#------------------------------------------------------------------------------ #$Date: 2016-09-17 04:25:38 +0300 (Sat, 17 Sep 2016) $ #$Revision: 186602 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/79/2107954.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2107954 loop_ _publ_author_name 'Arakcheeva, Alla' 'Chernyshov, Dmitry' 'Spina, Massimo' 'Forr\'o, L\'aszl\'o' 'Horv\'ath, Endre' _publ_section_title ; CH~3~NH~3~PbI~3~: precise structural consequences of water absorption at ambient conditions ; _journal_coeditor_code DK5045 _journal_issue 5 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first ; ; _journal_paper_doi 10.1107/S2052520616010428 _journal_volume 72 _journal_year 2016 _chemical_formula_moiety 'I3 Pb, C H6 N' _chemical_formula_sum 'C H6 I3 N Pb' _chemical_formula_weight 619.97 _chemical_name_systematic ' ?' _space_group_IT_number 97 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'I 4 2' _symmetry_space_group_name_H-M 'I 4 2 2' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.88375(18) _cell_length_b 8.88375(18) _cell_length_c 12.7010(3) _cell_measurement_reflns_used 4261 _cell_measurement_temperature 293 _cell_measurement_theta_max 31.27 _cell_measurement_theta_min 2.69 _cell_volume 1002.38(4) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_structure_refinement ; Petricek, V., Dusek, M. & Palatinus L. (2014). Z. Kristallogr. 229(5), 345-352 ; _computing_structure_solution ; Palatinus L. & Chapuis G. (2007). J. Appl. Cryst. 40, 786-790 ; _diffrn_ambient_temperature 293 _diffrn_measured_fraction_theta_full 0.97 _diffrn_measured_fraction_theta_max 0.83 _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type ; dectris-CrysAlisPro-abstract goniometer imported dectris images ; _diffrn_radiation_monochromator synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.68362 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 4261 _diffrn_reflns_theta_full 23.09 _diffrn_reflns_theta_max 31.27 _diffrn_reflns_theta_min 2.69 _exptl_absorpt_coefficient_mu 23.284 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.58149 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dark grey' _exptl_crystal_density_diffrn 4.1082 _exptl_crystal_description irregular _exptl_crystal_F_000 1040 _exptl_crystal_size_max 0.0025 _exptl_crystal_size_mid 0.0020 _exptl_crystal_size_min 0.0015 _refine_diff_density_max 0.40 _refine_diff_density_min -0.36 _refine_ls_abs_structure_details ' 305 of Friedel pairs used in the refinement' _refine_ls_abs_structure_Flack 0.25(13) _refine_ls_extinction_coef 394E1(9) _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_goodness_of_fit_ref 1.19 _refine_ls_hydrogen_treatment constr _refine_ls_number_constraints 31 _refine_ls_number_parameters 67 _refine_ls_number_reflns 773 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0129 _refine_ls_R_factor_gt 0.0118 _refine_ls_shift/su_max 0.0451 _refine_ls_shift/su_mean 0.0050 _refine_ls_structure_factor_coef F _refine_ls_weighting_details w=1/(\s^2^(F)+0.0001F^2^) _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_gt 