#======================================================================= data_global #======================================================================= _audit_creation_method 'Jana2006 Version : 11/03/2010' # 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 'Canadian Mineralogist' _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 'Canadian Mineralogist' _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 ; ; _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 'Fe0.322 Nb1 S2' _chemical_formula_weight 175 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63 2 2' _symmetry_space_group_name_Hall 'P 6c;2' 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 -x,-y,z+1/2 5 y,-x+y,z+1/2 6 x-y,x,z+1/2 7 y,x,-z 8 x-y,-y,-z 9 -x,-x+y,-z 10 -y,-x,-z+1/2 11 -x+y,y,-z+1/2 12 x,x-y,-z+1/2 _cell_length_a 5.7644 _cell_length_b 5.7644 _cell_length_c 12.1757 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 350.3748 _cell_formula_units_Z 6 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature ? _cell_special_details ; ? ; _exptl_crystal_density_diffrn 4.9749 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 8.418 _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 Cylindrical _exptl_absorpt_process_details 'Jana2006 (Petricek, Dusek & Palatinus, 2000)' _exptl_absorpt_correction_T_min 0.4119 _exptl_absorpt_correction_T_max 0.9443 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ? _diffrn_reflns_number 3820 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 29.29 _diffrn_reflns_theta_full 28.85 _diffrn_measured_fraction_theta_max 0.96 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0822 _diffrn_reflns_av_sigmaI/netI 0.0108 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 314 _reflns_number_gt 208 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_gt 0.1537 _refine_ls_R_factor_all 0.0632 _refine_ls_wR_factor_ref 0.1540 _refine_ls_goodness_of_fit_ref 8.39 _refine_ls_goodness_of_fit_gt 10.47 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 314 _refine_ls_number_parameters 19 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0418 _refine_ls_shift/su_mean 0.0125 _refine_diff_density_max 3.50 _refine_diff_density_min -2.75 _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 0.346 0.844 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Nb -2.073 0.622 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.125 0.123 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _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 Nb1 Nb 0.333333 0.666667 -0.0014(3) Uani 0.0056(13) 4 1 d . . . Nb2 Nb 