#------------------------------------------------------------------------------ #$Date: 2023-12-07 12:49:35 +0100 (Thu, 07 Dec 2023) $ #$Revision: 288136 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/29/2022917.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_2022917 loop_ _publ_author_name 'Irrou, Ezaddine' 'Ait Elmachkouri, Younesse' 'Mazzah, Ahmed' 'Hökelek, Tuncer' 'Haoudi, Amal' 'Mague, Joel T.' 'Taha, Mohamed Labd' 'Sebbar, Nada Kheira' _publ_section_title ; Crystal structure, Hirshfeld surface and crystal void analysis, inter-molecular inter-action energies, DFT calculations and energy frameworks of 2H-benzo[b][1,4]thia-zin-3(4H)-one 1,1-dioxide. ; _journal_coeditor_code WM5698 _journal_issue 'Pt 11' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 1037 _journal_page_last 1043 _journal_paper_doi 10.1107/S205698902300868X _journal_volume 79 _journal_year 2023 _chemical_formula_iupac 'C8 H7 N O3 S' _chemical_formula_moiety 'C8 H7 N O3 S' _chemical_formula_sum 'C8 H7 N O3 S' _chemical_formula_weight 197.21 _chemical_name_common ; 2,4-Dihydro-1\l^6^,4-benzothiazine-1,1,3-trione ; _chemical_name_systematic ; 2H-Benzo[b][1,4]thiazin-3(4H)-one 1,1-dioxide ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2019/1 _cell_angle_alpha 90 _cell_angle_beta 97.584(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.2179(6) _cell_length_b 9.5043(8) _cell_length_c 11.9945(9) _cell_measurement_reflns_used 9215 _cell_measurement_temperature 125(2) _cell_measurement_theta_max 36.3543 _cell_measurement_theta_min 2.8471 _cell_volume 815.64(11) _computing_cell_refinement ; SAINT (Bruker, 2021) ; _computing_data_collection ; APEX4 (Bruker, 2021) ; _computing_data_reduction ; SAINT (Bruker, 2021) ; _computing_molecular_graphics ; DIAMOND (Brandenburg & Putz, 2012) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2018/1 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 125(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device 'Bruker D8 QUEST PHOTON 3 diffractometer' _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON 3 diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_unetI/netI 0.0117 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 47688 _diffrn_reflns_theta_full 36.400 _diffrn_reflns_theta_max 36.442 _diffrn_reflns_theta_min 3.564 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 30.0 _diffrn_source_power 1.50 _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 0.366 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 408 _exptl_crystal_size_max 0.385 _exptl_crystal_size_mid 0.213 _exptl_crystal_size_min 0.162 _refine_diff_density_max 0.516 _refine_diff_density_min -0.356 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 122 _refine_ls_number_reflns 3957 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0252 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+0.2724P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.0744 _reflns_number_gt 3739 _reflns_number_total 3957 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5698sup1.cif _cod_data_source_block I _cod_depositor_comments 'Adding full bibliography for 2022917.cif.' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2022917 _cod_database_fobs_code 2022917 _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. ; _shelx_estimated_absorpt_t_min 0.872 _shelx_estimated_absorpt_t_max 0.943 _shelx_hkl_file ; -1 0 0 0.40 0.30 -1 0 0 0.10 0.20 1 0 0 0.50 0.30 1 0 0 0.10 0.30 1 0 0 0.10 0.30 1 0 0 0.30 0.30 -1 0 0 0.10 0.20 1 0 0 0.40 0.30 1 0 0 0.50 0.30 1 0 0 0.50 0.30 -1 0 0 0.60 0.30 -1 0 0 0.40 0.30 -1 0 0 0.20 0.30 -1 0 0 0.80 0.40 1 0 0 0.10 0.30 -1 0 0 0.30 0.30 -1 0 0 0.40 0.30 -2 0 0 53.89 2.40 -2 0 0 51.09 2.30 2 0 0 50.19 2.40 2 0 0 53.69 2.20 2 0 0 49.00 2.00 -2 0 0 52.49 2.10 -2 0 0 52.89 2.40 2 0 0 53.89 2.10 -2 0 0 48.50 2.00 2 0 0 55.79 2.70 -2 0 0 49.90 2.30 2 0 0 52.99 2.30 2 0 0 46.10 2.20 -2 0 0 48.00 2.20 2 0 0 51.39 2.40 2 0 0 51.19 2.00 -2 0 0 57.29 2.20 -2 0 0 49.99 2.60 2 0 0 54.19 2.40 3 0 0 1.40 0.80 -3 0 0 1.70 0.60 3 0 0 0.80 0.70 -3 0 0 1.70 0.70 -3 0 0 1.50 0.60 3 0 0 1.30 0.80 3 0 0 1.00 0.70 -3 0 0 2.00 0.80 -3 0 0 1.20 0.80 -3 0 0 1.60 0.80 -3 0 0 0.90 0.80 -3 0 0 2.10 0.80 3 0 0 1.20 0.70 3 0 0 2.50 1.00 -3 0 0 2.00 0.90 3 0 0 1.10 0.60 3 0 0 0.00 0.70 4 0 0 101.29 4.50 -4 0 0 90.69 3.80 -4 0 0 101.59 3.90 4 0 0 105.79 4.60 -4 0 0 100.99 4.10 -4 0 0 110.79 4.70 -4 0 0 98.79 5.10 -4 0 0 99.59 4.50 -4 0 0 100.29 4.40 4 0 0 100.59 4.60 4 0 0 96.99 4.00 -4 0 0 105.19 4.50 4 0 0 108.29 4.00 -4 0 0 99.39 3.90 -5 0 0 0.30 0.90 -5 0 0 1.00 0.80 -5 0 0 0.70 0.80 5 0 0 -1.20 0.70 5 0 0 0.30 0.90 -5 0 0 1.00 0.80 5 0 0 1.70 0.80 -5 0 0 1.80 1.10 5 0 0 1.30 1.20 -5 0 0 0.00 0.90 5 0 0 0.40 0.80 -6 0 0 2702.93 74.59 6 0 0 2705.43 74.89 6 0 0 2689.73 75.19 6 0 0 2659.63 74.79 6 0 0 2709.63 75.39 -6 0 0 2677.33 75.19 -6 0 0 2716.83 74.59 6 0 0 2725.83 73.59 -7 0 0 1.80 1.40 7 0 0 2.80 1.90 7 0 0 -1.50 1.30 7 0 0 0.80 1.00 -7 0 0 0.60 1.00 -7 0 0 -0.70 1.10 -7 0 0 3.10 1.60 7 0 0 2.20 1.40 7 0 0 -0.40 1.50 7 0 0 0.80 1.70 -8 0 0 108.89 6.60 -8 0 0 113.49 6.30 -8 0 0 109.99 6.50 8 0 0 106.19 6.70 -9 0 0 1.70 1.70 9 0 0 0.20 2.40 -9 0 0 2.90 2.00 9 0 0 2.40 2.10 -10 0 0 18.90 3.80 -10 0 0 20.90 4.50 10 0 0 22.90 4.80 10 0 0 20.70 4.20 11 0 0 0.80 2.70 -11 0 0 0.30 1.90 -11 0 0 2.60 2.70 11 0 0 2.80 5.00 0 -1 0 13.30 0.70 0 -1 0 14.00 0.60 0 1 0 15.60 0.70 -1 -1 0 1599.54 42.10 -1 -1 0 1533.75 42.50 -1 -1 0 1617.24 42.40 -1 -1 0 1604.64 42.40 -1 -1 0 1586.44 42.40 -1 -1 0 1520.35 42.40 1 -1 0 1531.45 42.20 -1 -1 0 1627.74 42.30 1 -1 0 1607.14 42.30 1 -1 0 1630.14 42.40 1 -1 0 1623.04 42.20 1 -1 0 1534.95 42.40 1 -1 0 1576.24 42.40 -1 -1 0 1681.83 42.20 -1 -1 0 1499.35 42.40 1 -1 0 1577.04 42.20 1 -1 0 1607.34 42.30 -1 -1 0 1575.94 42.50 1 -1 0 1529.65 42.40 1 -1 0 1665.93 42.50 -1 -1 0 1481.45 42.20 1 1 0 1583.34 42.50 1 1 0 1499.25 42.40 1 1 0 1555.24 42.40 1 1 0 1568.14 42.50 -1 1 0 1630.64 42.40 -1 1 0 1470.85 42.40 -1 1 0 1560.24 42.40 -1 1 0 1641.14 42.50 1 1 0 1629.24 42.40 -1 1 0 1620.14 42.40 1 1 0 1611.34 42.30 -1 1 0 1563.04 42.40 -1 1 0 1623.94 42.50 1 1 0 1542.45 42.30 1 1 0 1616.44 42.40 1 1 0 1535.85 42.40 -1 1 0 1525.05 42.20 -1 1 0 1620.14 42.30 -2 -1 0 1571.74 42.80 2 -1 0 1644.04 43.40 2 -1 0 1596.44 43.40 -2 -1 0 1570.44 43.40 2 -1 0 1634.84 43.50 2 -1 0 1559.94 43.40 2 -1 0 1615.14 43.00 2 -1 0 1621.74 43.30 -2 -1 0 1580.94 43.40 2 -1 0 1581.44 43.60 -2 -1 0 1549.94 43.60 -2 -1 0 1599.64 43.30 2 -1 0 1554.64 43.10 2 -1 0 1681.03 43.50 2 -1 0 1505.05 43.30 -2 -1 0 1692.23 43.60 -2 -1 0 1659.33 43.30 -2 -1 0 1604.34 43.40 -2 -1 0 1639.04 43.60 -2 -1 0 1590.04 43.50 2 1 0 1592.44 43.40 -2 1 0 1619.34 43.50 2 1 0 1488.35 43.40 2 1 0 1569.34 43.40 -2 1 0 1575.14 43.40 -2 1 0 1565.74 43.60 2 1 0 1582.44 43.60 -2 1 0 1603.84 43.40 2 1 0 1657.63 42.90 2 1 0 1627.14 43.40 -2 1 0 1619.84 43.00 2 1 0 1540.95 43.20 2 1 0 1678.03 43.50 -2 1 0 1643.24 43.50 -2 1 0 1651.83 43.60 2 1 0 1651.43 43.30 2 1 0 1597.84 43.20 2 1 0 1586.24 43.30 -2 1 0 1615.44 43.30 -2 1 0 1633.84 43.10 2 1 0 1456.45 43.30 -2 1 0 1603.74 43.30 3 -1 0 1943.91 51.19 3 -1 0 1943.51 51.29 3 -1 0 1969.20 50.99 -3 -1 0 1892.71 51.39 3 -1 0 1816.72 50.99 -3 -1 0 1776.02 51.19 -3 -1 0 1908.11 51.09 3 -1 0 1942.11 51.29 -3 -1 0 1920.01 50.99 3 -1 0 1965.70 51.09 -3 -1 0 1838.22 50.99 -3 -1 0 1963.50 51.29 3 -1 0 1871.21 51.19 -3 -1 0 1860.81 51.19 -3 -1 0 1909.71 50.79 3 -1 0 1927.01 51.49 -3 -1 0 1816.72 50.29 3 1 0 1906.61 51.19 -3 1 0 1910.61 51.29 3 1 0 1697.03 50.99 -3 1 0 1773.82 50.79 -3 1 0 1910.01 51.09 -3 1 0 1855.61 50.49 3 1 0 1849.42 51.19 -3 1 0 1741.33 50.89 -3 1 0 1952.80 51.29 3 1 0 1701.43 50.79 3 1 0 1836.02 50.69 -3 1 0 1839.32 51.09 3 1 0 1895.21 51.09 3 1 0 1768.62 50.79 -3 1 0 1887.11 50.49 3 1 0 1945.01 50.39 -3 1 0 1919.51 51.19 -3 1 0 1784.02 51.09 3 1 0 1919.21 51.49 -3 1 0 1904.31 50.69 -4 -1 0 229.48 7.80 -4 -1 0 203.58 7.50 -4 -1 0 210.98 7.30 4 -1 0 198.58 6.90 -4 -1 0 219.18 7.50 -4 -1 0 215.08 7.10 4 -1 0 219.38 7.80 -4 -1 0 202.68 7.70 4 -1 0 207.58 7.60 4 -1 0 196.08 7.70 4 -1 0 210.68 7.60 4 -1 0 216.58 7.20 -4 1 0 213.78 7.60 -4 1 0 213.18 7.10 -4 1 0 217.88 8.40 4 1 0 212.88 7.20 -4 1 0 216.68 7.70 4 1 0 211.98 7.70 4 1 0 221.08 7.60 -4 1 0 199.88 6.70 4 1 0 206.98 7.40 -4 1 0 182.08 8.20 4 1 0 209.78 6.70 -4 1 0 211.68 6.80 4 1 0 201.28 7.80 4 1 0 214.68 7.60 -5 -1 0 481.55 15.60 5 -1 0 510.85 15.40 -5 -1 0 499.05 16.00 5 -1 0 506.35 16.40 -5 -1 0 502.65 16.20 5 -1 0 489.55 15.90 -5 -1 0 505.85 15.80 -5 -1 0 492.05 15.20 5 -1 0 518.75 16.10 5 -1 0 519.05 16.10 5 1 0 505.25 15.90 -5 1 0 514.55 15.20 5 1 0 493.45 16.10 5 1 0 479.85 15.90 -5 1 0 512.25 16.20 -5 1 0 498.85 14.90 5 1 0 506.45 14.70 5 1 0 508.15 15.40 -5 1 0 502.75 15.80 -5 1 0 465.45 15.80 5 1 0 480.65 16.20 -5 1 0 515.65 16.20 6 -1 0 16.90 2.60 6 -1 0 18.00 2.00 -6 -1 0 16.40 2.10 -6 -1 0 20.20 2.60 6 -1 0 14.70 2.30 6 -1 0 14.90 2.50 -6 -1 0 16.40 2.40 -6 -1 0 18.70 2.00 6 -1 0 20.10 2.60 -6 -1 0 16.30 2.30 -6 1 0 15.00 1.80 -6 1 0 15.60 2.20 6 1 0 11.00 2.10 6 1 0 18.50 2.50 -6 1 0 15.70 2.30 -6 1 0 16.70 2.40 6 1 0 17.90 1.70 6 1 0 17.30 2.70 6 1 0 22.00 2.20 6 1 0 17.20 2.30 7 -1 0 1841.32 54.29 7 -1 0 1863.91 54.39 -7 -1 0 1884.71 52.89 7 -1 0 1933.21 54.39 -7 -1 0 1877.11 54.49 -7 -1 0 1891.11 54.69 -7 -1 0 1933.11 