0.0149 _refine_ls_wR_factor_ref 0.0153 _reflns_number_gt 721 _reflns_number_total 773 _reflns_threshold_expression I>3\s(I) _cod_data_source_file dk5045sup1.cif _cod_data_source_block I _cod_original_cell_volume 1002.38(5) _cod_database_code 2107954 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,z 3 -y,x,z 4 y,-x,z 5 -x,y,-z 6 x,-y,-z 7 y,x,-z 8 -y,-x,-z 9 x+1/2,y+1/2,z+1/2 10 -x+1/2,-y+1/2,z+1/2 11 -y+1/2,x+1/2,z+1/2 12 y+1/2,-x+1/2,z+1/2 13 -x+1/2,y+1/2,-z+1/2 14 x+1/2,-y+1/2,-z+1/2 15 y+1/2,x+1/2,-z+1/2 16 -y+1/2,-x+1/2,-z+1/2 loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy Pb Pb1 1 1 0.74980(5) 0.0374(3) Uani d 1 I I1_1 1 1 0.5 0.0764(7) Uani d 1 I I1_2 1 1 1 0.1027(12) Uani d 1 I I2 0.28604(17) 0.78604(17) 0.75 0.0873(4) Uani d 1 C C 1.0436(15) 0.4947(16) 0.5240(14) 0.066(6) Uiso d 0.25 N N 0.934(3) 0.574(3) 0.4677(11) 0.086(3) Uiso d 0.25 H H1n 0.850381 0.603186 0.516058 0.1031 Uiso d 0.25 H H2n 0.894125 0.509388 0.4098 0.1031 Uiso d 0.25 H H3n 0.980379 0.667029 0.43688 0.1031 Uiso d 0.25 H H1c 1.030773 0.384359 0.511218 0.0791 Uiso d 0.25 H H2c 1.032076 0.51604 0.600924 0.0791 Uiso d 0.25 H H3c 1.14599 0.526734 0.500292 0.0791 Uiso d 0.25 loop_ _atom_site_aniso_label _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 _atom_site_aniso_type_symbol Pb1 0.0369(3) 0.0369(3) 0.0385(6) 0 0 0 Pb I1_1 0.0951(12) 0.0951(12) 0.0389(15) 0 0 0 I I1_2 0.142(2) 0.142(2) 0.0233(13) 0 0 0 I I2 0.0711(5) 0.0711(5) 0.1198(10) 0.0413(4) -0.0037(5) 0.0037(5) I loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0031 0.0016 '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' I -0.4991 1.7187 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' N 0.0060 0.0031 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Pb -2.7699 9.6029 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' 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_3 _geom_angle I1_1 Pb1 I1_2 . . 180.0(5) I1_1 Pb1 I2 . 1_655 90.045(12) I1_1 Pb1 I2 . 2_675 90.045(12) I1_1 Pb1 I2 . 3_765 90.045(12) I1_1 Pb1 I2 . 4_565 90.045(12) I1_2 Pb1 I2 . 1_655 89.955(12) I1_2 Pb1 I2 . 2_675 89.955(12) I1_2 Pb1 I2 . 3_765 89.955(12) I1_2 Pb1 I2 . 4_565 89.955(12) I2 Pb1 I2 1_655 2_675 179.91(2) I2 Pb1 I2 1_655 3_765 90.00(4) I2 Pb1 I2 1_655 4_565 90.00(4) I2 Pb1 I2 2_675 3_765 90.00(4) I2 Pb1 I2 2_675 4_565 90.00(4) I2 Pb1 I2 3_765 4_565 179.91(2) Pb1 I1_1 Pb1 . 5_756 180.0(5) Pb1 I1_2 Pb1 . 5_757 180.0(5) Pb1 I2 Pb1 1_455 13_646 163.59(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Pb1 I1_1 . 3.1727(7) Pb1 I1_2 . 3.1777(7) Pb1 I2 1_655 3.1733(15) Pb1 I2 2_675 3.1733(15) Pb1 I2 3_765 3.1733(15) Pb1 I2 4_565 3.1733(15) C N . 1.40(3) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N H1n I2 4_565 1.00 3.18 4.017(17) 141.93 N H2n I2 9_544 1.00 3.00 3.99(2) 173.69 N H3n I1_1 . 