0 0 0 Uani 0.006(2) 2 1 d . . . S1 S 0.333(2) 0.0029(16) 0.3710(4) Uani 0.006(3) 12 1 d . . . Fe1 Fe 0.333333 0.666667 0.25 Uani 0.010(3) 2 0.96(7) 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 Nb1 Nb 0.0050(16) 0.0050(16) 0.007(2) 0.0025(8) 0 0 Nb2 Nb 0.005(3) 0.005(3) 0.007(4) 0.0025(13) 0 0 S1 S 0.003(4) 0.001(5) 0.010(2) -0.002(4) 0.001(5) 0.000(3) Fe1 Fe 0.010(4) 0.010(4) 0.011(5) 0.0048(19) 0 0 #======================================================================= # 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 Nb1 S1 . 4_664 2.464(7) yes Nb1 S1 . 5_564 2.464(10) yes Nb1 S1 . 6_554 2.464(11) yes Nb1 S1 . 10_565 2.505(9) yes Nb1 S1 . 11_665 2.505(8) yes Nb1 S1 . 12_555 2.505(13) yes Nb2 S1 . 4_554 2.476(10) yes Nb2 S1 . 5_554 2.476(12) yes Nb2 S1 . 6_554 2.476(8) yes Nb2 S1 . 10_555 2.476(10) yes Nb2 S1 . 11_555 2.476(12) yes Nb2 S1 . 12_555 2.476(8) yes S1 Fe1 . 1_545 2.434(9) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag ? ? ? ? ? ? ? ? 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 ? ? ? ? ? ? ? ? ? ? ? #======================================================================= # 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 0 1 0 483.35 402.46 13.17 o -1 2 0 24480.16 24648.64 35.13 o 0 2 0 386.49 343.37 15.90 o -1 3 0 318.76 229.11 16.37 o 0 3 0 81465.96 79533.48 134.50 o -2 4 0 13166.56 12879.07 36.63 o -1 4 0 152.30 107.38 21.00 o 0 4 0 76.32 100.26 31.09 o -2 5 0 140.14 128.85 22.42 o -1 5 0 8357.13 8372.66 27.06 o 0 5 0 76.29 121.38 48.29 < -3 6 0 38218.98 34951.50 114.17 o -2 6 0 119.09 101.21 32.15 o -1 6 0 118.98 99.66 36.31 < 0 6 0 29253.46 27120.25 92.97 o -3 7 0 15.03 65.14 41.29 < -2 7 0 4482.44 4756.19 45.18 o 0 1 1 1387.82 1545.88 10.32 o -1 2 1 7023.34 7394.11 15.35 o 0 2 1 1159.22 1225.05 14.59 o -2 3 1 758.49 847.27 15.31 o -1 3 1 762.78 799.22 18.51 o 0 3 1 0.01 301.37 11.08 o -3 4 1 429.63 450.27 20.76 o -2 4 1 3402.79 3231.48 16.30 o -1 4 1 428.34 490.14 21.71 o 0 4 1 366.40 360.57 25.75 o -4 5 1 2449.47 2645.99 22.87 o -3 5 1 446.56 407.20 25.98 o -2 5 1 439.52 421.32 23.97 o -1 5 1 2449.47 2727.96 22.39 o 0 5 1 403.18 326.40 33.46 o -5 6 1 175.26 203.48 40.22 o -4 6 1 154.19 186.99 35.71 o -3 6 1 0.01 3149.59 28.09 o -2 6 1 152.87 227.69 35.71 o -1 6 1 182.92 210.36 37.02 o 0 6 1 0.13 5211.60 44.39 o -6 7 1 79.84 116.16 83.29 < -5 7 1 1492.61 2335.29 35.76 o -4 7 1 122.61 133.72 42.59 o -3 7 1 126.41 143.80 37.26 o -2 7 1 1492.60 2262.74 36.55 o -1 7 1 75.63 67.51 245.25 < 0 0 2 26168.98 23540.65 75.80 o 0 1 2 469.64 392.96 10.92 o -1 2 2 21213.34 21340.50 20.73 o 0 2 2 