#======================================================================= data_global #======================================================================= _audit_creation_method 'Jana2006 Version : 28/01/2013' # 1. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_paper_category ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full 'Acta Crystallographica Section C' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 2. SUBMISSION DETAILS _publ_contact_author_name ? _publ_contact_author_address ; ? ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_requested_journal 'Acta Crystallographica Section C' _publ_requested_category ? _publ_contact_letter ; ? ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ? # name ; ? # footnote ; ; ? # address ; #======================================================================= # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_introduction ; ? ; _publ_section_experimental ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_exptl_solution ; ? ; _publ_section_discussion ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; Petricek, V., Dusek, M. & Palatinus L. (2006). Jana2006. Structure Determination Software Programs. Institute of Physics, Praha, Czech Republic. Palatinus L. & Chapuis G. (2007). J. Appl. Cryst. 40, 786-790. # enable this reference if Diamond ver. 2 was used for visualization #Brandenburg, K. (1999). DIAMOND. Version. 2.1c. #Crystal Impact GbR, Bonn, Germany. # enable this reference if Diamond ver. 3 was used for visualization #Brandenburg, K. & Putz, H. (2005). DIAMOND Version 3. #Crystal Impact GbR, Postfach 1251, D-53002 Bonn, Germany. # enable this reference if SIR97 was used for solving of the structure #Altomare, A., Burla, M. C., Camalli, M., Cascarano, G., Giacovazzo, C., #Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R. (1997). #SIR97. A Package for Crystal Structure Solution by Direct Methods #and Refinement, Bari, Rome, Italy. # use this reference if SIR2002 was used for solving of the structure #Burla, M.C., Camalli, M., Carrozzini, B., Cascarano, G., Giacovazzo, C., #Polidori, G., Spagna, R. #SIR2002: the program, J. Appl. Cryst, (2003). 36, 1103 # enable this reference if bond valences were calculated #Brown, I. D. (1996). J. Appl. Cryst. 29, 479-480. # enable this reference if Xshape wase used for crystal shape refinement #Stoe & Cie (1998). X-SHAPE. Stoe & Cie, Darmstadt, Germany. # enable this reference if Flack coefficient was refined #Flack, H. D. (1983). Acta Cryst. A39, 876-881. ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ? ; #======================================================================= data_I #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Fe2.911 H9 Na0 O15 S2' _chemical_formula_weight 475.7 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration . #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3 m' _symmetry_space_group_name_Hall '-R 3;-2"' _symmetry_Int_Tables_number 166 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z 3 -x+y,-x,z 4 y,x,-z 5 x-y,-y,-z 6 -x,-x+y,-z 7 -x,-y,-z 8 y,-x+y,-z 9 x-y,x,-z 10 -y,-x,z 11 -x+y,y,z 12 x,x-y,z 13 x+2/3,y+1/3,z+1/3 14 -y+2/3,x-y+1/3,z+1/3 15 -x+y+2/3,-x+1/3,z+1/3 16 y+2/3,x+1/3,-z+1/3 17 x-y+2/3,-y+1/3,-z+1/3 18 -x+2/3,-x+y+1/3,-z+1/3 19 -x+2/3,-y+1/3,-z+1/3 20 y+2/3,-x+y+1/3,-z+1/3 21 x-y+2/3,x+1/3,-z+1/3 22 -y+2/3,-x+1/3,z+1/3 23 -x+y+2/3,y+1/3,z+1/3 24 x+2/3,x-y+1/3,z+1/3 25 x+1/3,y+2/3,z+2/3 26 -y+1/3,x-y+2/3,z+2/3 27 -x+y+1/3,-x+2/3,z+2/3 28 y+1/3,x+2/3,-z+2/3 29 x-y+1/3,-y+2/3,-z+2/3 30 -x+1/3,-x+y+2/3,-z+2/3 31 -x+1/3,-y+2/3,-z+2/3 32 y+1/3,-x+y+2/3,-z+2/3 33 x-y+1/3,x+2/3,-z+2/3 34 -y+1/3,-x+2/3,z+2/3 35 -x+y+1/3,y+2/3,z+2/3 36 x+1/3,x-y+2/3,z+2/3 _cell_length_a 7.3401(3) _cell_length_b 7.3401(3) _cell_length_c 17.0484(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 795.46(6) loop_ _jana_cell_twin_matrix_id _jana_cell_twin_volume_fraction _jana_cell_twin_matrix_1_1 _jana_cell_twin_matrix_1_2 _jana_cell_twin_matrix_1_3 _jana_cell_twin_matrix_2_1 _jana_cell_twin_matrix_2_2 _jana_cell_twin_matrix_2_3 _jana_cell_twin_matrix_3_1 _jana_cell_twin_matrix_3_2 _jana_cell_twin_matrix_3_3 ? ? ? ? ? ? ? ? ? ? ? _cell_formula_units_Z 3 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 300 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 2.9784 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 710 _exptl_absorpt_coefficient_mu 4.419 _exptl_crystal_description ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad ? _exptl_crystal_colour ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 300 _diffrn_source ? _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_monochromator ? _diffrn_measurement_device ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ? _diffrn_measurement_specimen_support ? _diffrn_reflns_number ? _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max ? _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe X-ray #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 287 _reflns_number_gt 271 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0166 _refine_ls_wR_factor_gt 