#------------------------------------------------------------------------------ #$Date: 2025-01-18 04:36:03 +0200 (Sat, 18 Jan 2025) $ #$Revision: 297377 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/33/2023360.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_2023360 loop_ _publ_author_name 'Ruser, Niklas' 'N\"ather, Christian' 'Stock, Norbert' _publ_section_title ; Syntheses and crystal structures of the cerium-based coordination polymers poly[(acetic acid)bis(\m-5-carboxythiophene-2-carboxylato)bis(\m-thiophene-2,5-dicarboxylato)dicerium(III)] and poly[(\m-acetato)aqua(\m4-thiophene-2,5-dicarboxylato)cerium(III)] ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989025000210 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac '[Ce (C2 H3 O2) (C6 H2 O4 S) (H2 O)]' _chemical_formula_moiety 'C8 H7 Ce O7 S' _chemical_formula_sum 'C8 H7 Ce O7 S' _chemical_formula_weight 387.32 _chemical_name_systematic ; Poly[(\m-acetato)aqua(\m~4~-thiophene-2,5-dicarboxylato)cerium(III)] ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.3-ac4 (compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214) ; _cell_angle_alpha 90 _cell_angle_beta 102.3540(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.03100(10) _cell_length_b 14.67550(10) _cell_length_c 7.67650(10) _cell_measurement_reflns_used 10498 _cell_measurement_temperature 99.99(10) _cell_measurement_theta_max 79.8710 _cell_measurement_theta_min 3.0660 _cell_volume 1103.89(2) _computing_cell_refinement ; CrysAlisPro 1.171.42.100a (Rigaku OD, 2023) ; _computing_data_collection ; CrysAlisPro 1.171.42.100a (Rigaku OD, 2023) ; _computing_data_reduction ; CrysAlisPro 1.171.42.100a (Rigaku OD, 2023) ; _computing_molecular_graphics ; DIAMOND (Brandenburg & Putz, 1999) and XP in SHELXTL-PC (Sheldrick, 2008) ; _computing_publication_material ; Publcif (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2016/6 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014/4 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 99.99(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_unetI/netI 0.0151 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 13515 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 80.343 _diffrn_reflns_theta_min 4.512 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 33.888 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.30071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2023) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.330 _exptl_crystal_description