53.89 7 -1 0 1927.71 55.09 7 -1 0 1932.41 52.99 -7 1 0 1896.21 54.29 7 1 0 1861.51 54.49 -7 1 0 1924.91 52.89 7 1 0 1876.41 52.19 -7 1 0 1859.71 54.59 7 1 0 1987.10 55.09 -7 1 0 1856.91 52.39 7 1 0 1868.21 54.09 7 1 0 1878.21 53.19 -7 1 0 1906.41 54.59 -8 -1 0 110.39 6.60 8 -1 0 99.09 6.50 -8 -1 0 103.49 5.90 8 -1 0 108.29 6.50 -8 -1 0 101.39 6.30 8 -1 0 97.19 5.20 -8 1 0 105.09 6.50 8 1 0 104.79 6.70 8 1 0 96.49 6.30 -8 1 0 88.09 6.00 -9 -1 0 1274.97 39.20 9 -1 0 1242.38 38.70 -9 -1 0 1227.98 37.90 9 -1 0 1261.67 39.40 -9 1 0 1256.77 38.40 9 1 0 1217.58 39.00 -9 1 0 1264.87 39.10 9 1 0 1226.88 38.80 10 -1 0 338.17 15.00 -10 -1 0 348.87 14.90 10 -1 0 326.37 14.30 -10 -1 0 329.77 13.70 -10 1 0 319.77 13.90 -10 1 0 331.77 14.80 10 1 0 318.47 14.40 10 1 0 323.07 14.70 -11 -1 0 3.90 2.40 11 -1 0 -1.30 2.40 -11 -1 0 0.80 3.00 11 -1 0 0.00 3.70 -11 1 0 1.70 2.20 11 1 0 2.60 2.50 11 1 0 0.50 2.20 1 -2 0 394.16 11.00 -1 -2 0 391.76 11.00 -1 -2 0 369.56 10.60 1 -2 0 365.56 10.90 1 -2 0 377.16 11.00 1 -2 0 381.26 11.20 1 -2 0 384.56 11.00 -1 -2 0 388.06 10.80 1 -2 0 383.66 11.10 -1 -2 0 369.36 11.10 -1 -2 0 365.56 11.10 1 -2 0 396.06 10.90 -1 -2 0 395.76 11.10 -1 -2 0 386.66 11.10 -1 -2 0 380.96 11.00 1 -2 0 387.56 11.00 -1 -2 0 382.66 11.10 -1 -2 0 396.16 10.90 -1 -2 0 382.06 11.00 1 -2 0 381.46 10.60 1 2 0 385.46 11.00 -1 2 0 375.26 11.10 -1 2 0 396.16 11.00 -1 2 0 373.86 10.90 -1 2 0 371.96 11.00 1 2 0 386.16 11.10 1 2 0 393.96 11.10 -1 2 0 401.56 11.00 1 2 0 388.66 10.60 -1 2 0 385.86 11.10 1 2 0 374.76 10.80 -1 2 0 403.46 10.90 1 2 0 363.86 10.70 -1 2 0 406.16 10.70 1 2 0 369.36 11.00 1 2 0 371.36 11.00 -1 2 0 393.26 10.90 -1 2 0 387.06 11.10 1 2 0 386.66 11.10 -1 2 0 367.36 11.00 2 -2 0 286.07 8.70 -2 -2 0 296.87 9.10 2 -2 0 290.27 8.80 -2 -2 0 291.97 8.90 -2 -2 0 308.57 9.10 -2 -2 0 271.87 9.10 2 -2 0 311.97 8.70 -2 -2 0 303.07 8.80 -2 -2 0 305.37 8.90 2 -2 0 301.67 8.60 -2 -2 0 299.37 8.40 -2 -2 0 297.87 9.00 2 -2 0 259.37 9.20 2 -2 0 308.27 9.30 2 -2 0 302.47 9.10 -2 -2 0 297.27 8.40 2 -2 0 292.57 9.00 2 -2 0 296.57 9.00 -2 -2 0 271.97 9.10 2 -2 0 290.77 8.70 -2 -2 0 294.47 9.00 -2 -2 0 297.47 8.70 2 -2 0 300.17 9.10 -2 2 0 289.67 8.60 2 2 0 295.17 8.70 2 2 0 280.67 8.90 2 2 0 289.77 9.10 2 2 0 262.37 8.90 -2 2 0 298.47 8.90 -2 2 0 268.57 8.90 2 2 0 289.17 9.20 -2 2 0 296.57 8.80 -2 2 0 300.17 9.00 -2 2 0 285.97 9.00 -2 2 0 307.77 9.00 -2 2 0 300.07 9.10 2 2 0 294.87 9.00 2 2 0 303.97 9.00 -2 2 0 294.87 9.00 2 2 0 292.87 8.90 3 -2 0 178.68 6.20 3 -2 0 171.48 5.80 -3 -2 0 174.18 6.30 3 -2 0 180.08 6.50 3 -2 0 174.68 6.30 -3 -2 0 175.58 6.10 3 -2 0 173.58 6.20 3 -2 0 174.38 6.10 -3 -2 0 184.68 6.10 -3 -2 0 157.68 5.90 3 -2 0 173.98 5.60 3 -2 0 174.18 5.70 -3 -2 0 178.58 6.30 3 -2 0 158.48 5.90 -3 -2 0 151.68 5.70 3 -2 0 171.38 5.90 -3 -2 0 169.68 5.30 3 2 0 176.88 6.50 -3 2 0 176.48 6.20 3 2 0 174.98 6.20 -3 2 0 176.78 6.30 -3 2 0 162.58 6.10 -3 2 0 182.88 6.20 -3 2 0 171.18 6.10 3 2 0 177.08 6.20 -3 2 0 175.38 6.30 -3 2 0 177.68 5.80 3 2 0 156.68 6.40 3 2 0 177.58 6.10 3 2 0 168.68 5.90 4 -2 0 143.39 5.50 -4 -2 0 124.59 5.50 -4 -2 0 127.99 5.70 4 -2 0 125.69 5.30 -4 -2 0 136.09 4.60 4 -2 0 122.29 5.30 4 -2 0 140.89 5.70 4 -2 0 142.49 5.70 -4 -2 0 141.39 5.70 4 -2 0 141.59 6.00 -4 -2 0 142.79 5.50 -4 -2 0 129.09 5.20 -4 -2 0 150.28 5.40 4 2 0 127.99 5.40 4 2 0 144.59 5.40 4 2 0 145.69 6.10 -4 2 0 144.99 5.80 4 2 0 138.79 5.60 -4 2 0 135.19 5.70 -4 2 0 137.29 5.10 4 2 0 145.09 5.60 -4 2 0 132.09 4.80 4 2 0 120.39 5.40 4 2 0 135.49 4.60 -4 2 0 143.49 5.60 5 -2 0 256.07 9.20 5 -2 0 260.27 10.00 5 -2 0 260.97 9.60 -5 -2 0 259.27 9.80 -5 -2 0 253.47 9.20 5 -2 0 253.27 9.60 5 -2 0 263.87 9.40 -5 -2 0 262.17 9.20 -5 -2 0 264.37 9.70 -5 -2 0 250.57 9.00 5 2 0 262.47 9.10 -5 2 0 263.37 8.80 5 2 0 265.27 9.50 5 2 0 276.97 10.10 5 2 0 267.17 9.50 5 2 0 260.57 10.80 -5 2 0 259.07 8.50 5 2 0 264.67 8.20 -5 2 0 268.67 9.70 -5 2 0 261.87 9.70 -5 2 0 258.57 9.60 -5 2 0 263.37 9.50 -6 -2 0 1331.17 39.80 -6 -2 0 1350.66 38.90 -6 -2 0 1313.77 38.90 -6 -2 0 1368.66 38.50 6 -2 0 1361.76 38.80 -6 -2 0 1415.96 39.70 6 -2 0 1370.36 39.60 6 -2 0 1354.96 39.20 6 -2 0 1317.37 40.60 6 -2 0 1335.87 40.00 -6 2 0 1344.47 37.90 6 2 0 1331.27 40.00 -6 2 0 1356.86 39.60 -6 2 0 1362.06 39.30 -6 2 0 1385.86 39.70 6 2 0 1378.06 38.70 6 2 0 1340.77 39.40 6 2 0 1342.97 37.40 6 2 0 1389.96 39.40 6 2 0 1344.27 39.30 -6 2 0 1392.86 38.60 -7 -2 0 102.19 5.20 7 -2 0 102.99 6.00 -7 -2 0 104.29 6.00 7 -2 0 116.19 6.70 7 -2 0 98.89 5.90 7 -2 0 107.79 5.90 7 -2 0 100.69 5.30 -7 -2 0 108.29 6.30 -7 -2 0 111.99 5.70 -7 2 0 104.89 6.00 7 2 0 103.59 5.90 -7 2 0 97.79 5.00 7 2 0 90.69 5.70 -7 2 0 108.79 6.20 7 2 0 