0.0529 _refine_ls_R_factor_all 0.0180 _refine_ls_wR_factor_ref 0.0534 _refine_ls_goodness_of_fit_ref 2.03 _refine_ls_goodness_of_fit_gt 2.08 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 287 _refine_ls_number_parameters 31 _refine_ls_number_restraints 2 _refine_ls_number_constraints 1 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(I)+0.0004I^2^)' _refine_ls_hydrogen_treatment 'refall' _refine_ls_shift/su_max 0.0454 _refine_ls_shift/su_mean 0.0045 _refine_diff_density_max 0.15 _refine_diff_density_min -0.44 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe 0.3463 0.8444 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Na 0.0362 0.0249 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.333333 0.166667 0.166667 Uani 0.00950(19) 9 0.970(4) d . . . S1 S 0.666667 0.333333 0.02556(5) Uani 0.0107(3) 6 1 d . . . O1 O 0.666667 0.333333 -0.06013(15) Uani 0.0157(6) 6 1 d . . . O2 O 0.4472(2) 0.22362(12) 0.05494(8) Uani 0.0157(5) 18 1 d . . . O3 O 0.12726(13) 0.2545(3) 0.13504(10) Uani 0.0172(6) 18 1 d . . . O4 O 0 0 0 Uani 0.0229(11) 3 1 d . . . H1 H 0.1752(15) 0.350(3) 0.1094(16) Uiso 0.0206 18 1 d . . . H2 H -0.053(3) 0.053(3) -0.036(2) Uiso 0.046(19) 18 0.5 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 Fe 0.0074(3) 0.0098(2) 0.0105(3) 0.00368(13) 0.00027(13) 0.00014(7) S1 S 0.0119(3) 0.0119(3) 0.0082(4) 0.00594(16) 0 0 O1 O 0.0190(8) 0.0190(8) 0.0090(11) 0.0095(4) 0 0 O2 O 0.0108(8) 0.0209(6) 0.0120(7) 0.0054(4) 0.0007(5) 0.0003(3) O3 O 0.0101(6) 0.0133(8) 0.0293(9) 0.0066(4) 0.0048(3) 0.0097(7) O4 O 0.0263(14) 0.0263(14) 0.016(2) 0.0131(7) 0 0 loop_ _jana_atom_site_ADP_C_label _jana_atom_site_ADP_C_type_symbol _jana_atom_site_ADP_C_111 _jana_atom_site_ADP_C_112 _jana_atom_site_ADP_C_113 _jana_atom_site_ADP_C_122 _jana_atom_site_ADP_C_123 _jana_atom_site_ADP_C_133 _jana_atom_site_ADP_C_222 _jana_atom_site_ADP_C_223 _jana_atom_site_ADP_C_233 _jana_atom_site_ADP_C_333 ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_ADP_D_label _jana_atom_site_ADP_D_type_symbol _jana_atom_site_ADP_D_1111 _jana_atom_site_ADP_D_1112 _jana_atom_site_ADP_D_1113 _jana_atom_site_ADP_D_1122 _jana_atom_site_ADP_D_1123 _jana_atom_site_ADP_D_1133 _jana_atom_site_ADP_D_1222 _jana_atom_site_ADP_D_1223 _jana_atom_site_ADP_D_1233 _jana_atom_site_ADP_D_1333 _jana_atom_site_ADP_D_2222 _jana_atom_site_ADP_D_2223 _jana_atom_site_ADP_D_2233 _jana_atom_site_ADP_D_2333 _jana_atom_site_ADP_D_3333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_ADP_E_label _jana_atom_site_ADP_E_type_symbol _jana_atom_site_ADP_E_11111 _jana_atom_site_ADP_E_11112 _jana_atom_site_ADP_E_11113 _jana_atom_site_ADP_E_11122 _jana_atom_site_ADP_E_11123 _jana_atom_site_ADP_E_11133 _jana_atom_site_ADP_E_11222 _jana_atom_site_ADP_E_11223 _jana_atom_site_ADP_E_11233 _jana_atom_site_ADP_E_11333 _jana_atom_site_ADP_E_12222 _jana_atom_site_ADP_E_12223 _jana_atom_site_ADP_E_12233 _jana_atom_site_ADP_E_12333 _jana_atom_site_ADP_E_13333 _jana_atom_site_ADP_E_22222 _jana_atom_site_ADP_E_22223 _jana_atom_site_ADP_E_22233 _jana_atom_site_ADP_E_22333 _jana_atom_site_ADP_E_23333 _jana_atom_site_ADP_E_33333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_ADP_F_label _jana_atom_site_ADP_F_type_symbol _jana_atom_site_ADP_F_111111 _jana_atom_site_ADP_F_111112 _jana_atom_site_ADP_F_111113 _jana_atom_site_ADP_F_111122 _jana_atom_site_ADP_F_111123 _jana_atom_site_ADP_F_111133 _jana_atom_site_ADP_F_111222 _jana_atom_site_ADP_F_111223 _jana_atom_site_ADP_F_111233 _jana_atom_site_ADP_F_111333 _jana_atom_site_ADP_F_112222 _jana_atom_site_ADP_F_112223 _jana_atom_site_ADP_F_112233 _jana_atom_site_ADP_F_112333 _jana_atom_site_ADP_F_113333 _jana_atom_site_ADP_F_122222 _jana_atom_site_ADP_F_122223 _jana_atom_site_ADP_F_122233 _jana_atom_site_ADP_F_122333 _jana_atom_site_ADP_F_123333 _jana_atom_site_ADP_F_133333 _jana_atom_site_ADP_F_222222 _jana_atom_site_ADP_F_222223 _jana_atom_site_ADP_F_222233 _jana_atom_site_ADP_F_222333 _jana_atom_site_ADP_F_223333 _jana_atom_site_ADP_F_233333 _jana_atom_site_ADP_F_333333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 O2 . . 2.0377(13) ? Fe1 O2 . 18_555 2.0377(13) ? Fe1 O3 . . 1.9924(17) ? Fe1 O3 . 3_555 1.9924(10) ? Fe1 O3 . 17_555 1.992(2) ? Fe1 O3 . 18_555 1.9924(16) ? Fe1 H1 . . 2.38(2) ? Fe1 H1 . 3_555 2.384(14) ? Fe1 H1 . 17_555 2.38(3) ? Fe1 H1 . 18_555 2.38(2) ? Fe1 H2 . 13_555 2.91(3) ? Fe1 H2 . 14_555 2.91(4) ? Fe1 H2 . 4_555 2.91(3) ? Fe1 H2 . 6_555 2.91(4) ? S1 O1 . . 1.461(3) ? S1 O2 . . 1.4821(16) ? S1 O2 . 2_655 1.4821(19) ? S1 O2 . 3_665 1.4821(16) ? O1 O2 . . 2.407(2) ? O1 O2 . 2_655 2.407(3) ? O1 O2 . 3_665 2.407(2) ? O1 O3 . 4_555 2.915(2) ? O1 O3 . 5_665 2.915(2) ? O1 O3 . 6_655 2.915(2) ? O1 H1 . 4_555 2.18(2) ? O1 H1 . 5_665 2.18(2) ? O1 H1 . 6_655 2.18(2) ? O2 O2 . 2_655 2.416(2) ? O2 O2 . 3_665 2.4159(17) ? O2 O3 . . 2.822(2) ? O2 O3 . 3_555 2.8223(16) ? O2 O3 . 17_555 2.877(2) ? O2 O3 . 18_555 2.877(2) ? O2 O4 . . 2.9933(16) ? O2 H1 . . 2.75(2) ? O2 H1 . 3_555 2.752(13) ? O2 H1 . 4_555 2.87(3) ? O2 H2 . 3_555 2.67(3) ? O2 H2 . 4_555 2.593(18) ? O2 H2 . 6_555 2.59(2) ? O3 O3 . 