 77.00 0.00 54 59 \w 86.00 128.00 0.50 0.37 -- 110.00 77.00 0.00 84 60 \w 62.00 112.00 0.50 0.37 -- 110.00-125.00 0.00 100 61 \w 43.00 68.00 0.50 0.37 -- 110.00 -99.00 30.00 50 62 \w 71.00 101.00 0.50 0.37 -- 110.00 -99.00 30.00 60 63 \w 142.00 168.00 0.50 0.37 -- 110.00 57.00-180.00 52 64 \w 95.00 128.00 0.50 0.37 -- 110.00 57.00-180.00 66 65 \w 43.00 75.00 0.50 0.37 -- 110.00 -99.00 90.00 64 66 \w 92.00 176.00 0.50 0.37 -- 110.00 77.00 90.00 168 67 \w 42.00 96.00 0.50 0.37 -- 110.00 -99.00 -90.00 108 68 \w 141.00 176.00 0.50 0.37 -- 110.00 77.00 60.00 70 69 \w 86.00 129.00 0.50 0.37 -- 110.00 77.00 60.00 86 70 \w 40.00 71.00 0.50 0.37 -- 110.00 -99.00 60.00 62 71 \w 43.00 105.00 0.50 0.37 -- 110.00 -99.00-180.00 124 72 \w 105.00 178.00 0.50 0.37 -- 110.00 38.00 30.00 146 73 \w 142.00 167.00 0.50 0.37 -- 110.00 77.00 -90.00 50 74 \w 96.00 166.00 0.50 0.37 -- 110.00 125.00 120.00 140 75 \w 92.00 122.00 0.50 0.37 -- 110.00 77.00 -90.00 60 76 \w 88.00 116.00 0.50 0.37 -- 110.00 77.00-180.00 56 77 \w 89.00 171.00 0.50 0.37 -- 110.00 77.00 -30.00 164 78 \w 113.00 172.00 0.50 0.37 -- 110.00 125.00-120.00 118 79 \w 87.00 162.00 0.50 0.37 -- 110.00 77.00 -60.00 150 80 \w 134.00 169.00 0.50 0.37 -- 110.00 77.00-150.00 70 81 \w 98.00 172.00 0.50 0.37 -- 110.00 27.00-122.06 148 82 \w 44.00 87.00 0.50 0.37 -- 110.00 -99.00-150.00 86 83 \w 88.00 120.00 0.50 0.37 -- 110.00 77.00-150.00 64 84 \w 138.00 167.00 0.50 0.37 -- 110.00 68.00 147.71 58 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 300K' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0124741000 _diffrn_orient_matrix_UB_12 -0.0604996000 _diffrn_orient_matrix_UB_13 0.0198693000 _diffrn_orient_matrix_UB_21 -0.1415959000 _diffrn_orient_matrix_UB_22 -0.0066734000 _diffrn_orient_matrix_UB_23 -0.1436214000 _diffrn_orient_matrix_UB_31 0.0900212000 _diffrn_orient_matrix_UB_32 -0.0020890000 _diffrn_orient_matrix_UB_33 -0.1156840000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3958 _reflns_number_total 4378 _reflns_odcompleteness_completeness 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _refine_diff_density_max 0.288 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.047 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 266 _refine_ls_number_reflns 4378 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0367 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+1.0982P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0928 _refine_ls_wR_factor_ref 0.0948 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances O1-H1 0.93 with sigma of 0.02 3.a Ternary CH refined with riding coordinates: C1(H1A), C5(H5), C6(H6) 3.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B) 3.c Aromatic/amide H refined with riding coordinates: C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C18(H18), C19(H19), C1A(H1AA), C2A(H2AA), C3A(H3AA) 3.d Idealised Me refined as rotating group: C20(H20A,H20B,H20C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 0.65504(4) 0.68587(2) 0.22088(4) 0.01971(10) Uani 1 1 d . . . . . O1 O 0.86634(15) 0.67012(5) 0.77771(13) 0.0374(3) Uani 1 1 d D . . . . H1 H 0.811(2) 0.6989(8) 0.786(3) 0.056 Uiso 1 1 d D U . . . O2 O 0.73048(11) 0.73170(4) 0.30363(13) 0.0252(2) Uani 1 1 d . . . . . O3 O 0.65544(11) 0.67402(4) 0.06206(12) 0.0249(2) Uani 1 1 d . . . . . N1 N 0.73411(13) 0.63518(5) 0.33754(14) 0.0198(2) Uani 1 1 d . . . . . N2 N 0.66230(13) 0.58675(5) 0.27299(14) 0.0201(2) Uani 1 1 d . . . . . C1 C 0.87804(18) 0.67133(6) 0.61931(18) 0.0279(3) Uani 1 1 d . . . . . H1A H 0.864835 0.707536 0.577314 0.033 Uiso 1 1 calc R U . . . C2 C 1.02948(18) 0.65159(6) 0.63374(19) 0.0302(3) Uani 1 1 d . . . . . H2A H 1.101988 0.674006 0.707901 0.036 Uiso 1 1 calc R U . . . H2B H 1.043508 0.653639 0.529486 0.036 Uiso 1 1 calc R U . . . C3 C 1.05072(17) 0.59471(6) 0.69382(18) 0.0259(3) Uani 1 1 d . . . . . H3A H 1.148898 0.583048 0.704704 0.031 Uiso 1 1 calc R U . . . H3B H 1.037899 0.592495 0.798638 0.031 Uiso 1 1 calc R U . . . C4 C 0.93973(16) 0.55938(6) 0.57462(17) 0.0224(3) Uani 1 1 d . . . . . H4A H 0.953307 0.523219 0.613397 0.027 Uiso 1 1 calc R U . . . H4B H 0.956991 0.560378 0.471906 0.027 Uiso 1 1 calc R U . . . C5 C 0.78077(15) 0.57641(5) 0.54984(16) 0.0198(3) Uani 1 1 d . . . . . H5 H 0.748488 0.565344 0.639728 0.024 Uiso 1 1 calc R U . . . C6 C 0.75583(16) 0.63563(5) 0.51452(16) 0.0210(3) Uani 1 1 d . . . . . H6 H 0.663745 0.645849 0.530103 0.025 Uiso 1 1 calc R U . . . C7 C 0.68433(15) 0.55415(5) 0.39153(16) 0.0194(3) Uani 1 1 d . . . . . C8 C 0.63212(15) 0.49925(5) 0.36462(17) 0.0201(3) Uani 1 1 d . . . . . C9 C 0.66732(16) 0.46284(6) 0.49027(18) 0.0245(3) Uani 1 1 d . . . . . H9 H 0.722214 0.473586 0.593506 0.029 Uiso 1 1 calc R U . . . C10 C 0.62135(18) 0.41060(6) 0.46318(19) 0.0284(3) Uani 1 1 d . . . . . H10 H 0.646009 0.386579 0.547931 0.034 Uiso 1 1 calc R U . . . C11 C 0.53841(17) 0.39424(6) 0.30927(19) 0.0272(3) Uani 1 1 d . . . . . H11 H 0.509250 0.359144 0.290635 0.033 Uiso 1 1 calc R U . . . C12 C 0.49938(16) 0.43037(6) 0.18382(19) 0.0259(3) Uani 1 1 d . . . . . H12 H 0.442122 0.419731 0.081363 0.031 Uiso 1 1 calc R U . . . C13 C 0.54585(16) 0.48239(6) 0.21138(17) 0.0237(3) Uani 1 1 d . . . . . H13 H 0.519304 0.506452 0.126750 0.028 Uiso 1 1 calc R U . . . C14 C 0.47297(15) 0.68925(5) 0.21828(17) 0.0195(3) Uani 1 1 d . . . . . C15 C 0.43717(16) 0.72129(6) 0.32838(18) 0.0241(3) Uani 1 1 d . . . . . H15 H 0.508867 0.740923 0.403397 0.029 Uiso 1 1 calc R U . . . C16 C 0.29280(17) 0.72361(6) 0.32490(19) 0.0255(3) Uani 1 1 d . . . . . H16 H 0.268459 0.744551 0.399399 0.031 Uiso 1 1 calc R U . . . C17 C 0.18392(16) 0.69504(6) 0.21144(18) 0.0227(3) Uani 1 1 d . . . . . C18 C 0.22318(16) 0.66350(6) 0.10158(17) 0.0242(3) Uani 1 1 d . . . . . H18 H 0.151325 0.644499 0.024749 0.029 Uiso 1 1 calc R U . . . C19 C 0.36616(16) 0.65992(6) 0.10454(17) 0.0228(3) Uani 1 1 d . . . . . H19 H 0.390954 0.638294 0.031833 0.027 Uiso 1 1 calc R U . . . C20 C 0.02716(17) 0.69746(7) 0.2055(2) 0.0304(3) Uani 1 1 d . . . . . H20A H -0.000360 0.664170 0.239604 0.046 Uiso 1 1 calc R U . . . H20B H -0.034065 0.704792 0.097396 0.046 Uiso 1 1 calc R U . . . H20C H 0.015800 0.724951 0.275847 0.046 Uiso 1 1 calc R U . . . C1A C 1.0350(2) 0.54156(7) 0.1076(2) 0.0345(4) Uani 1 1 d . . . . . H1AA H 1.058771 0.569555 0.180150 0.041 Uiso 1 1 calc R U . . . C2A C 0.89140(19) 0.52517(7) 0.0439(2) 0.0354(4) Uani 1 1 d . . . . . H2AA H 0.818579 0.542034 0.073327 0.043 Uiso 1 1 calc R U . . . C3A C 0.85679(19) 0.48347(8) -0.0640(2) 0.0363(4) Uani 1 1 d . . . . . H3AA H 0.760394 0.472273 -0.107215 0.044 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 0.01778(17) 0.01774(17) 0.02263(18) 0.00354(12) 0.00524(13) -0.00016(12) O1 0.0500(7) 0.0332(6) 0.0227(6) -0.0059(5) 0.0031(5) 0.0169(5) O2 0.0210(5) 0.0196(5) 0.0323(6) 0.0031(4) 0.0051(4) -0.0033(4) O3 0.0240(5) 0.0282(5) 0.0230(5) 0.0058(4) 0.0084(4) 0.0016(4) N1 0.0204(6) 0.0178(6) 0.0196(6) 0.0005(4) 0.0044(4) 0.0006(4) N2 0.0207(6) 0.0177(5) 0.0217(6) -0.0007(4) 0.0065(5) -0.0006(4) C1 0.0348(8) 0.0188(7) 0.0238(7) -0.0021(6) 0.0010(6) 0.0017(6) C2 0.0290(8) 0.0293(8) 0.0271(8) -0.0002(6) 0.0019(6) -0.0059(6) C3 0.0232(7) 0.0289(8) 0.0230(7) 0.0000(6) 0.0037(6) 0.0035(6) C4 0.0245(7) 0.0213(7) 0.0207(7) 0.0008(5) 0.0062(5) 0.0050(5) C5 0.0225(7) 0.0186(6) 0.0186(6) 0.0002(5) 0.0071(5) 0.0013(5) C6 0.0228(7) 0.0205(7) 0.0190(6) 0.0010(5) 0.0059(5) 0.0035(5) C7 0.0188(6) 0.0199(7) 0.0200(6) 0.0008(5) 0.0070(5) 0.0025(5) C8 0.0205(6) 0.0192(6) 0.0217(7) 0.0000(5) 0.0083(5) 0.0015(5) C9 0.0277(7) 0.0233(7) 0.0221(7) 0.0018(6) 0.0077(6) 0.0005(6) C10 0.0329(8) 0.0236(7) 0.0304(8) 0.0065(6) 0.0127(6) 0.0009(6) C11 0.0278(8) 0.0206(7) 0.0362(8) -0.0017(6) 0.0145(6) -0.0028(6) C12 0.0246(7) 0.0258(7) 0.0268(7) -0.0048(6) 0.0078(6) -0.0019(6) C13 0.0262(7) 0.0228(7) 0.0209(7) 0.0006(5) 0.0061(6) 0.0003(6) C14 0.0179(6) 0.0176(6) 0.0219(7) 0.0033(5) 0.0048(5) 0.0014(5) C15 0.0224(7) 0.0196(7) 0.0265(7) -0.0031(5) 0.0029(6) 0.0000(5) C16 0.0263(7) 0.0215(7) 0.0290(8) -0.0028(6) 0.0094(6) 0.0034(6) C17 0.0199(7) 0.0224(7) 0.0242(7) 0.0056(5) 0.0048(5) 0.0019(5) C18 0.0218(7) 0.0266(7) 0.0212(7) -0.0003(6) 0.0028(5) -0.0040(6) C19 0.0238(7) 0.0229(7) 0.0212(7) -0.0012(5) 0.0067(6) -0.0010(5) C20 0.0214(7) 0.0342(8) 0.0353(8) 0.0037(7) 0.0085(6) 0.0033(6) C1A 0.0436(10) 0.0325(9) 0.0263(8) 0.0032(6) 0.0099(7) 0.0027(7) C2A 0.0353(9) 0.0438(10) 0.0285(8) 0.0079(7) 0.0122(7) 0.0138(7) C3A 0.0295(8) 0.0492(10) 0.0282(8) 0.0065(7) 0.0066(7) 0.0014(7) _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 O2 1.4354(10) . ? S1 O3 1.4283(11) . ? S1 N1 1.6644(12) . ? S1 C14 1.7579(14) . ? O1 H1 0.921(16) . ? O1 C1 1.433(2) . ? N1 N2 1.4314(16) . ? N1 C6 1.4995(17) . ? N2 C7 1.2906(18) . ? C1 H1A 0.9800 . ? C1 C2 1.515(2) . ? C1 C6 1.534(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C3 1.523(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.522(2) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 C5 1.5442(19) . ? C5 H5 0.9800 . ? C5 C6 1.5329(19) . ? C5 C7 1.5092(19) . ? C6 H6 0.9800 . ? C7 C8 1.4705(19) . ? C8 C9 1.392(2) . ? C8 C13 1.400(2) . ? C9 H9 0.9300 . ? C9 C10 1.390(2) . ? C10 H10 0.9300 . ? C10 C11 1.392(2) . ? C11 H11 0.9300 . ? C11 C12 1.386(2) . ? C12 H12 0.9300 . ? C12 C13 1.386(2) . ? C13 H13 0.9300 . ? C14 C15 1.390(2) . ? C14 C19 1.3948(19) . ? C15 H15 0.9300 . ? C15 C16 1.390(2) . ? C16 H16 0.9300 . ? C16 C17 1.394(2) . ? C17 C18 1.397(2) . ? C17 C20 1.503(2) . ? C18 H18 0.9300 . ? C18 C19 1.379(2) . ? C19 H19 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C1A H1AA 0.9300 . ? C1A C2A 1.383(3) . ? C1A C3A 1.381(3) 3_765 ? C2A H2AA 0.9300 . ? C2A C3A 1.384(3) . ? C3A H3AA 0.9300 . ? 