1.00 3.07 3.85(3) 135.68 N H3n I2 10_664 1.00 3.18 3.92(2) 131.83 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_observed_status _refln_F_squared_meas _refln_F_squared_calc 1 1 0 o 182552.00 166918.00 0 2 0 o 30568.00 31174.20 1 3 0 o 179057.00 178226.00 3 3 0 o 36372.90 35571.90 0 4 0 o 241487.00 230912.00 2 4 0 o 28399.10 28759.10 4 4 0 o 103536.00 108728.00 1 5 0 o 45366.10 46083.30 3 5 0 o 103923.00 109669.00 5 5 0 o 3399.57 3384.52 0 6 0 o 33144.70 34565.70 2 6 0 o 53924.40 55450.90 4 6 0 o 12418.70 12373.90 6 6 0 o 28402.60 29391.20 1 7 0 o 36868.10 36765.20 3 7 0 o 7211.78 7433.40 5 7 0 o 34889.20 33886.30 7 7 0 o 663.69 659.19 0 8 0 o 11845.30 11922.70 2 8 0 o 16712.00 17544.50 4 8 0 o 15069.70 14986.20 6 8 0 o 1761.54 1904.15 8 8 0 o 8053.44 8062.41 1 9 0 o 8910.37 9039.27 3 9 0 o 11657.70 11899.60 5 9 0 o 1879.94 1878.58 7 9 0 o 7362.59 7418.22 9 9 0 o 122.62 124.28 0 10 0 o 10943.30 10446.50 2 10 0 o 3186.93 3235.67 4 10 0 o 3885.08 3969.99 6 10 0 o 4244.44 4271.71 8 10 0 o 191.25 180.01 1 11 0 o 3256.93 3259.64 3 11 0 o 2823.32 2845.26 5 11 0 o 2512.89 2453.60 7 11 0 o 404.38 411.48 0 12 0 o 957.48 961.83 2 12 0 o 2927.37 2832.40 4 12 0 o 1016.88 1019.82 1 13 0 o 1155.49 1173.74 1 2 1 o 19050.60 19511.90 -1 2 1 o 18866.80 19511.70 2 3 1 o 5689.82 5391.65 -2 3 1 o 5632.58 5383.62 1 4 1 o 31938.70 31679.30 -1 4 1 o 31210.60 31668.20 3 4 1 o 9737.09 9812.25 -3 4 1 o 9816.05 9818.16 2 5 1 o 73.76 64.58 -2 5 1 o 53.47 64.20 4 5 1 o 216.77 243.51 -4 5 1 o 228.23 242.41 1 6 1 o 17804.70 17842.20 -1 6 1 o 18288.20 17863.90 3 6 1 o 7599.85 7748.65 -3 6 1 o 7919.87 7737.69 5 6 1 o 789.57 777.68 -5 6 1 o 790.10 778.99 0 7 1 < -0.13 33.35 2 7 1 o 777.83 778.31 -2 7 1 o 791.00 783.13 4 7 1 o 1036.34 1003.67 -4 7 1 o 1004.94 1001.52 6 7 1 o 168.08 175.47 -6 7 1 o 168.61 175.41 1 8 1 o 4912.44 4901.25 -1 8 1 o 4935.47 4884.70 3 8 1 o 3080.38 3115.32 -3 8 1 o 3099.35 3124.02 5 8 1 o 982.37 979.60 -5 8 1 o 990.42 977.29 7 8 1 o 54.78 49.35 -7 8 1 o 51.10 49.58 2 9 1 o 679.47 685.59 -2 9 1 o 678.42 681.78 4 9 1 o 1302.66 1266.48 -4 9 1 o 1314.79 1268.67 6 9 1 o 667.33 664.55 -6 9 1 o 660.60 664.50 8 9 1 o 71.90 71.81 -8 9 1 o 73.35 71.67 1 10 1 o 610.91 620.73 -1 10 1 o 617.75 625.70 3 10 1 o 656.43 688.39 -3 10 1 o 713.13 684.74 5 10 1 o 581.41 587.82 -5 10 1 o 599.21 589.61 7 10 1 o 229.07 233.27 -7 10 1 o 233.02 232.78 0 11 1 < 3.29 0.06 2 11 1 o 202.46 197.97 -2 11 1 o 191.52 199.12 4 11 1 o 472.04 478.37 -4 11 1 o 475.34 477.62 6 11 1 o 418.62 422.02 -6 11 1 o 412.82 422.05 1 12 1 o 21.20 23.93 -1 12 1 o 20.54 23.42 3 12 1 o 100.88 85.94 -3 12 1 o 83.36 86.75 5 12 1 o 171.62 180.16 -5 12 1 o 174.79 179.51 0 13 1 < 1.98 0.19 2 13 1 o 30.55 24.91 -2 13 1 o 24.49 24.81 1 1 2 o 15921.60 16340.80 0 2 2 o 46307.50 44472.30 2 2 2 o 104320.00 111603.00 1 3 2 o 33151.00 32980.50 -1 3 2 o 32453.60 32978.20 0 4 2 o 62616.40 63330.40 2 4 2 o 608.32 561.35 -2 4 2 o 616.02 554.14 4 4 2 o 37499.50 39091.10 1 5 2 o 5478.91 5495.79 -1 5 2 o 5384.61 5504.49 3 5 2 o 43819.10 45422.80 -3 5 2 o 42920.90 45415.30 0 6 2 o 7932.77 7684.16 2 6 2 o 19367.50 19525.50 -2 6 2 o 19675.60 19554.80 4 6 2 o 2432.36 2362.51 -4 6 2 o 2365.67 2356.57 6 6 2 o 16205.40 16338.40 1 7 2 o 14428.60 14299.40 -1 7 2 o 14406.10 14264.30 