block _exptl_crystal_F_000 740 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.429 _refine_diff_density_min -1.304 _refine_ls_extinction_coef 0.00097(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2016/6 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 162 _refine_ls_number_reflns 2360 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.152 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0265 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+2.3818P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0771 _refine_ls_wR_factor_ref 0.0772 _reflns_number_gt 2349 _reflns_number_total 2360 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file nx2017.cif _cod_data_source_block 2 _cod_original_cell_volume 1103.890(17) _cod_database_code 2023360 _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_hkl_file ; 0 0 1 3.04 0.89 0 0 2 14.69 1.43 0 0 2 11.09 1.78 0 0 3 1.31 1.09 0 0 3 1.11 1.74 0 0 4 5897.92 106.67 0 0 5 3.49 2.09 0 0 5 1.70 1.85 0 0 5 1.54 1.41 0 0 6 1024.35 26.12 0 0 6 1069.62 26.12 0 0 6 999.43 22.88 0 0 7 1.40 2.10 0 0 7 0.74 2.12 0 0 7 0.57 1.89 0 0 7 -0.60 2.06 0 0 8 427.46 11.45 0 0 8 463.44 12.21 0 0 9 0.39 1.46 0 0 9 2.48 1.68 0 0 9 1.18 1.65 0 -1 0 1.31 0.22 0 1 0 0.44 0.14 0 1 1 1233.55 22.45 0 1 1 1200.32 22.29 0 -1 2 1587.09 30.97 0 -1 -2 1522.55 29.69 0 -1 3 237.17 7.96 0 1 3 222.08 6.75 0 -1 4 254.71 8.76 0 -1 4 281.69 9.76 0 1 4 274.24 9.32 0 1 4 241.46 8.27 0 -1 5 696.59 16.58 0 1 5 684.23 16.37 0 1 5 739.98 19.21 0 -1 5 729.36 18.89 0 -1 6 1005.24 23.48 0 1 6 968.68 24.99 0 -1 6 998.69 24.81 0 -1 6 1044.16 25.46 0 1 6 949.07 21.99 0 -1 6 978.83 21.90 0 1 6 952.64 21.66 0 1 7 8.63 2.36 0 -1 7 10.04 2.30 0 -1 7 10.16 2.30 0 1 7 7.31 2.16 0 -1 7 10.60 2.63 0 1 7 15.09 2.60 0 -1 7 9.07 2.41 0 1 8 608.03 14.47 0 -1 8 645.34 15.14 0 1 8 595.22 14.39 0 -1 9 199.42 5.52 0 1 9 217.39 6.05 0 1 9 207.11 6.00 0 2 0 39.18 1.38 0 -2 0 71.27 1.86 0 2 1 727.57 5.38 0 -2 1 692.26 6.10 0 -2 -2 333.78 7.81 0 2 2 337.91 7.97 0 2 2 325.00 8.28 0 2 3 1281.32 24.04 0 -2 -3 1117.35 23.80 0 -2 3 1246.86 25.82 0 2 3 1165.76 24.76 0 2 3 1183.92 24.22 0 2 4 58.18 3.67 0 -2 4 51.45 3.80 0 2 4 55.00 3.82 0 -2 4 57.42 4.31 0 2 5 516.76 14.90 0 -2 5 540.76 15.09 0 2 5 531.77 13.88 0 2 5 488.07 12.85 0 -2 5 522.58 13.21 0 2 6 69.69 4.89 0 2 6 71.21 4.46 0 -2 6 80.10 4.76 0 2 6 76.59 5.53 0 -2 6 81.28 6.18 0 2 6 75.69 5.98 0 -2 6 70.52 5.46 0 2 -6 78.05 5.05 0 -2 6 84.07 5.38 0 2 7 986.81 22.31 0 -2 7 976.25 21.48 0 -2 7 997.46 21.88 0 -2 7 985.68 22.79 0 -2 7 1054.88 22.55 0 -2 7 1048.76 23.81 0 2 7 963.42 21.61 0 2 7 963.53 21.70 0 -2 8 3.67 2.03 0 2 8 3.36 2.09 0 -2 8 4.01 2.17 0 2 8 3.23 1.93 0 -2 9 6.92 1.66 0 -2 9 4.72 1.54 0 -2 9 4.38 1.57 0 2 9 5.57 1.68 0 2 9 6.85 1.66 0 -3 0 1.25 0.66 0 3 0 3.49 0.61 0 3 1 479.89 9.22 0 -3 1 434.79 9.43 0 3 2 1365.17 25.01 0 -3 -2 1309.62 25.28 0 3 2 1325.28 25.70 0 3 3 62.28 3.08 0 -3 -3 56.41 3.14 0 3 3 59.17 3.16 0 3 3 57.17 3.45 0 3 4 1347.14 27.58 0 -3 4 1347.18 29.68 0 3 4 1354.20 28.98 0 3 5 437.98 12.01 0 -3 5 482.67 12.49 0 3 5 452.42 13.53 0 -3 5 447.51 13.77 0 -3 5 511.57 15.46 0 3 5 475.68 13.03 0 3 6 894.28 20.64 0 -3 6 917.66 21.01 0 -3 6 897.40 20.71 0 -3 6 878.79 23.22 0 3 6 929.95 21.38 0 -3 7 33.48 3.75 0 -3 7 27.45 2.88 0 3 7 24.71 3.25 0 3 7 26.54 3.09 0 -3 7 31.76 4.00 0 -3 7 30.02 3.31 0 3 -7 27.31 2.84 0 -3 8 956.39 20.25 0 3 8 942.36 20.23 0 -3 8 931.55 20.40 0 -3 9 89.84 3.35 0 -3 9 91.29 3.34 0 3 9 92.13 3.41 0 3 9 88.66 3.32 0 -3 9 93.56 3.42 0 -4 0 2855.22 50.85 0 4 0 2992.74 51.48 0 -4 0 2924.60 51.80 0 -4 1 208.39 5.37 0 4 1 215.20 5.12 0 4 2 772.94 16.33 0 -4 -2 790.88 16.29 0 4 3 595.85 14.40 0 4 3 618.14 13.50 0 4 4 2950.98 54.76 0 4 4 2913.66 56.87 0 -4 4 2991.81 58.25 0 4 4 3158.14 55.67 0 -4 -4 2819.00 55.42 0 -4 4 2954.11 54.49 0 4 4 2778.68 54.44 0 4 5 104.87 5.41 0 -4 5 102.46 5.00 0 4 5 99.14 5.53 0 -4 5 89.91 5.66 0 4 5 96.09 6.22 0 -4 5 94.66 6.46 0 4 6 1009.96 23.18 0 4 6 1076.02 24.16 0 4 6 1070.02 27.35 0 -4 6 1015.18 25.83 0 -4 7 236.08 8.73 0 4 7 224.96 8.42 0 4 -7 231.60 7.66 0 4 8 535.70 13.40 0 -4 8 561.26 13.73 0 4 8 557.25 13.34 0 -4 8 566.68 13.35 0 4 8 548.58 13.29 0 -4 8 574.71 13.41 0 -4 9 12.75 1.64 0 4 9 12.04 1.36 0 4 9 9.86 1.34 0 -5 0 1.05 0.89 0 5 0 -0.25 0.70 0 -5 0 1.71 0.62 0 5 0 2.11 0.67 0 -5 1 1276.30 25.68 0 5 1 1328.56 24.44 0 -5 1 1303.39 24.65 0 -5 -2 420.07 10.43 0 5 2 422.58 9.68 0 -5 -3 280.98 8.45 0 5 3 294.39 8.05 0 5 3 289.95 8.92 0 -5 -4 6.56 1.73 0 5 4 9.06 1.88 0 5 4 6.29 1.93 0 -5 4 13.56 2.98 0 -5 4 8.23 1.64 0 5 4 6.00 1.62 0 -5 5 1284.21 26.56 0 5 5 1317.04 28.11 0 -5 5 1343.36 31.47 0 5 5 1281.82 30.64 0 -5 5 1278.56 29.50 0 5 5 1275.31 28.67 0 5 6 92.63 4.98 0 5 6 89.73 5.49 0 -5 6 93.44 6.21 0 5 6 97.99 5.54 0 5 -6 101.77 5.22 0 -5 7 2.50 2.06 0 5 7 3.33 2.08 0 5 -7 1.62 1.82 0 5 7 3.89 2.59 0 -5 8 276.74 8.17 0 -5 8 266.21 8.32 0 -5 8 236.68 6.88 0 5 8 255.72 7.36 0 5 8 243.80 7.31 0 5 8 262.21 7.96 0 5 9 553.79 11.45 0 -5 9 592.37 11.65 0 -6 0 105.45 3.35 0 6 