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 O2 S1 N1 104.73(6) . . ? O2 S1 C14 108.07(7) . . ? O3 S1 O2 120.09(6) . . ? O3 S1 N1 107.01(6) . . ? O3 S1 C14 108.62(6) . . ? N1 S1 C14 107.69(6) . . ? C1 O1 H1 106.9(15) . . ? N2 N1 S1 110.41(8) . . ? N2 N1 C6 107.65(10) . . ? C6 N1 S1 120.90(9) . . ? C7 N2 N1 107.22(11) . . ? O1 C1 H1A 110.1 . . ? O1 C1 C2 107.00(12) . . ? O1 C1 C6 106.29(13) . . ? C2 C1 H1A 110.1 . . ? C2 C1 C6 113.12(12) . . ? C6 C1 H1A 110.1 . . ? C1 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? C1 C2 C3 110.99(13) . . ? H2A C2 H2B 108.0 . . ? C3 C2 H2A 109.4 . . ? C3 C2 H2B 109.4 . . ? C2 C3 H3A 109.8 . . ? C2 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? C4 C3 C2 109.32(12) . . ? C4 C3 H3A 109.8 . . ? C4 C3 H3B 109.8 . . ? C3 C4 H4A 109.1 . . ? C3 C4 H4B 109.1 . . ? C3 C4 C5 112.41(12) . . ? H4A C4 H4B 107.9 . . ? C5 C4 H4A 109.1 . . ? C5 C4 H4B 109.1 . . ? C4 C5 H5 111.8 . . ? C6 C5 C4 112.67(12) . . ? C6 C5 H5 111.8 . . ? C7 C5 C4 108.37(11) . . ? C7 C5 H5 111.8 . . ? C7 C5 C6 99.71(11) . . ? N1 C6 C1 116.54(12) . . ? N1 C6 C5 99.33(10) . . ? N1 C6 H6 108.7 . . ? C1 C6 H6 108.7 . . ? C5 C6 C1 114.45(12) . . ? C5 C6 H6 108.7 . . ? N2 C7 C5 113.27(12) . . ? N2 C7 C8 121.07(12) . . ? C8 C7 C5 125.30(12) . . ? C9 C8 C7 120.98(13) . . ? C9 C8 C13 118.44(13) . . ? C13 C8 C7 120.58(13) . . ? C8 C9 H9 119.6 . . ? C10 C9 C8 120.74(14) . . ? C10 C9 H9 119.6 . . ? C9 C10 H10 120.0 . . ? C9 C10 C11 120.02(14) . . ? C11 C10 H10 120.0 . . ? C10 C11 H11 120.1 . . ? C12 C11 C10 119.87(14) . . ? C12 C11 H11 120.1 . . ? C11 C12 H12 120.1 . . ? C11 C12 C13 119.87(14) . . ? C13 C12 H12 120.1 . . ? C8 C13 H13 119.5 . . ? C12 C13 C8 121.02(14) . . ? C12 C13 H13 119.5 . . ? C15 C14 S1 119.73(11) . . ? C15 C14 C19 120.92(13) . . ? C19 C14 S1 119.35(11) . . ? C14 C15 H15 120.4 . . ? C14 C15 C16 119.12(13) . . ? C16 C15 H15 120.4 . . ? C15 C16 H16 119.5 . . ? C15 C16 C17 121.01(14) . . ? C17 C16 H16 119.5 . . ? C16 C17 C18 118.52(14) . . ? C16 C17 C20 121.59(14) . . ? C18 C17 C20 119.89(13) . . ? C17 C18 H18 119.3 . . ? C19 C18 C17 121.46(13) . . ? C19 C18 H18 119.3 . . ? C14 C19 H19 120.5 . . ? C18 C19 C14 118.97(14) . . ? C18 C19 H19 120.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C2A C1A H1AA 119.9 . . ? C3A C1A H1AA 119.9 3_765 . ? C3A C1A C2A 120.27(17) 3_765 . ? C1A C2A H2AA 120.2 . . ? C1A C2A C3A 119.54(17) . . ? C3A C2A H2AA 120.2 . . ? C1A C3A C2A 120.19(17) 3_765 . ? C1A C3A H3AA 119.9 3_765 . ? C2A C3A H3AA 119.9 . . ? 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 S1 N1 N2 C7 -154.51(10) . . . . ? S1 N1 C6 C1 -74.63(15) . . . . ? S1 N1 C6 C5 161.93(9) . . . . ? S1 C14 C15 C16 179.96(11) . . . . ? S1 C14 C19 C18 -178.91(11) . . . . ? O1 C1 C2 C3 62.17(16) . . . . ? O1 C1 C6 N1 173.23(11) . . . . ? O1 C1 C6 C5 -71.55(15) . . . . ? O2 S1 N1 N2 176.42(9) . . . . ? O2 S1 N1 C6 49.56(12) . . . . ? O2 S1 C14 C15 -19.91(13) . . . . ? O2 S1 C14 C19 159.61(11) . . . . ? O3 S1 N1 N2 -55.07(10) . . . . ? O3 S1 N1 C6 178.07(10) . . . . ? O3 S1 C14 C15 -151.71(11) . . . . ? O3 S1 C14 C19 27.81(13) . . . . ? N1 S1 C14 C15 92.72(12) . . . . ? N1 S1 C14 C19 -87.75(12) . . . . ? N1 N2 C7 C5 -2.83(16) . . . . ? N1 N2 C7 C8 -176.25(12) . . . . ? N2 N1 C6 C1 157.26(12) . . . . ? N2 N1 C6 C5 33.83(13) . . . . ? N2 C7 C8 C9 174.11(14) . . . . ? N2 C7 C8 C13 -5.8(2) . . . . ? C1 C2 C3 C4 60.80(16) . . . . ? C2 C1 C6 N1 -69.65(16) . . . . ? C2 C1 C6 C5 45.58(18) . . . . ? C2 C3 C4 C5 -58.61(16) . . . . ? C3 C4 C5 C6 49.68(16) . . . . ? C3 C4 C5 C7 159.03(12) . . . . ? C4 C5 C6 N1 82.32(13) . . . . ? C4 C5 C6 C1 -42.58(17) . . . . ? C4 C5 C7 N2 -94.13(14) . . . . ? C4 C5 C7 C8 78.97(16) . . . . ? C5 C7 C8 C9 1.5(2) . . . . ? C5 C7 C8 C13 -178.35(13) . . . . ? C6 N1 N2 C7 -20.60(14) . . . . ? C6 C1 C2 C3 -54.54(17) . . . . ? C6 C5 C7 N2 23.83(15) . . . . ? C6 C5 C7 C8 -163.08(13) . . . . ? C7 C5 C6 N1 -32.38(13) . . . . ? C7 C5 C6 C1 -157.28(12) . . . . ? C7 C8 C9 C10 -178.06(14) . . . . ? C7 C8 C13 C12 178.24(13) . . . . ? C8 C9 C10 C11 -0.4(2) . . . . ? C9 C8 C13 C12 -1.6(2) . . . . ? C9 C10 C11 C12 -1.3(2) . . . . ? C10 C11 C12 C13 1.4(2) . . . . ? C11 C12 C13 C8 0.0(2) . . . . ? C13 C8 C9 C10 1.8(2) . . . . ? C14 S1 N1 N2 61.56(10) . . . . ? C14 S1 N1 C6 -65.31(12) . . . . ? C14 C15 C16 C17 -1.0(2) . . . . ? C15 C14 C19 C18 0.6(2) . . . . ? C15 C16 C17 C18 0.5(2) . . . . ? C15 C16 C17 C20 -179.58(14) . . . . ? C16 C17 C18 C19 0.5(2) . . . . ? C17 C18 C19 C14 -1.1(2) . . . . ? C19 C14 C15 C16 0.4(2) . . . . ? C20 C17 C18 C19 -179.34(14) . . . . ? C1A C2A C3A C1A 0.0(3) . . . 3_765 ? C3A C1A C2A C3A 0.0(3) 3_765 . . . ? _shelx_res_file ; TITL ca061220_1_1_a.res in P2(1)/c ca061220_1_1.res created by SHELXL-2018/3 at 14:44:43 on 07-Dec-2020 REM Old TITL ca061220_1_1 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.099, Rweak 0.051, Alpha 0.025, Orientation as input REM Formula found by SHELXT: C23 N2 O3 S CELL 1.54184 9.6842 25.2973 8.7846 90 109.007 90 ZERR 4 0.0001 0.0002 0.0001 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O S UNIT 92 100 8 12 4 DFIX 0.93 O1 H1 L.S. 9 PLAN 20 CONF BOND $H list 4 MORE -1 fmap 2 acta REM REM REM WGHT 0.039100 1.098200 FVAR 0.63935 S1 5 0.655038 0.685871 0.220880 11.00000 0.01778 0.01774 = 0.02263 0.00354 0.00524 -0.00016 O1 4 0.866339 0.670123 0.777705 11.00000 0.05000 0.03322 = 0.02265 -0.00589 0.00312 0.01694 H1 2 0.810911 0.698930 0.785745 11.00000 -1.50000 O2 4 0.730479 0.731701 0.303628 11.00000 0.02103 0.01960 = 0.03234 0.00308 0.00512 -0.00327 O3 4 0.655444 0.674016 0.062062 11.00000 0.02399 0.02816 = 0.02303 0.00578 0.00840 0.00160 N1 3 0.734108 0.635176 0.337540 11.00000 0.02043 0.01777 = 0.01960 0.00049 0.00437 0.00058 N2 3 0.662303 0.586753 0.272993 11.00000 0.02065 0.01775 = 0.02168 -0.00070 0.00648 -0.00061 C1 1 0.878045 0.671335 0.619308 11.00000 0.03479 0.01883 = 0.02383 -0.00212 0.00096 0.00172 AFIX 13 H1A 2 0.864835 0.707536 0.577314 11.00000 -1.20000 AFIX 0 C2 1 1.029482 0.651595 0.633740 11.00000 0.02900 0.02933 = 0.02714 -0.00018 0.00195 -0.00587 AFIX 23 H2A 2 1.101988 0.674006 0.707901 11.00000 -1.20000 H2B 2 1.043508 0.653639 0.529486 11.00000 -1.20000 AFIX 0 C3 1 1.050725 0.594714 0.693822 11.00000 0.02318 0.02893 = 0.02295 -0.00001 0.00375 0.00348 AFIX 23 H3A 2 1.148898 0.583048 0.704704 11.00000 -1.20000 H3B 2 1.037899 0.592495 0.798638 11.00000 -1.20000 AFIX 0 C4 1 0.939729 0.559378 0.574615 11.00000 0.02451 0.02134 = 0.02066 0.00084 0.00624 0.00505 AFIX 23 H4A 2 0.953307 0.523219 0.613397 11.00000 -1.20000 H4B 2 0.956991 0.560378 0.471906 11.00000 -1.20000 AFIX 0 C5 1 0.780774 0.576412 0.549845 11.00000 0.02246 0.01859 = 0.01865 0.00020 0.00705 0.00133 AFIX 13 H5 2 0.748488 0.565344 0.639728 11.00000 -1.20000 AFIX 0 C6 1 0.755832 0.635629 0.514518 11.00000 0.02276 0.02054 = 0.01899 0.00099 0.00593 0.00350 AFIX 13 H6 2 0.663745 0.645849 0.530103 11.00000 -1.20000 AFIX 0 C7 1 0.684325 0.554149 0.391534 11.00000 0.01883 0.01993 = 0.02003 0.00083 0.00704 0.00253 C8 1 0.632121 0.499251 0.364616 11.00000 0.02053 0.01918 = 0.02168 -0.00001 0.00833 0.00153 C9 1 0.667320 0.462839 0.490272 11.00000 0.02773 0.02332 = 0.02213 0.00184 0.00766 0.00052 AFIX 43 H9 2 0.722214 0.473586 0.593506 11.00000 -1.20000 AFIX 0 C10 1 0.621346 0.410605 0.463182 11.00000 0.03291 0.02356 = 0.03036 0.00650 0.01266 0.00086 AFIX 43 H10 2 0.646009 0.386579 0.547931 11.00000 -1.20000 AFIX 0 C11 1 0.538415 0.394244 0.309270 11.00000 0.02779 0.02063 = 0.03619 -0.00168 0.01446 -0.00276 