3 7 2 o 1370.57 1343.38 -3 7 2 o 1375.52 1354.30 5 7 2 o 21574.20 21095.20 -5 7 2 o 21441.70 21095.20 7 7 2 o 192.32 186.58 0 8 2 o 4569.05 4457.59 2 8 2 o 8730.58 8652.12 -2 8 2 o 8806.41 8658.99 4 8 2 o 8362.87 8202.97 -4 8 2 o 8273.35 8208.75 6 8 2 o 781.87 786.42 -6 8 2 o 755.35 791.34 8 8 2 o 6384.79 6220.64 1 9 2 o 4416.90 4447.13 -1 9 2 o 4348.16 4456.82 3 9 2 o 7136.67 7120.28 -3 9 2 o 7148.85 7119.43 5 9 2 o 910.76 924.40 -5 9 2 o 945.58 923.52 7 9 2 o 5541.83 5682.60 -7 9 2 o 5729.54 5681.62 9 9 2 o 78.49 81.01 0 10 2 o 6826.34 7079.52 2 10 2 o 1784.39 1791.63 -2 10 2 o 1860.49 1790.86 4 10 2 o 2731.15 2685.34 -4 10 2 o 2748.81 2691.88 6 10 2 o 3337.36 3294.29 -6 10 2 o 3286.01 3293.17 8 10 2 o 133.29 135.74 -8 10 2 o 137.90 138.68 1 11 2 o 2200.80 2205.34 -1 11 2 o 2228.70 2220.94 3 11 2 o 1965.05 2030.74 -3 11 2 o 2066.06 2020.41 5 11 2 o 1801.84 1838.59 -5 11 2 o 1812.77 1844.30 7 11 2 o 300.11 310.30 -7 11 2 o 298.39 310.96 0 12 2 o 639.45 653.52 2 12 2 o 2189.57 2225.06 -2 12 2 o 2195.80 2221.82 4 12 2 o 772.74 793.55 -4 12 2 o 746.76 799.10 6 12 2 o 513.59 557.15 -6 12 2 o 545.88 555.93 1 13 2 o 936.69 970.12 -1 13 2 o 974.46 955.39 3 13 2 o 535.32 514.10 -3 13 2 o 500.64 527.20 1 2 3 o 15526.00 15037.40 -1 2 3 o 15410.40 15022.40 0 3 3 < 1.58 0.04 2 3 3 o 3509.88 3243.22 -2 3 3 o 3344.66 3237.23 1 4 3 o 22760.40 22882.60 -1 4 3 o 22661.40 22898.80 3 4 3 o 8395.25 8221.22 -3 4 3 o 8303.22 8216.42 2 5 3 o 17.12 22.76 -2 5 3 o 14.75 21.90 4 5 3 o 136.21 141.62 -4 5 3 o 147.41 141.09 1 6 3 o 13495.80 13812.50 -1 6 3 o 13518.20 13800.00 3 6 3 o 5706.31 5766.65 -3 6 3 o 5799.07 5772.64 5 6 3 o 596.66 591.68 -5 6 3 o 593.23 592.24 0 7 3 < 0.26 7.69 2 7 3 o 649.60 675.81 -2 7 3 o 666.89 671.03 4 7 3 o 768.84 817.35 -4 7 3 o 802.60 820.97 6 7 3 o 154.76 145.09 -6 7 3 o 148.71 144.14 1 8 3 o 3552.48 3752.72 -1 8 3 o 3661.91 3760.06 3 8 3 o 2386.27 2320.24 -3 8 3 o 2366.45 2317.55 5 8 3 o 779.65 776.24 -5 8 3 o 783.47 775.51 7 8 3 o 41.22 39.40 -7 8 3 o 45.96 39.73 0 9 3 < 0.53 3.12 2 9 3 o 554.07 568.58 -2 9 3 o 582.01 574.02 4 9 3 o 976.72 985.50 -4 9 3 o 969.88 980.79 6 9 3 o 523.12 542.13 -6 9 3 o 563.97 544.36 8 9 3 o 59.39 58.29 -8 9 3 o 64.92 57.84 1 10 3 o 460.46 451.75 -1 10 3 o 436.87 450.45 3 10 3 o 550.02 542.61 -3 10 3 o 530.51 542.75 5 10 3 o 446.86 446.33 -5 10 3 o 461.09 446.87 7 10 3 o 182.82 185.79 -7 10 3 o 177.82 185.17 0 11 3 < 4.74 5.91 2 11 3 o 147.12 150.28 -2 11 3 o 150.28 148.12 4 11 3 o 388.17 387.73 -4 11 3 o 389.22 390.23 6 11 3 o 319.48 331.97 -6 11 3 o 328.58 330.56 1 12 3 o 18.96 15.14 -1 12 3 o 14.22 15.07 3 12 3 o 61.37 65.92 -3 12 3 o 63.34 66.01 5 12 3 o 137.24 141.29 -5 12 3 o 152.25 140.90 0 13 3 < 1.71 0.03 2 13 3 o 23.31 20.08 -2 13 3 o 21.07 20.54 1 1 4 o 132440.00 134435.00 0 2 4 o 30700.50 31407.80 2 2 4 o 312834.00 286574.00 1 3 4 o 132967.00 132880.00 -1 3 4 o 134372.00 132870.00 3 3 4 o 31796.60 32271.60 0 4 4 o 150501.00 154241.00 2 4 4 o 28762.30 28662.80 -2 4 4 o 28898.90 28613.50 4 4 4 o 71924.60 76799.80 1 5 4 o 37670.10 38142.40 -1 5 4 