112.99 6.50 -7 2 0 119.69 6.30 7 2 0 108.59 5.40 -8 -2 0 4.20 1.80 -8 -2 0 4.00 2.40 8 -2 0 5.50 2.30 -8 -2 0 2.10 1.90 8 -2 0 4.40 2.20 8 -2 0 4.00 1.60 -8 -2 0 4.30 1.70 -8 2 0 3.80 1.90 8 2 0 2.90 1.60 8 2 0 5.60 3.40 -8 2 0 4.20 1.90 8 2 0 5.90 2.70 9 -2 0 8.50 2.70 -9 -2 0 6.20 2.30 9 -2 0 11.90 3.10 -9 -2 0 12.00 2.70 -9 2 0 4.70 2.40 9 2 0 13.70 3.20 -9 2 0 6.20 2.40 9 2 0 9.50 2.80 -10 -2 0 2.30 2.30 10 -2 0 7.10 2.90 -10 -2 0 5.60 2.60 10 -2 0 1.40 2.80 10 2 0 4.30 2.80 10 2 0 -0.50 2.50 -10 2 0 6.20 3.00 -10 2 0 6.50 3.00 -11 -2 0 342.57 16.10 11 -2 0 383.76 17.00 -11 2 0 393.36 16.10 11 2 0 358.46 16.60 11 2 0 385.56 16.30 -11 2 0 367.16 16.30 0 -3 0 1.00 0.70 0 -3 0 0.80 0.50 0 -3 0 1.70 0.70 0 -3 0 1.60 0.70 0 -3 0 0.70 0.40 0 -3 0 2.10 0.60 0 -3 0 1.40 0.60 0 -3 0 0.70 0.60 0 -3 0 1.70 0.40 0 3 0 0.90 0.60 0 3 0 1.20 0.60 0 3 0 1.00 0.50 0 3 0 0.90 0.50 0 3 0 0.30 0.50 0 3 0 1.80 0.60 0 3 0 0.70 0.60 0 3 0 0.40 0.60 1 -3 0 210.78 6.50 -1 -3 0 207.18 6.60 -1 -3 0 184.18 6.20 1 -3 0 197.88 6.30 -1 -3 0 206.78 6.50 -1 -3 0 180.88 6.30 1 -3 0 197.28 6.20 -1 -3 0 187.68 6.50 -1 -3 0 202.98 6.30 1 -3 0 193.88 6.40 1 -3 0 205.28 6.40 1 -3 0 199.28 6.30 1 -3 0 209.88 6.40 1 -3 0 192.68 6.40 -1 -3 0 210.68 6.40 1 -3 0 194.28 6.60 -1 -3 0 195.48 5.80 1 -3 0 195.18 6.40 -1 -3 0 193.08 6.40 1 -3 0 197.18 5.90 -1 -3 0 201.78 6.30 1 3 0 203.98 5.80 -1 3 0 203.98 6.40 -1 3 0 197.48 6.60 -1 3 0 199.58 6.20 -1 3 0 200.68 6.50 -1 3 0 192.78 6.30 -1 3 0 208.68 6.40 -1 3 0 202.18 6.50 1 3 0 193.38 6.20 -1 3 0 199.48 6.40 -1 3 0 199.18 6.20 1 3 0 210.08 6.50 1 3 0 194.18 6.50 1 3 0 178.28 6.20 1 3 0 205.68 6.40 1 3 0 212.58 6.50 1 3 0 196.38 6.40 1 3 0 184.28 6.30 -1 3 0 206.68 5.90 2 -3 0 1664.33 43.80 2 -3 0 1673.43 44.40 -2 -3 0 1575.64 44.10 -2 -3 0 1632.04 44.10 -2 -3 0 1531.55 43.70 2 -3 0 1616.94 43.40 2 -3 0 1537.25 43.80 -2 -3 0 1686.03 43.50 2 -3 0 1677.23 44.20 2 -3 0 1650.13 44.10 2 -3 0 1612.94 43.90 -2 -3 0 1541.05 43.90 -2 -3 0 1576.84 43.50 -2 -3 0 1658.33 44.00 2 -3 0 1683.93 44.30 -2 -3 0 1615.54 44.10 2 3 0 1564.84 43.70 -2 3 0 1462.85 43.90 2 3 0 1659.03 44.10 2 3 0 1652.53 44.40 2 3 0 1588.64 44.00 -2 3 0 1428.16 43.80 2 3 0 1628.44 43.50 -2 3 0 1642.94 43.90 -2 3 0 1685.33 44.10 -2 3 0 1572.74 43.70 2 3 0 1650.23 44.10 2 3 0 1590.94 44.20 -2 3 0 1538.05 44.00 -2 3 0 1533.55 44.00 -2 3 0 1661.83 44.20 -2 3 0 1698.43 44.30 -3 -3 0 63.49 3.30 3 -3 0 72.79 3.50 3 -3 0 68.89 3.00 3 -3 0 61.69 2.80 -3 -3 0 66.79 3.00 -3 -3 0 58.19 3.20 3 -3 0 62.99 3.30 3 -3 0 67.99 3.60 -3 -3 0 68.49 3.40 -3 -3 0 63.89 2.60 3 -3 0 59.09 2.90 3 -3 0 67.29 2.90 3 -3 0 65.69 3.40 3 -3 0 68.69 3.40 -3 -3 0 66.59 2.60 -3 -3 0 60.99 2.90 -3 -3 0 66.89 4.40 3 3 0 70.19 3.40 -3 3 0 70.89 3.10 -3 3 0 78.79 4.90 3 3 0 64.99 3.20 3 3 0 67.59 3.60 -3 3 0 65.19 2.80 3 3 0 71.59 3.40 3 3 0 74.49 3.50 3 3 0 67.89 3.00 -3 3 0 65.39 3.50 -3 3 0 70.99 3.30 -3 3 0 66.99 3.30 4 -3 0 28.00 1.80 4 -3 0 24.90 2.20 4 -3 0 29.30 2.10 -4 -3 0 22.00 1.40 -4 -3 0 26.70 2.00 -4 -3 0 25.30 2.20 4 -3 0 26.00 2.30 -4 -3 0 24.50 2.10 4 -3 0 25.40 2.20 -4 -3 0 25.50 2.10 -4 -3 0 19.10 2.00 -4 -3 0 25.60 1.50 4 -3 0 28.00 2.60 -4 -3 0 27.30 2.40 -4 3 0 24.70 2.20 4 3 0 28.60 2.10 -4 3 0 24.70 2.30 4 3 0 24.20 2.20 4 3 0 24.80 2.20 -4 3 0 21.30 1.70 -4 3 0 27.00 2.00 4 3 0 24.20 2.40 -4 3 0 21.70 2.10 -4 3 0 21.30 2.20 -5 -3 0 0.70 0.90 -5 -3 0 2.40 1.20 5 -3 0 3.90 1.30 -5 -3 0 1.20 0.80 5 -3 0 2.00 1.40 5 -3 0 1.30 1.00 -5 -3 0 0.90 1.10 5 -3 0 2.60 1.30 -5 -3 0 5.70 1.50 5 -3 0 1.00 0.90 -5 -3 0 2.30 1.10 5 3 0 -0.10 0.90 -5 3 0 2.20 1.30 5 3 0 0.40 1.00 -5 3 0 0.50 0.80 -5 3 0 2.60 1.30 5 3 0 1.00 0.90 -5 3 0 0.70 1.10 5 3 0 1.20 1.30 -5 3 0 0.80 1.00 5 3 0 2.10 1.20 -6 -3 0 10.30 2.20 6 -3 0 10.40 2.50 6 -3 0 11.00 2.20 -6 -3 0 10.70 2.10 -6 -3 0 12.10 2.20 6 -3 0 10.50 2.20 6 -3 0 13.50 2.70 -6 -3 0 10.00 2.30 6 -3 0 8.60 2.00 -6 3 0 10.10 2.20 -6 3 0 11.60 1.70 6 3 0 10.30 2.20 6 3 0 9.50 2.20 -6 3 0 8.20 2.20 6 3 0 12.00 2.00 6 3 0 12.50 2.10 6 3 0 14.20 2.10 -6 3 0 8.50 2.60 -6 3 0 7.70 1.60 -6 3 0 7.60 2.00 -7 -3 0 337.07 11.90 -7 -3 0 325.17 12.60 7 -3 0 334.17 12.10 7 -3 0 317.27 12.00 -7 -3 0 314.67 11.60 -7 -3 0 334.57 12.90 7 -3 0 324.17 13.20 7 3 0 333.07 12.50 -7 3 0 336.67 12.70 7 3 0 347.67 12.40 -7 3 0 302.97 12.50 -7 3 0 316.57 11.20 -7 3 0 308.97 12.50 7 3 0 325.57 11.90 7 3 0 335.77 13.20 8 -3 0 190.78 8.50 -8 -3 0 197.38 9.60 8 -3 0 192.78 9.90 -8 -3 0 184.98 8.20 -8 -3 0 194.28 9.30 8 -3 0 198.98 9.00 -8 -3 0 195.38 8.60 -8 3 0 197.68 9.40 8 3 0 195.78 8.50 -8 3 0 187.08 9.30 8 3 0 195.98 9.80 8 3 0 198.88 9.60 -9 -3 0 125.99 6.90 -9 -3 0 116.89 7.70 9 -3 0 124.09 7.90 9 -3 0 