AFIX 43 H11 2 0.509250 0.359144 0.290635 11.00000 -1.20000 AFIX 0 C12 1 0.499379 0.430368 0.183822 11.00000 0.02457 0.02576 = 0.02683 -0.00476 0.00779 -0.00193 AFIX 43 H12 2 0.442122 0.419731 0.081363 11.00000 -1.20000 AFIX 0 C13 1 0.545853 0.482388 0.211380 11.00000 0.02617 0.02284 = 0.02087 0.00059 0.00607 0.00033 AFIX 43 H13 2 0.519304 0.506452 0.126750 11.00000 -1.20000 AFIX 0 C14 1 0.472972 0.689251 0.218281 11.00000 0.01788 0.01759 = 0.02195 0.00327 0.00481 0.00137 C15 1 0.437168 0.721294 0.328383 11.00000 0.02239 0.01964 = 0.02652 -0.00311 0.00290 0.00005 AFIX 43 H15 2 0.508867 0.740923 0.403397 11.00000 -1.20000 AFIX 0 C16 1 0.292804 0.723614 0.324900 11.00000 0.02628 0.02153 = 0.02903 -0.00284 0.00936 0.00336 AFIX 43 H16 2 0.268459 0.744551 0.399399 11.00000 -1.20000 AFIX 0 C17 1 0.183920 0.695039 0.211444 11.00000 0.01985 0.02241 = 0.02418 0.00565 0.00482 0.00186 C18 1 0.223177 0.663502 0.101582 11.00000 0.02181 0.02658 = 0.02122 -0.00029 0.00280 -0.00404 AFIX 43 H18 2 0.151325 0.644499 0.024749 11.00000 -1.20000 AFIX 0 C19 1 0.366159 0.659923 0.104541 11.00000 0.02384 0.02285 = 0.02120 -0.00121 0.00674 -0.00102 AFIX 43 H19 2 0.390954 0.638294 0.031833 11.00000 -1.20000 AFIX 0 C20 1 0.027161 0.697456 0.205539 11.00000 0.02137 0.03418 = 0.03525 0.00366 0.00853 0.00335 AFIX 137 H20A 2 -0.000360 0.664170 0.239604 11.00000 -1.50000 H20B 2 -0.034065 0.704792 0.097396 11.00000 -1.50000 H20C 2 0.015800 0.724951 0.275847 11.00000 -1.50000 AFIX 0 C1A 1 1.034971 0.541562 0.107618 11.00000 0.04364 0.03247 = 0.02628 0.00322 0.00987 0.00269 AFIX 43 H1AA 2 1.058771 0.569555 0.180150 11.00000 -1.20000 AFIX 0 C2A 1 0.891398 0.525166 0.043906 11.00000 0.03532 0.04380 = 0.02854 0.00786 0.01221 0.01377 AFIX 43 H2AA 2 0.818579 0.542034 0.073327 11.00000 -1.20000 AFIX 0 C3A 1 0.856787 0.483468 -0.063987 11.00000 0.02954 0.04922 = 0.02817 0.00648 0.00658 0.00137 AFIX 43 H3AA 2 0.760394 0.472273 -0.107215 11.00000 -1.20000 AFIX 0 HKLF 4 REM ca061220_1_1_a.res in P2(1)/c REM wR2 = 0.0948, GooF = S = 1.089, Restrained GooF = 1.089 for all data REM R1 = 0.0367 for 3958 Fo > 4sig(Fo) and 0.0403 for all 4378 data REM 266 parameters refined using 1 restraints END WGHT 0.0391 1.0969 REM Highest difference peak 0.288, deepest hole -0.474, 1-sigma level 0.047 Q1 1 0.5576 0.6871 0.2208 11.00000 0.05 0.29 Q2 1 0.6651 0.5238 0.3659 11.00000 0.05 0.27 Q3 1 0.7719 0.6062 0.5394 11.00000 0.05 0.26 Q4 1 0.5978 0.4909 0.2953 11.00000 0.05 0.24 Q5 1 0.8623 0.5676 0.5583 11.00000 0.05 0.23 Q6 1 0.6844 0.6567 0.2910 11.00000 0.05 0.23 Q7 1 0.1102 0.6951 0.2174 11.00000 0.05 0.22 Q8 1 0.3674 0.7228 0.3239 11.00000 0.05 0.20 Q9 1 1.0275 0.6221 0.6594 11.00000 0.05 0.20 Q10 1 0.6179 0.4857 0.4213 11.00000 0.05 0.20 Q11 1 0.8172 0.6512 0.5654 11.00000 0.05 0.19 Q12 1 0.5022 0.4569 0.2147 11.00000 0.05 0.19 Q13 1 0.4552 0.7125 0.2587 11.00000 0.05 0.19 Q14 1 0.6302 0.4395 0.4696 11.00000 0.05 0.19 Q15 1 0.5392 0.4501 0.1888 11.00000 0.05 0.18 Q16 1 0.7316 0.5616 0.4643 11.00000 0.05 0.17 Q17 1 0.4182 0.6784 0.1603 11.00000 0.05 0.17 Q18 1 0.6035 0.4000 0.3796 11.00000 0.05 0.17 Q19 1 0.4661 0.6938 0.3065 11.00000 0.05 0.17 Q20 1 0.5177 0.4175 0.2541 11.00000 0.05 0.17 ; _shelx_res_checksum 53845 _shelx_hkl_file ; -1 0 0 684.37 35.65 1 0 0 680.71 36.32 -1 0 0 672.00 35.58 -1 0 0 683.74 35.79 2 0 0 214.05 12.53 2 0 0 216.15 13.70 -2 0 0 205.57 12.85 2 0 0 233.90 14.16 -2 0 0 207.53 13.33 3 0 0 3837.23 204.41 3 0 0 3854.61 202.89 -3 0 0 3957.05 202.89 3 0 0 3912.03 203.97 3 0 0 3854.92 203.22 -3 0 0 4013.71 203.63 -3 0 0 3847.59 203.09 -3 0 0 3909.70 202.66 -4 0 0 10.68 4.17 4 0 0 10.20 4.25 -4 0 0 12.03 3.44 4 0 0 7.73 3.18 -4 0 0 9.80 4.15 4 0 0 9.64 2.90 4 0 0 11.54 4.99 4 0 0 15.15 4.97 -4 0 0 8.18 3.73 -5 0 0 507.95 31.31 5 0 0 543.42 33.13 5 0 0 529.57 32.51 5 0 0 530.18 30.74 -5 0 0 546.60 34.05 5 0 0 489.54 30.23 -5 0 0 578.49 33.13 -5 0 0 538.89 33.20 -5 0 0 556.08 32.68 -5 0 0 565.43 32.71 5 0 0 497.14 30.01 6 0 0 1153.54 66.12 -6 0 0 1239.90 70.51 6 0 0 1282.21 71.15 -6 0 0 1313.21 72.61 -6 0 0 1260.06 71.07 -6 0 0 1326.17 70.33 -6 0 0 1268.76 71.87 6 0 0 1174.34 66.60 -7 0 0 592.44 38.80 -7 0 0 627.27 39.09 -7 0 0 572.39 32.15 7 0 0 566.38 37.87 -7 0 0 640.57 40.31 7 0 0 569.01 33.37 7 0 0 547.21 33.04 7 0 0 513.18 31.04 -8 0 0 116.22 14.89 -8 0 0 121.42 14.90 -8 0 0 113.09 9.33 -8 0 0 125.00 14.73 -8 0 0 108.82 13.83 -8 0 0 110.76 13.83 8 0 0 117.43 10.36 8 0 0 96.72 7.81 -9 0 0 218.60 20.73 -9 0 0 248.48 15.86 -9 0 0 264.00 22.43 9 0 0 234.31 16.79 9 0 0 224.44 16.53 9 0 0 237.68 15.66 9 0 0 236.74 15.42 -10 0 0 914.09 56.61 -10 0 0 928.46 50.71 10 0 0 965.00 50.51 -10 0 0 977.50 51.02 10 0 0 901.65 50.22 10 0 0 895.33 51.43 -11 0 0 4.48 1.97 11 0 0 5.00 2.36 1 -1 0 2659.73 140.60 1 1 0 2675.77 140.99 -1 -1 0 2907.02 141.26 -1 1 0 2907.60 141.26 -1 -1 0 2756.18 141.04 -1 1 0 2675.03 140.58 1 -1 0 2723.72 141.23 -2 1 0 124.62 8.13 -2 -1 0 126.87 8.19 2 -1 0 121.70 8.71 2 -1 0 124.60 9.30 -2 1 0 120.15 7.63 2 1 0 129.97 9.31 2 1 0 131.10 9.00 -2 -1 0 121.13 8.32 2 -1 0 115.58 7.61 -2 1 0 119.15 8.56 2 1 0 129.25 8.13 3 1 0 1282.60 70.29 -3 1 0 1340.74 69.21 -3 -1 0 1330.84 69.54 3 -1 0 1231.09 70.18 3 -1 0 1309.42 68.32 3 -1 0 1270.55 70.82 3 -1 0 1288.97 69.63 3 1 0 1235.95 70.59 -3 1 0 1292.76 69.84 3 -1 0 1266.15 69.21 -3 -1 0 1301.83 70.09 -3 -1 0 1335.80 69.46 -3 1 0 1261.89 69.36 4 -1 0 1685.72 92.56 -4 -1 0 1670.75 92.15 -4 1 0 1736.79 90.95 4 -1 0 1630.41 92.93 4 1 0 1672.25 92.55 4 -1 0 1638.35 89.86 4 -1 0 1674.72 89.36 -4 -1 0 1739.51 91.42 -4 -1 0 1621.78 90.37 -4 1 0 1779.34 92.22 4 -1 0 1576.52 90.28 4 1 0 1701.40 90.47 -4 1 0 1698.29 89.77 4 1 0 1794.07 91.71 4 1 0 1608.77 89.68 4 -1 0 1752.60 91.27 -4 1 0 1784.29 90.76 -4 -1 0 1760.14 91.85 -4 1 0 1739.34 91.40 -4 -1 0 1694.34 91.06 -4 1 0 1685.63 90.57 -5 -1 0 2000.36 104.15 -5 1 0 1923.98 101.71 5 1 0 1971.82 104.23 -5 1 0 1992.25 104.93 -5 1 0 2013.50 103.62 5 1 0 1854.20 103.23 5 -1 0 1910.47 103.16 5 1 0 1823.72 101.87 5 -1 0 1915.25 106.03 -5 -1 0 2034.53 105.71 5 1 0 1924.86 101.30 5 -1 0 1859.06 103.50 -5 -1 0 1928.63 102.65 5 -1 0 1714.19 100.15 5 -1 0 1856.98 100.99 -5 1 0 2025.00 103.12 -5 1 0 1879.82 103.61 -5 1 0 1887.77 102.71 -5 -1 0 1984.26 104.29 5 1 0 1965.89 100.83 5 -1 0 1887.30 100.72 6 1 0 135.07 12.27 -6 -1 0 129.20 11.98 -6 -1 0 149.16 14.77 -6 -1 0 153.35 13.79 -6 1 0 137.09 14.04 6 1 0 155.84 14.20 6 -1 0 126.91 12.97 6 1 0 137.90 10.39 -6 -1 0 161.39 14.68 -6 -1 0 156.14 13.61 -6 1 0 140.91 13.30 -6 1 0 124.12 13.29 -6 -1 0 134.40 13.47 6 1 0 126.94 10.52 6 -1 0 122.43 10.39 -7 -1 0 297.39 23.82 -7 1 0 290.99 17.43 -7 1 0 251.32 22.45 -7 -1 0 307.33 23.61 -7 1 0 285.85 22.57 -7 1 0 291.76 23.83 7 1 0 293.38 23.36 7 -1 0 264.03 21.99 -7 -1 0 318.45 24.97 7 -1 0 280.34 18.53 7 1 0 275.15 18.59 7 1 0 227.04 15.98 7 -1 0 273.31 18.46 7 1 0 284.19 18.49 7 -1 0 273.99 16.77 7 1 0 273.95 18.47 -8 1 0 322.45 26.01 -8 -1 0 326.25 26.12 -8 -1 0 315.90 25.70 -8 -1 0 321.21 26.12 -8 1 0 316.65 26.08 -8 1 0 310.27 25.23 -8 1 0 301.91 19.42 -8 -1 0 303.99 19.48 -8 1 0 310.77 26.92 -8 -1 0 283.32 25.90 -8 -1 0 341.75 28.27 8 1 0 335.57 20.94 8 -1 0 289.97 18.31 8 -1 0 302.08 19.41 8 -1 0 285.97 20.35 8 1 0 312.63 20.60 -9 -1 0 88.65 8.15 -9 1 0 101.23 8.22 -9 -1 0 101.94 13.01 -9 1 0 89.10 12.58 -9 1 0 85.66 12.55 -9 -1 0 83.52 11.97 9 -1 0 97.12 9.06 9 -1 0 78.13 7.59 9 1 0 98.36 7.99 9 -1 0 98.55 8.03 9 -1 0 98.65 9.27 9 1 0 85.07 8.64 9 1 0 77.92 7.75 -10 -1 0 46.07 8.08 -10 1 0 54.27 8.79 -10 1 0 52.27 5.15 -10 -1 0 49.61 5.25 10 1 0 40.34 4.78 -10 1 0 57.87 5.52 10 -1 0 44.20 4.60 10 1 0 46.47 5.93 10 -1 0 42.96 5.68 -10 -1 0 48.02 5.21 10 -1 0 40.10 4.79 10 1 0 47.79 4.99 11 -1 0 480.67 24.75 -11 1 0 503.93 25.69 -11 1 0 493.29 25.17 11 1 0 467.08 25.34 11 1 0 385.80 23.91 -11 -1 0 448.85 24.96 11 -1 0 483.05 25.31 0 2 0 159.41 8.90 0 -2 0 150.36 8.70 0 -2 0 151.69 8.54 -1 -2 0 109.65 6.87 1 2 0 99.46 6.70 -1 2 0 114.54 6.77 1 -2 0 109.76 6.45 -2 -2 0 1544.50 82.85 2 2 0 1520.18 83.02 -2 2 0 1589.78 83.52 -2 2 0 1690.89 83.02 -2 -2 0 1599.07 83.30 2 -2 0 1623.16 83.09 2 -2 0 1571.32 83.52 2 2 0 1524.92 83.72 -3 -2 0 133.47 9.85 3 -2 0 120.08 8.11 3 -2 0 134.63 9.92 3 -2 0 125.30 8.72 -3 -2 0 139.68 9.64 3 -2 0 126.01 10.83 3 2 0 122.10 8.97 -3 -2 0 127.61 10.14 3 -2 0 132.54 10.49 3 -2 0 128.62 9.42 3 2 0 131.59 10.45 -3 2 0 127.42 9.89 -3 2 0 140.72 8.62 -3 2 0 134.24 9.25 -3 2 0 121.81 9.33 -3 -2 0 129.70 9.80 4 -2 0 108.69 11.57 4 -2 0 136.03 10.71 -4 2 0 127.11 10.27 4 -2 0 126.69 9.70 4 2 0 121.70 9.45 4 -2 0 118.20 8.33 4 2 0 120.75 11.66 4 2 0 136.41 10.50 -4 2 0 