347.49 282.38 13.76 o -2 3 2 272.99 188.65 15.07 o -1 3 2 267.98 203.13 19.70 o 0 3 2 12077.11 12537.74 21.68 o -3 4 2 182.61 111.41 21.71 o -2 4 2 11911.65 11940.79 22.79 o -1 4 2 174.57 132.65 22.07 o 0 4 2 131.28 86.38 25.51 o -4 5 2 8476.80 8634.15 28.56 o -3 5 2 123.02 83.88 23.85 o -2 5 2 123.17 109.28 23.97 o -1 5 2 8476.38 8724.66 31.01 o 0 5 2 90.19 98.95 33.34 < -5 6 2 73.65 80.21 43.07 < -4 6 2 90.99 72.85 36.07 < -3 6 2 6179.08 6162.93 31.96 o -2 6 2 99.79 79.38 31.09 < -1 6 2 70.39 106.31 39.27 < 0 6 2 4886.21 5045.84 50.79 o -6 7 2 80.14 104.29 87.44 < -5 7 2 5207.61 5339.77 42.57 o -4 7 2 58.22 83.05 46.15 < -3 7 2 65.78 59.32 37.14 < -2 7 2 5208.27 5531.87 47.39 o -1 7 2 69.43 281.32 235.64 < 0 1 3 1556.51 1754.22 12.34 o -1 2 3 7056.31 7010.06 15.03 o 0 2 3 993.15 1120.16 14.48 o -2 3 3 880.76 910.63 18.75 o -1 3 3 886.33 856.53 19.70 o 0 3 3 0.00 13.61 11.95 < -3 4 3 639.90 647.35 21.48 o -2 4 3 3836.97 3656.35 17.33 o -1 4 3 639.31 611.28 27.65 o 0 4 3 519.79 514.46 25.27 o -4 5 3 2813.47 2364.48 20.89 o -3 5 3 335.23 333.28 23.85 o -2 5 3 326.75 330.08 24.56 o -1 5 3 2813.47 2730.81 31.01 o 0 5 3 186.19 246.67 37.97 o -5 6 3 249.01 208.11 41.65 o -4 6 3 332.95 285.82 35.95 o -3 6 3 0.00 21.68 24.92 < -2 6 3 330.32 249.16 36.54 o -1 6 3 258.59 234.92 41.76 o 0 6 3 0.08 123.90 37.19 o -6 7 3 200.98 232.43 100.97 < -5 7 3 1721.58 1863.58 40.67 o -4 7 3 207.18 177.38 42.95 o -3 7 3 210.90 207.40 39.63 o -2 7 3 1721.58 1753.68 43.67 o -1 7 3 197.18 184.50 226.74 < 0 0 4 7575.15 7114.18 23.97 o 0 1 4 403.56 315.25 12.10 o -1 2 4 67639.50 67776.81 53.25 o 0 2 4 267.74 173.58 13.64 o -2 3 4 193.56 167.29 17.80 o -1 3 4 192.96 156.26 16.97 o 0 3 4 4518.21 4599.06 15.90 o -3 4 4 172.93 128.26 20.05 o -2 4 4 39063.75 38331.71 42.33 o -1 4 4 172.02 113.31 27.05 o 0 4 4 204.74 129.92 24.56 o -4 5 4 27301.45 27112.26 56.73 o -3 5 4 92.46 32.98 27.41 < -2 5 4 92.54 33.58 31.56 < -1 5 4 27301.86 26704.79 49.69 o 0 5 4 92.05 51.73 37.14 < -5 6 4 27.95 61.58 41.17 < -4 6 4 39.21 50.31 35.95 < -3 6 4 1713.71 1760.80 29.91 o -2 6 4 40.23 62.29 35.59 < -1 6 4 27.52 39.04 46.04 < 0 6 4 1244.08 1406.27 39.64 o -5 7 4 15839.37 15408.67 64.80 o -4 7 4 102.18 81.75 50.66 < -3 7 4 103.00 28.00 62.41 < -2 7 4 15838.78 15888.22 87.90 o -1 7 4 40.00 59.92 167.41 < 0 1 5 753.47 802.90 13.64 o -1 2 5 3495.38 3625.65 13.61 o 0 2 5 460.55 515.77 15.19 o -2 3 5 449.61 459.53 17.09 o -1 3 5 447.53 460.59 17.80 o 0 3 5 0.01 15.43 11.55 < -3 4 5 347.62 356.78 22.66 o -2 4 5 2212.29 2031.87 20.89 o -1 4 5 349.45 357.49 25.87 o 0 4 5 279.23 285.11 23.61 o -4 5 