o 37709.10 38167.70 3 5 4 o 76267.20 79531.10 -3 5 4 o 75141.20 79536.70 5 5 4 o 4276.67 4266.00 0 6 4 o 30470.30 30202.00 2 6 4 o 40881.00 40643.80 -2 6 4 o 40675.10 40649.60 4 6 4 o 11847.10 11649.00 -4 6 4 o 11507.60 11618.40 6 6 4 o 21554.40 21447.90 1 7 4 o 28926.70 28266.70 -1 7 4 o 28251.30 28229.70 3 7 4 o 7392.84 7224.01 -3 7 4 o 7293.66 7238.14 5 7 4 o 24466.50 24617.00 -5 7 4 o 24583.60 24622.00 7 7 4 o 915.25 922.59 0 8 4 o 9991.87 9644.55 2 8 4 o 14573.50 14567.20 -2 8 4 o 14422.10 14555.60 4 8 4 o 11866.50 11392.80 -4 8 4 o 11810.50 11380.10 6 8 4 o 1957.70 1954.11 -6 8 4 o 1994.06 1951.58 8 8 4 o 5964.79 5884.74 1 9 4 o 7544.81 7507.35 -1 9 4 o 7264.48 7514.99 3 9 4 o 9134.37 9072.04 -3 9 4 o 9186.70 9073.17 5 9 4 o 1878.09 1903.11 -5 9 4 o 1875.34 1898.47 7 9 4 o 5350.49 5408.85 -7 9 4 o 5228.94 5408.31 9 9 4 o 190.72 176.26 0 10 4 o 8394.81 8222.52 2 10 4 o 2765.12 2750.53 -2 10 4 o 2778.96 2742.74 4 10 4 o 3435.51 3361.86 -4 10 4 o 3299.25 3360.02 6 10 4 o 3313.04 3230.02 -6 10 4 o 3279.63 3222.31 8 10 4 o 233.42 225.30 -8 10 4 o 252.78 227.92 1 11 4 o 2714.66 2650.50 -1 11 4 o 2799.07 2676.15 3 11 4 o 2384.11 2407.95 -3 11 4 o 2353.49 2385.80 5 11 4 o 1882.53 1894.21 -5 11 4 o 1964.89 1902.59 7 11 4 o 481.46 418.90 -7 11 4 o 409.39 418.44 0 12 4 o 827.68 859.42 2 12 4 o 2270.14 2243.26 -2 12 4 o 2252.76 2234.93 4 12 4 o 883.17 848.75 -4 12 4 o 847.94 855.90 1 13 4 o 949.07 976.62 -1 13 4 o 967.74 951.78 0 1 5 o 8.82 7.33 1 2 5 o 7701.11 7483.95 -1 2 5 o 7545.48 7476.29 2 3 5 o 2586.61 2544.31 -2 3 5 o 2615.07 2538.17 1 4 5 o 14544.00 14269.50 3 4 5 o 4074.34 3958.21 -3 4 5 o 4103.77 3959.95 0 5 5 < 6.19 1.57 2 5 5 o 93.12 84.65 -2 5 5 o 89.56 82.65 4 5 5 o 91.41 93.99 -4 5 5 o 108.00 93.73 1 6 5 o 8131.12 7987.67 -1 6 5 o 8006.10 7996.63 3 6 5 o 3585.29 3517.41 -3 6 5 o 3412.98 3511.47 5 6 5 o 301.75 315.58 -5 6 5 o 303.33 317.44 0 7 5 o 28.31 39.70 2 7 5 o 426.92 420.60 -2 7 5 o 436.02 421.02 4 7 5 o 557.12 546.66 -4 7 5 o 543.41 547.58 6 7 5 o 111.55 107.23 -6 7 5 o 106.42 106.37 1 8 5 o 2235.53 2129.91 -1 8 5 o 2093.83 2119.21 3 8 5 o 1419.42 1434.14 -3 8 5 o 1444.60 1441.08 5 8 5 o 427.11 433.66 -5 8 5 o 449.65 430.61 7 8 5 o 20.94 23.68 -7 8 5 o 31.21 24.20 0 9 5 < 1.84 7.47 2 9 5 o 334.15 334.95 -2 9 5 o 351.01 335.29 4 9 5 o 707.43 670.41 -4 9 5 o 691.88 669.05 6 9 5 o 335.71 336.29 -6 9 5 o 349.93 337.70 8 9 5 o 38.32 42.01 -8 9 5 o 40.69 41.57 1 10 5 o 252.80 251.75 -1 10 5 o 261.10 255.31 3 10 5 o 282.45 287.75 -3 10 5 o 292.73 284.47 5 10 5 o 272.96 284.11 -5 10 5 o 287.72 286.42 7 10 5 o 120.51 117.96 -7 10 5 o 113.92 117.04 0 11 5 < 5.00 1.50 2 11 5 o 107.60 103.54 -2 11 5 o 98.51 103.03 4 11 5 o 227.23 230.25 -4 11 5 o 233.29 231.21 6 11 5 o 215.10 215.90 -6 11 5 o 219.71 215.01 1 12 5 < 5.66 6.78 -1 12 5 < 10.14 6.43 3 12 5 o 35.03 35.61 -3 12 5 o 39.37 36.44 0 13 5 < -0.13 0.35 0 0 6 o 71538.00 66476.00 1 1 6 o 6017.36 6132.35 0 2 6 o 5804.44 5681.67 2 2 6 o 42051.00 42723.40 1 3 6 o 15010.10 15190.90 -1 3 6 o 14627.30 15201.70 3 3 6 o 939.89 981.03 0 4 6 o 