119.29 7.30 -9 3 0 130.69 7.60 9 3 0 119.89 8.10 9 3 0 125.39 7.30 -9 3 0 129.59 7.60 10 -3 0 145.29 9.50 -10 -3 0 153.68 9.20 -10 -3 0 145.89 8.10 -10 3 0 157.78 9.20 10 3 0 156.68 9.70 -10 3 0 150.08 9.10 10 3 0 157.98 9.00 11 -3 0 101.59 8.30 -11 -3 0 115.99 8.30 -11 3 0 96.39 7.50 11 3 0 111.99 8.70 -11 3 0 108.79 8.30 11 3 0 106.79 7.70 0 -4 0 3206.48 85.19 0 -4 0 3121.99 85.39 0 -4 0 3185.88 85.09 0 -4 0 3017.20 85.29 0 -4 0 3292.87 85.49 0 -4 0 3095.59 85.09 0 -4 0 2984.70 85.09 0 -4 0 3272.17 84.59 0 -4 0 3180.18 84.59 0 4 0 3109.09 85.29 0 4 0 3320.17 85.29 0 4 0 3034.50 84.89 0 4 0 2988.30 85.09 0 4 0 3300.97 85.29 0 4 0 3284.07 85.69 0 4 0 3217.18 84.89 0 4 0 3260.57 85.39 -1 -4 0 21.30 1.60 1 -4 0 24.40 1.80 1 -4 0 21.90 1.20 1 -4 0 19.40 1.60 -1 -4 0 18.50 1.00 -1 -4 0 14.80 1.50 -1 -4 0 22.80 1.70 1 -4 0 19.60 1.60 1 -4 0 22.10 1.90 -1 -4 0 20.40 1.60 -1 -4 0 19.50 1.70 -1 -4 0 18.80 1.50 1 -4 0 20.50 1.40 1 -4 0 21.30 1.50 1 -4 0 18.30 1.50 1 4 0 20.70 1.60 -1 4 0 23.60 1.80 1 4 0 21.90 1.60 -1 4 0 19.60 1.60 1 4 0 17.20 1.70 1 4 0 19.50 1.60 1 4 0 17.90 1.40 -1 4 0 20.50 1.60 -1 4 0 20.40 1.30 1 4 0 20.10 1.50 -1 4 0 22.90 1.90 1 4 0 20.20 1.10 -1 4 0 21.10 1.40 1 4 0 17.00 1.40 1 4 0 18.30 1.50 -1 4 0 19.10 1.60 1 4 0 17.70 1.50 1 4 0 15.40 1.70 -1 4 0 18.00 1.30 -2 -4 0 21.70 2.10 -2 -4 0 17.80 1.40 -2 -4 0 18.10 1.70 -2 -4 0 19.30 1.50 2 -4 0 16.30 1.50 2 -4 0 14.80 1.60 -2 -4 0 19.00 1.60 -2 -4 0 19.60 1.90 2 -4 0 16.00 1.20 -2 -4 0 19.80 1.70 2 -4 0 19.70 1.70 -2 -4 0 17.00 1.20 2 -4 0 17.80 1.60 2 -4 0 19.80 1.90 2 -4 0 19.50 1.80 -2 4 0 17.80 1.30 2 4 0 17.90 1.80 2 4 0 18.30 1.20 2 4 0 18.60 1.50 2 4 0 18.80 1.70 -2 4 0 19.20 1.70 -2 4 0 18.60 1.50 2 4 0 15.60 1.70 -2 4 0 22.70 1.90 -2 4 0 16.40 1.50 -2 4 0 15.00 1.60 2 4 0 15.90 1.30 -2 4 0 18.00 1.70 -2 4 0 16.10 1.30 2 4 0 23.80 1.80 2 4 0 17.60 1.60 -2 4 0 20.00 1.60 -3 -4 0 61.99 2.70 -3 -4 0 67.19 3.50 -3 -4 0 66.49 3.40 3 -4 0 67.99 4.30 3 -4 0 64.29 2.80 3 -4 0 66.99 3.40 -3 -4 0 66.19 3.10 -3 -4 0 63.99 2.70 3 -4 0 70.69 3.10 3 -4 0 64.99 3.50 -3 -4 0 65.59 3.40 -3 -4 0 62.99 2.90 3 -4 0 61.79 3.60 3 -4 0 62.69 2.80 -3 -4 0 62.39 3.30 -3 -4 0 60.19 3.40 -3 4 0 62.39 3.40 3 4 0 57.49 3.20 -3 4 0 67.39 3.20 3 4 0 61.19 2.80 -3 4 0 68.59 3.60 3 4 0 62.49 3.70 3 4 0 63.69 3.40 -3 4 0 67.29 3.30 3 4 0 73.09 3.70 -3 4 0 66.59 3.50 3 4 0 62.19 3.30 4 -4 0 81.89 4.40 4 -4 0 94.89 4.90 4 -4 0 88.69 4.60 -4 -4 0 92.39 4.60 4 -4 0 94.49 3.90 -4 -4 0 86.79 4.40 -4 -4 0 82.79 4.20 4 -4 0 86.69 4.50 -4 -4 0 87.59 4.50 -4 -4 0 91.49 3.50 4 -4 0 99.29 4.10 -4 -4 0 73.39 4.20 -4 -4 0 92.69 4.60 -4 4 0 90.69 4.50 -4 4 0 83.89 4.10 4 4 0 92.09 4.50 -4 4 0 92.69 4.40 -4 4 0 83.39 4.60 4 4 0 93.59 4.00 -4 4 0 88.79 4.60 4 4 0 97.69 4.60 4 4 0 97.99 4.90 -5 -4 0 45.50 3.20 5 -4 0 43.00 3.00 5 -4 0 43.70 3.40 5 -4 0 45.30 3.40 5 -4 0 46.70 3.60 5 -4 0 45.70 3.40 -5 -4 0 47.10 3.00 -5 -4 0 44.70 3.40 5 -4 0 45.50 2.60 -5 -4 0 51.99 3.40 -5 -4 0 53.49 3.70 -5 -4 0 46.00 2.30 -5 4 0 42.10 3.30 5 4 0 45.70 3.30 -5 4 0 48.10 3.60 -5 4 0 42.10 3.40 -5 4 0 41.30 2.80 -5 4 0 41.90 3.30 5 4 0 39.50 2.90 5 4 0 43.60 3.30 5 4 0 44.10 3.70 5 4 0 46.40 3.40 6 -4 0 791.32 25.30 -6 -4 0 783.72 24.00 -6 -4 0 766.42 23.70 6 -4 0 767.12 24.40 -6 -4 0 796.52 24.70 6 -4 0 793.32 23.90 6 -4 0 781.62 25.80 6 -4 0 784.42 26.10 -6 -4 0 791.42 24.90 -6 4 0 804.22 24.60 -6 4 0 754.12 24.70 6 4 0 758.12 25.10 6 4 0 787.02 24.40 -6 4 0 780.32 23.40 6 4 0 798.52 23.90 6 4 0 817.12 24.30 -7 -4 0 168.18 8.10 -7 -4 0 179.48 8.70 7 -4 0 181.58 9.20 -7 -4 0 167.08 7.60 7 -4 0 162.38 7.80 7 -4 0 170.48 7.70 -7 -4 0 177.58 7.50 7 4 0 159.48 7.90 -7 4 0 205.98 11.40 7 4 0 167.18 7.60 7 4 0 187.28 9.20 -7 4 0 155.88 8.10 -7 4 0 171.28 8.20 7 4 0 171.48 7.80 -7 4 0 164.48 7.10 -8 -4 0 30.30 3.70 8 -4 0 30.50 4.10 -8 -4 0 31.50 3.40 8 -4 0 32.70 3.60 8 -4 0 29.30 3.40 -8 -4 0 33.80 3.40 -8 -4 0 33.90 4.00 -8 4 0 28.50 3.70 8 4 0 33.70 4.20 8 4 0 32.00 3.40 8 4 0 27.30 3.40 -8 4 0 39.70 4.30 9 -4 0 6.00 2.40 9 -4 0 2.30 2.30 -9 -4 0 1.40 1.70 -9 -4 0 0.00 1.80 9 4 0 4.30 2.70 -9 4 0 2.80 2.30 -9 4 0 2.40 2.50 9 4 0 2.80 1.90 -10 -4 0 74.59 8.20 10 -4 0 61.69 8.00 -10 4 0 71.39 6.50 -10 4 0 58.39 5.80 10 4 0 63.49 6.50 10 4 0 59.99 5.50 11 -4 0 70.59 6.90 -11 -4 0 68.49 6.70 -11 4 0 71.79 6.70 -11 4 0 55.79 6.30 11 4 0 76.59 7.00 0 -5 0 0.90 0.50 0 -5 0 -0.10 0.80 0 -5 0 -0.30 0.80 0 -5 0 0.30 0.70 0 -5 0 -0.10 0.40 0 -5 0 0.10 0.60 0 -5 0 1.90 0.90 0 -5 0 1.30 0.70 0 5 0 3.40 1.10 0 5 0 1.00 0.60 0 5 0 0.60 0.60 1 -5 0 386.96 12.00 -1 -5 0 390.66 11.80 -1 -5 0 427.86 14.80 -1 -5 0 353.76 11.80 1 -5 0 366.86 11.80 1 -5 0 403.46 11.60 1 -5 0 366.36 