2_555 2.8023(18) ? O3 O3 . 3_555 2.802(2) ? O3 O3 . 16_455 2.833(3) ? O3 O3 . 18_555 2.8331(14) ? O3 O4 . . 2.8139(16) ? O3 H1 . . 0.75(2) ? O3 H1 . 16_455 2.82(2) ? O3 H1 . 18_555 2.817(16) ? O3 H2 . 4_555 2.64(3) ? O3 H2 . 5_555 2.64(3) ? O3 H2 . 6_555 1.93(4) ? O4 H1 . . 2.91(2) ? O4 H1 . 2_555 2.91(2) ? O4 H1 . 3_555 2.91(2) ? O4 H1 . 4_555 2.91(2) ? O4 H1 . 5_555 2.91(2) ? O4 H1 . 6_555 2.91(2) ? O4 H2 . . 0.91(3) ? O4 H2 . 2_555 0.91(3) ? O4 H2 . 3_555 0.91(3) ? O4 H2 . 4_555 0.91(3) ? O4 H2 . 5_555 0.91(3) ? O4 H2 . 6_555 0.91(3) ? H1 H1 . 16_455 2.80(3) ? H1 H1 . 18_555 2.80(3) ? H1 H2 . 4_555 2.91(3) ? H1 H2 . 5_555 2.91(3) ? H1 H2 . 6_555 1.99(4) ? H2 H2 . 2_555 1.16(4) ? H2 H2 . 3_555 1.16(4) ? H2 H2 . 4_555 1.83(5) ? H2 H2 . 5_555 1.41(5) ? H2 H2 . 6_555 1.41(5) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag ? ? ? ? ? ? ? ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O3 H1 O1 . . 4_555 0.75(2) 2.18(2) 2.915(2) 167(3) ? O4 H2 O2 . . 2_555 0.91(3) 2.67(3) 2.9933(19) 102(3) ? O4 H2 O2 . . 4_555 0.91(3) 2.593(18) 2.9933(16) 107.2(14) ? O4 H2 O2 . . 6_555 0.91(3) 2.593(18) 2.9933(16) 107.2(14) ? O4 H2 O3 . . 4_555 0.91(3) 2.64(3) 2.8139(16) 91.2(18) ? O4 H2 O3 . . 5_555 0.91(3) 2.64(3) 2.8139(16) 91.2(18) ? O4 H2 O3 . . 6_555 0.91(3) 1.93(4) 2.8139(18) 162(3) ? #======================================================================= # 11. STRUCTURE-FACTOR LIST loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status -1 2 0 2857.30 2860.87 22.02 o 0 3 0 1349.89 1623.99 15.61 o -2 4 0 73230.10 68170.40 412.14 o -1 5 0 724.96 765.52 9.73 o -3 6 0 9622.45 9555.47 76.57 o 0 6 0 14280.90 14364.00 120.57 o -2 7 0 77.63 67.98 5.38 o -4 8 0 12645.10 12790.60 126.73 o -1 8 0 574.85 616.76 14.55 o -3 9 0 23.00 33.44 6.58 o -1 1 1 3199.09 3176.09 25.71 o 0 2 1 57258.50 55354.40 305.42 o -2 3 1 388.89 402.86 4.62 o -4 4 1 18506.30 18104.20 116.65 o -1 4 1 22.38 25.32 2.96 o -3 5 1 2455.44 2533.03 20.82 o 0 5 1 79.80 91.86 6.79 o -5 6 1 4.37 7.90 4.30 < -2 6 1 12786.30 13249.30 72.52 o -7 7 1 131.91 138.74 9.32 o -4 7 1 3.24 13.58 4.57 < -1 7 1 780.68 762.58 13.58 o -6 8 1 9135.91 9062.72 65.84 o -3 8 1 153.15 154.60 7.67 o 0 8 1 3743.91 3792.28 73.61 o -8 9 1 390.58 338.68 48.11 o -5 9 1 231.53 240.41 10.05 o -2 9 1 83.34 92.14 9.50 o 0 1 2 20993.80 21902.20 143.92 o -2 2 2 6391.38 6706.29 42.14 o -1 3 2 256.27 359.82 4.13 o -3 4 2 8252.83 8535.93 42.49 o 0 4 2 18430.20 19094.40 132.06 o -5 5 2 25.07 13.53 5.31 < -2 5 2 8528.28 8562.18 46.18 o -4 6 2 3456.04 3597.73 27.30 o -1 