26144.40 25789.70 2 4 6 o 1003.32 997.30 -2 4 6 o 957.83 983.39 4 4 6 o 17314.40 17921.70 1 5 6 o 4340.91 4308.36 -1 5 6 o 4241.20 4312.28 3 5 6 o 22471.20 22211.30 -3 5 6 o 22021.70 22204.50 5 5 6 o 438.52 432.30 0 6 6 o 6253.97 6349.78 2 6 6 o 9712.93 9657.36 -2 6 6 o 9919.42 9706.50 4 6 6 o 2815.30 2659.07 -4 6 6 o 2710.31 2655.27 6 6 6 o 8402.59 8615.65 1 7 6 o 8561.95 8438.45 -1 7 6 o 8470.60 8404.34 3 7 6 o 1779.35 1674.38 -3 7 6 o 1757.37 1679.28 5 7 6 o 10388.50 10657.60 -5 7 6 o 10303.90 10661.20 7 7 6 o 401.12 413.37 0 8 6 o 2886.01 2859.14 2 8 6 o 5819.39 5845.19 -2 8 6 o 5774.37 5855.61 4 8 6 o 4691.40 4677.00 -4 8 6 o 4789.18 4691.22 6 8 6 o 946.60 928.65 -6 8 6 o 972.03 936.42 8 8 6 o 3423.54 3320.99 1 9 6 o 3217.25 3171.27 -1 9 6 o 3154.21 3170.60 3 9 6 o 4192.10 4117.54 -3 9 6 o 4239.42 4128.36 5 9 6 o 976.98 989.90 -5 9 6 o 984.78 984.91 7 9 6 o 3068.76 3014.42 -7 9 6 o 3117.72 3014.59 9 9 6 o 140.27 151.43 0 10 6 o 4393.99 4324.34 2 10 6 o 1301.16 1311.91 -2 10 6 o 1291.11 1316.27 4 10 6 o 1914.40 1915.21 -4 10 6 o 1889.65 1922.26 6 10 6 o 1941.36 1880.77 -6 10 6 o 1861.32 1881.88 8 10 6 o 185.85 195.38 -8 10 6 o 196.26 199.60 1 11 6 o 1475.70 1469.29 -1 11 6 o 1544.31 1501.93 3 11 6 o 1490.31 1449.43 -3 11 6 o 1377.44 1426.98 5 11 6 o 1059.14 1116.30 -5 11 6 o 1102.09 1130.17 0 12 6 o 518.46 534.91 2 12 6 o 1407.41 1397.89 -2 12 6 o 1409.82 1390.56 4 12 6 o 571.07 554.20 0 1 7 o 10.27 9.53 1 2 7 o 3909.69 3795.98 -1 2 7 o 3820.64 3786.94 0 3 7 o 7.90 5.68 2 3 7 o 775.49 766.30 -2 3 7 o 765.34 764.46 1 4 7 o 6161.76 6112.78 -1 4 7 o 6019.93 6118.25 3 4 7 o 2264.78 2250.58 -3 4 7 o 2173.87 2251.82 0 5 7 o 81.52 66.03 2 5 7 o 9.22 3.88 -2 5 7 o 8.69 3.53 4 5 7 o 17.12 22.50 -4 5 7 o 17.12 22.17 1 6 7 o 3869.26 3783.18 -1 6 7 o 3772.76 3784.84 3 6 7 o 1477.46 1553.38 -3 6 7 o 1533.11 1551.56 5 6 7 o 133.82 143.52 -5 6 7 o 138.96 144.70 0 7 7 < 4.87 7.62 2 7 7 o 232.66 247.74 -2 7 7 o 235.83 245.30 4 7 7 o 308.58 306.87 -4 7 7 o 305.28 309.49 6 7 7 o 62.16 56.39 -6 7 7 o 57.15 55.45 1 8 7 o 1000.35 999.14 -1 8 7 o 1011.05 997.23 3 8 7 o 596.53 605.73 -3 8 7 o 596.13 607.49 5 8 7 o 242.64 221.57 -5 8 7 o 221.96 220.10 7 8 7 o 11.85 15.66 -7 8 7 o 11.32 15.88 0 9 7 < 2.90 1.13 2 9 7 o 199.96 200.71 -2 9 7 o 189.55 203.66 4 9 7 o 311.72 319.34 -4 9 7 o 310.80 316.48 6 9 7 o 189.28 187.34 -6 9 7 o 187.17 188.98 8 9 7 o 19.75 23.71 -8 9 7 o 25.55 23.39 1 10 7 o 90.61 99.22 -1 10 7 o 95.09 100.00 3 10 7 o 150.15 144.11 -3 10 7 o 138.82 142.94 5 10 7 o 135.52 129.89 -5 10 7 o 124.59 130.70 7 10 7 o 60.05 62.19 -7 10 7 o 60.84 61.75 0 11 7 < 3.16 9.40 2 11 7 o 47.01 44.72 -2 11 7 o 58.07 43.62 4 11 7 o 128.94 126.35 -4 11 7 o 126.70 127.82 6 11 7 o 96.80 107.04 -6 11 7 o 99.56 106.21 1 12 7 < 2.37 1.19 -1 12 7 < 4.21 1.09 3 12 7 < 20.15 18.52 -3 12 7 < 13.83 18.71 0 0 8 o 166517.00 163577.00 1 1 8 o 68447.80 69317.30 0 2 8 o 30832.50 30334.40 2 2 8 o 96938.50 98913.80 1 3 8 o 59372.10 61403.30 -1 3 8 o 59806.90 61417.20 3 3 8 o 22055.50 22454.70 0 4 8 o 56650.70 59266.80 2 4 8 o 22677.90 