133.71 9.21 -4 -2 0 132.49 10.91 -4 2 0 125.48 10.92 4 2 0 139.02 11.30 -4 -2 0 128.30 11.37 -4 2 0 114.83 9.61 -4 -2 0 120.39 10.81 -4 2 0 118.94 10.38 -4 2 0 131.20 9.92 -4 -2 0 132.67 10.83 -4 -2 0 139.26 10.90 5 -2 0 10.48 2.88 5 2 0 7.84 5.40 5 2 0 4.16 4.59 -5 2 0 16.52 5.05 -5 -2 0 11.64 4.22 5 -2 0 13.19 4.31 -5 -2 0 2.88 4.53 -5 -2 0 8.11 4.59 5 2 0 8.30 2.75 5 -2 0 5.42 4.29 5 2 0 9.54 3.79 5 2 0 5.92 4.55 -5 2 0 5.06 4.12 -5 2 0 7.39 3.18 -5 2 0 7.47 3.72 -5 -2 0 6.91 3.95 -5 -2 0 17.65 5.28 -5 -2 0 8.50 4.15 5 -2 0 8.85 3.34 5 2 0 8.13 3.40 -6 2 0 26.28 5.69 -6 -2 0 31.65 6.79 -6 2 0 28.75 3.79 -6 2 0 27.13 6.69 -6 -2 0 14.98 6.09 6 2 0 19.84 4.36 -6 -2 0 17.89 4.83 6 2 0 32.57 6.90 6 2 0 25.80 3.98 6 2 0 23.05 5.34 -6 2 0 23.66 6.22 -6 -2 0 29.46 6.56 6 -2 0 17.27 5.55 6 -2 0 19.18 4.36 6 -2 0 28.81 4.77 6 2 0 17.43 4.23 -7 2 0 62.56 6.43 -7 2 0 72.63 10.55 -7 -2 0 99.38 12.27 -7 -2 0 64.60 9.87 -7 2 0 101.23 12.27 -7 2 0 80.61 10.78 -7 -2 0 76.63 11.05 7 -2 0 79.06 10.68 7 2 0 64.79 10.40 -7 -2 0 72.20 11.23 -7 2 0 66.27 10.61 7 2 0 70.71 8.13 -7 -2 0 83.58 7.44 7 -2 0 79.27 8.08 7 2 0 65.09 7.62 7 -2 0 81.39 6.83 -8 2 0 16.04 3.74 -8 -2 0 18.20 7.03 -8 -2 0 24.19 7.14 -8 2 0 8.89 5.89 -8 -2 0 10.43 5.92 -8 2 0 27.05 8.07 -8 -2 0 17.55 4.18 -8 -2 0 27.64 8.15 -8 2 0 16.56 7.06 -8 2 0 10.85 5.49 8 2 0 16.54 5.14 8 -2 0 11.17 4.82 8 -2 0 16.79 4.04 8 2 0 23.33 5.03 8 -2 0 12.37 3.29 -9 -2 0 23.22 4.11 -9 2 0 19.46 3.74 -9 -2 0 27.11 7.71 -9 2 0 20.33 6.78 -9 -2 0 14.68 6.32 -9 -2 0 32.27 7.80 -9 2 0 25.21 7.66 9 2 0 17.70 3.92 9 2 0 22.04 4.82 -9 2 0 25.72 4.55 9 -2 0 26.23 4.08 9 -2 0 15.82 4.60 9 -2 0 21.00 4.00 -10 -2 0 24.75 3.85 -10 2 0 23.70 6.38 10 2 0 25.10 3.68 10 -2 0 25.17 3.81 10 -2 0 22.09 3.23 -10 -2 0 24.51 3.80 -10 2 0 28.24 4.01 10 -2 0 31.73 4.77 10 2 0 29.44 4.95 11 2 0 107.63 6.95 -11 2 0 123.73 8.13 11 -2 0 109.68 7.26 11 2 0 96.23 6.72 -11 2 0 120.12 7.67 -11 -2 0 119.56 7.57 11 2 0 111.67 7.88 11 -2 0 112.22 7.72 0 -3 0 0.75 0.98 0 -3 0 1.98 1.27 0 -3 0 0.95 1.09 -1 3 0 338.14 18.47 1 3 0 311.09 18.71 -1 -3 0 345.04 19.02 1 -3 0 345.99 18.14 -2 3 0 127.57 7.89 -2 3 0 117.45 8.43 2 3 0 113.72 8.16 2 -3 0 119.43 7.29 2 -3 0 128.85 8.12 -2 -3 0 109.83 8.45 -2 -3 0 126.74 8.44 3 -3 0 933.60 48.86 3 3 0 916.54 51.75 -3 -3 0 920.69 50.09 -3 -3 0 911.19 49.56 -3 3 0 964.90 49.65 3 3 0 912.40 50.13 3 3 0 877.14 48.57 -3 -3 0 910.93 49.30 -3 3 0 915.31 48.89 -3 3 0 865.94 46.81 -3 -3 0 882.66 49.45 -3 3 0 812.39 49.18 -4 3 0 38.23 5.88 4 -3 0 35.68 5.34 -4 -3 0 34.70 6.07 4 3 0 38.23 6.28 -4 -3 0 44.53 6.23 4 3 0 26.36 4.43 4 -3 0 34.86 4.39 4 -3 0 34.20 6.52 4 3 0 30.20 6.21 -4 -3 0 46.29 6.36 -4 3 0 28.18 5.44 -4 -3 0 36.99 5.13 -4 -3 0 31.69 5.61 -4 3 0 34.13 5.27 -4 -3 0 31.36 5.87 5 3 0 109.85 10.96 5 3 0 102.08 10.18 -5 -3 0 117.58 10.68 5 -3 0 116.41 8.99 5 -3 0 104.74 12.24 5 3 0 95.36 11.46 -5 -3 0 122.46 12.26 -5 3 0 115.54 11.33 5 3 0 108.72 9.23 5 3 0 107.98 11.24 5 -3 0 113.42 10.71 -5 -3 0 113.95 11.18 -5 -3 0 118.11 11.11 -5 -3 0 121.48 11.35 -5 3 0 107.38 11.15 -5 3 0 114.63 10.78 -5 -3 0 132.47 11.86 5 -3 0 113.25 8.79 5 3 0 93.46 8.47 -6 3 0 40.17 7.53 -6 -3 0 45.09 7.99 6 -3 0 40.54 4.04 -6 3 0 48.26 4.67 -6 -3 0 50.29 8.36 -6 -3 0 38.43 7.48 6 -3 0 40.17 8.21 -6 3 0 41.97 7.59 6 3 0 44.90 5.63 -6 -3 0 59.44 7.82 6 3 0 46.44 8.09 6 3 0 37.24 6.29 6 -3 0 45.18 7.24 6 3 0 47.05 7.12 6 -3 0 42.52 5.75 6 3 0 38.57 5.65 6 3 0 36.72 5.37 6 -3 0 38.69 5.49 -7 3 0 1.60 2.61 -7 3 0 3.96 4.91 -7 3 0 2.66 4.65 -7 -3 0 8.23 5.81 -7 -3 0 1.38 5.00 -7 -3 0 3.16 4.52 -7 -3 0 1.06 3.31 7 3 0 1.40 4.20 -7 -3 0 3.51 3.07 7 3 0 -1.83 3.86 7 3 0 2.32 3.56 7 -3 0 1.26 2.91 7 -3 0 2.85 3.65 7 -3 0 1.49 2.61 -8 -3 0 9.28 6.09 -8 -3 0 1.53 3.21 -8 3 0 7.49 5.58 -8 3 0 1.78 2.65 -8 3 0 2.96 5.68 -8 -3 0 6.06 4.75 -8 3 0 9.02 5.09 -8 -3 0 3.54 5.54 -8 3 0 1.64 5.54 -8 -3 0 6.29 3.14 8 3 0 4.51 3.87 8 -3 0 7.06 3.06 8 -3 0 9.28 4.62 8 -3 0 6.97 2.87 8 -3 0 6.24 3.92 8 3 0 6.96 4.13 8 -3 0 4.81 3.22 -9 -3 0 200.46 13.52 -9 -3 0 164.85 17.84 -9 -3 0 195.87 18.82 -9 3 0 173.75 18.19 -9 -3 0 180.53 18.39 9 -3 0 203.14 12.99 9 -3 0 164.56 11.93 -9 3 0 208.33 13.52 9 -3 0 199.87 14.40 9 3 0 187.82 14.14 9 -3 0 189.62 12.67 -10 3 0 30.78 6.89 -10 -3 0 36.33 4.50 -10 3 0 32.93 4.01 10 -3 0 42.63 4.48 -10 3 0 28.30 4.28 10 -3 0 26.57 3.42 10 -3 0 40.19 5.18 10 3 0 27.26 4.85 -10 -3 0 37.41 4.50 -11 3 0 6.89 2.30 11 -3 0 3.20 1.82 11 -3 0 3.56 2.07 11 3 0 5.13 2.33 11 3 0 3.93 1.52 -11 3 0 3.07 1.88 0 4 0 151.20 9.57 0 -4 0 143.92 8.81 0 -4 0 149.98 9.19 0 -4 0 141.82 9.25 -1 4 0 43.95 3.63 1 -4 0 44.67 3.24 1 -4 0 47.82 4.55 -1 -4 0 39.64 4.21 -1 -4 0 39.24 3.15 1 -4 0 42.66 3.73 -1 4 0 50.66 3.37 1 -4 0 40.19 4.65 1 4 0 48.79 4.40 2 -4 0 29.64 2.48 -2 -4 0 31.43 4.31 2 4 0 33.36 3.91 -2 4 0 33.82 4.63 2 -4 0 34.68 3.48 -2 -4 0 31.67 4.06 2 4 0 34.12 5.45 -2 4 0 29.66 3.57 -2 4 0 33.29 3.98 -2 4 0 33.21 2.91 -3 -4 0 55.22 5.92 3 -4 0 45.47 4.16 -3 4 0 46.11 5.34 3 4 0 46.93 7.00 3 -4 0 53.88 5.15 3 4 0 50.99 6.29 -3 -4 0 46.11 5.71 3 4 0 57.70 5.44 -3 4 0 48.06 5.57 -4 -4 0 12.34 4.91 4 4 0 22.65 5.30 4 -4 0 22.48 3.42 4 4 0 12.99 3.62 4 4 0 14.27 5.33 4 -4 0 23.09 5.91 4 -4 0 18.56 4.26 -4 -4 0 18.89 4.65 -4 4 0 13.91 4.22 -4 -4 0 17.45 4.51 -4 4 0 16.22 4.32 -4 -4 0 16.56 4.53 -4 -4 0 24.68 5.05 -5 -4 0 215.71 16.46 5 -4 0 174.99 16.72 -5 4 0 209.79 17.12 5 4 0 176.27 14.94 5 -4 0 185.70 14.55 5 4 0 212.70 16.60 5 4 0 160.58 13.27 5 4 0 227.79 17.59 -5 -4 0 224.32 17.51 5 -4 0 188.31 13.30 -5 4 0 188.76 15.49 -5 -4 0 187.39 15.64 -5 -4 0 179.64 15.69 -5 4 0 196.03 15.76 -5 -4 0 191.86 15.75 5 -4 0 187.19 12.87 5 4 0 179.46 12.77 -6 4 0 1.09 3.81 -6 -4 0 1.10 4.09 -6 4 0 -1.09 4.29 -6 -4 0 1.10 3.97 -6 -4 0 -3.50 4.35 6 -4 0 3.70 3.54 -6 4 0 5.19 5.38 -6 -4 0 6.66 4.34 6 -4 0 -1.43 3.65 6 4 0 3.33 2.48 6 4 0 -0.89 3.23 6 4 0 -1.19 4.29 -6 -4 0 2.29 4.02 6 4 0 -1.79 3.88 6 4 0 2.16 3.16 6 -4 0 2.93 3.24 6 4 0 4.49 3.16 -7 4 0 323.45 24.58 -7 4 0 313.74 25.65 -7 -4 0 319.65 26.00 -7 -4 0 311.42 25.92 -7 4 0 347.50 26.35 -7 4 0 324.79 25.54 -7 -4 0 370.18 26.90 7 4 0 374.13 27.49 7 -4 0 318.77 22.67 -7 -4 0 334.43 27.51 -7 -4 0 286.19 23.77 -7 -4 0 311.35 19.79 -7 -4 0 345.17 20.91 7 4 0 321.70 21.34 7 -4 0 313.89 19.72 7 4 0 311.58 21.01 7 -4 0 308.94 20.89 7 -4 0 330.04 19.68 -8 4 0 78.22 11.63 -8 4 0 76.09 11.59 -8 -4 0 63.58 11.09 -8 -4 0 58.38 10.59 -8 -4 0 72.64 7.40 -8 4 0 69.76 11.09 -8 -4 0 79.38 12.60 -8 4 0 86.26 12.63 -8 -4 0 73.19 7.23 8 4 0 70.49 8.26 8 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313.00 17.46 -2 5 0 325.72 19.00 3 -5 0 47.05 4.76 -3 -5 0 39.66 5.30 3 5 0 40.42 5.56 -3 -5 0 34.06 5.29 3 -5 0 37.39 3.51 -3 5 0 35.36 5.69 3 5 0 33.49 6.24 -3 5 0 37.14 4.77 3 5 0 40.76 4.97 -3 5 0 41.98 4.54 -3 -5 0 43.40 5.56 -3 5 0 46.95 5.42 -4 -5 0 9.68 4.31 4 -5 0 10.25 2.53 -4 -5 0 11.47 4.78 -4 5 0 10.07 4.09 -4 5 0 14.09 5.21 4 -5 0 6.10 3.25 4 5 0 9.25 4.95 -4 -5 0 10.51 4.23 4 5 0 10.92 6.85 -4 -5 0 13.69 4.68 -4 -5 0 11.47 4.61 -4 5 0 8.95 3.43 -4 5 0 5.29 3.52 -4 5 0 9.39 2.21 -4 5 0 11.66 2.69 5 5 0 486.89 32.57 5 -5 0 523.69 34.90 5 5 0 526.73 34.05 -5 -5 0 523.62 33.51 5 5 0 517.68 30.96 -5 5 0 544.38 34.49 -5 -5 0 517.33 34.31 5 5 0 503.93 33.46 5 -5 0 507.85 31.49 -5 5 0 467.00 32.14 -5 -5 0 537.84 33.26 -5 -5 0 552.85 33.62 -5 5 0 498.99 32.63 -5 -5 0 531.09 33.34 -5 5 0 483.59 31.25 5 5 0 512.41 29.39 5 -5 0 479.23 29.09 -6 -5 0 233.41 20.08 -6 5 0 240.39 18.38 6 -5 0 225.98 14.38 -6 5 0 235.96 19.44 -6 -5 0 234.76 19.91 -6 5 0 264.54 20.21 -6 -5 0 239.57 19.81 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109.96 8.14 -3 -6 0 6.22 3.47 3 -6 0 7.23 2.59 3 6 0 5.92 2.75 -3 -6 0 -1.79 3.65 -3 6 0 2.69 2.76 3 6 0 3.40 4.34 -3 6 0 5.17 3.92 -3 6 0 1.65 2.23 -3 6 0 -0.52 3.11 -3 -6 0 3.96 3.58 -3 6 0 1.01 2.75 -3 6 0 4.41 2.68 -4 -6 0 2650.63 139.01 -4 -6 0 2698.33 138.29 -4 -6 0 2686.01 138.47 4 6 0 2641.71 141.35 -4 6 0 2843.44 139.44 -4 -6 0 2724.12 138.56 -4 6 0 2453.34 133.84 -4 6 0 2514.32 136.01 -4 6 0 2618.39 133.50 -4 6 0 2513.12 137.37 -4 -6 0 2651.73 138.32 -4 6 0 2582.58 137.40 4 -6 0 2427.66 134.39 -5 6 0 55.86 8.35 5 6 0 43.49 7.62 -5 -6 0 39.77 7.72 5 6 0 57.28 6.65 5 6 0 35.04 7.28 -5 -6 0 50.61 8.41 5 -6 0 46.18 8.34 -5 6 0 35.44 6.52 -5 -6 0 39.35 7.16 -5 -6 0 26.72 6.56 -5 -6 0 54.33 8.03 -5 6 0 35.15 6.37 -5 6 0 44.41 4.13 -5 6 0 41.81 5.90 5 -6 0 39.67 5.19 -6 -6 0 614.64 39.11 6 -6 0 560.86 32.22 -6 6 0 584.32 32.17 -6 6 0 598.35 38.12 -6 -6 0 590.84 38.98 -6 -6 0 599.35 38.87 -6 6 0 549.14 37.52 -6 -6 0 545.36 37.81 6 -6 0 574.58 40.50 6 6 0 510.40 36.98 6 -6 0 