6 2 5155.73 5238.96 39.47 o -6 7 2 1071.34 1103.48 15.99 o -3 7 2 2719.79 2753.62 26.68 o 0 7 2 1944.47 1985.83 36.33 o -8 8 2 1394.28 1375.69 36.70 o -5 8 2 4326.45 4380.18 39.06 o -2 8 2 7297.68 7348.00 62.69 o -7 9 2 940.49 937.22 25.19 o -4 9 2 309.70 325.08 11.94 o -1 9 2 2045.05 2108.55 80.77 o 0 0 3 18599.60 18429.70 242.97 o -1 2 3 32274.60 31063.70 123.83 o -3 3 3 1899.76 1721.11 15.86 o 0 3 3 53643.30 52529.20 325.80 o -2 4 3 11158.20 11243.80 52.82 o -4 5 3 10468.50 10082.20 54.55 o -1 5 3 7556.29 7610.25 46.81 o -6 6 3 265.92 307.12 10.88 o -3 6 3 6123.45 6151.54 39.95 o 0 6 3 7998.30 7976.46 79.71 o -5 7 3 4988.15 4963.01 36.13 o -2 7 3 7017.18 7163.07 51.89 o -7 8 3 1597.87 1630.56 24.71 o -4 8 3 1343.73 1286.33 19.05 o -1 8 3 2035.58 2148.42 29.56 o -6 9 3 863.27 892.80 18.12 o -3 9 3 4915.22 4950.19 54.85 o -1 1 4 3431.39 3713.45 24.56 o 0 2 4 21444.40 20009.70 111.19 o -2 3 4 595.11 622.27 6.31 o -4 4 4 21932.40 21186.50 136.03 o -1 4 4 7908.82 8180.43 41.86 o -3 5 4 3695.74 3664.64 24.43 o 0 5 4 24.21 69.48 6.84 o -5 6 4 1843.37 1858.12 17.93 o -2 6 4 12303.70 12151.50 69.34 o -7 7 4 2843.73 2766.63 44.32 o -4 7 4 84.16 89.98 5.66 o -1 7 4 687.97 735.82 14.83 o -6 8 4 6988.45 6985.17 56.51 o -3 8 4 939.72 935.70 16.52 o 0 8 4 2225.95 2194.10 61.47 o -8 9 4 373.03 374.18 47.66 o -5 9 4 551.11 515.93 14.91 o -2 9 4 484.32 490.31 23.15 o 0 1 5 2203.33 2249.38 16.12 o -2 2 5 4128.45 3765.16 25.69 o -1 3 5 204.75 242.26 3.52 o -3 4 5 5369.81 5654.19 30.30 o 0 4 5 16753.80 17341.20 116.74 o -5 5 5 110.66 104.76 6.61 o -2 5 5 506.75 486.57 7.69 o -4 6 5 20438.20 20151.90 109.78 o -1 6 5 2356.58 2376.06 22.28 o -6 7 5 137.10 136.13 6.86 o -3 7 5 337.77 339.20 9.98 o 0 7 5 232.14 223.71 15.38 o -8 8 5 8792.48 8717.93 115.26 o -5 8 5 1895.11 1885.70 24.73 o -2 8 5 9287.35 9421.36 76.38 o -7 9 5 104.03 104.91 17.12 o -4 9 5 1.55 9.30 7.14 < -1 9 5 39.75 78.03 26.87 < 0 0 6 38913.70 36247.50 333.55 o -1 2 6 864.81 1040.03 7.97 o -3 3 6 344.36 355.69 7.51 o 0 3 6 110.02 101.13 4.87 o -2 4 6 27735.20 27516.10 125.25 o -4 5 6 1056.02 1026.81 12.57 o -1 5 6 4.24 13.85 3.69 o -6 6 6 12398.90 12275.00 102.74 o -3 6 6 560.61 551.10 10.05 o 0 6 6 10920.70 11168.70 100.61 o -5 7 6 7.99 4.73 5.58 < -2 7 6 984.90 901.17 15.54 o -7 8 6 7.80 2.71 5.78 < -4 8 6 7198.13 7196.10 62.27 o -1 8 6 29.96 32.81 8.58 o -6 9 6 121.41 120.01 12.60 o -3 9 6 3.28 10.13 11.26 < -1 1 7 38438.60 37500.60 189.80 o 0 2 7 24253.40 24210.00 149.28 o -2 3 7 2120.15 1950.08 13.93 o -4 4 7 15708.40 15805.00 109.10 o -1 4 7 5170.86 