data_p21_c_a _audit_creation_date 2018-06-20 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2018/1' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _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 'C21 H19 N O4 S3' _chemical_formula_sum 'C21 H19 N O4 S3' _chemical_formula_weight 445.55 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 19.557(4) _cell_length_b 5.4170(11) _cell_length_c 21.739(4) _cell_angle_alpha 90 _cell_angle_beta 102.53(3) _cell_angle_gamma 90 _cell_volume 2248.1(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15010 _cell_measurement_temperature 100 _cell_measurement_theta_max 22.974 _cell_measurement_theta_min 1.067 _shelx_estimated_absorpt_T_max 0.996 _shelx_estimated_absorpt_T_min 0.993 _exptl_absorpt_coefficient_mu 0.356 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 928 _exptl_crystal_preparation 'slow diffusion of pentane into dichloromethane' _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.4271 _diffrn_reflns_av_unetI/netI 0.4337 _diffrn_reflns_Laue_measured_fraction_full 0.818 _diffrn_reflns_Laue_measured_fraction_max 0.818 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 15010 _diffrn_reflns_point_group_measured_fraction_full 0.818 _diffrn_reflns_point_group_measured_fraction_max 0.818 _diffrn_reflns_theta_full 22.974 _diffrn_reflns_theta_max 22.974 _diffrn_reflns_theta_min 1.067 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.818 _diffrn_measured_fraction_theta_max 0.818 _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'Phi Scan' _diffrn_radiation_monochromator 'Silicon Double Crystal' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'MX1 Beamline Australian Synchrotron' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1269 _reflns_number_total 2537 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _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 'XDS (Kabsch, 1993)' _computing_data_collection 'AS QEGUI' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.063 _refine_diff_density_min -1.106 _refine_diff_density_rms 0.258 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.226 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 264 _refine_ls_number_reflns 2537 _refine_ls_number_restraints 141 _refine_ls_R_factor_all 0.3022 _refine_ls_R_factor_gt 0.1801 _refine_ls_restrained_S_all 1.195 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.4042 _refine_ls_wR_factor_ref 0.4696 _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 O(H) groups 2. Rigid bond restraints C12, C17, C16, C14, C13, C15 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C6, C1, C2, C3, C4, C5 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 N1, C10, C9, C8, C7 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 S3, C18, S2 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 3. Uiso/Uaniso restraints and constraints C3 \\sim C2 \\sim C1 \\sim C6 \\sim C5 \\sim C4: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 C17 \\sim C16 \\sim C15 \\sim C14 \\sim C13 \\sim C12: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 N1 \\sim C10 \\sim C9 \\sim C8 \\sim C7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 4. Rigid body (RIGU) restrains S1, C18 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5.a Ternary CH refined with riding coordinates: C9(H9), C8(H8) 5.b Secondary CH2 refined with riding coordinates: C19(H19A,H19B), C11(H11A,H11B), C20(H20A,H20B) 5.c Aromatic/amide H refined with riding coordinates: C6(H6), C5(H5), C4(H4A), C17(H17), C2(H2), C3(H3), C14(H14), C13(H13), C15(H15), C16(H16) 5.d Idealised tetrahedral OH refined with riding coordinates: O4(H4) ; _atom_sites_solution_hydrogens geom _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 0.7216(2) 1.1775(6) 0.24618(18) 0.0534(14) Uani 1 1 d . U . . . S2 S 0.6291(2) 0.8239(7) 0.2983(2) 0.0627(15) Uani 1 1 d . U . . . S3 S 0.5880(3) 1.0666(8) 0.1716(2) 0.0695(16) Uani 1 1 d . U . . . O1 O 0.7004(6) 1.3250(17) 0.3836(4) 0.053(3) Uani 1 1 d . . . . . O3 O 0.5163(7) 0.552(2) 0.0741(5) 0.069(3) Uani 1 1 d . . . . . O4 O 0.4439(7) 0.7764(18) 0.0043(5) 0.079(4) Uani 1 1 d . . . . . H4 H 0.452799 0.673414 -0.021758 0.118 Uiso 1 1 calc R . . . . O2 O 0.8304(7) 0.6242(17) 0.4339(5) 0.068(3) Uani 1 1 d . . . . . N1 N 0.7619(7) 0.972(2) 0.4235(5) 0.047(3) Uani 1 1 d . U . . . C6 C 0.6979(8) 0.773(2) 0.4923(6) 0.043(3) Uani 1 1 d . U . . . H6 H 0.685674 0.644691 0.462115 0.051 Uiso 1 1 calc R . . . . C1 C 0.7414(7) 0.964(2) 0.4810(6) 0.041(3) Uani 1 1 d . U . . . C7 C 0.7393(9) 1.161(3) 0.3774(7) 0.052(4) Uani 1 1 d . U . . . C5 C 0.6722(9) 0.767(2) 0.5467(7) 0.049(3) Uani 1 1 d . U . . . H5 H 0.642226 0.638096 0.554279 0.059 Uiso 1 1 calc R . . . . C9 C 0.8065(8) 0.838(2) 0.3331(7) 0.044(3) Uani 1 1 d . U . . . H9 H 0.776022 0.717799 0.304908 0.053 Uiso 1 1 calc R . . . . C4 C 0.6922(8) 0.964(2) 0.5915(7) 0.047(3) Uani 1 1 d . U . . . H4A H 0.676782 0.965071 0.630068 0.057 Uiso 1 1 calc R . . . . C17 C 0.9249(8) 1.097(2) 0.2452(8) 0.048(3) Uani 1 1 d . U . . . H17 H 0.947841 1.197754 0.279246 0.057 Uiso 1 1 calc R . . . . C12 C 0.8881(8) 0.893(3) 0.2587(7) 0.053(4) Uani 1 1 d . U . . . C2 C 0.7577(8) 1.159(2) 0.5233(7) 0.047(3) Uani 1 1 d . U . . . H2 H 0.784652 1.294754 0.514343 0.056 Uiso 1 1 calc R . . . . C8 C 0.7734(9) 1.110(2) 0.3235(7) 0.051(4) Uani 1 1 d . U . . . H8 H 0.814354 1.224972 0.329383 0.062 Uiso 1 1 calc R . . . . C3 C 0.7346(9) 1.151(2) 0.5773(7) 0.055(4) Uani 1 1 d . U . . . H3 H 0.747991 1.280237 0.607091 0.066 Uiso 1 1 calc R . . . . C10 C 0.8042(9) 0.790(3) 0.4034(8) 0.054(4) Uani 1 1 d . U . . . C19 C 0.5091(10) 0.873(3) 0.1751(8) 0.069(5) Uani 1 1 d . . . . . H19A H 0.522937 0.698942 0.184620 0.082 Uiso 1 1 calc R . . . . H19B H 0.485899 0.935009 0.208277 0.082 Uiso 1 1 calc R . . . . C14 C 0.8607(9) 0.813(3) 0.1445(8) 0.059(4) Uani 1 1 d . U . . . H14 H 0.838580 0.717086 0.109236 0.071 Uiso 1 1 calc R . . . . C13 C 0.8531(9) 0.751(3) 0.2042(8) 0.051(4) Uani 1 1 d . U . . . H13 H 0.824652 0.614554 0.209751 0.062 Uiso 1 1 calc R . . . . C15 C 0.9010(9) 1.018(3) 0.1361(7) 0.063(4) Uani 1 1 d . U . . . H15 H 0.908415 1.058665 0.095575 0.076 Uiso 1 1 calc R . . . . C18 C 0.6434(8) 1.011(2) 0.2458(6) 0.042(3) Uani 1 1 d . U . . . C11 C 0.8841(10) 0.824(3) 0.3235(9) 0.062(5) Uani 1 1 d . . . . . H11A H 0.914212 0.936288 0.353686 0.074 Uiso 1 1 calc R . . . . H11B H 0.902110 0.653764 0.332367 0.074 Uiso 1 1 calc R . . . . C16 C 0.9297(10) 