22638.60 -2 4 8 o 22155.70 22607.20 4 4 8 o 31300.90 31548.50 1 5 8 o 22266.60 22005.20 -1 5 8 o 21888.00 22007.70 3 5 8 o 33930.10 33851.20 -3 5 8 o 33298.90 33859.60 5 5 8 o 4866.14 4904.11 0 6 8 o 18699.50 18925.90 2 6 8 o 18561.90 18534.00 -2 6 8 o 18312.90 18537.40 4 6 8 o 8166.42 8418.58 -4 6 8 o 8030.66 8393.67 6 6 8 o 8882.77 9313.59 1 7 8 o 14005.90 13811.60 -1 7 8 o 13137.30 13799.50 3 7 8 o 5655.73 5653.89 -3 7 8 o 5541.71 5649.76 5 7 8 o 10545.70 10410.40 -5 7 8 o 10320.60 10415.70 7 7 8 o 1241.35 1209.58 0 8 8 o 5585.78 5574.76 2 8 8 o 8269.54 8217.01 -2 8 8 o 8107.14 8202.75 4 8 8 o 5511.87 5518.93 -4 8 8 o 5431.49 5508.57 6 8 8 o 1637.64 1675.07 -6 8 8 o 1758.62 1671.37 8 8 8 o 2693.34 2505.47 1 9 8 o 4341.19 4348.10 -1 9 8 o 4469.71 4335.07 3 9 8 o 4367.39 4388.58 -3 9 8 o 4504.15 4398.93 5 9 8 o 1554.63 1575.99 -5 9 8 o 1620.04 1565.85 7 9 8 o 2349.77 2303.22 -7 9 8 o 2294.53 2303.12 0 10 8 o 4200.24 4139.94 2 10 8 o 1761.61 1728.29 -2 10 8 o 1711.97 1725.65 4 10 8 o 2081.78 1999.80 -4 10 8 o 1993.06 1991.63 6 10 8 o 1533.73 1517.38 -6 10 8 o 1523.85 1513.02 1 11 8 o 1534.24 1489.43 -1 11 8 o 1585.05 1517.14 3 11 8 o 1410.18 1419.42 -3 11 8 o 1416.24 1394.10 5 11 8 o 955.84 954.75 -5 11 8 o 938.54 965.17 0 12 8 o 596.13 590.29 2 12 8 o 1122.82 1150.48 -2 12 8 o 1229.97 1140.45 0 1 9 o 8.30 9.44 1 2 9 o 1187.03 1263.24 -1 2 9 o 1247.56 1262.88 0 3 9 < 4.21 4.00 2 3 9 o 400.07 408.14 -2 3 9 o 404.68 407.51 1 4 9 o 2434.94 2474.91 -1 4 9 o 2471.68 2472.38 3 4 9 o 634.47 646.31 -3 4 9 o 649.49 648.15 0 5 9 < 4.08 1.99 2 5 9 o 22.39 21.61 -2 5 9 o 18.96 21.28 4 5 9 o 8.03 11.58 -4 5 9 o 13.17 11.53 1 6 9 o 1396.63 1381.66 -1 6 9 o 1351.44 1385.57 3 6 9 o 601.04 593.46 -3 6 9 o 564.66 591.09 5 6 9 o 44.64 43.18 -5 6 9 o 45.96 43.84 0 7 9 o 8.82 9.79 2 7 9 o 107.21 106.29 -2 7 9 o 104.44 105.49 4 7 9 o 129.21 130.80 -4 7 9 o 132.76 131.80 6 7 9 o 34.11 32.58 -6 7 9 o 33.05 32.18 1 8 9 o 333.48 338.54 -1 8 9 o 332.43 335.90 3 8 9 o 239.49 242.15 -3 8 9 o 236.33 244.06 5 8 9 o 78.49 75.03 -5 8 9 o 78.09 74.11 7 8 9 < 8.69 7.17 -7 8 9 < 5.79 7.32 0 9 9 < 3.69 8.66 2 9 9 o 72.69 70.44 -2 9 9 o 66.50 71.23 4 9 9 o 150.28 149.59 -4 9 9 o 146.73 148.71 6 9 9 o 72.17 74.89 -6 9 9 o 82.97 75.31 1 10 9 o 38.06 31.10 -1 10 9 o 37.40 31.79 3 10 9 o 46.35 44.36 -3 10 9 o 44.38 43.60 5 10 9 o 51.10 54.67 -5 10 9 o 59.26 55.23 0 11 9 < 3.29 0.77 2 11 9 o 24.10 23.28 -2 11 9 o 21.73 22.99 4 11 9 o 46.35 46.17 -4 11 9 o 40.56 46.49 1 1 10 o 1977.27 1899.50 0 2 10 o 295.43 274.86 2 2 10 o 8633.85 8523.62 1 3 10 o 4478.71 4353.75 -1 3 10 o 4499.85 4366.53 3 3 10 o 1071.16 1055.64 0 4 10 o 5832.96 5920.88 2 4 10 o 1525.67 1512.70 -2 4 10 o 1530.73 1507.29 4 4 10 o 4925.48 4997.97 1 5 10 o 2293.47 2328.53 -1 5 10 o 2194.39 2323.49 3 5 10 o 6178.40 6345.82 -3 5 10 o 6016.68 6352.56 5 5 10 o 761.07 807.83 0 6 10 o 3360.91 3253.97 2 6 10 o 3172.30 3171.18 -2 6 10 o 3192.16 3193.02 4 6 10 o 1889.72 1871.67 -4 6 10 o 1920.10 1873.52 6 6 10 o 2930.57 2862.44 1 7 10 o 3226.24 3260.98 -1 7 10 o 3229.64 3264.72 