11.30 1 -5 0 366.96 11.90 -1 -5 0 373.56 11.60 1 -5 0 370.46 11.40 -1 -5 0 374.06 11.70 -1 -5 0 376.76 11.90 -1 -5 0 358.56 10.70 -1 5 0 371.06 11.00 1 5 0 347.77 11.60 1 5 0 384.26 11.80 1 5 0 378.56 11.80 -1 5 0 373.66 11.30 1 5 0 375.56 11.50 1 5 0 389.56 11.70 -1 5 0 375.16 11.80 -1 5 0 371.16 11.70 -1 5 0 376.56 11.90 1 5 0 378.46 12.80 -1 5 0 377.16 12.00 -1 5 0 374.16 11.80 -2 -5 0 1304.07 36.00 -2 -5 0 1201.78 34.70 -2 -5 0 1325.47 36.20 2 -5 0 1316.27 36.20 2 -5 0 1170.78 36.00 -2 -5 0 1314.87 35.60 -2 -5 0 1314.07 36.00 2 -5 0 1302.97 36.50 2 -5 0 1236.48 35.90 -2 -5 0 1225.68 36.10 -2 -5 0 1312.97 36.30 2 -5 0 1339.87 36.00 2 -5 0 1191.28 35.70 2 5 0 1295.37 36.00 2 5 0 1277.57 34.80 -2 5 0 1304.67 36.00 -2 5 0 1334.77 36.10 2 5 0 1286.57 36.00 2 5 0 1204.68 35.80 -2 5 0 1309.57 35.60 -2 5 0 1295.07 36.10 -2 5 0 1287.27 35.00 2 5 0 1278.87 36.10 -2 5 0 1281.27 36.20 2 5 0 1295.27 36.40 3 -5 0 1378.96 38.80 3 -5 0 1347.57 38.30 -3 -5 0 1224.38 37.00 -3 -5 0 1392.76 37.40 -3 -5 0 1349.86 37.70 3 -5 0 1376.06 37.80 3 -5 0 1369.06 38.50 -3 -5 0 1352.46 38.30 3 -5 0 1252.27 37.00 3 -5 0 1382.66 38.50 -3 -5 0 1350.66 38.40 -3 -5 0 1347.47 37.90 -3 -5 0 1386.36 38.30 3 5 0 1360.86 38.60 3 5 0 1353.96 38.20 -3 5 0 1377.46 38.60 3 5 0 1364.76 38.20 -3 5 0 1346.47 38.40 -3 5 0 1342.97 38.20 3 5 0 1376.66 38.70 -3 5 0 1360.76 37.90 3 5 0 1346.87 37.10 -4 -5 0 55.19 3.60 4 -5 0 57.99 3.60 4 -5 0 51.69 3.00 -4 -5 0 54.39 3.60 -4 -5 0 54.69 3.20 -4 -5 0 57.29 3.30 4 -5 0 56.69 3.00 4 -5 0 52.19 3.70 4 -5 0 56.09 3.60 -4 -5 0 53.49 2.60 4 -5 0 50.49 3.80 -4 -5 0 51.19 3.50 -4 5 0 53.59 3.50 -4 5 0 51.19 3.50 4 5 0 53.39 3.80 -4 5 0 52.49 3.30 4 5 0 55.39 2.90 4 5 0 56.99 3.50 -4 5 0 52.59 3.20 -4 5 0 58.59 3.80 4 5 0 53.09 3.40 4 5 0 55.99 3.70 -5 -5 0 2.80 1.40 5 -5 0 4.60 1.80 5 -5 0 3.10 1.40 -5 -5 0 5.70 1.80 -5 -5 0 2.70 1.70 5 -5 0 1.40 1.70 -5 -5 0 1.00 1.20 -5 -5 0 1.10 1.40 5 -5 0 1.60 1.60 -5 5 0 4.20 1.90 -5 5 0 1.90 1.20 5 5 0 1.10 1.10 -5 5 0 0.90 1.10 -5 5 0 0.90 1.20 5 5 0 3.30 1.50 5 5 0 5.60 1.70 5 5 0 2.10 1.60 5 5 0 2.40 1.30 -6 -5 0 453.15 15.50 6 -5 0 455.15 14.80 -6 -5 0 449.66 15.90 6 -5 0 463.05 16.00 -6 -5 0 479.35 16.30 6 -5 0 444.46 15.90 6 -5 0 450.25 16.50 -6 -5 0 465.75 15.00 6 5 0 463.25 15.80 -6 5 0 424.26 15.60 -6 5 0 453.65 15.60 6 5 0 455.95 14.90 6 5 0 445.76 15.50 -6 5 0 473.95 16.30 6 5 0 438.16 16.40 -6 5 0 443.16 14.80 -7 -5 0 811.52 26.30 7 -5 0 758.22 25.40 -7 -5 0 825.32 25.70 7 -5 0 848.22 27.30 -7 -5 0 814.92 25.20 -7 -5 0 840.82 26.80 7 -5 0 836.42 26.30 7 5 0 811.62 25.20 7 5 0 821.52 25.90 7 5 0 818.12 26.20 -7 5 0 790.72 24.80 -7 5 0 864.71 27.00 -7 5 0 801.62 26.00 7 5 0 851.61 27.40 8 -5 0 479.45 18.10 -8 -5 0 429.26 17.10 8 -5 0 477.65 16.90 -8 -5 0 408.06 16.70 -8 -5 0 426.36 17.90 -8 -5 0 465.45 15.90 -8 5 0 477.85 17.70 8 5 0 473.55 16.20 8 5 0 463.35 18.00 -8 5 0 441.26 16.70 -9 -5 0 65.09 4.90 9 -5 0 78.19 5.80 9 -5 0 70.09 6.40 -9 -5 0 63.79 5.70 9 5 0 84.39 5.60 -9 5 0 72.39 6.10 9 5 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732.73 25.60 -1 -11 -9 726.03 25.60 -1 -11 -9 745.93 24.30 1 -11 9 738.03 26.20 1 -11 9 731.83 25.10 1 -11 9 675.43 24.50 1 11 9 689.83 25.20 -1 11 -9 712.03 25.00 -1 11 -9 698.43 25.80 1 11 9 725.63 25.40 1 11 9 747.73 24.00 -1 11 -9 717.73 24.90 2 -11 9 7.90 3.20 -2 -11 -9 4.80 2.40 2 -11 9 8.10 3.30 -2 -11 -9 12.50 3.70 2 -11 9 8.80 3.30 -2 -11 -9 6.90 2.50 -2 11 -9 4.80 2.50 -2 11 -9 6.00 2.60 2 11 9 4.20 2.50 -2 11 -9 5.40 3.10 2 11 9 7.40 2.70 2 11 9 6.00 2.70 -3 -11 -9 12.60 3.20 3 -11 9 13.40 3.80 -3 -11 -9 8.90 3.00 3 11 9 19.10 5.60 -3 11 -9 13.00 3.80 -3 11 -9 13.00 3.40 -3 11 -9 13.30 6.00 3 11 9 11.60 3.80 -4 -11 -9 96.89 6.80 4 -11 9 104.99 8.20 -4 -11 -9 103.89 7.80 4 -11 9 99.99 7.90 4 11 9 95.69 6.60 -4 11 -9 81.89 7.30 4 11 9 96.29 8.00 4 11 9 113.49 7.70 -5 -11 -9 373.86 16.50 5 -11 9 334.77 16.40 -5 -11 -9 355.56 15.10 5 -11 9 375.46 16.70 5 11 9 374.36 17.10 5 11 9 360.86 16.00 -5 11 -9 348.67 16.50 5 11 9 343.87 14.80 -6 -11 -9 12.30 3.10 6 -11 9 22.00 4.40 6 -11 9 11.50 4.10 -6 11 -9 15.10 4.10 6 11 9 10.70 3.70 6 11 9 13.40 3.80 -6 11 -9 4.30 4.70 6 -12 -9 46.70 5.70 6 -12 -9 44.60 5.90 6 -12 -9 54.19 6.30 -6 -12 9 43.60 6.20 -6 12 9 47.40 5.90 -6 12 9 48.90 5.70 -6 12 9 43.60 5.80 6 12 -9 56.09 6.10 5 -12 -9 9.50 3.50 5 -12 -9 14.30 3.80 -5 -12 9 5.60 2.90 -5 -12 9 3.40 3.20 5 -12 -9 3.10 2.80 5 12 -9 13.80 3.90 -5 12 9 7.30 3.40 -5 12 9 7.30 3.40 5 12 -9 4.50 3.10 -5 12 9 12.60 3.80 4 -12 -9 215.68 11.50 4 -12 -9 208.48 10.70 4 -12 -9 203.58 11.50 -4 -12 9 201.78 11.20 -4 -12 9 191.98 11.20 4 12 -9 204.38 11.40 -4 12 9 211.08 10.70 4 12 -9 201.28 