4953.82 28.54 o -3 5 7 15257.80 14463.70 87.99 o 0 5 7 1322.55 1307.21 19.93 o -5 6 7 1588.84 1576.40 18.70 o -2 6 7 1777.46 1886.93 21.57 o -7 7 7 2638.11 2670.57 41.65 o -4 7 7 4328.61 4320.81 40.83 o -1 7 7 1105.92 1100.89 19.56 o -6 8 7 3774.77 3702.66 40.75 o -3 8 7 670.33 644.69 15.21 o 0 8 7 297.50 288.63 31.12 o -5 9 7 976.84 995.06 28.89 o -2 9 7 797.14 847.72 65.09 o 0 1 8 1944.08 1607.50 14.56 o -2 2 8 12445.60 12470.00 88.59 o -1 3 8 10912.50 10521.00 52.37 o -3 4 8 2004.95 1966.42 17.27 o 0 4 8 2107.99 2076.73 25.89 o -5 5 8 4959.58 4766.82 51.64 o -2 5 8 1024.76 1080.34 13.47 o -4 6 8 5310.00 5253.25 43.56 o -1 6 8 2588.32 2687.64 26.83 o -6 7 8 4024.86 3978.86 33.79 o -3 7 8 1685.59 1750.98 22.78 o 0 7 8 394.13 405.77 21.06 o -8 8 8 3509.68 3185.52 149.90 o -5 8 8 2919.89 2983.95 34.66 o -2 8 8 1393.14 1311.22 23.25 o -4 9 8 1745.31 1673.45 47.23 o 0 0 9 45524.90 46872.80 399.54 o -1 2 9 1457.08 1430.05 10.98 o -3 3 9 289.92 308.86 9.37 o 0 3 9 9429.50 9144.40 66.70 o -2 4 9 12530.90 12410.40 63.58 o -4 5 9 1868.54 1888.88 19.91 o -1 5 9 297.71 332.09 8.07 o -6 6 9 2666.12 2580.04 37.53 o -3 6 9 24.94 47.77 6.41 o 0 6 9 7257.90 7146.20 83.46 o -5 7 9 40.30 34.62 6.48 o -2 7 9 1222.70 1276.15 20.79 o -7 8 9 487.66 498.96 28.08 o -4 8 9 4756.40 4686.33 46.33 o -1 8 9 695.19 697.51 28.35 o -1 1 10 93.59 99.96 4.90 o 0 2 10 71534.20 67987.40 457.63 o -2 3 10 141.88 142.67 4.58 o -4 4 10 19973.30 19813.30 166.63 o -1 4 10 2659.02 2543.84 21.02 o -3 5 10 4.27 6.04 4.75 < 0 5 10 51.32 68.45 8.77 o -5 6 10 2022.35 1983.38 25.84 o -2 6 10 15598.00 15560.80 101.46 o -7 7 10 204.12 231.10 15.96 o -4 7 10 159.01 148.52 9.51 o -1 7 10 5.05 15.01 7.82 < -6 8 10 5891.65 5781.52 80.97 o -3 8 10 1392.79 1419.43 28.16 o 0 1 11 165.85 202.59 7.29 o -2 2 11 20467.40 19659.70 126.28 o -1 3 11 22.23 21.22 3.52 o -3 4 11 3.19 14.66 3.95 o 0 4 11 17252.50 17205.70 139.34 o -5 5 11 9.76 29.51 8.05 o -2 5 11 68.43 85.60 6.13 o -4 6 11 9654.46 9523.07 72.55 o -1 6 11 123.99 104.88 7.47 o -6 7 11 62.49 69.24 7.51 o -3 7 11 251.59 248.88 11.29 o 0 7 11 268.83 271.38 22.67 o -5 8 11 105.23 108.03 11.57 o -2 8 11 6483.34 6426.37 129.95 o 0 0 12 2028.12 2090.95 42.36 o -1 2 12 2093.67 2193.12 16.24 o -3 3 12 862.09 833.51 17.20 o 0 3 12 4813.15 4802.42 51.44 o -2 4 12 6423.77 6368.22 43.92 o -4 5 12 2068.08 2044.85 25.77 o -1 5 12 944.84 933.09 15.24 o -6 6 12 2281.36 2216.50 44.65 o -3 6 12 4390.68 4346.07 41.91 o 0 6 12 9642.44 9594.27 106.64 o -5 7 12 282.89 251.29 11.62 o -2 7 12 1021.99 999.61 23.88 o -4 8 