606.66 36.69 -6 -6 0 592.99 39.05 6 6 0 528.20 36.54 6 6 0 584.44 35.75 -6 -6 0 563.36 39.67 6 -6 0 584.84 36.35 6 6 0 636.10 40.04 -6 6 0 581.18 37.43 -6 6 0 635.16 40.00 6 6 0 552.27 34.01 6 6 0 587.85 34.37 6 -6 0 609.53 33.67 6 6 0 573.06 33.78 6 -6 0 579.00 32.33 6 -6 0 561.45 33.49 7 -6 0 57.15 5.49 -7 6 0 56.18 9.69 -7 6 0 67.44 5.84 -7 -6 0 57.12 10.27 -7 -6 0 57.63 9.74 -7 -6 0 55.15 9.50 -7 6 0 53.34 9.74 -7 6 0 48.82 8.47 -7 -6 0 63.46 11.31 -7 -6 0 57.16 10.10 7 6 0 46.98 9.37 7 -6 0 46.92 7.40 7 -6 0 38.71 7.33 -7 -6 0 52.08 9.29 -7 -6 0 47.22 5.98 7 6 0 64.24 6.41 -7 -6 0 61.37 7.10 7 6 0 53.26 7.15 7 6 0 57.44 7.47 7 -6 0 56.44 5.71 7 -6 0 52.10 7.02 7 -6 0 51.65 5.48 7 -6 0 45.99 6.42 7 6 0 57.18 7.20 -8 -6 0 316.65 26.86 -8 6 0 290.89 25.50 -8 6 0 309.13 19.08 -8 6 0 327.25 27.05 -8 -6 0 321.19 27.95 -8 6 0 314.40 25.05 8 6 0 306.90 21.04 -8 -6 0 325.93 20.43 -8 -6 0 282.91 19.29 -8 6 0 311.64 19.61 8 -6 0 309.72 19.21 8 -6 0 322.26 19.00 8 -6 0 307.33 20.47 -9 6 0 396.08 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21 0 -1.99 6.73 -4 -21 0 -1.28 4.78 -4 -21 0 0.56 3.60 4 21 0 4.52 4.51 -4 21 0 -2.96 3.78 4 -21 0 -1.18 3.70 4 21 0 5.43 4.75 4 21 0 -3.40 5.79 -4 -21 0 1.13 3.73 -4 21 0 2.69 2.50 4 21 0 1.45 3.03 4 -21 0 3.96 2.78 -4 21 0 -4.95 4.84 -5 21 0 28.76 9.75 -5 -21 0 27.58 6.57 5 -21 0 30.11 5.27 -5 21 0 25.90 8.65 -5 -21 0 24.76 4.79 5 21 0 23.93 6.10 -5 -21 0 28.97 5.22 5 21 0 27.97 5.93 5 -21 0 32.29 5.51 -5 21 0 27.97 5.53 -5 21 0 27.51 4.03 -5 21 0 30.64 6.01 -6 21 0 15.99 6.84 6 -21 0 10.33 3.58 -6 21 0 8.61 6.80 6 21 0 12.52 4.80 6 21 0 17.18 4.40 -6 -21 0 17.36 4.20 6 -21 0 12.83 3.82 -6 -21 0 15.24 4.62 -6 21 0 8.47 2.70 6 -21 0 10.67 3.20 7 -21 0 3.74 2.75 -7 21 0 6.98 5.64 -7 -21 0 7.10 3.27 -7 -21 0 3.30 2.85 7 -21 0 5.72 2.48 -7 21 0 2.61 2.95 7 21 0 10.80 3.85 -7 21 0 3.55 1.90 -8 -21 0 122.63 8.45 -8 21 0 129.17 8.72 8 21 0 115.58 8.08 8 21 0 118.45 8.99 8 -21 0 119.21 7.86 0 22 0 764.14 54.25 0 22 0 805.42 45.11 0 22 0 731.53 42.93 0 22 0 734.31 44.10 0 -22 0 755.18 42.96 0 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3 -22 0 1122.08 58.54 3 22 0 1090.83 59.74 4 -22 0 80.16 7.84 -4 22 0 91.90 13.91 4 22 0 85.22 14.54 -4 -22 0 71.21 11.82 4 22 0 67.12 8.52 -4 -22 0 63.24 7.22 -4 -22 0 71.81 7.89 4 -22 0 85.11 8.38 -4 22 0 80.54 8.03 -4 22 0 57.09 8.39 4 22 0 64.02 8.64 4 22 0 87.80 10.09 -4 22 0 88.16 8.85 -4 22 0 67.24 6.35 -4 -22 0 82.08 8.16 4 -22 0 77.67 6.59 5 -22 0 49.35 6.26 -5 22 0 64.09 11.27 5 22 0 69.37 8.02 -5 -22 0 39.41 5.75 5 22 0 54.84 7.50 -5 -22 0 52.41 7.24 5 -22 0 55.44 6.61 -5 -22 0 49.88 6.38 -5 22 0 58.27 6.71 -5 22 0 50.89 5.05 -5 22 0 61.52 7.12 5 -22 0 51.00 5.36 6 -22 0 17.65 3.95 6 -22 0 13.80 3.68 6 22 0 7.81 4.48 -6 22 0 11.39 3.81 -6 -22 0 13.99 4.23 -6 -22 0 13.64 3.58 6 22 0 18.39 4.20 7 -22 0 29.66 3.98 -7 -22 0 22.35 4.20 -7 -22 0 25.79 4.09 -7 22 0 28.95 4.56 7 -22 0 24.31 3.33 7 22 0 26.21 4.87 -7 22 0 36.36 4.25 -8 22 0 -1.41 1.98 -8 22 0 -0.82 1.58 -8 -22 0 2.72 1.92 8 22 0 1.97 1.91 8 -22 0 2.34 1.52 8 -22 0 0.39 1.15 0 -23 0 0.41 2.65 0 23 0 6.68 7.79 0 23 0 2.50 2.96 0 23 0 9.58 4.85 0 23 0 1.35 4.59 0 -23 0 -1.59 3.52 1 23 0 353.90 32.54 1 -23 0 325.11 20.93 -1 -23 0 325.60 21.42 -1 23 0 302.79 21.02 -1 23 0 359.39 23.30 1 23 0 335.86 23.15 1 -23 0 348.66 22.00 1 23 0 316.97 22.62 1 -23 0 338.79 20.86 -1 23 0 355.31 22.86 -1 23 0 370.11 22.76 -1 -23 0 345.58 21.81 -2 -23 0 381.29 23.61 2 23 0 420.44 37.07 2 23 0 410.35 34.18 2 -23 0 453.92 25.71 -2 -23 0 356.76 23.77 2 23 0 380.83 26.25 2 -23 0 391.11 23.92 -2 23 0 408.78 25.08 -2 -23 0 436.90 25.52 -2 23 0 385.93 26.31 2 23 0 436.39 27.10 -2 -23 0 460.01 25.82 2 23 0 412.15 24.55 2 -23 0 396.57 24.46 -2 23 0 438.09 26.42 3 -23 0 132.56 10.79 3 23 0 186.55 20.55 -3 -23 0 145.33 16.37 -3 -23 0 123.01 10.14 -3 -23 0 147.27 11.55 -3 23 0 149.36 12.79 -3 23 0 137.60 11.09 3 -23 0 142.32 11.44 3 23 0 127.59 12.15 -3 -23 0 130.11 10.43 -3 -23 0 153.36 11.72 3 23 0 159.35 13.53 3 -23 0 135.15 9.44 -3 23 0 156.80 12.42 3 -23 0 119.82 9.75 4 -23 0 559.24 31.10 -4 23 0 468.43 37.88 4 23 0 499.73 40.93 -4 -23 0 535.08 31.26 -4 23 0 513.34 32.06 4 -23 0 518.65 31.33 -4 23 0 516.84 31.07 4 23 0 515.84 32.32 4 23 0 519.15 32.30 4 -23 0 500.76 29.25 -4 -23 0 512.15 31.02 4 23 0 577.29 33.63 -4 23 0 543.67 31.75 -5 23 0 124.58 15.23 5 -23 0 130.07 10.60 5 -23 0 135.06 10.94 -5 -23 0 148.46 11.80 -5 -23 0 151.34 11.21 -5 23 0 142.05 11.99 5 23 0 139.99 11.79 -5 23 0 148.50 11.15 5 23 0 135.33 11.85 -5 -23 0 145.46 10.82 5 -23 0 141.66 9.66 -5 23 0 127.49 11.05 6 23 0 123.23 9.55 -6 23 0 123.61 10.15 -6 -23 0 125.81 10.17 -6 23 0 132.25 9.69 -6 -23 0 119.66 9.43 -6 -23 0 107.99 8.62 6 -23 0 125.92 9.45 7 -23 0 1.77 2.10 7 23 0 0.89 2.17 -7 -23 0 2.16 2.40 -7 23 0 -1.15 2.26 -7 23 0 -0.35 2.87 -7 -23 0 2.81 2.40 7 23 0 -1.67 2.91 7 -23 0 1.23 1.77 -8 -23 0 67.61 4.64 8 23 0 56.59 4.67 0 24 0 259.13 27.24 0 24 0 266.36 19.49 0 24 0 246.75 18.69 0 -24 0 287.12 18.22 1 24 0 104.37 15.08 -1 24 0 107.67 17.12 1 24 0 132.00 19.13 1 24 0 135.67 12.29 -1 24 0 109.73 11.48 1 -24 0 119.25 9.83 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11.86 -5 24 0 142.62 10.85 -5 -24 0 135.04 10.53 5 -24 0 139.02 10.95 5 -24 0 155.57 9.81 -5 24 0 148.07 11.31 5 -24 0 155.71 11.15 6 -24 0 16.75 3.40 -6 -24 0 15.73 3.42 -6 -24 0 16.73 3.93 -6 24 0 18.02 4.05 -6 24 0 13.72 3.17 -6 -24 0 12.69 2.68 6 -24 0 16.38 2.75 -7 24 0 0.87 2.23 -7 24 0 0.39 1.62 -7 -24 0 -0.25 1.91 -7 -24 0 1.70 1.90 7 24 0 2.34 2.16 0 25 0 -6.69 7.27 0 25 0 2.17 4.39 0 -25 0 5.56 3.65 0 -25 0 3.18 3.68 0 25 0 3.94 4.32 1 -25 0 2.99 2.87 1 25 0 4.65 7.27 1 25 0 5.14 5.36 -1 25 0 -2.13 7.69 -1 -25 0 0.46 2.78 -1 -25 0 5.84 3.69 1 -25 0 2.68 3.02 -1 25 0 2.84 4.50 1 25 0 9.44 4.78 1 -25 0 5.91 3.80 1 25 0 4.14 4.45 -1 -25 0 2.74 3.77 2 25 0 50.14 12.83 2 25 0 37.86 9.69 -2 -25 0 57.82 6.31 -2 -25 0 41.27 5.20 2 25 0 54.37 7.37 -2 25 0 49.81 7.40 -2 -25 0 52.81 6.62 -2 25 0 43.06 5.54 2 -25 0 45.66 6.25 2 25 0 52.70 7.87 2 -25 0 54.60 5.95 -2 -25 0 49.07 6.51 2 -25 0 52.95 5.88 -2 25 0 53.69 7.31 3 25 0 -1.82 4.94 -3 -25 0 4.97 2.58 -3 -25 0 -1.90 2.65 -3 25 0 2.62 4.27 -3 25 0 1.33 2.73 3 25 0 -2.53 4.00 3 -25 0 9.69 4.13 -3 -25 0 0.53 3.43 -3 -25 0 -1.07 3.71 3 25 0 6.42 4.91 -3 25 0 5.93 4.51 -3 25 0 -3.04 3.43 4 -25 0 9.46 3.42 -4 -25 0 6.17 2.89 4 25 0 4.00 3.91 -4 -25 0 1.95 3.72 -4 25 0 6.20 3.00 -4 25 0 4.75 4.66 4 -25 0 2.46 3.10 4 25 0 8.17 4.26 -4 25 0 15.17 4.44 -4 25 0 6.28 3.31 5 -25 0 1.60 2.84 -5 25 0 8.02 3.87 -5 25 0 6.26 2.79 -5 -25 0 10.74 3.77 5 -25 0 14.27 2.97 5 -25 0 8.53 3.23 5 25 0 12.03 3.54 -5 25 0 8.96 3.66 6 -25 0 169.37 10.26 -6 25 0 167.22 11.18 -6 -25 0 169.69 11.16 -6 -25 0 161.90 10.37 6 25 0 179.30 10.76 -6 25 0 141.91 9.82 6 25 0 178.25 11.71 6 -25 0 167.91 10.69 -6 25 0 154.48 10.47 -7 -25 0 37.74 3.62 -7 -25 0 38.14 3.43 -7 25 0 36.61 3.70 7 25 0 40.98 3.98 0 26 0 15.15 5.45 0 -26 0 23.14 4.52 0 26 0 21.81 5.35 0 -26 0 16.83 4.38 1 26 0 87.17 15.04 -1 26 0 51.31 12.48 1 26 0 87.70 9.17 1 -26 0 90.29 8.29 -1 -26 0 93.60 8.34 -1 26 0 73.98 8.89 -1 -26 0 77.87 7.44 -1 -26 0 88.92 8.35 1 26 0 83.55 9.12 2 -26 0 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-3 -3 1773.37 94.62 3 3 -3 147.60 12.96 3 3 -3 144.83 11.38 -3 3 3 145.44 8.87 3 -3 -3 147.82 11.44 -3 -3 3 138.92 11.16 -3 -3 3 126.67 11.95 3 -3 -3 139.41 9.43 2 3 -3 527.18 30.96 -2 3 3 514.55 30.14 -2 -3 3 508.45 30.42 2 3 -3 469.19 27.05 2 -3 -3 520.38 27.44 1 3 -3 42.54 5.88 -1 3 3 41.21 3.21 -1 -3 3 41.47 5.11 1 3 -3 42.47 5.67 -1 3 3 38.21 3.50 -1 -3 3 46.50 5.90 -1 -3 3 45.74 4.85 -1 -3 3 39.95 5.29 -1 3 3 45.24 5.72 -1 3 3 48.02 4.71 1 -3 -3 44.08 6.00 1 -3 -3 36.07 3.73 0 3 -3 16.67 4.37 0 3 3 8.15 1.63 0 3 -3 6.45 2.90 0 -3 3 9.78 3.64 0 3 3 13.06 4.20 0 3 3 7.92 3.77 0 -3 3 9.87 4.49 0 3 3 9.78 1.72 0 3 3 10.18 4.10 0 -3 3 8.44 3.25 0 3 -3 10.27 2.84 0 -3 -3 9.61 2.38 0 -3 -3 12.36 3.15 0 -3 -3 9.67 3.26 0 3 -3 10.06 1.81 0 -3 3 12.94 2.04 0 -3 -3 10.55 3.56 0 -3 3 10.62 3.61 1 -3 3 462.39 29.39 1 3 3 423.62 27.57 -1 -3 -3 457.83 27.01 1 3 3 529.09 30.03 1 3 3 448.03 28.48 1 3 3 438.93 28.35 1 -3 3 452.08 28.04 -1 -3 -3 446.03 26.44 1 3 3 429.60 24.38 1 -3 3 462.53 24.48 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3 58.22 5.24 -4 3 -3 46.99 5.04 -4 -3 -3 50.71 7.87 4 -3 3 44.77 9.14 4 3 3 62.97 10.71 4 -3 3 56.17 10.37 -4 -3 -3 66.82 9.20 4 3 3 56.96 8.75 -4 3 -3 52.52 8.23 4 -3 3 57.81 9.62 4 3 3 55.62 5.63 -4 -3 -3 54.10 6.20 4 -3 3 49.09 5.05 4 3 3 57.73 6.74 -4 3 -3 56.62 5.16 -4 -3 -3 52.06 4.79 -5 -3 -3 84.08 10.35 -5 3 -3 