1.159(3) 0.1875(8) 0.062(4) Uani 1 1 d . U . . . H16 H 0.953905 1.306375 0.181507 0.075 Uiso 1 1 calc R . . . . C20 C 0.4608(9) 0.892(3) 0.1120(7) 0.051(4) Uani 1 1 d . . . . . H20A H 0.460191 1.065327 0.097331 0.061 Uiso 1 1 calc R . . . . H20B H 0.412796 0.849538 0.116106 0.061 Uiso 1 1 calc R . . . . C21 C 0.4814(10) 0.723(3) 0.0617(8) 0.065(5) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.083(3) 0.042(2) 0.032(3) 0.0008(15) 0.003(2) 0.0003(18) S2 0.079(3) 0.053(2) 0.047(3) 0.0089(19) -0.005(2) -0.012(2) S3 0.085(3) 0.069(3) 0.043(3) 0.010(2) -0.011(2) -0.007(2) O1 0.093(9) 0.041(5) 0.027(6) -0.002(4) 0.015(5) 0.020(6) O3 0.097(9) 0.064(7) 0.033(7) -0.005(5) -0.011(6) 0.027(7) O4 0.135(11) 0.038(5) 0.042(8) -0.009(5) -0.025(7) 0.027(6) O2 0.105(9) 0.034(5) 0.059(8) 0.013(5) 0.006(6) 0.032(6) N1 0.079(8) 0.039(6) 0.017(6) -0.009(4) -0.002(5) -0.011(5) C6 0.076(10) 0.023(6) 0.024(7) -0.002(5) -0.001(6) 0.002(5) C1 0.055(8) 0.037(6) 0.024(7) 0.003(5) -0.007(6) 0.005(5) C7 0.074(10) 0.041(7) 0.030(8) -0.003(5) -0.011(6) -0.001(6) C5 0.072(10) 0.040(7) 0.033(8) -0.006(6) 0.006(6) -0.003(6) C9 0.066(9) 0.028(6) 0.031(7) -0.005(5) -0.006(6) -0.004(6) C4 0.071(9) 0.039(7) 0.030(8) -0.009(5) 0.005(6) 0.001(6) C17 0.053(9) 0.038(7) 0.049(7) -0.005(6) 0.004(7) -0.001(5) C12 0.067(10) 0.038(7) 0.045(8) -0.007(6) -0.005(7) 0.000(6) C2 0.070(10) 0.026(6) 0.035(7) 0.005(5) -0.008(6) -0.006(6) C8 0.084(11) 0.030(6) 0.037(8) -0.006(5) 0.006(7) -0.002(6) C3 0.092(11) 0.028(6) 0.038(8) -0.006(6) 0.000(7) 0.000(6) C10 0.083(11) 0.030(6) 0.041(7) -0.003(6) -0.005(7) -0.005(6) C19 0.092(13) 0.066(10) 0.047(12) -0.020(8) 0.013(9) 0.022(9) C14 0.074(11) 0.055(8) 0.038(7) -0.009(6) -0.012(7) 0.001(6) C13 0.070(10) 0.035(7) 0.050(8) -0.006(6) 0.016(7) -0.010(6) C15 0.083(11) 0.066(9) 0.032(7) 0.018(6) -0.006(7) 0.004(7) C18 0.076(10) 0.040(7) 0.011(7) -0.011(5) 0.008(6) 0.008(7) C11 0.072(12) 0.053(9) 0.062(12) 0.001(8) 0.016(9) 0.003(8) C16 0.087(11) 0.037(7) 0.057(8) 0.003(6) 0.003(8) 0.007(7) C20 0.067(10) 0.056(9) 0.026(9) -0.012(7) 0.000(7) 0.011(8) C21 0.081(13) 0.058(10) 0.042(11) -0.001(8) -0.019(9) 0.009(10) _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 C8 1.802(15) . ? S1 C18 1.774(16) . ? S2 C18 1.596(15) . ? S3 C19 1.88(2) . ? S3 C18 1.762(13) . ? O1 C7 1.196(19) . ? O3 C21 1.144(19) . ? O4 C21 1.34(2) . ? O2 C10 1.166(17) . ? N1 C1 1.393(18) . ? N1 C7 1.433(19) . ? N1 C10 1.42(2) . ? C6 C1 1.40(2) . ? C6 C5 1.38(2) . ? C1 C2 1.39(2) . ? C7 C8 1.50(2) . ? C5 C4 1.44(2) . ? C9 C8 1.603(19) . ? C9 C10 1.56(2) . ? C9 C11 1.58(2) . ? C4 C3 1.39(2) . ? C17 C12 1.39(2) . ? C17 C16 1.32(2) . ? C12 C13 1.45(2) . ? C12 C11 1.48(2) . ? C2 C3 1.35(2) . ? C19 C20 1.49(2) . ? C14 C13 1.38(2) . ? C14 C15 1.39(2) . ? C15 C16 1.37(2) . ? C20 C21 1.55(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C18 S1 C8 102.2(7) . . ? C18 S3 C19 102.4(8) . . ? C1 N1 C7 123.0(13) . . ? C1 N1 C10 123.7(12) . . ? C10 N1 C7 113.2(13) . . ? C5 C6 C1 121.0(13) . . ? N1 C1 C6 119.1(12) . . ? C2 C1 N1 120.0(13) . . ? C2 C1 C6 120.5(15) . . ? O1 C7 N1 123.9(15) . . ? O1 C7 C8 129.0(14) . . ? N1 C7 C8 107.1(13) . . ? C6 C5 C4 117.9(14) . . ? C10 C9 C8 100.7(11) . . ? C10 C9 C11 110.8(13) . . ? C11 C9 C8 113.6(12) . . ? C3 C4 C5 118.6(15) . . ? C16 C17 C12 123.5(15) . . ? C17 C12 C13 115.1(15) . . ? C17 C12 C11 122.7(14) . . ? C13 C12 C11 122.2(14) . . ? C3 C2 C1 118.8(14) . . ? C7 C8 S1 115.9(12) . . ? C7 C8 C9 107.7(12) . . ? C9 C8 S1 115.9(9) . . ? C2 C3 C4 123.1(13) . . ? O2 C10 N1 125.1(16) . . ? O2 C10 C9 125.8(15) . . ? N1 C10 C9 109.1(12) . . ? C20 C19 S3 106.6(13) . . ? C13 C14 C15 119.7(14) . . ? C14 C13 C12 120.8(14) . . ? C16 C15 C14 118.8(16) . . ? S2 C18 S1 127.2(8) . . ? S2 C18 S3 126.5(9) . . ? S3 C18 S1 106.0(7) . . ? C12 C11 C9 111.4(14) . . ? C17 C16 C15 122.0(16) . . ? C19 C20 C21 113.5(13) . . ? O3 C21 O4 125.0(16) . . ? O3 C21 C20 123.2(15) . . ? O4 C21 C20 110.9(15) . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 -0.115 0.000 130.7 67.6 ? 2 0.000 -0.380 0.500 130.7 67.6 ? _shelx_fab_file ; -19 0 6 1.0872 0.0026 -18 0 2 1.9350 0.0001 -18 0 4 3.4825 0.0034 -18 0 6 1.9798 0.0020 -18 0 8 -1.6037 -0.0018 -18 0 10 -3.7231 -0.0020 -18 0 12 -4.5069 0.0002 -18 0 14 -5.5883 -0.0006 -18 1 1 0.4437 -0.0018 -18 1 2 0.0310 -0.0018 -18 1 3 -1.8674 0.0003 -18 1 4 0.0064 0.0041 -18 1 5 -3.5259 -0.0005 -18 1 6 0.4073 0.0036 -18 1 7 -3.4936 -0.0021 -18 1 8 -0.0759 -0.0028 -18 1 9 -1.5754 -0.0025 -18 1 10 -0.6515 -0.0042 -18 1 11 0.8370 -0.0016 -18 2 7 2.5819 0.0054 -18 2 8 -0.4329 0.0003 -18 2 9 0.7031 0.0013 -18 2 10 0.0347 0.0010 -18 2 11 -1.6921 -0.0021 -18 2 12 -0.4647 0.0006 -18 2 13 -2.1328 0.0030 -18 2 14 -1.0168 -0.0019 -17 0 2 5.1171 -0.0005 -17 0 4 6.1312 0.0013 -17 0 6 3.6670 0.0000 -17 0 8 -0.0848 -0.0015 -17 0 10 -1.9844 -0.0005 -17 0 12 -3.4139 0.0014 -17 0 14 -5.9719 0.0001 -17 0 16 -7.6372 -0.0048 -17 0 18 -5.8923 -0.0087 -17 1 1 -1.0289 0.0008 -17 1 2 1.3108 -0.0010 -17 1 3 -4.2861 0.0016 -17 1 4 1.0712 0.0047 -17 1 5 -6.4697 -0.0000 -17 1 6 0.3883 0.0037 -17 1 7 -6.1551 -0.0009 -17 1 8 -1.3288 -0.0018 -17 1 9 -3.2399 -0.0005 -17 1 10 -1.7707 -0.0020 -17 1 11 0.0836 -0.0001 -17 1 12 -0.1650 0.0017 -17 1 13 2.0566 -0.0011 -17 1 14 0.8056 -0.0023 -17 1 15 1.9053 -0.0018 -17 2 1 1.1705 -0.0033 -17 2 2 -0.5872 -0.0004 -17 2 3 2.2447 -0.0036 -17 2 4 -1.2169 -0.0001 -17 2 5 3.9437 0.0004 -17 2 6 -0.5008 0.0003 -17 2 7 3.7856 0.0022 -17 2 8 1.0756 0.0006 -17 2 9 1.0625 -0.0011 -17 2 10 0.7123 0.0014 -17 2 11 -1.9938 -0.0017 -17 2 12 -0.9129 0.0013 -17 2 13 -2.7256 0.0051 -17 2 14 -1.9590 -0.0019 -16 0 2 7.8810 -0.0019 -16 0 4 8.0918 -0.0011 -16 0 6 5.3389 -0.0018 -16 0 8 2.6805 -0.0015 -16 0 10 1.6685 0.0004 -16 0 12 -0.4617 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4 0 8 -6.8438 0.0003 4 0 10 -15.2034 0.0001 4 0 12 -13.6969 0.0011 4 0 14 -5.7243 0.0018 4 0 16 -2.4051 -0.0009 4 0 18 -5.0615 0.0047 4 1 0 -9.4644 0.0067 4 1 1 -14.4587 0.0004 4 1 2 -3.1182 0.0079 4 1 3 -16.0941 0.0012 4 1 4 5.3218 -0.0003 4 1 5 -17.2030 0.0019 4 1 6 5.0428 -0.0056 4 1 7 -13.6571 0.0024 4 1 8 -1.8352 -0.0018 4 1 9 -3.8510 0.0013 4 1 10 -9.2049 0.0013 4 1 11 3.2682 -0.0019 4 1 12 -13.9094 -0.0011 4 1 13 4.3285 -0.0030 4 1 14 -14.0552 -0.0029 4 1 15 4.2174 -0.0016 4 1 16 -9.5982 -0.0007 4 1 17 3.9298 -0.0023 4 1 18 -4.0649 -0.0003 4 1 19 1.5747 -0.0028 4 2 0 10.1602 -0.0017 4 2 1 1.0940 0.0028 4 2 2 17.1600 -0.0011 4 2 3 -1.5389 