12 3353.92 3295.20 52.12 o -1 1 13 6631.02 7026.59 58.53 o 0 2 13 2398.30 2511.91 31.23 o -2 3 13 11025.60 10905.10 63.62 o -4 4 13 1715.19 1798.06 31.10 o -1 4 13 8686.77 8715.38 60.38 o -3 5 13 3748.31 3825.09 38.39 o 0 5 13 7131.67 7089.84 77.48 o -5 6 13 4255.33 4249.39 46.79 o -2 6 13 2331.80 2319.73 30.25 o -7 7 13 3736.01 3229.36 150.35 o -4 7 13 2658.64 2727.58 35.37 o -1 7 13 3002.83 3008.13 48.67 o 0 1 14 763.09 709.73 15.84 o -2 2 14 3928.51 4060.66 48.04 o -1 3 14 5011.28 5072.34 39.75 o -3 4 14 3209.76 3198.69 30.01 o 0 4 14 3207.48 3253.52 47.51 o -5 5 14 3599.47 3666.89 59.83 o -2 5 14 174.29 182.18 8.10 o -4 6 14 4971.85 4883.65 47.23 o -1 6 14 2274.62 2382.88 33.34 o -6 7 14 1119.56 1065.35 41.18 o -3 7 14 942.21 994.31 25.29 o 0 7 14 729.64 803.12 68.76 o 0 0 15 4005.22 4379.55 87.44 o -1 2 15 221.38 205.36 7.17 o -3 3 15 378.63 326.66 14.55 o 0 3 15 724.58 706.51 23.15 o -2 4 15 7449.15 7446.04 56.46 o -4 5 15 232.91 238.57 10.98 o -1 5 15 83.78 80.27 7.64 o -6 6 15 9383.54 8852.81 169.24 o -3 6 15 1365.48 1352.90 25.85 o 0 6 15 4262.04 4261.40 86.76 o -5 7 15 10.25 45.50 27.96 < -2 7 15 56.92 41.90 11.92 o -1 1 16 87.01 114.78 7.80 o 0 2 16 17121.70 17378.90 151.76 o -2 3 16 53.46 56.71 5.70 o -4 4 16 12778.20 12720.70 131.10 o -1 4 16 103.26 109.30 8.63 o -3 5 16 6.50 21.12 8.62 < 0 5 16 10.72 8.02 12.34 < -5 6 16 36.11 65.52 13.78 o -2 6 16 6702.73 6750.62 65.56 o -4 7 16 119.76 163.08 77.43 < 0 1 17 1139.77 1232.45 24.53 o -2 2 17 10380.80 10269.20 100.53 o -1 3 17 2957.41 3010.78 32.90 o -3 4 17 48.05 54.45 7.04 o 0 4 17 2512.29 2585.35 52.12 o -5 5 17 2341.18 2309.09 61.97 o -2 5 17 439.51 432.67 15.84 o -4 6 17 2955.53 3096.12 60.01 o -1 6 17 53.35 44.72 17.02 < 0 0 18 5101.91 4991.04 100.63 o -1 2 18 1696.23 1759.02 23.85 o -3 3 18 2751.51 2673.88 42.24 o 0 3 18 1700.38 1694.44 40.30 o -2 4 18 1720.99 1615.39 29.87 o -4 5 18 1196.97 1235.39 36.40 o -1 5 18 1415.97 1396.71 34.19 o -3 6 18 635.33 636.90 43.09 o -1 1 19 853.61 807.95 24.26 o 0 2 19 4733.41 4838.97 69.09 o -2 3 19 3088.02 3113.40 36.40 o -4 4 19 1257.30 1254.53 44.35 o -1 4 19 441.75 432.75 16.32 o -3 5 19 327.73 320.48 23.61 o 0 5 19 2258.31 2328.47 125.90 o 0 1 20 151.60 121.92 12.67 o -2 2 20 10045.20 10420.70 120.94 o -1 3 20 141.49 150.03 10.10 o -3 4 20 54.58 75.52 11.79 o 0 4 20 8437.24 8355.26 195.26 o -2 5 20 56.50 203.98 53.40 o 0 0 21 4626.74 4637.38 128.56 o -1 2 21 39.10 50.81 9.61 o -3 3 21 353.27 419.30 36.23 o 0 3 21 63.83 75.75 18.40 o -2 4 21 5546.49 5790.55 160.21 o -1 1 22 3.66 1.99 15.73 <