92.91 10.96 -5 3 -3 96.13 7.65 -5 -3 -3 82.41 10.50 -5 -3 -3 93.59 7.61 5 -3 3 90.90 7.17 5 -3 3 84.51 13.14 5 -3 3 100.08 13.34 5 3 3 108.70 12.55 5 3 3 81.92 13.28 5 3 3 120.80 15.65 -5 3 -3 97.86 12.20 5 -3 3 97.48 12.63 -5 -3 -3 87.32 11.87 5 -3 3 107.04 11.18 5 -3 3 112.87 13.92 -5 -3 -3 83.83 7.89 5 3 3 88.72 8.90 5 3 3 83.73 7.85 5 -3 3 93.43 7.98 -5 -3 -3 83.59 8.74 5 -3 3 94.32 8.80 5 3 3 94.90 9.18 -5 3 -3 78.69 7.17 5 -3 3 93.99 7.50 -5 -3 -3 96.99 7.25 5 -3 3 75.06 6.87 -6 -3 -3 268.46 22.64 -6 3 -3 304.41 18.86 -6 3 -3 323.03 24.05 -6 -3 -3 305.13 25.23 -6 -3 -3 282.34 18.78 6 -3 3 294.61 17.80 -6 3 -3 281.08 22.32 6 -3 3 295.43 24.34 6 3 3 351.60 28.30 6 3 3 274.34 23.53 -6 -3 -3 295.04 25.81 -6 3 -3 274.42 24.82 6 3 3 285.09 26.96 6 3 3 335.85 26.34 6 -3 3 292.09 23.30 6 3 3 316.01 20.55 6 3 3 294.45 19.27 -6 -3 -3 326.15 20.76 -6 3 -3 307.91 19.76 6 -3 3 319.82 19.12 6 3 3 284.71 20.48 6 3 3 291.26 18.29 -6 3 -3 314.74 18.76 6 -3 3 292.78 18.44 -6 -3 -3 287.47 18.20 6 -3 3 294.48 18.03 6 -3 3 294.45 20.09 -7 3 -3 521.99 36.91 -7 3 -3 574.50 32.96 -7 -3 -3 587.08 33.14 -7 3 -3 614.13 40.05 7 3 3 509.62 39.62 -7 3 -3 656.92 41.83 -7 -3 -3 608.42 41.63 -7 3 -3 526.48 33.17 7 3 3 611.66 34.69 7 3 3 578.48 33.36 -7 3 -3 572.20 33.90 7 3 3 618.42 35.04 7 -3 3 563.11 33.11 7 3 3 519.00 31.72 -7 3 -3 594.00 32.87 -7 -3 -3 592.09 32.49 7 -3 3 564.03 34.20 -8 -3 -3 96.53 11.66 -8 -3 -3 89.64 11.89 -8 3 -3 100.10 7.94 -8 3 -3 116.12 12.62 -8 -3 -3 98.06 8.00 -8 -3 -3 97.78 8.47 -8 3 -3 108.30 8.93 -8 -3 -3 91.79 8.42 8 -3 3 89.19 7.62 -8 -3 -3 96.11 7.37 8 -3 3 92.03 7.46 8 -3 3 87.21 8.68 8 3 3 89.75 8.93 -9 3 -3 17.20 2.85 -9 -3 -3 18.39 2.97 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116.16 8.97 8 4 -3 106.70 8.14 8 4 -3 112.35 10.59 8 -4 -3 121.70 9.57 8 -4 -3 105.19 8.41 8 4 -3 133.08 10.30 8 -4 -3 107.23 9.68 -7 -4 3 143.54 13.62 -7 4 3 147.25 13.67 7 4 -3 140.69 16.12 7 4 -3 193.24 17.33 -7 -4 3 156.49 14.16 7 -4 -3 155.80 15.21 -7 4 3 145.16 13.42 -7 4 3 162.25 13.35 -7 -4 3 166.85 16.05 7 4 -3 160.54 12.41 7 4 -3 164.05 11.15 7 -4 -3 161.01 10.87 7 4 -3 144.84 10.17 7 -4 -3 186.59 11.99 7 -4 -3 156.64 11.87 7 4 -3 169.76 12.24 7 4 -3 157.62 10.52 7 4 -3 164.98 12.81 7 -4 -3 143.09 10.57 7 -4 -3 162.94 11.46 7 -4 -3 147.52 11.58 -6 4 3 215.05 13.10 -6 4 3 202.71 16.00 6 -4 -3 225.74 14.76 6 4 -3 238.53 18.89 -6 -4 3 214.64 16.70 6 -4 -3 229.58 17.84 -6 4 3 194.82 15.23 -6 4 3 213.08 15.89 -6 4 3 217.85 15.70 -6 -4 3 229.22 16.76 -5 -4 3 1201.90 67.72 5 4 -3 1200.18 71.23 5 4 -3 1256.01 68.97 -5 -4 3 1226.75 68.75 -5 -4 3 1261.67 70.39 -5 4 3 1157.55 65.96 5 -4 -3 1222.29 68.26 -5 4 3 1233.40 66.22 -5 -4 3 1188.26 67.88 4 -4 -3 1288.56 69.34 4 4 -3 1308.03 72.02 -4 -4 3 1289.48 70.76 4 4 -3 1257.59 69.35 -4 4 3 1188.43 66.48 4 -4 -3 1252.80 66.44 3 4 -3 224.16 17.26 3 4 -3 242.52 15.69 -3 -4 3 224.82 15.60 3 -4 -3 226.81 15.59 -3 -4 3 261.85 17.22 -3 4 3 205.65 12.68 -3 4 3 215.76 13.16 3 -4 -3 230.51 13.66 -2 -4 3 88.13 8.04 2 4 -3 64.82 7.97 -2 -4 3 71.54 7.35 -2 4 3 75.33 7.55 -2 -4 3 72.72 7.11 2 -4 -3 73.44 5.70 1 4 -3 343.13 21.38 -1 -4 3 341.46 20.77 -1 4 3 319.92 18.49 1 4 -3 320.64 21.71 -1 -4 3 302.24 20.67 -1 -4 3 321.53 19.70 -1 4 3 341.35 20.26 -1 4 3 352.84 21.13 -1 -4 3 330.22 19.31 -1 4 3 314.86 21.08 -1 4 3 325.65 19.78 1 4 -3 304.68 17.78 -1 -4 3 326.88 20.32 1 -4 -3 346.99 19.31 1 -4 -3 333.59 21.61 1 -4 -3 328.27 18.41 0 -4 3 698.26 36.45 0 4 3 668.35 37.68 0 4 3 659.02 37.58 0 -4 3 634.97 37.09 0 4 -3 635.50 37.88 0 4 3 580.04 33.03 0 -4 -3 627.09 36.35 0 -4 3 591.35 36.22 0 -4 -3 622.98 33.70 0 -4 -3 699.53 37.97 0 -4 3 627.69 33.45 0 4 -3 646.52 36.20 1 4 3 138.59 11.36 1 4 3 115.09 11.44 1 -4 3 126.68 8.02 1 4 3 109.85 11.50 1 4 3 141.79 12.50 1 -4 3 128.09 12.46 1 4 3 118.19 9.11 -1 -4 -3 121.47 9.41 1 -4 3 121.23 11.11 1 -4 3 132.01 8.06 -1 4 -3 119.73 7.91 1 -4 3 121.96 8.15 -1 4 -3 133.13 10.72 -1 -4 -3 117.14 11.37 2 -4 3 2102.27 104.73 2 -4 3 2122.93 111.14 2 -4 3 2064.08 109.56 -2 -4 -3 1890.63 106.66 2 4 3 2093.52 110.21 2 4 3 2066.31 110.68 2 4 3 1970.14 109.42 -2 4 -3 1968.07 108.73 -2 -4 -3 2013.10 108.45 2 -4 3 2117.75 104.78 -2 4 -3 1947.90 108.20 2 4 3 2014.49 110.03 -2 -4 -3 1870.96 109.28 -2 4 -3 1975.01 107.08 2 -4 3 2022.24 105.03 2 4 3 1965.10 105.31 -2 4 -3 1979.95 108.36 -2 4 -3 1968.68 104.63 -2 4 -3 1949.95 104.60 3 -4 3 47.88 8.51 -3 -4 -3 45.24 7.12 3 -4 3 46.53 8.79 3 4 3 49.71 8.24 -3 4 -3 39.48 6.84 3 -4 3 42.27 7.72 3 4 3 48.62 8.24 -3 -4 -3 33.39 5.13 3 4 3 44.30 4.87 -3 4 -3 32.86 6.19 3 4 3 38.98 7.60 -3 4 -3 41.90 4.07 3 4 3 41.00 5.10 3 -4 3 44.40 4.87 -3 -4 -3 37.95 4.03 -3 4 -3 36.04 5.54 3 -4 3 30.94 3.92 3 -4 3 38.51 4.86 3 4 3 40.36 5.35 -3 4 -3 41.12 4.20 -4 -4 -3 42.51 6.33 -4 4 -3 52.63 7.42 -4 4 -3 35.95 4.36 -4 -4 -3 43.90 7.53 -4 -4 -3 40.19 4.42 -4 4 -3 46.49 6.57 4 4 3 50.04 5.64 4 -4 3 44.19 4.08 4 -4 3 41.55 8.81 4 -4 3 42.27 8.54 4 -4 3 37.73 8.92 -4 -4 -3 50.39 8.35 4 4 3 49.50 8.34 -4 4 -3 37.15 7.15 4 4 3 42.33 5.06 -4 -4 -3 40.31 5.57 4 4 3 36.04 5.66 -4 4 -3 40.49 4.41 -5 -4 -3 44.29 7.29 -5 4 -3 44.11 7.19 -5 4 -3 56.79 8.25 -5 4 -3 66.94 5.77 -5 -4 -3 48.59 5.34 -5 -4 -3 34.64 7.35 5 -4 3 47.17 4.98 5 4 3 53.02 11.23 5 -4 3 41.67 10.14 5 -4 3 56.65 10.28 5 4 3 42.83 10.45 5 -4 3 58.66 8.17 5 -4 3 55.36 9.88 5 4 3 47.69 8.58 -5 -4 -3 51.44 9.38 -5 4 -3 42.91 8.59 5 4 3 57.09 7.07 5 4 3 45.73 5.79 5 -4 3 44.90 5.36 -5 -4 -3 54.84 6.08 -5 -4 -3 46.22 6.45 5 -4 3 44.61 6.50 5 4 3 34.82 6.11 5 -4 3 50.19 5.38 -5 4 -3 51.34 5.34 5 -4 3 41.59 4.90 -5 -4 -3 57.57 5.13 -6 -4 -3 354.37 25.40 -6 4 -3 310.50 24.83 -6 -4 -3 355.73 28.32 -6 -4 -3 336.06 21.05 -6 4 -3 339.38 20.94 -6 4 -3 313.88 24.63 -6 4 -3 371.51 27.50 6 4 3 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17.34 3.84 1 3 -9 11.22 4.05 -1 3 9 11.85 3.03 1 -3 -9 7.90 3.18 1 3 -9 14.45 3.83 1 3 -9 6.74 2.69 1 -3 -9 12.24 3.42 0 3 9 532.93 31.98 0 -3 9 572.31 32.00 0 3 -9 571.75 33.03 0 3 9 508.20 30.67 0 -3 9 560.58 31.82 0 -3 -9 599.26 32.01 0 3 -9 560.98 32.07 1 3 9 132.17 9.85 1 -3 9 129.19 9.53 -1 -3 -9 119.14 8.98 -1 3 -9 138.35 10.30 1 3 9 123.76 8.55 1 -3 9 129.00 9.27 -1 -3 -9 116.36 9.12 -1 3 -9 142.84 9.78 -1 -3 -9 117.08 8.66 2 -3 9 56.06 4.81 -2 3 -9 47.06 5.13 2 3 9 49.48 4.05 2 3 9 46.60 4.35 -2 -3 -9 46.41 4.50 -2 3 -9 61.58 5.08 2 -3 9 47.41 4.39 -2 -3 -9 38.57 3.53 2 -3 9 47.51 4.51 -3 3 -9 4.37 1.71 -3 -3 -9 4.32 1.48 -3 3 -9 7.41 1.78 3 -3 9 6.04 1.65 3 3 9 5.57 1.77 9 4 -9 22.96 3.02 8 -4 -9 0.30 2.12 8 4 -9 0.32 2.25 7 -4 -9 52.39 5.46 7 4 -9 50.21 5.55 7 -4 -9 54.47 5.67 -6 4 9 2.71 4.59 -6 -4 9 5.02 2.34 6 4 -9 12.88 3.97 6 4 -9 13.86 3.37 6 -4 -9 6.74 2.94 6 4 -9 2.68 2.87 6 -4 -9 9.28 3.74 -5 4 9 83.85 12.36 -5 -4 9 87.04 7.69 5 4 -9 93.89 8.05 5 -4 -9 87.80 8.28 5 4 -9 105.05 9.43 5 -4 -9 101.00 8.44 5 4 -9 108.13 8.78 5 -4 -9 98.71 8.46 5 -4 -9 93.84 8.51 -4 -4 9 74.54 6.47 -4 4 9 67.12 11.64 -4 -4 9 64.54 5.87 -4 -4 9 54.88 5.92 -4 4 9 51.68 10.16 4 4 -9 72.46 7.75 4 -4 -9 56.06 6.38 4 -4 -9 64.17 6.53 4 -4 -9 73.05 7.03 4 -4 -9 65.32 6.89 -3 -4 9 27.67 4.14 -3 -4 9 21.28 3.74 -3 4 9 19.09 7.29 3 4 -9 18.31 4.69 3 4 -9 24.12 4.42 3 -4 -9 27.50 4.69 -2 4 9 234.39 24.04 -2 -4 9 261.32 16.95 -2 4 9 241.61 23.58 2 4 -9 277.80 18.61 2 -4 -9 278.56 17.32 2 4 -9 279.86 17.63 2 -4 -9 252.13 17.42 -1 4 9 1.68 6.46 -1 -4 9 3.21 2.21 -1 4 9 0.51 3.02 -1 -4 9 -2.25 2.94 -1 4 9 3.83 2.73 1 -4 -9 -2.19 2.83 1 4 -9 6.84 3.97 1 -4 -9 3.07 2.71 1 4 -9 4.78 3.06 1 -4 -9 4.33 3.20 0 4 9 257.40 16.75 0 -4 9 281.78 16.53 0 -4 -9 242.58 15.79 0 4 -9 290.30 17.79 0 4 9 237.16 15.36 0 -4 9 256.45 16.24 0 -4 -9 258.43 16.10 0 4 -9 229.65 16.06 0 -4 -9 229.09 15.84 1 4 9 26.64 4.25 1 -4 9 20.48 3.66 -1 4 -9 24.67 4.41 1 4 9 17.49 3.19 -1 -4 -9 30.92 3.83 -1 4 -9 22.05 3.68 1 -4 9 20.01 3.50 1 -4 9 22.01 3.47 -1 -4 -9 19.27 3.21 2 -4 9 10.69 2.53 -2 4 -9 6.68 2.77 2 4 9 7.33 2.11 2 -4 9 10.14 2.39 -2 -4 -9 8.38 2.17 -2 4 -9 6.36 2.30 2 4 9 8.68 2.23 2 -4 9 6.86 2.22 -2 -4 -9 2.75 1.43 -3 4 -9 13.88 2.40 -3 -4 -9 6.83 1.58 -3 4 -9 9.92 1.93 3 -4 9 11.94 1.85 3 4 9 10.75 1.92 9 5 -9 12.92 2.51 8 5 -9 28.97 3.89 8 5 -9 18.66 3.19 8 -5 -9 25.04 3.37 7 -5 -9 107.24 8.05 7 5 -9 108.43 8.21 7 -5 -9 93.46 8.22 -6 -5 9 73.73 6.95 -6 5 9 77.67 11.87 6 5 -9 106.15 8.18 6 5 -9 81.68 8.19 6 -5 -9 94.25 7.63 6 5 -9 96.96 7.88 6 -5 -9 88.65 8.07 -5 5 9 25.19 7.66 -5 -5 9 27.90 4.10 5 5 -9 29.91 5.11 5 5 -9 26.19 4.29 5 -5 -9 23.94 4.17 5 5 -9 30.94 4.56 5 -5 -9 26.18 4.47 5 -5 -9 31.29 5.05 -4 -5 9 2.84 2.11 -4 -5 9 1.70 2.24 -4 5 9 1.57 5.31 4 5 -9 0.62 3.45 4 5 -9 2.97 2.49 4 -5 -9 