0.0018 4 2 4 13.9928 -0.0001 4 2 5 -0.0057 0.0006 4 2 6 13.9926 0.0004 4 2 7 -1.1074 0.0023 4 2 8 17.5220 -0.0000 4 2 9 -1.5164 0.0025 4 2 10 14.6383 -0.0004 4 2 11 2.8130 -0.0018 4 2 12 5.1697 0.0003 4 2 13 7.6326 -0.0033 4 2 14 -2.7628 0.0016 4 2 15 8.2725 0.0016 4 2 16 -5.8382 0.0009 4 2 17 5.6329 0.0028 4 2 18 -4.5592 -0.0009 4 2 19 2.5278 -0.0046 4 3 0 -10.9830 -0.0005 4 3 1 1.6996 -0.0001 4 3 2 -3.8840 0.0004 4 3 3 1.4107 0.0003 4 3 4 -0.6151 0.0005 4 3 5 -0.5269 -0.0013 4 3 6 -1.0323 0.0004 4 3 7 -3.4070 -0.0007 4 3 8 1.2556 -0.0002 4 3 9 -5.8656 0.0034 4 3 10 2.9254 -0.0000 4 3 11 -6.0962 0.0041 4 3 12 -0.9403 0.0012 4 3 13 -2.9735 -0.0000 4 3 14 -3.6935 0.0012 4 3 15 0.8065 0.0006 4 3 16 -1.0009 0.0011 4 3 17 1.4528 0.0070 4 3 18 0.9755 0.0024 4 4 0 -5.1454 -0.0003 4 4 1 -6.6111 -0.0007 4 4 2 -6.8771 0.0034 4 4 3 -2.9415 -0.0030 4 4 4 -5.0870 0.0026 4 4 5 -0.3988 -0.0032 4 4 6 -2.3819 -0.0015 4 4 7 -0.3179 -0.0016 4 4 8 -0.4685 -0.0031 4 4 9 1.0744 0.0011 4 4 10 0.9416 -0.0006 4 4 11 2.9489 0.0022 4 4 12 0.6914 0.0035 4 5 0 3.4962 0.0006 4 5 1 1.4526 0.0011 4 5 2 2.4561 0.0028 4 5 3 1.4396 0.0006 4 5 4 0.8255 0.0036 4 5 5 1.9950 0.0009 4 5 6 0.1326 0.0003 4 5 7 1.4269 0.0012 5 0 0 -2.1995 0.0115 5 0 2 9.6829 -0.0029 5 0 4 12.4449 -0.0108 5 0 6 7.2310 -0.0044 5 0 8 -2.5451 0.0007 5 0 10 -10.8225 0.0000 5 0 12 -9.2798 0.0013 5 0 14 -1.8084 0.0018 5 0 16 -0.8620 -0.0011 5 0 18 -6.0408 0.0051 5 1 0 -15.1518 0.0046 5 1 1 -6.9954 0.0046 5 1 2 -6.8701 0.0013 5 1 3 -11.8579 0.0045 5 1 4 4.2312 -0.0065 5 1 5 -16.7710 0.0029 5 1 6 4.5370 -0.0069 5 1 7 -14.6482 0.0001 5 1 8 -3.3705 -0.0005 5 1 9 -4.5584 -0.0019 5 1 10 -11.3733 0.0019 5 1 11 3.4064 -0.0031 5 1 12 -15.0112 -0.0010 5 1 13 4.9577 -0.0026 5 1 14 -13.1403 -0.0024 5 1 15 4.5026 -0.0014 5 1 16 -7.5195 0.0011 5 1 17 3.9927 -0.0021 5 1 18 -2.2020 0.0059 5 1 19 2.0750 -0.0017 5 2 0 8.4160 0.0000 5 2 1 4.9483 0.0032 5 2 2 14.3988 -0.0003 5 2 3 0.6117 0.0018 5 2 4 12.8960 -0.0006 5 2 5 -1.9629 0.0018 5 2 6 14.8309 0.0006 5 2 7 -5.6141 0.0034 5 2 8 17.6430 0.0016 5 2 9 -5.8539 0.0015 5 2 10 12.5655 0.0005 5 2 11 -0.1366 -0.0034 5 2 12 2.3909 -0.0001 5 2 13 6.4677 -0.0030 5 2 14 -4.8528 0.0006 5 2 15 8.4386 0.0032 5 2 16 -7.3449 -0.0019 5 2 17 5.8412 0.0039 5 2 18 -5.5427 -0.0063 5 2 19 2.2433 -0.0033 5 3 0 -11.0484 0.0016 5 3 1 4.7552 -0.0001 5 3 2 -3.2422 0.0010 5 3 3 3.5729 0.0001 5 3 4 0.4116 0.0002 5 3 5 0.5539 -0.0013 5 3 6 1.4397 0.0010 5 3 7 -3.4795 -0.0001 5 3 8 5.2931 0.0011 5 3 9 -7.0138 0.0030 5 3 10 6.6272 0.0005 5 3 11 -7.9797 0.0013 5 3 12 1.2680 0.0006 5 3 13 -4.8708 -0.0038 5 3 14 -2.6473 0.0019 5 3 15 -0.3268 -0.0025 5 3 16 -0.9800 0.0038 5 3 17 1.3070 0.0041 5 4 0 -7.4115 0.0007 5 4 1 -4.8667 -0.0002 5 4 2 -8.8619 0.0039 5 4 3 -0.9656 -0.0022 5 4 4 -6.9768 0.0001 5 4 5 0.7026 -0.0012 5 4 6 -4.0530 -0.0053 5 4 7 -0.2631 0.0015 5 4 8 -1.2221 -0.0047 5 4 9 0.0102 0.0041 5 4 10 1.2558 0.0009 5 4 11 1.0957 0.0034 5 5 0 3.3053 -0.0002 5 5 1 0.6563 0.0025 5 5 2 2.5843 0.0030 5 5 3 1.5888 0.0012 5 5 4 0.8852 0.0020 5 5 5 2.5567 0.0016 5 5 8 0.8848 -0.0136 6 0 0 -5.8301 -0.0014 6 0 2 5.4363 -0.0107 6 0 4 9.6595 -0.0105 6 0 6 8.3352 -0.0020 6 0 8 1.4847 0.0009 6 0 10 -5.9134 -0.0005 6 0 12 -4.4036 0.0010 6 0 14 1.8551 0.0007 6 0 16 0.3619 -0.0026 6 0 18 -6.6799 0.0028 6 1 0 -16.1955 0.0009 6 1 1 -3.7986 0.0045 6 1 2 -5.2842 -0.0044 6 1 3 -9.3414 0.0044 6 1 4 6.4477 -0.0089 6 1 5 -15.7773 0.0016 6 1 6 5.3978 -0.0045 6 1 7 -14.3424 -0.0022 6 1 8 -3.9734 0.0020 6 1 9 -4.3812 -0.0031 6 1 10 -12.0995 0.0025 6 1 11 3.8116 -0.0020 6 1 12 -14.3901 -0.0004 6 1 13 5.2766 -0.0006 6 1 14 -11.1008 -0.0012 6 1 15 4.1345 0.0001 6 1 16 -5.4040 0.0038 6 1 17 3.5082 -0.0005 6 1 18 -1.0307 0.0136 6 2 0 5.8366 0.0020 6 2 1 6.5226 0.0017 6 2 2 10.6629 0.0003 6 2 3 0.7076 -0.0002 6 2 4 10.7385 -0.0012 6 2 5 -5.2952 0.0009 6 2 6 14.0029 0.0007 6 2 7 -10.4556 0.0024 6 2 8 15.7271 0.0027 6 2 9 -9.6980 -0.0002 6 2 10 9.0997 0.0006 6 2 11 -2.2888 -0.0035 6 2 12 -0.5353 -0.0012 6 2 13 5.7805 -0.0007 6 2 14 -6.0728 -0.0009 6 2 15 8.4858 0.0055 6 2 16 -7.5708 -0.0052 6 2 17 5.7689 0.0051 6 2 18 -5.5351 -0.0110 6 2 19 1.9809 -0.0019 6 3 0 -9.3969 0.0032 6 3 1 7.0024 0.0000 6 3 2 -1.6955 0.0013 6 3 3 5.3636 -0.0001 6 3 4 2.0268 0.0003 6 3 5 1.5729 -0.0011 6 3 6 4.2907 0.0019 6 3 7 -3.4704 0.0003 6 3 8 8.9479 0.0017 6 3 9 -7.8849 0.0013 6 3 10 9.2484 -0.0007 6 3 11 -9.3823 -0.0023 6 3 12 2.5327 -0.0014 6 3 13 -6.3847 -0.0069 6 3 14 -1.9746 0.0015 6 3 15 -1.4542 -0.0051 6 3 16 -0.8932 0.0050 6 4 0 -8.4512 0.0018 6 4 1 -3.2998 0.0004 6 4 2 -9.7514 0.0033 6 4 3 0.2906 -0.0003 6 4 4 -8.0559 -0.0029 6 4 5 1.2758 0.0021 6 4 6 -5.0811 -0.0072 6 4 7 -0.1700 0.0049 6 4 8 -1.5210 -0.0038 6 4 9 -0.5855 0.0055 6 4 10 1.6340 0.0025 6 5 0 3.0290 -0.0004 6 5 1 -0.1629 0.0029 6 5 2 2.7784 0.0027 6 5 3 1.2838 -0.0001 6 5 4 0.9771 -0.0023 7 0 0 -4.4177 -0.0039 7 0 2 2.5515 -0.0083 7 0 4 6.0371 -0.0050 7 0 6 8.4321 0.0008 7 0 8 5.2591 0.0006 7 0 10 -0.7159 -0.0009 7 0 12 0.4689 0.0006 7 0 14 5.0639 -0.0007 7 0 16 1.5709 -0.0049 7 1 0 -12.5233 -0.0016 7 1 1 -1.7510 0.0008 7 1 2 -0.4800 -0.0063 7 1 3 -6.3347 0.0016 7 1 4 9.1737 -0.0062 7 1 5 -12.8640 -0.0006 7 1 6 5.8927 0.0004 7 1 7 -12.1706 -0.0029 7 1 8 -3.9389 0.0041 7 1 9 -3.3538 -0.0016 7 1 10 -11.0729 0.0025 7 1 11 4.1457 0.0005 7 1 12 -12.0321 0.0005 7 1 13 5.0150 0.0014 7 1 14 -8.3871 -0.0001 7 1 15 3.0918 0.0016 7 1 16 -3.7497 0.0052 7 1 17 2.5248 0.0015 7 1 18 -0.7536 0.0184 7 2 0 2.6347 0.0031 7 2 1 6.3125 -0.0010 7 2 2 6.3180 0.0006 7 2 3 -0.1302 -0.0032 7 2 4 7.1199 -0.0018 7 2 5 -8.2989 -0.0010 7 2 6 10.6319 0.0008 7 2 7 -13.9155 0.0006 7 2 8 11.3313 0.0029 7 2 9 -11.9412 -0.0011 7 2 10 4.5124 -0.0004 7 2 11 -3.2743 -0.0015 7 2 12 -3.1479 -0.0024 7 2 13 5.5326 0.0026 7 2 14 -6.2802 -0.0019 7 2 15 8.3758 0.0075 7 2 16 -6.7084 -0.0071 7 2 17 5.4877 0.0063 7 2 18 -4.7927 -0.0131 7 3 0 -6.7199 0.0034 7 3 1 8.0724 0.0004 7 3 2 0.2555 0.0009 7 3 3 6.7352 -0.0003 7 3 4 3.7596 0.0006 7 3 5 2.7480 -0.0004 7 3 6 6.7949 0.0024 7 3 7 -2.8908 0.0006 7 3 8 11.4061 0.0010 7 3 9 -7.8454 -0.0003 7 3 10 10.3053 -0.0027 7 3 11 -9.7509 -0.0042 7 3 12 2.7558 -0.0036 7 3 13 -7.1354 -0.0072 7 3 14 -1.6308 0.0005 7 3 15 -2.3212 -0.0056 7 4 0 -8.0146 0.0026 7 4 1 -2.0978 0.0008 7 4 2 -9.4249 0.0017 7 4 3 0.8407 0.0015 7 4 4 -8.2219 -0.0049 7 4 5 1.3848 0.0050 7 4 6 -5.4129 -0.0057 7 4 7 -0.0561 0.0060 7 4 8 -1.4940 -0.0008 7 4 9 -0.7026 0.0029 7 5 0 2.6768 