5 1664.20 1629.07 28.96 o -3 5 5 138.78 168.48 30.37 o -2 5 5 143.44 132.06 33.22 o -1 5 5 1664.20 1538.16 23.97 o 0 5 5 61.55 92.55 38.56 < -5 6 5 130.65 123.39 44.61 < -4 6 5 189.75 137.63 42.71 o -3 6 5 0.01 12.90 31.33 < -2 6 5 189.54 133.84 36.90 o -1 6 5 125.91 104.17 46.39 < 0 6 5 0.16 52.85 46.28 < -5 7 5 1029.53 867.70 52.85 o -4 7 5 114.33 113.31 57.54 < -3 7 5 110.92 135.73 65.02 < -2 7 5 1029.53 845.07 52.38 o 0 0 6 21097.63 22297.84 60.13 o 0 1 6 282.45 199.09 14.00 o -1 2 6 11726.52 12370.09 19.23 o 0 2 6 201.99 138.58 16.49 o -2 3 6 169.65 140.01 17.68 o -1 3 6 173.65 149.26 18.27 o 0 3 6 12963.03 13403.15 25.87 o -3 4 6 139.85 83.88 26.34 o -2 4 6 7823.10 7941.62 26.66 o -1 4 6 146.65 77.48 26.70 < 0 4 6 125.04 66.44 24.44 < -4 5 6 5895.13 5897.09 33.15 o -3 5 6 76.60 75.82 32.98 < -2 5 6 76.48 81.75 32.27 < -1 5 6 5895.50 5966.00 35.37 o 0 5 6 57.45 61.93 39.51 < -5 6 6 44.26 58.02 52.21 < -4 6 6 75.38 86.61 41.29 < -3 6 6 7424.70 7612.00 40.43 o -2 6 6 67.82 59.80 40.34 < -1 6 6 47.05 23.97 45.92 < 0 6 6 5923.81 5941.08 117.26 o -5 7 6 3739.27 3273.01 58.79 o -4 7 6 73.11 42.24 63.83 < -3 7 6 66.63 80.80 73.80 < -2 7 6 3738.69 3313.29 117.97 o 0 1 7 958.31 983.60 16.85 o -1 2 7 4704.65 4883.09 14.95 o 0 2 7 867.07 876.22 17.80 o -2 3 7 658.26 712.49 19.10 o -1 3 7 652.78 709.40 22.66 o 0 3 7 0.00 25.08 15.74 < -3 4 7 434.63 457.39 27.41 o -2 4 7 3335.38 3406.96 22.39 o -1 4 7 434.70 399.73 28.83 o 0 4 7 385.27 380.74 28.95 o -4 5 7 2563.46 2400.01 27.85 o -3 5 7 420.99 393.08 36.43 o -2 5 7 429.42 370.66 35.00 o -1 5 7 2563.46 2433.64 30.94 o 0 5 7 380.91 261.62 40.82 o -5 6 7 226.24 244.77 47.70 o -4 6 7 203.65 255.57 39.51 o -3 6 7 0.00 41.14 27.77 < -2 6 7 206.85 227.45 41.76 o -1 6 7 216.55 202.41 44.37 o 0 6 7 0.03 189.65 144.47 < -5 7 7 1594.14 1174.45 102.30 o -4 7 7 169.70 124.23 79.14 < -3 7 7 166.49 67.16 143.68 < -2 7 7 1594.14 1134.41 103.57 o 0 0 8 68422.80 72703.50 95.18 o 0 1 8 175.09 106.31 16.97 o -1 2 8 11967.42 11952.02 22.15 o 0 2 8 161.61 142.97 21.71 o -2 3 8 147.73 95.04 21.00 o -1 3 8 148.65 102.99 22.78 o 0 3 8 45602.29 45197.70 48.42 o -3 4 8 79.61 60.75 31.68 < -2 4 8 7832.66 8090.83 27.45 o -1 4 8 81.07 24.92 32.63 < 0 4 8 41.11 59.32 31.68 < -4 5 8 5635.00 5658.70 34.18 o -3 5 8 77.70 75.94 36.19 < -2 5 8 77.58 75.58 36.78 < -1 5 8 5634.32 5659.81 34.65 o 0 5 8 43.70 62.41 46.15 < -5 6 8 75.07 -6.17 88.87 < -4 6 8 76.82 54.10 60.75 < -3 6 8 25899.08 25868.11 63.06 o -2 6 8 75.18 57.66 60.99 < -1 6 8 75.76 1.19 84.36 < 0 1 9 228.61 215.35 20.41 o -1 2 9 1509.87 1429.53 15.11 o 0 2 9 251.47 