0.90 2.59 4 -5 -9 1.55 2.87 4 -5 -9 -2.45 3.31 -3 5 9 1.74 6.14 -3 -5 9 25.33 3.73 -3 -5 9 20.54 3.62 -3 5 9 -1.64 5.78 3 5 -9 13.93 4.39 3 -5 -9 17.04 4.08 -2 5 9 7.00 6.13 2 -5 -9 7.60 2.98 -2 5 9 -2.65 3.54 -2 -5 9 2.98 2.81 -2 -5 9 6.11 2.66 -2 5 9 1.66 6.00 2 -5 -9 12.31 3.41 2 5 -9 8.18 3.70 2 -5 -9 3.02 2.69 2 5 -9 11.43 3.37 2 -5 -9 7.34 3.36 2 -5 -9 6.84 2.76 -1 5 9 224.70 22.75 -1 5 9 225.73 16.26 -1 -5 9 239.45 15.73 1 -5 -9 265.85 15.77 1 5 -9 254.97 17.17 1 5 -9 226.95 15.96 -1 -5 9 239.71 15.76 1 -5 -9 246.92 15.69 1 5 -9 246.52 15.97 1 -5 -9 234.16 16.15 0 5 9 232.50 16.46 0 -5 9 278.35 16.37 0 -5 -9 233.73 15.38 0 5 -9 276.92 17.50 0 5 9 233.63 15.45 0 -5 9 265.81 16.16 0 -5 -9 264.96 15.89 0 5 -9 252.55 16.12 0 -5 -9 238.60 16.08 1 5 9 36.44 5.13 1 -5 9 51.80 5.01 -1 5 -9 50.49 5.67 1 5 9 42.69 4.50 1 -5 9 33.17 4.37 -1 -5 -9 46.28 4.62 -1 5 -9 43.30 4.82 1 -5 9 40.33 4.25 -2 5 -9 17.90 3.53 2 5 9 21.29 2.81 -2 -5 -9 20.00 2.76 -2 5 -9 22.55 3.04 2 -5 9 20.98 2.97 -2 -5 -9 22.35 2.55 2 -5 9 28.69 3.29 -3 5 -9 40.75 3.84 -3 5 -9 35.89 3.25 3 -5 9 40.78 3.25 3 5 9 39.25 3.17 9 6 -9 18.00 2.76 8 6 -9 57.61 5.43 8 -6 -9 49.79 4.94 7 6 -9 67.78 6.36 7 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18.68 2.61 8 8 -9 68.69 5.82 8 -8 -9 53.51 5.05 7 8 -9 130.32 9.42 7 -8 -9 106.20 7.88 7 -8 -9 124.34 9.11 6 8 -9 168.85 12.27 6 8 -9 178.38 12.05 6 -8 -9 163.72 11.00 6 -8 -9 164.31 12.19 -5 -8 9 18.21 3.45 5 8 -9 18.08 3.89 5 -8 -9 24.05 3.43 5 -8 -9 22.12 3.88 5 -8 -9 21.47 4.36 -4 8 9 3.52 5.95 -4 8 9 -2.85 2.90 -4 -8 9 0.87 2.42 4 8 -9 6.82 3.25 4 8 -9 -1.44 2.98 -4 -8 9 -0.56 2.14 4 -8 -9 5.29 2.67 4 -8 -9 3.97 2.66 4 -8 -9 4.32 3.24 -3 8 9 10.79 6.90 -3 8 9 3.94 2.83 -3 -8 9 6.01 2.42 -3 -8 9 2.65 2.50 3 8 -9 2.71 2.99 3 8 -9 2.24 2.83 3 -8 -9 3.94 2.60 -3 -8 9 2.71 2.40 3 -8 -9 6.81 3.42 -2 8 9 53.37 10.70 2 -8 -9 48.21 5.88 -2 -8 9 48.60 5.46 -2 8 9 49.28 6.47 -2 8 9 51.75 5.85 -2 -8 9 51.21 5.13 2 8 -9 59.44 6.40 -2 -8 9 42.15 3.98 2 -8 -9 40.13 5.57 2 -8 -9 48.62 5.11 -1 8 9 -3.39 6.67 -1 8 9 0.52 3.22 -1 -8 9 5.30 2.50 1 8 -9 4.64 3.30 1 -8 -9 2.50 2.06 -1 -8 9 2.19 2.58 -1 -8 9 2.60 2.03 1 -8 -9 4.88 2.99 0 -8 9 21.34 3.58 0 8 9 24.30 4.52 0 -8 9 19.25 3.41 0 8 -9 19.55 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-2 9 9 36.70 9.79 2 -9 -9 36.38 5.26 -2 9 9 36.79 5.69 -2 9 9 38.64 5.11 -2 -9 9 34.17 4.26 -2 -9 9 39.15 4.81 2 9 -9 40.25 5.20 2 -9 -9 44.02 5.48 2 -9 -9 31.83 4.34 -2 -9 9 41.32 4.62 -1 9 9 26.13 8.52 -1 -9 9 39.51 4.67 -1 9 9 43.92 5.59 -1 -9 9 32.05 4.26 1 9 -9 46.50 5.37 -1 -9 9 34.94 4.28 -1 -9 9 24.71 3.05 1 -9 -9 40.28 5.06 0 -9 9 2.72 2.22 0 9 9 0.45 3.16 0 -9 9 5.61 2.54 0 9 -9 8.60 2.97 0 -9 -9 5.47 2.61 0 9 9 6.06 2.78 0 -9 9 3.20 2.27 0 9 -9 2.02 1.91 0 -9 9 4.28 1.84 0 -9 -9 3.32 2.74 1 9 9 39.87 4.76 1 -9 9 42.84 4.23 -1 9 -9 49.70 4.91 1 9 9 37.35 4.34 -1 -9 -9 34.10 4.23 -1 9 -9 35.81 3.59 1 -9 9 33.15 3.33 -1 -9 -9 37.22 4.22 1 -9 9 47.02 4.30 -2 9 -9 1.99 1.74 -2 9 -9 1.53 1.68 2 9 9 4.60 1.89 -2 9 -9 1.10 1.12 2 -9 9 1.95 1.28 -2 -9 -9 -0.19 1.37 9 10 -9 31.38 2.92 8 10 -9 11.42 2.72 8 -10 -9 9.25 2.36 7 10 -9 19.93 3.90 7 -10 -9 15.36 3.42 6 10 -9 4.22 3.12 6 10 -9 1.03 1.87 6 -10 -9 6.92 3.30 -5 10 9 -4.89 4.88 -5 -10 9 -0.28 1.97 -5 10 9 5.07 2.71 -5 -10 9 0.38 1.99 5 10 -9 1.00 3.09 5 10 -9 0.89 2.04 5 -10 -9 -0.46 3.14 -4 10 9 25.52 8.17 -4 -10 9 33.85 4.35 -4 10 9 32.11 4.64 -4 -10 9 26.91 4.00 4 10 -9 39.84 4.94 4 10 -9 37.47 4.18 4 -10 -9 34.13 4.59 4 -10 -9 36.47 5.05 -3 -10 9 24.40 3.98 -3 10 9 23.39 4.30 -3 -10 9 27.07 3.27 -3 -10 9 27.15 3.95 3 10 -9 20.34 3.98 3 10 -9 26.43 4.56 3 -10 -9 26.29 4.34 -3 -10 9 26.40 3.46 3 10 -9 30.01 3.80 3 -10 -9 29.95 4.54 -2 10 9 8.32 6.37 -2 -10 9 3.49 2.74 -2 10 9 -1.55 3.13 -2 10 9 -0.47 2.97 -2 -10 9 2.80 2.14 -2 -10 9 0.39 2.24 2 10 -9 3.23 2.51 2 -10 -9 6.02 2.80 -2 -10 9 1.56 2.18 2 -10 -9 3.47 3.07 2 -10 -9 0.32 2.37 -1 10 9 24.62 7.71 -1 -10 9 23.92 3.81 -1 10 9 12.57 4.06 -1 -10 9 22.97 3.57 1 10 -9 26.98 4.50 1 10 -9 28.95 4.25 1 10 -9 24.01 3.29 1 -10 -9 25.60 4.25 0 -10 9 0.97 2.22 0 10 9 -2.97 3.09 0 -10 9 -2.16 2.18 0 10 -9 4.63 2.66 0 10 -9 -1.95 2.57 0 -10 -9 -0.38 2.14 0 10 9 -2.81 2.78 0 10 -9 0.74 1.76 0 -10 9 -1.04 1.53 0 -10 -9 1.61 2.33 0 -10 9 0.60 2.11 1 10 9 4.05 2.39 -1 10 -9 7.61 2.45 -1 10 -9 4.58 2.28 1 10 9 3.42 2.42 -1 -10 -9 3.49 2.14 -1 10 -9 2.18 1.43 1 -10 9 1.45 1.51 -1 -10 -9 6.16 2.14 1 -10 9 4.34 2.09 -2 10 -9 -0.22 1.41 2 10 9 2.28 1.65 2 10 9 1.61 1.19 8 11 -9 4.52 1.94 8 -11 -9 1.07 1.68 7 11 -9 13.50 3.49 7 -11 -9 12.86 3.07 6 11 -9 49.76 5.80 6 11 -9 44.90 4.05 6 -11 -9 52.24 5.66 -5 -11 9 18.56 2.89 -5 11 9 14.64 3.38 5 11 -9 14.26 3.07 5 11 -9 15.86 3.87 5 11 -9 17.17 2.75 5 -11 -9 19.63 4.10 -4 11 9 6.46 5.46 -4 -11 9 -0.98 2.32 -4 11 9 4.82 2.80 -4 -11 9 3.77 2.31 4 11 -9 1.50 3.29 4 11 -9 2.19 1.89 4 -11 -9 2.38 2.32 4 -11 -9 3.06 2.88 -3 11 9 34.05 9.35 -3 -11 9 53.90 5.48 -3 -11 9 63.15 5.74 -3 11 9 51.15 5.91 3 -11 -9 54.04 6.10 3 11 -9 54.07 4.92 3 -11 -9 62.59 6.30 -3 -11 9 58.78 4.78 3 -11 -9 48.85 5.62 -2 11 9 6.24 5.64 -2 -11 9 -0.37 2.58 -2 11 9 3.41 3.17 -2 11 9 0.93 2.81 -2 -11 9 -0.57 1.99 2 11 -9 1.25 2.71 2 11 -9 -0.84 2.51 2 -11 -9 1.67 2.51 -2 -11 9 0.57 2.17 2 -11 -9 0.46 2.60 2 -11 -9 -1.45 2.40 -1 -11 9 84.86 6.93 -1 11 9 68.65 7.39 -1 -11 9 81.69 6.57 1 11 -9 90.11 7.35 1 11 -9 76.55 7.41 1 -11 -9 90.13 7.58 0 -11 9 84.66 6.65 0 11 9 73.23 6.95 0 11 -9 83.49 6.87 0 11 -9 85.05 7.21 0 -11 -9 79.59 6.69 0 11 9 79.64 6.83 0 -11 9 89.54 6.55 0 -11 -9 76.24 6.95 -1 11 -9 9.74 2.42 -1 11 -9 6.87 2.30 1 11 9 14.72 2.71 -1 -11 -9 8.89 2.35 1 -11 9 8.33 2.14 -1 -11 -9 4.25 2.03 -2 11 -9 33.57 3.27 2 11 9 43.46 3.47 8 12 -9 16.55 2.66 8 -12 -9 16.18 2.24 7 12 -9 39.76 4.55 7 -12 -9 42.13 4.53 6 12 -9 24.59 4.15 6 -12 -9 25.45 4.19 5 12 -9 269.53 15.99 5 12 -9 233.89 14.19 5 -12 -9 253.61 15.33 -4 -12 9 245.99 14.24 -4 12 9 204.34 14.70 4 -12 -9 237.76 15.33 4 12 -9 263.42 15.89 4 12 -9 213.59 14.21 4 12 -9 207.39 13.27 4 -12 -9 258.26 14.68 4 -12 -9 213.68 14.69 -3 -12 9 -0.67 2.81 -3 12 9 2.23 2.96 3 -12 -9 0.45 2.81 3 12 -9 -1.37 1.73 3 -12 -9 -0.40 2.21 3 -12 -9 4.69 2.61 -2 -12 9 229.49 12.97 -2 12 9 182.58 13.31 -2 12 9 169.87 13.03 2 12 -9 220.90 13.49 2 -12 -9 196.30 12.96 2 12 -9 174.02 11.49 2 -12 -9 224.86 13.47 -2 -12 9 204.34 11.97 2 -12 -9 163.99 11.60 -1 -12 9 50.88 4.86 -1 12 9 41.51 5.22 1 12 -9 37.31 3.60 -1 -12 9 36.99 4.07 1 -12 -9 53.34 5.35 0 -12 9 9.17 2.47 0 12 9 9.50 2.94 0 12 -9 15.15 3.31 0 12 9 15.03 2.98 0 -12 -9 7.80 2.68 0 -12 9 14.16 2.57 -1 12 -9 66.65 5.21 -1 12 -9 63.13 5.47 1 12 9 65.71 5.32 -1 -12 -9 66.65 5.33 2 12 9 70.22 4.71 8 13 -9 0.92 1.37 8 -13 -9 0.65 1.06 7 13 -9 34.52 4.14 7 -13 -9 40.29 4.08 6 13 -9 258.11 17.02 6 -13 -9 294.30 17.21 5 13 -9 23.87 4.23 5 -13 -9 23.26 4.04 -4 -13 9 6.51 2.23 -4 13 9 7.61 2.98 4 13 -9 6.01 2.19 4 13 -9 3.55 2.71 4 -13 -9 6.92 3.04 4 -13 -9 9.54 3.16 -3 13 9 126.27 9.73 3 -13 -9 137.78 9.88 3 13 -9 148.41 9.14 3 13 -9 110.33 7.61 3 -13 -9 139.39 9.34 3 -13 -9 119.21 8.85 -2 -13 9 4.47 2.57 -2 13 9 4.16 2.98 -2 13 9 0.42 2.68 2 13 -9 0.62 1.91 2 13 -9 0.76 2.78 2 -13 -9 3.42 2.66 2 13 -9 1.18 1.25 2 -13 -9 1.46 2.16 -2 -13 9 -0.22 1.68 2 -13 -9 0.60 1.73 -1 -13 9 5.40 2.35 -1 13 9 3.38 2.85 1 13 -9 3.76 2.08 -1 -13 9 3.23 1.79 1 -13 -9 3.83 2.19 0 -13 9 39.43 3.98 0 13 9 41.06 4.50 0 13 -9 40.12 4.59 0 13 9 33.63 4.11 0 -13 -9 42.76 4.32 -1 13 -9 5.12 1.90 -1 13 -9 3.19 1.36 1 13 9 6.38 1.96 -1 -13 -9 8.32 1.81 8 14 -9 22.34 2.22 7 14 -9 5.00 2.14 7 -14 -9 7.09 2.09 6 14 -9 1.99 2.20 6 -14 -9 -0.31 2.29 5 14 -9 31.41 4.41 5 -14 -9 27.48 3.97 4 -14 -9 40.94 5.02 4 14 -9 51.36 5.47 4 14 -9 41.28 3.90 4 -14 -9 49.50 4.29 4 -14 -9 49.80 5.05 -3 14 9 46.18 5.23 3 14 -9 45.98 5.21 3 -14 -9 46.04 5.12 3 14 -9 39.08 3.98 3 -14 -9 46.88 4.46 3 -14 -9 41.39 4.32 -2 -14 9 393.09 18.93 -2 14 9 327.09 19.28 2 14 -9 334.95 18.22 2 -14 -9 342.82 19.14 2 -14 -9 354.17 18.87 -1 -14 9 63.11 5.25 -1 14 9 66.72 5.81 1 14 -9 55.45 4.82 1 -14 -9 62.30 5.42 0 14 -9 9.58 1.89 0 14 9 11.56 2.53 0 -14 -9 9.10 2.13 1 14 9 60.23 4.71 -1 -14 -9 68.19 4.72 7 15 -9 49.65 4.17 7 -15 -9 51.52 4.06 6 15 -9 11.66 2.72 6 -15 -9 6.29 2.20 5 15 -9 40.79 4.57 5 -15 -9 39.13 4.26 4 15 -9 28.45 4.06 -3 -15 9 -0.96 1.69 -3 15 9 1.76 2.51 3 15 -9 1.94 1.26 3 15 -9 -0.35 2.29 3 -15 -9 0.35 2.14 3 -15 -9 0.22 1.97 -2 -15 9 18.03 2.79 -2 15 9 20.87 3.47 2 15 -9 15.01 2.06 2 -15 -9 20.03 3.12 2 -15 -9 17.50 2.68 1 15 -9 1.60 1.19 1 15 -9 0.24 1.89 1 -15 -9 0.75 1.45 0 15 9 18.50 2.62 0 -15 -9 15.72 2.41 1 15 9 6.11 1.39 -1 -15 -9 