0.0004 7 5 1 -1.0652 0.0017 7 5 2 2.9730 0.0024 7 5 7 1.1973 0.0126 8 0 0 -4.4254 0.0000 8 0 2 -2.4550 -0.0013 8 0 4 1.1446 0.0010 8 0 6 8.1027 0.0021 8 0 8 8.8171 0.0000 8 0 10 4.1494 -0.0005 8 0 12 4.6746 0.0008 8 0 14 7.5843 -0.0018 8 0 16 2.8941 -0.0068 8 1 0 -6.9204 -0.0020 8 1 1 1.4379 -0.0031 8 1 2 3.6338 -0.0045 8 1 3 -1.7141 -0.0013 8 1 4 9.5296 -0.0007 8 1 5 -7.9113 -0.0019 8 1 6 4.9888 0.0049 8 1 7 -8.5695 -0.0016 8 1 8 -3.2429 0.0041 8 1 9 -1.9902 0.0011 8 1 10 -8.2716 0.0016 8 1 11 4.0701 0.0023 8 1 12 -8.2783 0.0013 8 1 13 4.1246 0.0018 8 1 14 -5.3985 -0.0002 8 1 15 1.5787 0.0019 8 1 16 -2.6173 0.0034 8 1 17 1.2602 0.0028 8 1 18 -1.0573 0.0174 8 2 0 -0.5410 0.0030 8 2 1 5.9653 -0.0035 8 2 2 1.6691 0.0002 8 2 3 -0.1755 -0.0052 8 2 4 1.8172 -0.0023 8 2 5 -9.2485 -0.0021 8 2 6 4.6415 0.0007 8 2 7 -14.7387 -0.0003 8 2 8 5.0032 0.0022 8 2 9 -12.1195 -0.0002 8 2 10 -0.3897 -0.0020 8 2 11 -3.2578 0.0013 8 2 12 -5.0432 -0.0029 8 2 13 5.3537 0.0044 8 2 14 -5.6651 -0.0009 8 2 15 7.8591 0.0075 8 2 16 -5.2369 -0.0061 8 2 17 4.8899 0.0069 8 2 18 -3.6920 -0.0119 8 3 0 -4.0933 0.0017 8 3 1 7.9191 0.0007 8 3 2 1.7262 -0.0004 8 3 3 7.6648 -0.0003 8 3 4 4.6932 0.0004 8 3 5 4.1430 0.0007 8 3 6 7.9675 0.0016 8 3 7 -1.4929 0.0012 8 3 8 12.0251 -0.0005 8 3 9 -6.5605 -0.0010 8 3 10 9.7838 -0.0037 8 3 11 -8.7929 -0.0030 8 3 12 2.2582 -0.0035 8 3 13 -6.8508 -0.0036 8 3 14 -1.3937 0.0007 8 4 0 -6.3060 0.0027 8 4 1 -0.9875 0.0008 8 4 2 -8.0381 -0.0005 8 4 3 1.1964 0.0025 8 4 4 -7.5608 -0.0050 8 4 5 1.3998 0.0057 8 4 6 -5.1837 -0.0013 8 4 7 0.1081 0.0034 8 4 8 -1.4053 0.0028 8 5 0 2.1441 0.0024 9 0 0 -7.9236 0.0038 9 0 2 -8.9355 0.0035 9 0 4 -3.0459 0.0030 9 0 6 8.5045 0.0011 9 0 8 11.9390 -0.0001 9 0 10 7.8377 0.0011 9 0 12 7.5376 0.0017 9 0 14 9.1147 -0.0019 9 0 16 4.1088 -0.0073 9 1 0 -3.0597 -0.0010 9 1 1 5.6478 -0.0043 9 1 2 3.9495 -0.0012 9 1 3 3.6496 -0.0022 9 1 4 6.4524 0.0040 9 1 5 -2.3093 -0.0016 9 1 6 2.9934 0.0062 9 1 7 -4.8354 0.0007 9 1 8 -1.6742 0.0015 9 1 9 -1.0194 0.0029 9 1 10 -4.1482 0.0001 9 1 11 3.4210 0.0016 9 1 12 -3.8307 0.0018 9 1 13 2.8219 -0.0001 9 1 14 -2.4874 -0.0020 9 1 15 -0.0007 0.0007 9 1 16 -1.8086 -0.0021 9 1 17 0.0773 0.0028 9 2 0 -2.8734 0.0020 9 2 1 6.8494 -0.0041 9 2 2 -2.8185 -0.0005 9 2 3 1.5413 -0.0045 9 2 4 -4.5423 -0.0023 9 2 5 -7.5197 -0.0011 9 2 6 -2.6677 0.0009 9 2 7 -12.8161 0.0006 9 2 8 -1.5969 0.0012 9 2 9 -10.5878 0.0017 9 2 10 -4.4124 -0.0032 9 2 11 -2.7701 0.0026 9 2 12 -5.9184 -0.0016 9 2 13 4.8034 0.0022 9 2 14 -4.5663 0.0028 9 2 15 6.7026 0.0039 9 2 16 -3.6550 -0.0020 9 2 17 3.8781 0.0062 9 3 0 -2.3660 -0.0010 9 3 1 6.7698 0.0004 9 3 2 1.9737 -0.0020 9 3 3 7.9916 -0.0000 9 3 4 4.0614 -0.0008 9 3 5 5.4067 0.0024 9 3 6 7.2013 -0.0005 9 3 7 0.3816 0.0019 9 3 8 10.7513 -0.0017 9 3 9 -4.3448 -0.0009 9 3 10 8.1772 -0.0018 9 3 11 -6.7577 0.0005 9 3 12 1.5808 0.0004 9 3 13 -5.6081 0.0023 9 4 0 -3.8980 0.0019 9 4 1 0.4016 0.0005 9 4 2 -5.9864 -0.0027 9 4 3 1.9292 0.0020 9 4 4 -6.3112 -0.0032 9 4 5 1.6939 0.0039 9 4 6 -4.5919 0.0044 9 4 7 0.3345 -0.0023 9 4 8 -1.4194 0.0052 9 5 2 2.5008 0.0025 9 5 3 -1.2608 -0.0108 10 0 0 -12.3834 0.0034 10 0 2 -13.3814 0.0031 10 0 4 -4.0129 0.0008 10 0 6 10.1927 -0.0007 10 0 8 13.9849 0.0010 10 0 10 9.5967 0.0033 10 0 12 8.6187 0.0024 10 0 14 9.3829 -0.0015 10 0 16 4.7651 -0.0061 10 1 0 -3.0970 -0.0002 10 1 1 8.9058 -0.0021 10 1 2 0.0437 0.0010 10 1 3 7.7200 -0.0011 10 1 4 1.2393 0.0057 10 1 5 2.0026 -0.0004 10 1 6 1.1401 0.0038 10 1 7 -2.2855 0.0021 10 1 8 0.7233 -0.0025 10 1 9 -0.8869 0.0022 10 1 10 0.3281 -0.0010 10 1 11 2.3512 -0.0014 10 1 12 0.3766 0.0017 10 1 13 1.5134 -0.0028 10 1 14 -0.0020 -0.0056 10 1 15 -1.1927 -0.0008 10 1 16 -1.1423 -0.0100 10 1 17 -0.6648 0.0017 10 2 0 -3.8409 0.0009 10 2 1 8.9402 -0.0027 10 2 2 -6.5317 -0.0012 10 2 3 4.5196 -0.0014 10 2 4 -10.5052 -0.0018 10 2 5 -3.9037 0.0014 10 2 6 -9.0848 0.0016 10 2 7 -9.1126 0.0023 10 2 8 -6.4686 0.0004 10 2 9 -8.1801 0.0030 10 2 10 -6.5628 -0.0034 10 2 11 -2.3088 0.0003 10 2 12 -5.7167 0.0016 10 2 13 3.6992 -0.0051 10 2 14 -3.3130 0.0084 10 2 15 4.9331 -0.0034 10 3 0 -1.7247 -0.0031 10 3 1 4.9788 -0.0007 10 3 2 0.8725 -0.0030 10 3 3 7.4300 0.0004 10 3 4 1.8082 -0.0025 10 3 5 5.8949 0.0039 10 3 6 4.7062 -0.0031 10 3 7 1.9470 0.0016 10 3 8 8.1895 -0.0016 10 3 9 -2.0158 -0.0014 10 3 10 6.2079 0.0035 10 3 11 -4.3354 0.0037 10 4 0 -1.4966 0.0007 10 4 1 2.1267 -0.0003 10 4 2 -3.7867 -0.0041 10 4 3 3.1978 -0.0001 10 4 4 -4.7878 -0.0000 10 4 5 2.3332 0.0005 10 4 6 -3.7880 0.0093 10 4 7 0.5565 -0.0084 10 4 8 -1.4770 0.0054 10 4 9 -0.3061 -0.0229 11 0 0 -13.7506 -0.0003 11 0 2 -12.7285 -0.0008 11 0 4 -0.9587 -0.0025 11 0 6 12.4073 -0.0012 11 0 8 14.1425 0.0031 11 0 10 9.1399 0.0041 11 0 12 7.9172 0.0011 11 0 14 8.3263 -0.0015 11 1 0 -6.4690 -0.0003 11 1 1 9.3388 0.0016 11 1 2 -5.8137 0.0013 11 1 3 8.9930 0.0004 11 1 4 -3.4987 0.0042 11 1 5 3.8757 0.0001 11 1 6 0.5383 -0.0004 11 1 7 -1.4112 0.0017 11 1 8 3.3457 -0.0055 11 1 9 -1.4311 -0.0002 11 1 10 3.9450 -0.0008 11 1 11 1.2949 -0.0038 11 1 12 3.4643 0.0008 11 1 13 0.6153 -0.0033 11 1 14 1.7331 -0.0106 11 1 15 -1.6963 -0.0010 11 1 16 -0.6134 -0.0179 11 2 0 -3.5484 0.0001 11 2 1 10.8638 -0.0004 11 2 2 -8.9543 -0.0016 11 2 3 7.2119 0.0020 11 2 4 -14.4946 -0.0006 11 2 5 0.0153 0.0033 11 2 6 -12.6774 0.0025 11 2 7 -4.9947 0.0031 11 2 8 -8.3988 -0.0002 11 2 9 -5.6683 0.0022 11 2 10 -6.6408 -0.0028 11 2 11 -2.0239 -0.0056 11 2 12 -4.7214 0.0056 11 2 13 2.2579 -0.0156 11 2 14 -2.1463 0.0138 11 2 15 2.9012 -0.0120 11 3 0 -1.7339 -0.0031 11 3 1 2.8936 -0.0024 11 3 2 -1.0113 -0.0025 11 3 3 5.7906 0.0010 11 3 4 -1.3007 -0.0035 11 3 5 5.1201 0.0046 11 3 6 1.4420 -0.0049 11 3 7 2.5091 -0.0011 11 3 8 5.2797 0.0004 11 3 9 -0.3745 -0.0047 11 3 10 4.4308 0.0106 11 3 11 -2.2585 0.0039 11 4 0 0.3231 -0.0005 11 4 1 3.7920 -0.0018 11 4 2 -1.9210 -0.0043 11 4 3 4.5869 -0.0036 11 4 4 -3.2977 0.0034 11 4 5 2.9982 -0.0032 11 4 6 -2.8524 0.0120 11 4 7 0.6415 -0.0119 11 4 8 -1.3734 0.0038 12 0 0 -10.0582 -0.0036 12 0 2 -6.9717 -0.0037 12 0 4 4.3484 -0.0034 12 0 6 13.4940 0.0010 12 0 8 12.0215 0.0050 12 0 10 6.8834 0.0017 12 0 12 5.9127 -0.0036 12 0 14 6.2230 -0.0031 12 1 0 -10.5674 -0.0007 12 1 1 6.8249 0.0041 12 1 2 -10.3446 0.0008 12 1 3 7.6325 0.0006 12 1 4 -5.6128 0.0018 12 1 5 3.6035 -0.0009 12 1 6 1.3312 -0.0035 12 1 7 -1.6806 -0.0001 12 1 8 5.2060 -0.0053 12 1 9 -2.0161 -0.0019 12 1 10 5.7724 0.0011 12 1 11 0.7221 -0.0024 12 1 12 4.9437 -0.0011 12 1 