11.30 -4 12 9 192.58 11.00 -4 12 9 195.48 11.00 3 -12 -9 115.49 8.10 3 -12 -9 95.89 10.50 -3 -12 9 100.79 9.30 3 -12 -9 104.49 7.80 3 12 -9 114.89 10.30 -3 12 9 109.49 7.70 -3 12 9 87.39 9.20 -3 12 9 93.59 7.80 2 -12 -9 214.48 12.60 -2 -12 9 209.98 11.00 2 -12 -9 217.68 12.30 -2 -12 9 262.57 18.10 2 -12 -9 218.68 11.40 -2 12 9 225.98 12.80 2 12 -9 221.88 11.40 -2 12 9 251.87 13.00 2 12 -9 218.78 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4.40 -3 3 19 12.40 3.50 -2 -3 19 37.60 3.30 -2 -3 19 35.60 5.20 2 3 -19 35.10 5.40 -2 3 19 28.50 4.80 2 3 -19 31.70 3.30 -2 3 19 35.80 5.00 -1 -3 19 40.70 5.50 -1 -3 19 37.30 5.30 -1 -3 19 41.50 3.50 1 3 -19 42.00 5.70 1 3 -19 39.60 3.50 0 -3 19 47.60 5.80 0 -3 19 48.50 3.60 0 -3 19 48.90 5.50 0 3 -19 32.00 5.60 0 3 -19 42.70 3.60 1 -3 19 35.30 5.20 1 -3 19 36.70 3.30 -1 3 -19 32.60 5.60 -1 3 -19 35.80 5.50 -1 3 -19 31.60 3.10 -3 -4 19 90.19 7.50 -3 -4 19 94.19 5.50 -3 4 19 84.29 7.40 3 4 -19 81.59 7.40 3 4 -19 80.89 5.20 -2 -4 19 24.00 3.10 -2 -4 19 25.90 5.20 2 4 -19 24.30 3.20 2 4 -19 27.60 4.90 -2 4 19 29.40 4.90 -1 -4 19 380.86 17.40 -1 -4 19 391.26 17.00 -1 -4 19 356.66 13.40 1 4 -19 379.56 17.20 1 4 -19 374.56 13.50 0 -4 19 17.90 4.60 0 -4 19 30.90 4.80 0 -4 19 19.80 2.80 0 4 -19 24.50 3.00 0 4 -19 25.20 4.80 -2 -5 19 -1.50 2.20 -2 0 20 37.00 5.40 -1 0 20 -1.70 1.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 13640 _shelx_res_file ; TITL JTM1553_0m_a.res in P2(1)/n JTM1553_0m_a.res created by SHELXL-2019/1 at 11:04:10 on 09-Sep-2022 REM Old TITL JTM1553_0m in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.073, Rweak 0.002, Alpha 0.021 REM 2.766 for 109 systematic absences, Orientation as input REM Formula found by SHELXT: C8 N O3 S CELL 0.71073 7.2179 9.5043 11.9945 90.000 97.584 90.000 ZERR 4.000 0.0006 0.0008 0.0009 0.000 0.002 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O S UNIT 32 28 4 12 4 TEMP -148 SIZE 0.162 0.213 0.385 L.S. 5 BOND $H LIST 4 FMAP 2 PLAN 5 OMIT 0 1 1 OMIT 4 0 0 CONF EQIV $1 x+1, y, z HTAB N1 O3_$1 EQIV $2 -x+3/2, y-1/2, -z+3/2 HTAB C5 O1_$2 EQIV $3 -x+1/2, y-1/2, -z+3/2 HTAB C8 O2_$3 ACTA 72.8 DFIX 0.91 0.01 N1 H1 WGHT 0.038300 0.272400 FVAR 1.27876 S1 5 0.160679 0.521433 0.717541 11.00000 0.00776 0.01295 = 0.01219 -0.00153 0.00109 0.00109 O1 4 0.612285 0.595297 0.908593 11.00000 0.01733 0.02361 = 0.01736 -0.00209 -0.00298 -0.00682 O2 4 0.162679 0.667209 0.683518 11.00000 0.02050 0.01289 = 0.01996 0.00015 0.00061 0.00460 O3 4 -0.018818 0.457936 0.726666 11.00000 0.00783 0.02623 = 0.02137 -0.00439 0.00373 -0.00199 N1 3 0.578058 0.479753 0.742108 11.00000 0.00778 0.01949 = 0.01491 0.00008 0.00092 -0.00112 H1 2 0.700060 0.490023 0.739801 11.00000 0.02701 C1 1 0.279589 0.420442 0.627998 11.00000 0.00917 0.01142 = 0.01134 -0.00003 0.00190 0.00061 C2 1 0.179969 0.356153 0.534118 11.00000 0.01379 0.01366 = 0.01253 -0.00101 0.00073 -0.00096 AFIX 43 H2 2 0.047397 0.361237 0.521776 11.00000 -1.20000 AFIX 0 C3 1 0.276510 0.284601 0.458823 11.00000 0.02125 0.01502 = 0.01402 -0.00282 0.00385 -0.00101 AFIX 43 H3 2 0.210847 0.242727 0.393292 11.00000 -1.20000 AFIX 0 C4 1 0.470922 0.274809 0.480358 11.00000 0.02185 0.01660 = 0.01841 -0.00242 0.00877 0.00246 AFIX 43 H4 2 0.536825 0.224837 0.429380 11.00000 -1.20000 AFIX 0 C5 1 0.569850 0.336809 0.574993 11.00000 0.01325 0.01773 = 0.01905 0.00041 0.00638 0.00328 AFIX 43 H5 2 0.701938 0.327605 0.588942 11.00000 -1.20000 AFIX 0 C6 1 0.474864 0.412736 0.649657 11.00000 0.00929 0.01295 = 0.01295 0.00133 0.00242 0.00103 C7 1 0.511720 0.532876 0.834988 11.00000 0.01136 0.01426 = 0.01331 0.00154 -0.00035 -0.00146 C8 1 0.308634 0.502135 0.846035 11.00000 0.01151 0.01618 = 0.01130 -0.00122 0.00154 -0.00114 AFIX 23 H8A 2 0.266578 0.566751 0.902374 11.00000 -1.20000 H8B 2 0.298167 0.404753 0.873825 11.00000 -1.20000 AFIX 0 HKLF 4 REM JTM1553_0m_a.res in P2(1)/n REM wR2 = 0.0744, GooF = S = 1.042, Restrained GooF = 1.042 for all data REM R1 = 0.0252 for 3739 Fo > 4sig(Fo) and 0.0268 for all 3957 data REM 122 parameters refined using 1 restraints END WGHT 0.0383 0.2728 REM Highest difference peak 0.516, deepest hole -0.356, 1-sigma level 0.057 Q1 1 0.5234 0.3730 0.6141 11.00000 0.05 0.52 Q2 1 0.3739 0.4209 0.6394 11.00000 0.05 0.51 Q3 1 0.3726 0.2836 0.4700 11.00000 0.05 0.47 Q4 1 0.2308 0.3187 0.4977 11.00000 0.05 0.47 Q5 1 0.2311 0.3832 0.5864 11.00000 0.05 0.47 ; _shelx_res_checksum 12631 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-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 _atom_site_disorder_assembly _atom_site_disorder_group S S1 0.16068(2) 0.52143(2) 0.71754(2) 0.01099(4) Uani d 1 . . O O1 0.61228(8) 0.59530(6) 0.90859(5) 