3 7 10 o 1378.36 1357.13 -3 7 10 o 1341.81 1354.47 5 7 10 o 3287.81 3286.83 -5 7 10 o 3371.95 3293.30 7 7 10 o 515.69 524.16 0 8 10 o 1415.37 1403.22 2 8 10 o 2568.61 2572.97 -2 8 10 o 2559.70 2578.11 4 8 10 o 1819.04 1806.68 -4 8 10 o 1811.98 1817.32 6 8 10 o 700.96 731.67 -6 8 10 o 730.09 736.10 8 8 10 o 1004.59 1108.45 1 9 10 o 1542.11 1563.42 -1 9 10 o 1534.52 1550.90 3 9 10 o 1608.53 1603.60 -3 9 10 o 1596.43 1620.35 5 9 10 o 709.50 718.98 -5 9 10 o 673.25 715.16 0 10 10 o 1779.50 1704.01 2 10 10 o 740.24 721.69 -2 10 10 o 765.66 728.95 4 10 10 o 945.92 932.97 -4 10 10 o 924.42 934.36 1 11 10 o 701.98 693.84 -1 11 10 o 696.92 716.32 3 11 10 o 732.51 705.54 -3 11 10 o 670.46 690.39 0 1 11 < 2.37 2.30 1 2 11 o 431.15 426.31 -1 2 11 o 434.18 425.12 0 3 11 < 2.50 0.49 2 3 11 o 91.53 87.57 -2 3 11 o 90.22 87.28 1 4 11 o 710.57 716.55 -1 4 11 o 667.31 717.34 3 4 11 o 249.65 247.09 -3 4 11 o 245.83 247.39 0 5 11 < 2.37 14.39 2 5 11 < 3.69 9.10 -2 5 11 < 2.90 8.96 4 5 11 < 5.14 2.34 -4 5 11 < 1.32 2.27 1 6 11 o 439.24 429.99 -1 6 11 o 440.43 430.57 3 6 11 o 187.57 174.68 -3 6 11 o 192.44 174.41 5 6 11 o 18.04 16.38 -5 6 11 < 10.53 16.43 0 7 11 < 6.58 11.91 2 7 11 o 40.30 39.84 -2 7 11 o 37.14 39.71 4 7 11 o 48.33 53.76 -4 7 11 o 51.36 53.91 6 7 11 < 11.32 10.65 -6 7 11 < 3.42 10.64 1 8 11 o 99.30 105.53 -1 8 11 o 92.98 105.07 3 8 11 o 65.45 65.97 -3 8 11 o 72.56 66.12 5 8 11 o 29.23 25.72 -5 8 11 o 26.73 25.74 7 8 11 < 2.24 3.99 -7 8 11 < 1.19 3.94 0 9 11 < -0.92 0.30 2 9 11 o 25.55 33.67 -2 9 11 o 33.58 33.83 4 9 11 o 41.61 46.18 -4 9 11 o 43.72 46.18 6 9 11 o 37.27 28.99 -6 9 11 o 32.79 28.85 1 10 11 < 8.03 8.07 -1 10 11 < 8.30 8.11 3 10 11 o 25.15 14.15 -3 10 11 < 15.41 14.14 0 11 11 < 1.19 3.48 0 2 12 o 18508.80 18215.10 2 2 12 o 28631.00 27575.20 1 3 12 o 22377.20 21979.30 -1 3 12 o 21972.40 21984.90 3 3 12 o 11591.30 11546.60 0 4 12 o 18843.70 18195.40 2 4 12 o 11960.10 11536.90 -2 4 12 o 11838.30 11528.70 4 4 12 o 10403.10 10135.50 1 5 12 o 9782.04 9701.79 -1 5 12 o 9496.67 9694.20 3 5 12 o 10777.10 10710.50 -3 5 12 o 10569.60 10711.90 5 5 12 o 3335.85 3334.75 -2 6 12 o 6643.88 6726.34 4 6 12 o 4010.42 4132.24 -4 6 12 o 3981.09 4124.02 6 6 12 o 2995.95 3059.26 1 7 12 o 5158.40 5134.88 -1 7 12 o 5040.90 5138.14 3 7 12 o 3063.72 3051.78 -3 7 12 o 3117.16 3041.68 5 7 12 o 3123.26 3229.72 -5 7 12 o 3256.82 3230.02 0 8 12 o 2542.66 2554.53 2 8 12 o 3230.24 3229.73 -2 8 12 o 3120.84 3222.08 4 8 12 o 2047.63 2065.90 -4 8 12 o 2053.22 2060.86 6 8 12 o 900.03 947.26 -6 8 12 o 942.90 944.92 1 9 12 o 1824.06 1846.01 -1 9 12 o 1982.49 1832.86 3 9 12 o 1633.18 1617.84 -3 9 12 o 1522.79 1623.48 5 9 12 o 851.23 853.67 -5 9 12 o 829.10 846.59 0 1 13 < 0.92 2.72 1 2 13 o 131.71 108.95 0 3 13 < 5.00 10.09 2 3 13 o 38.98 40.90 -2 3 13 o 42.27 40.01 1 4 13 o 207.87 202.98 -1 4 13 o 210.10 205.09 3 4 13 o 74.41 60.38 -3 4 13 o 55.71 59.45 0 5 13 < 11.06 17.61 2 5 13 < -3.03 11.94 -2 5 13 < 8.95 11.76 4 5 13 < 5.79 10.95 -4 5 13 < 6.85 10.90 1 6 13 o 125.51 117.65 3 6 13 o 45.70 50.49 -3 6 13 o 64.13 51.45