13 0.3458 0.0009 12 1 14 2.5190 -0.0162 12 1 15 -1.5018 0.0013 12 2 0 -2.6592 -0.0005 12 2 1 11.0029 0.0011 12 2 2 -9.9207 -0.0017 12 2 3 8.1846 0.0033 12 2 4 -15.6594 0.0009 12 2 5 2.8778 0.0027 12 2 6 -12.8422 0.0031 12 2 7 -1.5018 0.0020 12 2 8 -7.6134 -0.0014 12 2 9 -3.4309 -0.0002 12 2 10 -5.3514 -0.0025 12 2 11 -1.7235 -0.0126 12 2 12 -3.4538 0.0084 12 2 13 0.9413 -0.0252 12 3 0 -1.7790 -0.0009 12 3 1 0.8071 -0.0036 12 3 2 -2.7863 -0.0002 12 3 3 3.2506 0.0019 12 3 4 -4.0871 -0.0031 12 3 5 3.1847 0.0037 12 3 6 -1.3958 -0.0046 12 3 7 1.9608 -0.0069 12 3 8 2.8184 0.0038 12 3 9 0.2749 -0.0115 12 3 10 3.0060 0.0167 12 4 0 1.2828 -0.0011 12 4 1 4.7796 -0.0043 12 4 2 -0.7031 -0.0031 12 4 3 5.3776 -0.0080 12 4 4 -2.0741 0.0061 12 4 5 3.2069 -0.0057 12 4 6 -1.8499 0.0121 12 4 7 0.4836 -0.0114 13 0 0 -2.8997 -0.0036 13 0 2 0.7783 -0.0031 13 0 4 8.7544 -0.0006 13 0 6 12.1613 0.0047 13 0 8 8.1611 0.0048 13 0 10 3.8583 -0.0047 13 0 12 3.4012 -0.0114 13 0 14 3.6657 -0.0063 13 1 0 -12.6335 -0.0005 13 1 1 3.0980 0.0040 13 1 2 -11.3623 0.0008 13 1 3 5.2185 -0.0009 13 1 4 -4.6667 0.0002 13 1 5 2.4652 -0.0027 13 1 6 2.6682 -0.0040 13 1 7 -2.0883 -0.0016 13 1 8 5.5218 -0.0020 13 1 9 -2.0243 -0.0006 13 1 10 5.6335 0.0036 13 1 11 0.8288 0.0043 13 1 12 4.9041 -0.0041 13 1 13 0.6080 0.0097 13 1 14 2.3904 -0.0211 13 1 15 -0.8843 0.0057 13 2 0 -1.9509 -0.0012 13 2 1 8.7627 0.0009 13 2 2 -9.6591 -0.0016 13 2 3 7.1006 0.0016 13 2 4 -14.2619 0.0022 13 2 5 4.2134 -0.0002 13 2 6 -10.4951 0.0025 13 2 7 0.9634 0.0002 13 2 8 -5.4927 -0.0040 13 2 9 -1.5126 -0.0021 13 2 10 -3.8205 -0.0037 13 2 11 -1.1613 -0.0170 13 3 0 -1.5390 0.0022 13 3 1 -1.0152 -0.0035 13 3 2 -3.7597 0.0030 13 3 3 0.4350 0.0033 13 3 4 -5.5941 -0.0009 13 3 5 0.8343 0.0012 13 3 6 -2.9804 -0.0020 13 3 7 0.8440 -0.0148 13 3 8 1.1489 0.0074 13 3 9 0.2134 -0.0200 13 4 0 1.4157 -0.0011 13 4 1 4.6723 -0.0079 13 4 2 -0.2105 -0.0012 13 4 3 5.0514 -0.0126 13 4 4 -1.2350 0.0074 13 4 5 2.6757 -0.0069 13 4 6 -0.8869 0.0101 14 0 0 3.9503 -0.0008 14 0 2 6.5369 0.0002 14 0 4 9.9015 0.0034 14 0 6 8.5566 0.0070 14 0 8 3.9739 0.0012 14 0 10 1.2739 -0.0138 14 0 12 1.1873 -0.0199 14 1 0 -11.4739 0.0007 14 1 1 0.3981 0.0023 14 1 2 -8.8885 0.0016 14 1 3 3.4601 -0.0027 14 1 4 -1.9155 -0.0005 14 1 5 1.6467 -0.0038 14 1 6 3.4236 -0.0029 14 1 7 -1.9558 -0.0012 14 1 8 4.2687 0.0024 14 1 9 -1.3175 0.0042 14 1 10 4.1818 0.0055 14 1 11 1.3922 0.0147 14 1 12 3.9100 -0.0079 14 1 13 1.0448 0.0198 14 2 0 -1.8127 -0.0020 14 2 1 5.0275 -0.0005 14 2 2 -8.6014 -0.0012 14 2 3 4.8253 -0.0017 14 2 4 -11.3850 0.0027 14 2 5 4.3791 -0.0031 14 2 6 -7.3361 -0.0001 14 2 7 2.4547 0.0004 14 2 8 -3.5912 -0.0084 14 2 9 0.0889 -0.0009 14 3 0 -1.1325 0.0046 14 3 1 -2.3132 -0.0014 14 3 2 -3.7556 0.0057 14 3 3 -1.8094 0.0053 14 3 4 -5.5303 0.0024 14 3 5 -0.9503 -0.0018 14 3 6 -3.1716 0.0020 14 3 7 -0.0646 -0.0222 14 3 8 0.1816 0.0096 15 0 0 7.3150 0.0021 15 0 2 8.0719 0.0027 15 0 4 7.6993 0.0048 15 0 6 4.2730 0.0054 15 0 8 1.0403 -0.0052 15 0 10 -0.0581 -0.0224 15 0 12 -0.2177 -0.0260 15 1 0 -7.9113 0.0024 15 1 1 -0.1303 0.0006 15 1 2 -4.7322 0.0021 15 1 3 2.9967 -0.0032 15 1 4 0.7687 -0.0021 15 1 5 1.4541 -0.0033 15 1 6 3.0398 -0.0026 15 1 7 -1.3372 0.0008 15 1 8 2.2461 0.0052 15 1 9 -0.3036 0.0103 15 1 10 2.4890 0.0054 15 2 0 -2.0525 -0.0024 15 2 1 1.5179 -0.0018 15 2 2 -7.1323 -0.0003 15 2 3 2.6818 -0.0040 15 2 4 -8.2397 0.0024 15 2 5 3.9922 -0.0029 15 2 6 -4.7770 -0.0043 15 2 7 3.1205 0.0044 15 2 8 -2.6960 -0.0138 15 2 9 1.2279 0.0041 15 3 0 -0.8772 0.0048 15 3 1 -2.8807 0.0025 15 3 2 -3.0603 0.0067 15 3 3 -2.8394 0.0078 15 3 4 -4.2829 0.0055 15 3 5 -1.5492 -0.0040 15 3 6 -2.4079 0.0058 15 3 7 -0.3094 -0.0260 15 3 8 -0.3468 0.0097 16 0 0 6.5648 0.0027 16 0 2 5.9770 0.0018 16 0 4 4.0602 0.0015 16 0 6 1.2615 -0.0003 16 0 8 0.1879 -0.0121 16 0 10 -0.0945 -0.0271 16 1 0 -3.8939 0.0035 16 1 1 0.9608 0.0001 16 1 2 -1.0737 0.0010 16 1 3 3.2018 -0.0023 16 1 4 2.1295 -0.0060 16 1 5 1.3823 -0.0017 16 1 6 1.8439 -0.0053 16 1 7 -0.7701 0.0030 16 1 8 0.5660 0.0045 16 2 0 -2.1437 -0.0014 16 2 1 -0.3941 -0.0020 16 2 2 -5.4760 0.0016 16 2 3 1.5094 -0.0035 16 2 4 -5.5834 0.0016 16 2 5 3.4045 0.0015 16 2 6 -3.2810 -0.0089 16 2 7 3.0237 0.0119 16 2 8 -2.5636 -0.0182 17 0 0 3.4906 0.0012 17 0 2 2.6727 -0.0024 17 0 4 1.2861 -0.0054 17 0 6 0.4977 -0.0077 17 1 0 -1.0927 0.0033 17 1 1 2.1476 0.0003 17 1 2 0.8474 -0.0021 17 1 3 3.0001 -0.0011 17 1 4 2.0756 -0.0121 17 1 5 0.8376 -0.0007 17 1 8 -0.0678 0.0011 17 2 0 -1.7002 0.0014 17 2 1 -0.5020 -0.0010 17 2 2 -3.7675 0.0044 17 2 3 1.2411 -0.0006 17 2 4 -3.5835 0.0010 17 2 5 2.6111 0.0084 18 0 0 0.5849 -0.0001 18 0 2 0.4087 -0.0071 18 1 0 -0.0072 0.0022 18 1 1 2.2468 -0.0000 18 1 2 1.1285 -0.0058 18 1 3 1.8968 -0.0011 0 0 0 0.0 0.0 ; loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 0 -1 0.78 2.68 0 0 2 51.48 22.04 0 0 -2 60.72 25.84 0 0 -2 11.82 7.2 0 0 3 14.6 8.51 0 0 -3 7.88 7.4 0 0 -3 26.32 12.26 0 0 4 1321.52 552.74 0 0 -4 1269.46 531.33 0 0 -4 1139.06 476.59 0 0 5 5.16 12.6 0 0 5 0.49 8.22 0 0 -5 3.45 12.94 0 0 -5 6.81 10.41 0 0 6 28.37 18.2 0 0 6 32.45 16.69 0 0 -6 29.19 16.69 0 0 -6 29.97 17.47 0 0 7 9.44 13.58 0 0 7 0.78 8.66 0 0 -7 2.82 11.48 0 0 -7 5.64 10.9 0 0 8 120.13 52.01 0 0 8 168.11 70.84 0 0 -8 96.73 41.94 0 0 -8 148.31 62.96 0 0 9 2.68 12.5 0 0 9 4.62 7.2 0 0 -9 1.12 9.29 0 0 -9 5.01 9.54 0 0 10 93.28 41.02 0 0 10 126.46 53.38 0 0 -10 126.85 53.86 0 0 -10 178.52 75.27 0 0 11 0.29 5.74 0 0 11 -1.31 13.38 0 0 -11 4.28 7.69 0 0 -11 5.45 9 0 0 12 1269.46 531.33 0 0 12 1250 523.06 0 0 -12 1537.56 643.24 0 0 -12 1258.76 526.47 0 0 13 -0.15 10.95 0 0 13 1.75 4.82 0 0 14 422.63 176.92 0 0 14 376.46 158.09 0 0 15 -1.9 3.5 0 0 15 -3.11 12.26 0 0 16 499.22 209.42 0 0 16 447.16 187.13 0 0 17 -1.27 4.23 1 0 18 54.89 23.36 1 0 17 8.37 11.53 1 0 17 1.95 6.67 1 0 16 163.54 69.77 1 0 16 182.03 76.29 1 0 15 2.34 12.94 1 0 15 0.78 3.31 1 0 14 67.93 28.76 1 0 14 69.04 31.53 1 0 13 -1.85 5.16 1 0 13 9.59 12.46 1 0 12 1099.16 459.86 1 0 12 947.35 396.6 1 0 11 4.04 7.15 1 0 11 -2.34 13.23 1 0 10 542.52 227.18 1 0 10 525.98 220.56 -1 0 -9 -2.09 9.39 -1 0 -9 1.36 8.95 1 0 9 3.65 13.04 1 0 9 -0.63 6.91 -1 0 -8 243.63 102.52 -1 0 -8 291.31 122.37 1 0 8 263.23 110.5 1 0 8 232.92 98.14 -1 0 -7 -1.56 10.07 -1 0 -7 -3.89 11.43 1 0 7 0.97 8.9 1 0 7 3.45 11.39 -1 0 -6 67.05 30.7 -1 0 -6 40.58 20.48 1 0 6 62.67 29.05 1 0 6 39.8 19.46 -1 0 -5 -2.63 12.99 -1 0 -5 -1.65 11.48 1 0 5 6.23 12.7 1 0 5 5.84 