233.26 21.48 o -2 3 9 160.12 182.84 23.02 o -1 3 9 160.49 175.84 26.22 o 0 3 9 0.00 22.94 17.41 < -3 4 9 89.31 98.12 33.93 < -2 4 9 1142.01 1171.92 23.10 o -1 4 9 87.32 94.80 32.87 < 0 4 9 80.23 97.29 36.07 < -4 5 9 889.90 828.14 30.78 o -3 5 9 135.45 117.70 37.02 o -2 5 9 133.15 111.53 36.54 o -1 5 9 889.91 791.51 27.85 o 0 5 9 147.57 106.43 44.02 < -5 6 9 44.62 80.44 132.89 < -4 6 9 29.68 40.22 59.21 < -3 6 9 0.01 70.10 40.67 < -2 6 9 30.98 68.70 72.61 < -1 6 9 46.58 30.14 71.90 < 0 0 10 5564.80 6019.17 58.31 o 0 1 10 117.13 93.50 22.42 o -1 2 10 10013.35 9304.29 25.95 o 0 2 10 118.31 74.39 24.56 o -2 3 10 100.02 76.88 26.10 < -1 3 10 97.15 79.38 31.56 < 0 3 10 4140.43 4050.68 28.40 o -3 4 10 65.77 61.70 36.07 < -2 4 10 7648.51 7796.19 37.42 o -1 4 10 60.76 51.02 35.59 < 0 4 10 39.43 39.51 37.73 < -4 5 10 6052.75 5889.97 42.57 o -3 5 10 65.44 37.85 40.58 < -2 5 10 65.51 25.63 47.10 < -1 5 10 6052.47 5817.18 40.19 o 0 5 10 52.65 78.19 81.99 < -4 6 10 48.17 61.70 87.80 < -3 6 10 2629.84 2284.02 83.08 o -2 6 10 53.71 34.88 91.12 < 0 1 11 570.14 613.89 28.36 o -1 2 11 3112.28 3093.73 21.36 o 0 2 11 453.46 455.97 28.83 o -2 3 11 428.73 392.85 35.12 o -1 3 11 433.37 360.81 38.44 o 0 3 11 0.00 4.98 24.53 < -3 4 11 356.51 316.32 39.04 o -2 4 11 2414.73 2461.09 37.27 o -1 4 11 356.68 331.74 42.71 o 0 4 11 312.42 316.79 42.24 o -4 5 11 1896.52 1850.13 44.54 o -3 5 11 244.68 264.23 47.46 o -2 5 11 237.68 210.01 51.97 o -1 5 11 1896.51 1719.50 55.86 o 0 5 11 170.28 246.20 140.84 < 0 0 12 2702.34 2813.73 66.70 o 0 1 12 88.93 73.21 35.24 < -1 2 12 21633.35 23155.02 51.98 o 0 2 12 69.98 33.10 39.75 < -2 3 12 54.63 68.10 40.70 < -1 3 12 53.67 36.43 48.29 < 0 3 12 1891.60 1787.62 30.46 o -3 4 12 57.13 54.93 46.15 < -2 4 12 16454.38 15785.28 63.30 o -1 4 12 55.60 53.63 48.05 < 0 4 12 71.14 30.73 53.39 < -4 5 12 12870.08 12585.85 178.65 o -3 5 12 36.81 103.46 142.14 < -2 5 12 36.93 1.07 115.21 < -1 5 12 12870.79 12579.20 171.21 o 0 1 13 70.86 81.99 36.54 < -1 2 13 597.89 715.40 30.62 o 0 2 13 35.80 63.95 39.39 < -2 3 13 48.21 125.65 51.14 < -1 3 13 48.77 39.27 74.99 < 0 3 13 0.00 29.12 35.13 < -3 4 13 49.56 37.37 79.26 < -2 4 13 470.94 434.05 64.72 o -1 4 13 51.31 32.51 97.41 < 0 4 13 40.73 63.24 111.53 < 0 0 14 8775.04 9787.95 133.32 o 0 1 14 60.30 49.83 43.19 < -1 2 14 3577.65 3786.97 38.06 o 0 2 14 40.43 55.05 42.59 < -2 3 14 39.13 52.21 73.09 < -1 3 14 40.93 -10.56 114.38 < 0 3 14 6983.98 6194.90 68.99 o 0 1 15 312.47 359.98 51.02 o -1 2 15 1836.83 2161.70 41.70 o 0 2 15 300.24 362.00 68.82 o -2 3 15 261.35 144.16 109.39 < -1 2 16 3771.97 3950.51 105.23 o