0.01991(10) Uani d 1 . . O O2 0.16268(8) 0.66721(6) 0.68352(5) 0.01797(10) Uani d 1 . . O O3 -0.01882(7) 0.45794(7) 0.72667(5) 0.01832(10) Uani d 1 . . N N1 0.57806(8) 0.47975(6) 0.74211(5) 0.01411(10) Uani d 1 . . H H1 0.7001(12) 0.4900(15) 0.7398(13) 0.027(3) Uiso d 1 . . C C1 0.27959(8) 0.42044(6) 0.62800(5) 0.01059(9) Uani d 1 . . C C2 0.17997(9) 0.35615(7) 0.53412(5) 0.01342(10) Uani d 1 . . H H2 0.047397 0.361237 0.521776 0.016 Uiso calc 1 . . C C3 0.27651(11) 0.28460(7) 0.45882(6) 0.01663(11) Uani d 1 . . H H3 0.210847 0.242727 0.393292 0.020 Uiso calc 1 . . C C4 0.47092(11) 0.27481(8) 0.48036(6) 0.01841(12) Uani d 1 . . H H4 0.536825 0.224837 0.429380 0.022 Uiso calc 1 . . C C5 0.56985(10) 0.33681(8) 0.57499(6) 0.01630(11) Uani d 1 . . H H5 0.701938 0.327605 0.588942 0.020 Uiso calc 1 . . C C6 0.47486(8) 0.41274(7) 0.64966(5) 0.01164(10) Uani d 1 . . C C7 0.51172(9) 0.53288(7) 0.83499(5) 0.01315(10) Uani d 1 . . C C8 0.30863(9) 0.50214(7) 0.84603(5) 0.01299(10) Uani d 1 . . H H8A 0.266578 0.566751 0.902374 0.016 Uiso calc 1 . . H H8B 0.298167 0.404753 0.873825 0.016 Uiso calc 1 . . 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 S1 0.00776(7) 0.01295(7) 0.01219(7) 0.00109(4) 0.00109(4) -0.00153(4) O1 0.0173(2) 0.0236(3) 0.0174(2) -0.00682(19) -0.00298(17) -0.00209(18) O2 0.0205(2) 0.0129(2) 0.0200(2) 0.00460(17) 0.00061(18) 0.00015(16) O3 0.00783(18) 0.0262(3) 0.0214(2) -0.00199(17) 0.00373(16) -0.00439(19) N1 0.0078(2) 0.0195(2) 0.0149(2) -0.00112(17) 0.00092(16) 0.00008(18) C1 0.0092(2) 0.0114(2) 0.0113(2) 0.00061(16) 0.00190(16) -0.00003(16) C2 0.0138(2) 0.0137(2) 0.0125(2) -0.00096(19) 0.00073(18) -0.00101(18) C3 0.0212(3) 0.0150(3) 0.0140(2) -0.0010(2) 0.0038(2) -0.00282(19) C4 0.0218(3) 0.0166(3) 0.0184(3) 0.0025(2) 0.0088(2) -0.0024(2) C5 0.0133(2) 0.0177(3) 0.0190(3) 0.0033(2) 0.0064(2) 0.0004(2) C6 0.0093(2) 0.0130(2) 0.0130(2) 0.00103(17) 0.00242(17) 0.00133(17) C7 0.0114(2) 0.0143(2) 0.0133(2) -0.00146(18) -0.00035(18) 0.00154(18) C8 0.0115(2) 0.0162(2) 0.0113(2) -0.00114(19) 0.00154(18) -0.00122(18) 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' 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 _geom_angle_publ_flag O2 S1 O3 . . 117.64(4) ? O2 S1 C1 . . 109.21(3) ? O3 S1 C1 . . 109.56(3) ? O2 S1 C8 . . 108.59(3) ? O3 S1 C8 . . 109.59(3) ? C1 S1 C8 . . 100.95(3) ? C7 N1 C6 . . 127.24(6) ? C7 N1 H1 . . 116.1(10) ? C6 N1 H1 . . 116.7(10) ? C2 C1 C6 . . 121.72(6) ? C2 C1 S1 . . 119.61(5) ? C6 C1 S1 . . 118.58(5) ? C3 C2 C1 . . 119.34(6) ? C3 C2 H2 . . 120.3 ? C1 C2 H2 . . 120.3 ? C2 C3 C4 . . 119.38(6) ? C2 C3 H3 . . 120.3 ? C4 C3 H3 . . 120.3 ? C5 C4 C3 . . 121.22(6) ? C5 C4 H4 . . 119.4 ? C3 C4 H4 . . 119.4 ? C4 C5 C6 . . 119.96(6) ? C4 C5 H5 . . 120.0 ? C6 C5 H5 . . 120.0 ? C5 C6 C1 . . 118.33(6) ? C5 C6 N1 . . 119.08(6) ? C1 C6 N1 . . 122.58(6) ? O1 C7 N1 . . 122.05(6) ? O1 C7 C8 . . 121.31(6) ? N1 C7 C8 . . 116.53(6) ? C7 C8 S1 . . 112.57(4) ? C7 C8 H8A . . 109.1 ? S1 C8 H8A . . 109.1 ? C7 C8 H8B . . 109.1 ? S1 C8 H8B . . 109.1 ? H8A C8 H8B . . 107.8 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 O2 . 1.4450(6) ? S1 O3 . 1.4464(6) ? S1 C1 . 1.7478(6) ? S1 C8 . 1.7649(7) ? O1 C7 . 1.2203(8) ? N1 C7 . 1.3661(9) ? N1 C6 . 1.4043(9) ? N1 H1 . 0.890(8) ? C1 C2 . 1.3945(9) ? C1 C6 . 1.4010(9) ? C2 C3 . 1.3892(10) ? C2 H2 . 0.9500 ? C3 C4 . 1.3960(11) ? C3 H3 . 0.9500 ? C4 C5 . 1.3898(11) ? C4 H4 . 0.9500 ? C5 C6 . 1.3982(9) ? C5 H5 . 0.9500 ? C7 C8 . 1.5175(9) ? C8 H8A . 0.9900 ? C8 H8B . 0.9900 ? 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 _geom_hbond_publ_flag N1 H1 O3 1_655 0.890(8) 2.078(9) 2.9472(8) 165.0(13) yes C5 H5 O1 2_646 0.95 2.58 3.2330(9) 126 yes C8 H8A Cg2 2_556 0.99 2.93 3.7933(8) 146 y C8 H8B O2 2_546 0.99 2.39 3.2126(9) 140 yes 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 O2 S1 C1 C2 . . . . -93.69(6) ? O3 S1 C1 C2 . . . . 36.48(6) ? C8 S1 C1 C2 . . . . 152.03(5) ? O2 S1 C1 C6 . . . . 82.92(6) ? O3 S1 C1 C6 . . . . -146.91(5) ? C8 S1 C1 C6 . . . . -31.36(6) ? C6 C1 C2 C3 . . . . -1.16(10) ? S1 C1 C2 C3 . . . . 175.34(5) ? C1 C2 C3 C4 . . . . 1.92(10) ? C2 C3 C4 C5 . . . . -0.81(11) ? C3 C4 C5 C6 . . . . -1.12(11) ? C4 C5 C6 C1 . . . . 1.86(10) ? C4 C5 C6 N1 . . . . -177.23(6) ? C2 C1 C6 C5 . . . . -0.74(9) ? S1 C1 C6 C5 . . . . -177.28(5) ? C2 C1 C6 N1 . . . . 178.32(6) ? S1 C1 C6 N1 . . . . 1.78(8) ? C7 N1 C6 C5 . . . . -165.40(7) ? C7 N1 C6 C1 . . . . 15.55(10) ? C6 N1 C7 O1 . . . . -176.50(7) ? C6 N1 C7 C8 . . . . 7.37(10) ? O1 C7 C8 S1 . . . . 141.26(6) ? N1 C7 C8 S1 . . . . -42.58(7) ? O2 S1 C8 C7 . . . . -64.45(5) ? O3 S1 C8 C7 . . . . 165.81(5) ? C1 S1 C8 C7 . . . . 50.29(5) ?