10.12 -1 0 -4 298.41 125.34 -1 0 -4 341.67 143.34 1 0 4 411.59 172.39 1 0 4 273.21 114.78 -1 0 -3 5.06 6.91 1 0 3 30.12 14.69 -1 0 -2 226.25 94.88 -1 0 -2 354.47 148.5 -1 0 -1 6.03 6.18 -1 0 -1 6.03 7.59 1 0 1 -1.27 5.55 1 0 1 12.16 9.1 -1 0 0 0 1.07 -1 0 0 98.09 41.46 1 0 0 167.04 70.11 1 0 0 -0.39 1.02 -1 0 1 3.16 5.45 -1 0 1 12.46 6.71 1 0 -1 11.92 8.17 1 0 -1 5.94 4.72 -1 0 2 1664.07 696.28 -1 0 3 36.25 17.08 1 0 -3 6.71 6.52 1 0 -3 47.93 21.56 -1 0 4 45.88 21.12 1 0 -4 40.43 19.17 1 0 -4 41.21 18.93 -1 0 5 7.79 12.07 -1 0 5 3.26 11.97 1 0 -5 9.29 11.24 1 0 -5 1.99 13.28 -1 0 6 25.01 17.22 -1 0 6 27.83 15.81 1 0 -6 25.2 15.67 1 0 -6 31.29 17.27 -1 0 7 -0.39 12.89 -1 0 7 5.25 9.44 1 0 -7 -0.73 10.07 1 0 -7 0.15 10.9 -1 0 8 63.5 27.98 -1 0 8 32.79 18.88 1 0 -8 33.48 17.57 1 0 -8 59.51 26.71 -1 0 9 -2.04 7.49 -1 0 9 -3.89 12.8 1 0 -9 -1.56 8.81 1 0 -9 2.68 9.97 -1 0 10 798.95 334.61 -1 0 10 816.95 341.86 1 0 -10 803.33 336.22 1 0 -10 1050.02 439.42 -1 0 11 4.38 12.75 -1 0 11 2.24 5.74 1 0 -11 6.91 8.95 1 0 -11 1.61 7.06 -1 0 12 3.31 12.46 -1 0 12 12.07 7.49 1 0 -12 5.74 7.35 1 0 -12 2.82 8.47 -1 0 13 -0.63 11.19 -1 0 13 -0.54 4.67 1 0 -13 2.58 6.86 1 0 -13 1.41 7.74 -1 0 14 159.74 67.05 -1 0 14 162.76 69 1 0 -14 167.62 70.55 1 0 -14 154.44 65.01 -1 0 15 2.68 10.95 -1 0 15 0.83 3.65 -1 0 16 9.93 5.11 1 0 -16 4.43 6.47 -1 0 17 -1.41 2.43 2 0 18 -0.34 3.02 2 0 18 1.65 10.8 2 0 17 0.92 8.03 2 0 17 0.68 12.75 2 0 16 0.92 7.3 2 0 16 566.37 237.49 2 0 15 1.02 4.53 2 0 15 -0.92 14.5 2 0 14 311.6 131.28 2 0 14 350.72 146.85 2 0 13 0.49 5.11 2 0 13 12.12 13.92 2 0 12 31.09 14.35 2 0 12 3.75 13.38 2 0 11 0.68 6.28 2 0 11 -5.45 13.77 -2 0 -10 1260.7 527.44 -2 0 -10 1145.38 479.42 2 0 10 1129.33 472.65 2 0 10 1260.7 527.44 -2 0 -9 -2.24 10.66 -2 0 -9 -3.16 8.56 2 0 9 -2.82 8.08 2 0 9 -6.57 12.7 -2 0 -8 1994.93 834.47 -2 0 -8 2568.11 1074.35 2 0 8 1900.54 795.54 2 0 8 2154.53 901.13 -2 0 -7 -9.88 11.29 -2 0 -7 1.31 12.7 2 0 7 1.61 10.07 2 0 7 0.29 12.89 -2 0 -6 546.42 229.13 -2 0 -6 538.15 225.67 2 0 6 658.81 275.98 2 0 6 448.76 188.3 -2 0 -5 -3.16 11.68 -2 0 -5 5.45 15.47 2 0 5 3.11 15.03 2 0 5 1.65 13.28 -2 0 -4 239 101.11 -2 0 -4 184.36 78.29 2 0 4 220.9 93.57 2 0 4 242.12 102.18 -2 0 -3 0.15 9.49 -2 0 -3 -0.24 12.94 2 0 3 1.75 10.61 2 0 3 2.19 9.39 -2 0 -2 111.57 47.88 -2 0 -2 160.96 67.93 2 0 2 119.36 51.19 -2 0 -1 21.17 11.77 -2 0 -1 4.72 9.63 2 0 1 30.02 16.3 2 0 0 599.94 251.26 2 0 0 0.39 1.9 -2 0 1 0.29 1.85 2 0 -1 56.25 25.54 2 0 -1 7.79 7.44 -2 0 2 3.6 6.76 2 0 -2 434.56 182.12 2 0 -2 10.41 8.37 -2 0 3 2.68 6.57 2 0 -3 41.21 20.1 2 0 -3 65.1 28.95 -2 0 4 759.05 317.73 -2 0 4 2.63 7.79 2 0 -4 704.55 295.06 2 0 -4 702.61 294.13 -2 0 5 0.49 14.79 -2 0 5 2.09 11.53 2 0 -5 3.89 14.84 2 0 -5 -1.12 11.63 -2 0 6 1846.04 772.67 -2 0 6 1572.11 657.84 2 0 -6 1509.34 631.57 2 0 -6 1411.54 590.7 -2 0 7 8.32 14.31 -2 0 7 -10.7 13.62 2 0 -7 5.25 10.17 2 0 -7 5.55 14.4 -2 0 8 392.81 164.8 -2 0 8 417.04 175.16 2 0 -8 443.46 186.16 2 0 -8 407.7 170.93 -2 0 9 13.77 13.96 -2 0 9 0.34 8.56 2 0 -9 -3.89 10.7 2 0 -9 -1.36 8.66 -2 0 10 1837.29 768.78 -2 0 10 2201.73 921.08 2 0 -10 1783.76 746.4 2 0 -10 1891.3 791.16 -2 0 11 -4.09 13.28 -2 0 11 1.41 6.52 2 0 -11 0.88 9.49 2 0 -11 -3.36 7.74 -2 0 12 390.67 163.63 -2 0 12 342.45 143.98 2 0 -12 364 152.54 2 0 -12 365.02 153.07 -2 0 13 -6.42 10.66 -2 0 13 1.36 5.69 -2 0 17 -0.83 2.63 3 0 19 -1.36 2.34 3 0 18 1.65 3.02 3 0 18 1.36 14.4 3 0 17 -4.77 14.5 3 0 17 -1.7 8.86 3 0 16 10.61 15.47 3 0 16 -1.02 8.61 3 0 15 19.07 17.13 3 0 15 -2.68 8.03 3 0 14 116.39 51.04 3 0 14 26.91 13.04 3 0 13 1.65 14.06 3 0 13 -1.46 4.91 -3 0 -12 266.83 112.2 -3 0 -12 291.84 122.52 3 0 12 265.52 111.28 3 0 12 243.28 102.62 -3 0 -11 -3.11 10.51 -3 0 -11 -3.55 8.51 3 0 11 -3.5 6.47 3 0 11 2.04 11.77 -3 0 -10 425.21 178.18 -3 0 -10 373.98 156.92 3 0 10 367.8 154.1 3 0 10 377.92 158.77 -3 0 -9 0.24 11.19 -3 0 -9 0.05 8.76 3 0 9 -5.45 7.59 3 0 9 -13.19 13.87 -3 0 -8 2024.13 847.12 -3 0 -8 1541.45 645.19 3 0 8 1875.24 784.84 3 0 8 1861.13 779 -3 0 -7 -2.97 10.12 -3 0 -7 -4.96 14.45 3 0 7 0.34 9.88 3 0 7 -6.23 14.21 -3 0 -6 902.1 377.72 -3 0 -6 929.35 389.11 3 0 6 833.01 348.77 3 0 6 960.97 402.39 -3 0 -5 0.19 12.55 -3 0 -5 10.41 15.67 3 0 5 1.22 13.23 3 0 5 3.16 14.11 -3 0 -4 503.6 211.61 -3 0 -4 605.29 253.84 3 0 4 492.89 207.08 3 0 4 641.3 268.83 -3 0 -3 -0.63 15.42 -3 0 -3 15.03 19.32 3 0 3 -8.17 17.66 3 0 3 4.72 12.02 -3 0 -2 2918.44 1221.29 3 0 2 2932.55 1226.64 -3 0 -1 -2.53 14.06 -3 0 -1 2.24 9.73 3 0 1 -0.92 13.04 3 0 1 -0.24 3.21 -3 0 0 18.68 12.41 -3 0 0 41.07 21.17 3 0 0 10.27 13.82 -3 0 1 0 2.63 3 0 -1 4.28 9.39 3 0 -1 4.23 14.06 -3 0 2 1.17 2.87 3 0 -2 -2.14 8.61 3 0 -2 1336.61 559.55 -3 0 3 5.35 9.88 -3 0 3 10.95 13.04 3 0 -3 8.56 14.01 3 0 -3 1.61 11.09 -3 0 4 8.42 11.63 -3 0 4 4506.61 1884.97 -3 0 5 -5.74 13.19 -3 0 5 4.82 12.8 3 0 -5 -0.78 16.15 3 0 -5 -2.09 18.1 -3 0 6 8.81 13.19 -3 0 6 -3.8 12.12 3 0 -6 2.58 16.84 3 0 -6 16.74 16.01 -3 0 7 5.89 13.14 -3 0 7 -1.61 10.66 3 0 -7 -3.5 15.76 3 0 -7 -1.61 13.09 -3 0 8 5.89 12.12 -3 0 8 -3.36 8.71 3 0 -8 7.88 12.21 3 0 -8 8.86 15.62 -3 0 9 -1.85 7.4 -3 0 9 -4.72 10.9 3 0 -9 1.02 14.21 3 0 -9 -1.46 11.29 -3 0 10 255.84 107.63 -3 0 10 1.17 5.98 3 0 -10 295.01 124.27 3 0 -10 267.56 112.54 4 0 19 -43.3 22.28 4 0 19 -1.27 3.16 4 0 18 12.85 17.22 4 0 18 -0.24 3.41 4 0 17 2.43 7.3 4 0 17 2.19 15.91 4 0 16 34.06 20.78 4 0 16 -2.19 10.66 4 0 15 0 9 4 0 15 2.34 15.72 -4 0 -14 34.89 20.24 4 0 14 1.65 8.51 4 0 14 12.46 15.18 -4 0 -13 4.77 10.07 -4 0 -13 3.45 8.13 4 0 13 1.12 8.32 4 0 13 -7.64 13.96 -4 0 -12 43.65 20.29 -4 0 -12 39.51 19.41 4 0 12 27 17.08 4 0 12 53.04 23.26 -4 0 -11 3.02 8.81 -4 0 -11 -1.9 11.34 4 0 11 1.7 6.47 4 0 11 -1.85 12.7 -4 0 -10 131.71 56.34 -4 0 -10 146.51 62.04 4 0 10 112.25 47.59 4 0 10 146.26 62.62 -4 0 -9 -3.5 11.09 -4 0 -9 -2.53 8.66 4 0 9 -3.84 7.59 4 0 9 12.31 14.26 -4 0 -8 62.13 27.83 -4 0 -8 63.84 29.53 4 0 8 59.85 26.32 4 0 8 70.16 32.16 -4 0 -7 1.17 9.73 -4 0 -7 11.63 14.89 4 0 7 -1.46 13.43 4 0 7 0.05 8.9 -4 0 -6 489.49 205.62 -4 0 -6 466.28 195.6 4 0 6 463.99 194.82 4 0 6 553.23 231.75 -4 0 -5 12.94 17.61 -4 0 -5 4.72 13.67 4 0 5 3.26 14.94 4 0 5 -0.92 12.31 -4 0 -4 1755.54 734.72 -4 0 -4 1452.9 608.21 4 0 4 1830.47 765.86 4 0 4 1335.63 559.07 -4 0 -3 -0.19 18.54 -4 0 -3 12.75 18.49 4 0 3 1.51 17.71 4 0 3 -6.96 15.81 4 0 2 0.73 7.06 -4 0 -1 -3.5 15.13 -4 0 -1 -0.68 21.99 4 0 1 0.1 6.03 4 0 1 -4.77 22.04 -4 0 0 1248.05 522.09 -4 0 0 822.3 344.78 4 0 0 2.04 5.74 4 0 0 1336.61 559.55 -4 0 1 -3.11 19.75 -4 0 1 -0.15 4.72 -4 0 2 1.12 5.3 -4 0 2 2193.45 917.67 4 0 -2 2105.87 881.18 4 0 -2 9.49 14.21 -4 0 3 0.73 6.03 -4 0 3 -10.7 20.73 4 0 -3 10.8 20.63 4 0 -3 1.07 15.18 -4 0 4 1204.75 504.57 -4 0 4 1254.38 525.01 4 0 -4 -2.38 15.81 4 0 -4 1029.09 431.1 -4 0 5 6.33 14.79 -4 0 5 6.18 14.89 4 0 -5 9.44 20.97 4 0 -5 -3.55 18.49 -4 0 6 -15.33 15.03 -4 0 6 2000.29 836.9 4 0 -6 1603.73 671.47 4 0 -6 1774.52 742.99 -4 0 7 -1.02 12.31 -4 0 7 0.83 10.9 4 0 -7 -11.77 18.3 4 0 -7 1.46 14.74 -4 0 8 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5 -3 20.34 27.25 3 5 -3 14.45 9.59 -3 -5 4 26.03 15.33 -3 -5 4 18.68 19.9 3 5 -4 30.07 14.55 3 5 -4 14.89 28.61 -3 -5 5 -15.33 16.88 -3 -5 5 7.3 10.85 3 5 -5 1.99 7.98 3 5 -5 -8.42 26.13 -3 -5 6 0.97 15.38 -3 -5 6 -0.19 10.66 3 5 -6 1.8 7.88 3 5 -6 -28.22 28.42 -3 -5 7 34.94 21.07 -3 -5 7 43.55 21.65 3 5 -7 16.3 26.71 3 5 -7 25.69 13.04 -3 -5 8 32.6 20.83 -3 -5 8 28.8 15.67 3 5 -8 15.47 27.39 3 5 -8 28.12 14.11 -3 -5 9 0.29 15.42 -3 -5 9 6.23 9.73 3 5 -9 7.06 7.93 3 5 -9 4.28 30.56 3 5 -10 -13.67 29.78 -4 -5 -4 -4.43 14.99 -4 -5 -4 6.96 11.09 4 5 4 17.27 24.47 -4 -5 -3 72.4 34.11 -4 -5 -3 63.69 29 4 5 3 69 37.51 4 5 3 50.17 22.24 -4 -5 -2 -0.44 11.34 -4 -5 -2 3.26 16.59 4 5 2 -2.24 7.49 4 5 2 -34.89 28.17 -4 -5 -1 -3.31 11.19 -4 -5 -1 8.22 18.73 4 5 1 0.68 6.71 4 5 1 -9 23.74 -4 -5 0 92.98 42.43 -4 -5 0 63.84 29.34 4 5 0 115.17 56.34 4 5 0 56.2 24.62 -4 -5 1 -3.41 15.91 -4 -5 1 2.53 10.56 4 5 -1 30.12 27.78 4 5 -1 3.84 6.96 -4 -5 2 13.09 18.25 -4 -5 2 6.96 11.39 4 5 -2 -24.86 28.95 4 5 -2 10.27 8.13 -4 -5 3 13.92 12.26 -4 -5 3 30.36 21.17 4 5 -3 17.81 10.27 4 5 -3 19.32 27.59 -4 -5 4 15.96 16.98 -4 -5 4 6.33 9.63 4 5 -4 13.28 9.78 4 5 -4 9.39 27.69 -4 -5 5 42.96 24.38 -4 -5 5 11.77 11.58 4 5 -5 37.37 31.19 4 5 -5 33.28 15.96 -4 -5 6 -7.44 16.25 -4 -5 6 0.24 10.75 4 5 -6 -0.88 6.76 4 5 -6 2.29 24.52 -4 -5 7 20.44 13.96 -4 -5 7 24.67 18.59 4 5 -7 14.94 9.68 4 5 -7 23.11 27.64 -4 -5 8 12.7 11.43 -4 -5 8 12.36 16.4 4 5 -8 9.88 8.13 4 5 -8 26.81 29.1 -4 -5 9 11.34 15.47 -4 -5 9 8.66 10.07 4 5 -9 5.94 31.34 4 5 -9 10.27 8.42 4 5 -10 0 25.79 -5 -5 -3 33.18 17.81 -5 -5 -3 37.76 23.36 5 5 3 44.52 28.85 -5 -5 -2 -0.92 14.35 -5 -5 -2 -1.95 10.9 5 5 2 6.33 7.25 5 5 2 1.8 21.36 -5 -5 -1 20.29 13.72 -5 -5 -1 15.13 16.4 5 5 1 0.44 7.2 5 5 1 7.3 22.92 -5 -5 0 30.95 17.32 -5 -5 0 64.28 31.72 5 5 0 36.98 16.98 5 5 0 27.05 30.26 -5 -5 1 7.74 17.42 -5 -5 1 13.67 12.5 5 5 -1 2.14 24.04 5 5 -1 16.98 10.36 -5 -5 2 14.84 16.49 -5 -5 2 7.98 11.68 5 5 -2 25.84 30.02 5 5 -2 6.42 7.79 -5 -5 3 7.54 11.63 -5 -5 3 23.4 19.95 5 5 -3 10.51 8.66 5 5 -3 5.5 27.49 -5 -5 4 9.44 11.63 -5 -5 4 -0.49 16.74 5 5 -4 -19.37 28.22 5 5 -4 7.35 7.54 -5 -5 5 -5.06 15.81 -5 -5 5 14.5 12.07 5 5 -5 5.98 8.03 5 5 -5 -1.41 26.13 -5 -5 6 28.9 18.49 -5 -5 6 15.18 13.43 5 5 -6 25.2 28.08 5 5 -6 33.77 16.15 -5 -5 7 40.97 23.11 -5 -5 7 30.65 17.22 5 5 -7 -3.21 25.35 5 5 -7 47 20.97 -5 -5 8 -3.6 14.16 -5 -5 8 6.81 11.29 5 5 -8 -1.8 28.56 5 5 -8 2.43 7.4 5 5 -9 15.62 33.77 5 5 -9 30.46 15.52 5 5 -10 -30.07 20.97 -6 -5 -2 12.36 15.76 -6 -5 -2 -2.63 12.99 6 5 2 16.11 26.96 -6 -5 -1 5.06 12.07 -6 -5 -1 -2.29 15.62 6 5 1 6.03 7.15 6 5 1 1.8 25.4 -6 -5 0 54.35 25.3 -6 -5 0 52.35 26.57 6 5 0 72.01 39.41 6 5 0 68.65 29.78 -6 -5 1 9.49 16.3 -6 -5 1 6.13 10.9 6 5 -1 -6.23 25.93 6 5 -1 -3.7 7.01 -6 -5 2 36.64 21.99 -6 -5 2 40.34 20.73 6 5 -2 57.56 25.11 6 5 -2 31.77 29.44 -6 -5 3 -2.09 16.3 -6 -5 3 7.44 12.07 6 5 -3 -1.75 6.37 6 5 -3 -9.05 27.25 -6 -5 4 -10.41 11.68 -6 -5 4 22.77 17.95 6 5 -4 11 26.66 6 5 -4 -1.95 7.15 -6 -5 5 -6.67 16.45 -6 -5 5 1.41 11.29 6 5 -5 9.73 26.96 6 5 -5 -2.48 6.71 -6 -5 6 19.56 18.3 -6 -5 6 8.56 11.14 6 5 -6 -5.06 25.69 6 5 -6 11.77 8.17 6 5 -7 5.25 7.44 6 5 -7 14.21 27.39 6 5 -8 0.97 8.42 6 5 -8 -6.13 30.65 6 5 -9 51.77 23.31 6 5 -9 30.7 30.9 -7 -5 0 2.19 12.16 -7 -5 0 -4.48 16.49 7 5 0 12.75 27.59 7 5 0 1.56 6.71 -7 -5 1 -9.54 12.6 -7 -5 1 -1.7 14.74 7 5 -1 1.85 27.05 7 5 -1 6.23 7.2 -7 -5 2 30.22 17.03 -7 -5 2 50.55 26.27 7 5 -2 38.78 30.26 7 5 -2 46.03 20.58 -7 -5 3 -0.29 12.12 -7 -5 3 -3.99 15.62 7 5 -3 9.63 7.93 7 5 -3 5.35 26.86 -7 -5 4 -1.12 12.02 -7 -5 4 -8.13 17.22 7 5 -4 3.6 6.33 7 5 -4 3.7 26.62 -7 -5 5 22.24 17.61 -7 -5 5 -12.21 13.04 7 5 -5 -14.45 27.05 7 5 -5 -1.7 7.06 -7 -5 6 -12.36 37.56 7 5 -6 13.19 25.11 7 5 -6 6.86 9.34 7 5 -7 3.36 8.66 7 5 -7 10.17 27.2 7 5 -8 28.37 14.5 7 5 -8 10.32 28.71 7 5 -9 20 17.76 7 5 -9 32.26 16.2 -8 -5 2 11.05 16.54 -8 -5 2 13.82 13.14 8 5 -2 -25.01 27.64 8 5 -2 1.7 7.2 -8 -5 3 14.45 16.84 -8 -5 3 1.99 10.9 8 5 -3 29.63 26.76 8 5 -3 16.45 9.24 -8 -5 4 22.58 38.78 8 5 -4 -8.56 23.74 8 5 -4 10.27 8.9 8 5 -5 33.77 28.56 8 5 -5 58.19 25.74 8 5 -6 -1.51 23.6 8 5 -6 -6.47 9.1 8 5 -7 15.38 21.75 8 5 -7 9.63 9.83 8 5 -8 12.8 16.01 8 5 -8 15.91 10.8 8 5 -9 36.4 21.36 8 5 -9 30.8 16.06 9 5 -4 1.75 22.87 9 5 -5 18.3 20.24 9 5 -5 2.19 7.88 9 5 -6 4.67 15.62 9 5 -6 -7.06 9.63 9 5 -7 -6.67 14.6 9 5 -7 9.88 10.32 9 5 -8 -10.46 14.11 9 5 -8 19.46 12.26 9 5 -9 -5.11 13.53 9 5 -9 -2.82 11.43 10 5 -7 -6.62 12.89 10 5 -8 -3.45 12.65 10 5 -8 -0.39 10.22 _iucr_refine_instructions_details ; TITL p21_c_a.res in P2(1)/c p21_c_a.res created by SHELXL-2018/1 at 13:14:42 on 20-Jun-2018 REM Old TITL p21_c in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.586, Rweak 0.025, Alpha 0.070, Orientation as input REM Formula found by SHELXT: C20 N2 O6 S3 CELL 0.71073 19.557 5.417 21.739 90 102.534 90 ZERR 4 0.0039 0.0011 0.0043 0 0.03 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O S UNIT 84 76 4 16 12 DELU C12 C17 C16 C14 C13 C15 DELU C6 C1 C2 C3 C4 C5 DELU N1 C10 C9 C8 C7 DELU S3 C18 S2 SIMU 0.04 0.08 1.7 C3 C2 C1 C6 C5 C4 SIMU 0.04 0.08 1.7 C17 C16 C15 C14 C13 C12 SIMU 0.04 0.08 1.7 N1 C10 C9 C8 C7 RIGU S1 C18 L.S. 20 PLAN 20 SIZE 0.01 0.01 0.02 TEMP -173.15 LIST 6 ABIN fmap 2 acta REM REM REM WGHT 0.200000 SWAT 0.578679 2.9655 FVAR 0.34579 S1 5 0.721570 1.177450 0.246176 11.00000 0.08261 0.04196 = 0.03150 0.00083 0.00323 0.00031 S2 5 0.629073 0.823866 0.298313 11.00000 0.07881 0.05334 = 0.04727 0.00893 -0.00541 -0.01185 S3 5 0.588026 1.066598 0.171632 11.00000 0.08474 0.06898 = 0.04338 0.01026 -0.01131 -0.00676 O1 4 0.700369 1.324994 0.383622 11.00000 0.09279 0.04119 = 0.02711 -0.00213 0.01499 0.01976 O3 4 0.516290 0.552463 0.074053 11.00000 0.09680 0.06422 = 0.03330 -0.00512 -0.01129 0.02738 O4 4 0.443877 