3.56 1.10 7 16 -9 1.16 1.00 7 -16 -9 2.21 1.03 6 16 -9 9.62 2.02 6 -16 -9 7.49 1.91 5 16 -9 18.21 2.93 5 -16 -9 15.95 2.68 4 16 -9 3.76 2.37 -4 -16 9 -0.31 1.36 3 16 -9 7.07 2.45 3 -16 -9 4.41 2.21 3 -16 -9 4.93 1.48 3 -16 -9 2.59 1.44 2 16 -9 10.50 2.55 2 -16 -9 9.70 2.33 2 -16 -9 12.23 2.17 -1 16 9 -0.22 2.02 1 16 -9 -0.19 1.56 1 -16 -9 1.19 1.51 0 16 9 10.37 1.98 0 -16 -9 11.36 1.74 0 -16 9 12.65 1.81 6 17 -9 -0.18 1.29 6 -17 -9 0.15 1.14 5 17 -9 47.48 4.38 5 -17 -9 50.10 4.04 4 17 -9 11.31 2.49 4 -17 -9 7.29 1.76 3 17 -9 3.88 2.11 2 17 -9 6.89 1.96 -2 -17 9 5.57 1.61 1 17 -9 9.61 1.66 -1 17 9 16.97 2.28 1 -17 -9 13.42 1.75 -1 -17 9 16.85 2.12 0 17 9 5.68 1.31 5 18 -9 16.32 2.19 5 -18 -9 13.92 1.75 4 18 -9 29.42 3.22 3 18 -9 0.20 1.47 -3 -18 9 0.24 1.09 2 18 -9 1.51 1.32 -2 -18 9 3.91 1.38 -1 18 9 44.11 3.73 -1 -18 9 61.88 3.78 4 19 -9 5.81 1.39 3 19 -9 13.39 1.79 -2 19 9 14.97 1.79 7 0 -10 27.20 3.57 6 0 -10 92.19 7.43 5 0 -10 0.82 2.35 5 0 -10 3.85 2.61 4 0 -10 94.06 8.23 4 0 -10 117.86 8.79 -3 0 10 91.07 6.91 3 0 -10 77.06 7.20 2 0 -10 5.03 2.63 -1 0 10 5.02 2.33 1 0 -10 6.36 2.35 -1 0 10 1.24 2.37 1 0 -10 1.66 2.37 0 0 -10 177.49 10.95 0 0 10 161.64 10.79 0 0 -10 179.65 11.11 -1 0 -10 7.89 1.52 -1 0 -10 8.69 1.80 1 0 10 7.87 1.74 7 -1 -10 59.75 5.20 7 1 -10 55.12 5.12 6 -1 -10 4.36 2.48 6 1 -10 5.83 2.61 5 -1 -10 14.41 3.26 5 1 -10 8.13 3.12 5 -1 -10 7.44 3.08 5 1 -10 15.63 3.44 4 -1 -10 22.53 3.77 4 1 -10 22.59 4.21 4 -1 -10 22.68 3.89 4 1 -10 28.91 4.28 -3 -1 10 30.25 3.75 3 -1 -10 23.98 3.86 3 1 -10 36.26 4.66 -2 -1 10 21.52 3.36 2 -1 -10 22.16 3.49 2 1 -10 21.99 3.75 2 -1 -10 17.70 2.96 -1 -1 10 116.93 8.61 -1 1 10 124.64 8.81 1 -1 -10 124.20 8.73 1 1 -10 140.71 9.40 -1 -1 10 129.10 8.86 1 -1 -10 112.90 8.71 1 1 -10 121.05 8.90 0 1 -10 276.13 15.76 0 -1 10 273.71 15.51 0 1 10 269.30 15.48 0 -1 -10 264.95 15.48 0 1 -10 276.12 15.70 0 -1 10 225.88 14.74 -1 -1 -10 12.70 1.96 -1 1 -10 13.26 2.09 1 -1 10 9.80 1.73 1 1 10 9.28 1.82 7 -2 -10 0.80 1.70 7 2 -10 0.55 1.92 6 -2 -10 192.17 12.39 6 2 -10 190.31 12.55 5 -2 -10 193.15 12.17 5 2 -10 192.32 12.81 -5 -2 10 176.36 10.97 5 -2 -10 179.48 12.00 5 2 -10 155.16 11.79 4 -2 -10 298.95 17.99 4 2 -10 298.34 18.60 4 -2 -10 298.95 17.97 4 2 -10 271.07 17.90 -3 2 10 10.53 2.66 -3 -2 10 7.82 2.55 3 -2 -10 18.40 3.17 3 2 -10 9.49 3.23 3 -2 -10 8.94 2.50 -2 2 10 -0.30 2.16 -2 -2 10 2.77 2.11 2 -2 -10 9.44 2.63 2 2 -10 5.51 2.82 -2 -2 10 8.69 2.69 2 -2 -10 4.03 2.11 -1 -2 10 1.47 2.08 -1 2 10 2.27 2.24 1 2 -10 1.11 2.25 1 -2 -10 -0.30 2.02 1 2 -10 2.57 2.37 -1 -2 10 -1.77 2.15 0 -2 -10 24.10 2.83 0 2 -10 27.99 3.59 0 -2 -10 31.38 3.33 0 2 -10 23.35 3.24 0 -2 10 27.77 3.24 0 2 10 21.45 3.24 -1 2 -10 41.84 3.56 -1 -2 -10 37.92 3.30 -1 2 -10 45.91 3.56 1 -2 10 34.07 3.03 1 2 10 34.98 3.22 7 -3 -10 0.25 1.69 7 3 -10 1.30 1.90 6 -3 -10 13.96 2.84 6 3 -10 15.47 2.99 5 -3 -10 14.64 2.96 5 3 -10 18.96 3.71 5 -3 -10 13.57 2.93 5 3 -10 15.18 3.24 -4 3 10 9.24 2.55 4 -3 -10 4.55 2.35 4 3 -10 7.44 3.14 -4 -3 10 5.21 2.30 4 -3 -10 5.92 2.62 4 3 -10 11.94 3.13 -3 3 10 20.27 3.34 3 3 -10 27.22 4.42 3 -3 -10 25.78 3.75 3 -3 -10 24.39 3.63 -2 3 10 -0.94 2.18 -2 -3 10 -1.17 1.93 2 3 -10 0.87 2.66 -2 -3 10 0.92 2.17 2 -3 -10 1.90 2.00 1 -3 -10 9.07 2.12 1 3 -10 12.21 2.97 1 3 -10 10.74 2.52 -1 -3 10 9.81 2.14 -1 -3 10 12.50 2.80 0 3 -10 85.86 6.27 0 3 10 72.25 5.65 0 -3 -10 74.03 5.50 0 3 -10 62.06 5.44 0 -3 -10 64.88 4.88 0 -3 10 77.29 5.65 -1 3 -10 34.78 3.20 -1 3 -10 32.45 2.93 1 3 10 24.18 2.69 7 -4 -10 3.13 1.81 7 4 -10 2.42 1.81 6 -4 -10 -1.64 2.05 6 4 -10 0.89 1.98 5 4 -10 31.78 4.58 5 -4 -10 34.90 4.08 5 4 -10 36.67 4.39 -4 4 10 47.31 5.01 4 4 -10 64.21 6.27 -4 -4 10 55.64 4.85 4 -4 -10 54.93 5.25 4 4 -10 57.22 5.51 -3 4 10 -0.33 2.23 3 -4 -10 0.31 2.05 3 4 -10 0.45 2.66 -3 -4 10 0.86 2.13 3 -4 -10 -1.61 2.20 3 4 -10 -1.07 2.55 3 -4 -10 3.85 2.35 -2 4 10 32.73 3.96 2 4 -10 41.30 4.80 2 -4 -10 31.60 3.44 -2 -4 10 18.77 2.61 2 -4 -10 22.46 3.55 -2 -4 10 30.34 3.65 1 4 -10 7.52 2.64 1 4 -10 6.64 2.32 -1 -4 10 1.90 2.02 -1 -4 10 4.59 1.72 1 -4 -10 6.60 2.03 0 4 -10 3.61 2.02 0 -4 10 0.23 1.67 0 4 -10 0.23 1.62 0 -4 10 -0.85 1.36 0 -4 -10 1.05 1.30 -1 4 -10 12.05 1.84 1 4 10 15.68 2.07 7 -5 -10 5.92 1.87 7 5 -10 1.98 1.76 6 -5 -10 1.73 1.83 6 5 -10 3.28 2.01 5 5 -10 2.00 2.49 5 -5 -10 6.43 2.25 5 5 -10 6.21 2.31 -4 5 10 -0.64 2.48 4 -5 -10 1.70 1.85 4 5 -10 -0.85 2.72 4 -5 -10 0.30 2.17 4 5 -10 1.32 2.04 -4 -5 10 0.45 1.72 -3 5 10 84.45 7.69 3 5 -10 113.13 8.69 -3 -5 10 109.38 7.51 3 -5 -10 118.15 7.88 3 5 -10 109.28 8.03 3 -5 -10 96.58 7.85 -2 5 10 9.65 2.72 2 5 -10 11.80 3.15 -2 -5 10 7.31 1.64 2 -5 -10 13.83 2.83 -1 -5 10 2.75 2.02 1 5 -10 -0.72 2.27 -1 -5 10 0.26 1.75 -1 -5 10 -0.83 1.38 1 -5 -10 -1.33 1.72 0 5 -10 53.89 4.63 0 5 -10 45.37 3.96 0 -5 10 59.44 4.29 -1 5 -10 15.12 2.21 1 5 10 11.27 1.82 7 6 -10 34.46 3.41 6 6 -10 1.49 1.73 5 6 -10 171.89 11.85 5 6 -10 177.31 11.28 -4 6 10 44.97 4.86 4 6 -10 54.29 5.52 4 6 -10 55.54 4.90 4 -6 -10 38.01 4.56 -3 6 10 17.59 3.38 3 6 -10 23.80 3.82 -3 6 10 14.36 2.15 -3 -6 10 22.89 2.92 3 6 -10 17.09 3.09 3 -6 -10 13.43 2.97 2 6 -10 8.79 2.83 -2 6 10 7.10 1.74 2 -6 -10 6.38 2.41 -1 -6 10 101.42 6.33 1 6 -10 99.19 6.87 1 -6 -10 92.38 6.16 -1 -6 10 99.96 6.15 0 6 -10 7.47 2.15 -1 6 -10 18.91 2.10 1 6 10 9.37 1.58 6 -7 -10 47.43 3.96 5 7 -10 0.34 2.11 5 -7 -10 6.85 2.56 -4 -7 10 6.81 2.45 -4 7 10 8.74 2.66 4 7 -10 9.57 2.81 4 7 -10 10.64 2.46 4 -7 -10 5.96 2.39 -3 -7 10 52.53 4.89 3 7 -10 60.87 5.65 -3 7 10 48.55 4.15 3 7 -10 58.48 4.95 3 -7 -10 54.78 5.30 -3 -7 10 50.73 4.39 -2 -7 10 20.14 2.96 2 7 -10 18.78 3.28 -2 7 10 11.44 2.11 -2 -7 10 15.51 2.62 2 -7 -10 15.11 2.45 2 7 -10 14.68 2.68 2 -7 -10 14.37 2.80 1 7 -10 82.04 6.19 -1 7 10 58.61 4.67 1 -7 -10 74.00 5.03 1 -7 -10 73.75 5.60 -1 -7 10 69.22 5.36 0 7 -10 58.93 4.56 0 -7 -10 42.13 3.77 -1 7 -10 0.14 0.89 6 8 -10 1.99 1.48 6 -8 -10 0.51 1.97 5 8 -10 123.93 8.58 5 -8 -10 114.74 8.23 -4 -8 10 70.41 5.69 -4 8 10 67.72 6.24 4 8 -10 86.61 6.52 4 -8 -10 68.18 6.02 -3 -8 10 4.64 2.20 -3 8 10 6.46 1.94 3 8 -10 7.14 2.66 3 -8 -10 8.07 2.53 -2 -8 10 114.96 7.55 -2 8 10 94.31 7.77 2 8 -10 113.12 7.89 -2 8 10 99.40 6.78 2 -8 -10 97.44 7.54 1 8 -10 10.65 2.48 -1 8 10 8.08 1.78 1 -8 -10 10.56 2.27 0 8 -10 46.02 3.85 0 8 -10 35.70 2.99 0 -8 -10 41.51 3.38 6 9 -10 25.18 2.43 6 -9 -10 25.28 3.14 5 9 -10 17.51 2.66 5 9 -10 11.16 2.07 5 -9 -10 12.54 2.67 4 9 -10 9.46 2.40 4 9 -10 10.87 2.07 4 -9 -10 8.95 2.34 -3 -9 10 1.77 1.76 -3 9 10 -0.67 2.30 3 9 -10 1.82 1.94 3 9 -10 2.58 1.64 3 -9 -10 5.39 2.18 2 9 -10 12.01 2.45 -2 9 10 7.84 1.99 2 9 -10 6.66 1.73 2 -9 -10 13.67 2.58 1 9 -10 66.32 5.04 -1 9 10 52.22 4.22 1 9 -10 56.23 4.10 1 -9 -10 63.92 4.94 0 9 -10 9.78 1.78 0 -9 -10 6.95 1.47 6 -10 -10 3.92 1.91 5 10 -10 3.79 1.26 5 -10 -10 6.57 1.96 4 10 -10 5.00 1.45 3 10 -10 93.44 6.76 3 10 -10 85.86 5.90 3 -10 -10 103.76 6.94 -2 10 10 51.42 4.22 2 10 -10 46.53 3.65 2 -10 -10 52.08 4.60 1 10 -10 2.45 1.48 -1 10 10 3.31 1.40 1 -10 -10 5.63 1.64 0 10 -10 6.24 1.28 0 -10 -10 4.36 1.14 6 11 -10 63.61 4.80 6 -11 -10 80.95 5.31 5 -11 -10 19.81 2.70 4 11 -10 41.38 3.77 -3 11 10 -0.55 1.54 3 -11 -10 0.67 1.43 -2 11 10 34.03 3.28 2 -11 -10 40.75 3.63 -1 11 10 3.60 1.28 1 -11 -10 2.11 1.35 -3 12 10 29.99 3.10 3 12 -10 33.71 3.01 2 12 -10 5.05 1.31 -2 12 10 6.14 1.61 2 -12 -10 8.50 1.65 1 -12 -10 6.65 1.38 -3 13 10 6.42 1.50 2 -13 -10 10.58 1.57 6 0 -11 1.60 1.05 5 0 -11 0.17 1.27 4 0 -11 0.54 1.30 3 0 -11 -1.33 1.14 3 0 -11 1.53 1.27 2 0 -11 1.74 1.01 6 -1 -11 4.32 1.15 6 1 -11 4.15 1.15 5 -1 -11 69.93 4.81 5 1 -11 65.00 4.78 4 -1 -11 1.19 1.31 4 1 -11 -1.61 1.36 3 1 -11 19.40 2.32 3 -1 -11 22.31 2.38 3 1 -11 22.03 2.42 2 -1 -11 3.95 1.13 2 1 -11 2.80 1.15 6 2 -11 1.56 0.92 5 -2 -11 82.72 5.23 5 2 -11 72.40 5.20 4 -2 -11 43.47 3.34 4 2 -11 34.60 3.28 3 2 -11 0.53 1.24 3 -2 -11 0.86 1.05 3 2 -11 3.19 1.38 2 2 -11 9.89 1.50 5 -3 -11 -0.12 1.01 5 3 -11 1.00 1.13 4 -3 -11 0.53 1.00 4 3 -11 2.33 1.32 3 -3 -11 19.22 1.89 3 3 -11 18.35 2.04 5 4 -11 134.15 7.88 4 4 -11 28.93 2.61 3 4 -11 -0.17 1.10 3 4 -11 -0.63 1.00 3 5 -11 0.60 0.92 TITL ca061220_1_1 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 9.684234 25.297270 8.784584 90.0000 109.0073 90.0000 ZERR 4.00 0.000099 0.000209 0.000088 0.0000 0.0011 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O S UNIT 80.00 88.00 8.00 12.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 17489 _olex2_date_sample_submission 2020-12-04 _olex2_submission_original_sample_id ca061220_1_1 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.460 _oxdiff_exptl_absorpt_empirical_full_min 0.708