0.776386 0.004309 11.00000 0.13525 0.03780 = 0.04245 -0.00862 -0.02548 0.02697 AFIX 143 H4 2 0.452799 0.673414 -0.021758 11.00000 -1.50000 AFIX 0 O2 4 0.830435 0.624172 0.433883 11.00000 0.10547 0.03418 = 0.05876 0.01336 0.00579 0.03197 N1 3 0.761888 0.972403 0.423518 11.00000 0.07887 0.03921 = 0.01666 -0.00889 -0.00207 -0.01115 C6 1 0.697853 0.772970 0.492305 11.00000 0.07619 0.02269 = 0.02431 -0.00210 -0.00128 0.00190 AFIX 43 H6 2 0.685674 0.644691 0.462115 11.00000 -1.20000 AFIX 0 C1 1 0.741434 0.964226 0.481012 11.00000 0.05526 0.03675 = 0.02385 0.00315 -0.00657 0.00533 C7 1 0.739307 1.161150 0.377432 11.00000 0.07368 0.04147 = 0.02978 -0.00341 -0.01103 -0.00107 C5 1 0.672169 0.767436 0.546726 11.00000 0.07226 0.03983 = 0.03347 -0.00552 0.00618 -0.00282 AFIX 43 H5 2 0.642226 0.638096 0.554279 11.00000 -1.20000 AFIX 0 C9 1 0.806539 0.838347 0.333126 11.00000 0.06584 0.02752 = 0.03126 -0.00518 -0.00556 -0.00436 AFIX 13 H9 2 0.776022 0.717799 0.304908 11.00000 -1.20000 AFIX 0 C4 1 0.692229 0.963748 0.591544 11.00000 0.07053 0.03930 = 0.02953 -0.00856 0.00453 0.00071 AFIX 43 H4A 2 0.676782 0.965071 0.630068 11.00000 -1.20000 AFIX 0 C17 1 0.924885 1.097056 0.245206 11.00000 0.05331 0.03819 = 0.04875 -0.00535 0.00402 -0.00068 AFIX 43 H17 2 0.947841 1.197754 0.279246 11.00000 -1.20000 AFIX 0 C12 1 0.888054 0.892646 0.258660 11.00000 0.06678 0.03821 = 0.04501 -0.00725 -0.00504 0.00033 C2 1 0.757719 1.158832 0.523338 11.00000 0.07042 0.02605 = 0.03523 0.00482 -0.00795 -0.00571 AFIX 43 H2 2 0.784652 1.294754 0.514343 11.00000 -1.20000 AFIX 0 C8 1 0.773436 1.110029 0.323512 11.00000 0.08380 0.02992 = 0.03721 -0.00588 0.00578 -0.00151 AFIX 13 H8 2 0.814354 1.224972 0.329383 11.00000 -1.20000 AFIX 0 C3 1 0.734622 1.151169 0.577324 11.00000 0.09202 0.02836 = 0.03789 -0.00634 -0.00037 -0.00046 AFIX 43 H3 2 0.747991 1.280237 0.607091 11.00000 -1.20000 AFIX 0 C10 1 0.804164 0.789552 0.403355 11.00000 0.08308 0.02956 = 0.04064 -0.00258 -0.00533 -0.00543 C19 1 0.509056 0.872899 0.175104 11.00000 0.09158 0.06567 = 0.04744 -0.02048 0.01280 0.02200 AFIX 23 H19A 2 0.522937 0.698942 0.184620 11.00000 -1.20000 H19B 2 0.485899 0.935009 0.208277 11.00000 -1.20000 AFIX 0 C14 1 0.860701 0.813337 0.144491 11.00000 0.07373 0.05482 = 0.03832 -0.00878 -0.01237 0.00076 AFIX 43 H14 2 0.838580 0.717086 0.109236 11.00000 -1.20000 AFIX 0 C13 1 0.853111 0.751382 0.204233 11.00000 0.06989 0.03514 = 0.05020 -0.00646 0.01554 -0.00983 AFIX 43 H13 2 0.824652 0.614554 0.209751 11.00000 -1.20000 AFIX 0 C15 1 0.901019 1.017998 0.136141 11.00000 0.08314 0.06641 = 0.03239 0.01826 -0.00600 0.00394 AFIX 43 H15 2 0.908415 1.058665 0.095575 11.00000 -1.20000 AFIX 0 C18 1 0.643381 1.010846 0.245771 11.00000 0.07583 0.04014 = 0.01055 -0.01074 0.00764 0.00762 C11 1 0.884143 0.823843 0.323494 11.00000 0.07209 0.05315 = 0.06182 0.00124 0.01647 0.00340 AFIX 23 H11A 2 0.914212 0.936288 0.353686 11.00000 -1.20000 H11B 2 0.902110 0.653764 0.332367 11.00000 -1.20000 AFIX 0 C16 1 0.929746 1.159226 0.187520 11.00000 0.08694 0.03697 = 0.05736 0.00251 0.00280 0.00673 AFIX 43 H16 2 0.953905 1.306375 0.181507 11.00000 -1.20000 AFIX 0 C20 1 0.460819 0.892108 0.111963 11.00000 0.06703 0.05633 = 0.02562 -0.01207 0.00002 0.01105 AFIX 23 H20A 2 0.460191 1.065327 0.097331 11.00000 -1.20000 H20B 2 0.412796 0.849538 0.116106 11.00000 -1.20000 AFIX 0 C21 1 0.481368 0.722580 0.061730 11.00000 0.08118 0.05842 = 0.04165 -0.00148 -0.01867 0.00894 HKLF 4 REM p21_c_a.res in P2(1)/c REM R1 = 0.1801 for 1269 Fo > 4sig(Fo) and 0.3022 for all 2537 data REM 264 parameters refined using 141 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.063, deepest hole -1.106, 1-sigma level 0.258 Q1 1 0.6941 0.7797 0.2984 11.00000 0.05 1.06 Q2 1 0.5212 1.0183 0.2402 11.00000 0.05 1.01 Q3 1 0.6941 0.9551 0.4065 11.00000 0.05 0.97 Q4 1 0.7778 1.1625 0.2527 11.00000 0.05 0.90 Q5 1 0.3884 0.8299 -0.0071 11.00000 0.05 0.85 Q6 1 0.6592 1.1961 0.2494 11.00000 0.05 0.82 Q7 1 0.8087 0.7398 0.1589 11.00000 0.05 0.82 Q8 1 0.7504 0.6344 0.2084 11.00000 0.05 0.78 Q9 1 0.5659 0.8198 0.2909 11.00000 0.05 0.74 Q10 1 0.5271 0.8216 0.1888 11.00000 0.05 0.72 Q11 1 0.4791 1.1589 0.2188 11.00000 0.05 0.68 Q12 1 0.6230 0.7901 0.5299 11.00000 0.05 0.68 Q13 1 1.0025 1.1663 0.1970 11.00000 0.05 0.66 Q14 1 0.6764 0.8381 0.3714 11.00000 0.05 0.65 Q15 1 0.5199 1.1777 0.1821 11.00000 0.05 0.64 Q16 1 0.7349 0.8084 0.5700 11.00000 0.05 0.63 Q17 1 0.8741 0.8419 0.4070 11.00000 0.05 0.63 Q18 1 0.7678 0.4444 0.1754 11.00000 0.05 0.62 Q19 1 0.9343 0.2599 0.4632 11.00000 0.05 0.62 Q20 1 0.7883 0.4659 0.2271 11.00000 0.05 0.60 REM The information below was added by Olex2. REM REM R1 = 0.1801 for 1269 Fo > 4sig(Fo) and 0.3022 for all 16161 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.06, deepest hole -1.11 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.3022 REM R1_gt = 0.1801 REM wR_ref = 0.4696 REM GOOF = 1.226 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 16161 REM Reflections_gt = 1269 REM Parameters = n/a REM Hole = -1.11 REM Peak = 1.06 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received' # start Validation Reply Form _vrf_RINTA01_p21_c_a ; PROBLEM: The value of Rint is greater than 0.25 RESPONSE: The crystals were ultra thin needles that diffracted very weakly. So, all the alerts regarding Rint, high R1 (and wR2), low bond precision arise because of the weak signal from the microcrystals. Synchrotron radiation was required to get diffraction from the crystals. ; _vrf_THETM01_p21_c_a ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: As for the reasons written above ; _vrf_PLAT020_p21_c_a ; PROBLEM: The Value of Rint is Greater Than 0.12 ......... 0.427 Report RESPONSE: As for the reasons written above ; _vrf_PLAT029_p21_c_a ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.818 Why? RESPONSE: Synchrotron radiation was required to get diffraction from the crystals. Data from Synchrotron sources are collected on one axis and typically have completion values less than 100%. ; _vrf_PLAT084_p21_c_a ; PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.47 Report RESPONSE: As for the reasons written above ; _vrf_PLAT082_p21_c_a ; PROBLEM: High R1 Value .................................. 0.18 Report RESPONSE: As for the reasons written above ; _vrf_PLAT340_p21_c_a ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02068 Ang. RESPONSE: As for the reasons written above ; # end Validation Reply Form