0 108.52 3.87 0 -6 0 105.76 4.11 0 6 0 112.21 3.33 0 -6 1 735.46 16.50 0 6 1 751.42 15.12 0 -6 1 729.67 15.24 0 -6 -2 154.68 5.70 0 6 2 150.33 4.90 0 6 3 1245.06 24.77 0 -6 -3 1180.49 25.50 0 -6 4 324.22 9.25 0 -6 -4 310.35 10.23 0 6 4 311.57 9.45 0 -6 5 106.87 7.15 0 -6 5 102.88 4.81 0 6 5 101.39 5.83 0 6 5 101.54 5.69 0 6 6 177.94 7.04 0 6 6 186.24 7.85 0 6 -6 196.85 7.32 0 -6 6 200.85 8.60 0 -6 7 615.11 15.29 0 6 -7 568.88 13.82 0 -6 7 564.67 13.95 0 6 7 561.24 14.04 0 -6 7 621.91 15.88 0 6 7 592.19 15.41 0 6 8 118.49 4.23 0 6 8 127.31 5.15 0 -6 8 130.42 5.33 0 -6 8 118.01 4.27 0 6 9 8.11 0.99 0 7 0 0.74 0.65 0 7 0 0.85 0.93 0 -7 0 0.27 0.71 0 -7 0 2.16 1.19 0 -7 1 250.06 6.94 0 7 1 249.85 6.88 0 -7 1 270.61 8.30 0 7 -1 247.39 7.36 0 -7 2 4451.17 84.28 0 -7 -2 4541.60 83.84 0 7 2 4726.63 82.15 0 -7 3 15.50 2.07 0 7 3 16.08 1.94 0 -7 -3 19.59 2.41 0 7 3 16.41 1.81 0 -7 4 586.41 14.09 0 7 4 607.38 15.04 0 7 5 27.56 3.36 0 7 5 23.24 3.65 0 7 5 28.14 4.57 0 -7 5 26.13 2.99 0 -7 5 24.65 4.08 0 -7 5 22.52 4.07 0 -7 5 29.90 3.89 0 7 -5 27.64 3.14 0 -7 6 1016.63 22.57 0 7 6 828.69 20.10 0 7 6 896.52 21.50 0 -7 6 982.02 22.82 0 7 6 898.97 20.22 0 -7 7 2.53 2.41 0 -7 7 10.76 2.58 0 -7 7 2.60 2.81 0 7 -7 3.84 1.77 0 7 8 1043.42 20.79 0 -7 8 1068.77 20.56 0 -7 8 1020.02 20.75 0 7 -8 999.99 19.72 0 7 8 999.49 20.37 0 -8 0 4134.42 73.93 0 8 0 4174.85 75.31 0 -8 1 812.35 17.36 0 8 1 836.70 17.62 0 -8 1 828.67 19.39 0 8 1 830.05 17.55 0 8 -1 790.44 18.13 0 -8 -1 801.47 16.71 0 8 -2 70.12 3.76 0 -8 2 81.61 4.14 0 8 2 75.32 3.52 0 8 -2 76.68 4.31 0 -8 2 77.59 4.87 0 -8 -2 90.97 4.99 0 8 2 90.15 4.05 0 -8 3 567.02 14.15 0 8 3 543.43 13.50 0 -8 3 585.33 14.70 0 -8 -3 549.11 15.27 0 -8 4 1622.37 32.52 0 8 4 1654.70 33.30 0 -8 4 1576.30 35.30 0 -8 4 1623.65 33.61 0 -8 5 8.84 2.98 0 8 5 7.98 2.38 0 8 5 5.85 2.50 0 8 -5 9.86 2.28 0 -8 5 8.98 3.40 0 -8 5 5.54 3.15 0 -8 5 5.36 2.66 0 8 5 7.63 2.52 0 -8 5 6.21 2.28 0 -8 6 579.67 15.84 0 8 6 504.74 14.58 0 8 6 567.54 15.81 0 8 6 541.83 13.96 0 8 -6 537.60 13.58 0 -8 7 399.66 11.28 0 -8 7 397.54 10.74 0 8 -7 402.18 10.60 0 8 7 359.27 10.99 0 -8 7 384.63 11.19 0 8 -7 382.62 9.85 0 8 8 214.44 6.51 0 -8 8 211.62 6.40 0 -8 8 210.95 6.03 0 8 8 218.43 6.31 0 8 8 193.90 5.59 0 -8 8 184.96 5.28 0 -8 -8 244.86 6.50 0 9 0 0.81 1.24 0 -9 0 0.65 1.51 0 -9 1 617.13 15.23 0 9 1 645.05 14.55 0 9 -1 600.32 14.48 0 9 -1 611.87 15.40 0 9 1 650.69 14.85 0 -9 1 629.31 16.64 0 9 2 10.73 1.67 0 9 -2 10.97 2.12 0 -9 -2 9.09 2.38 0 -9 2 11.18 2.15 0 9 2 9.65 1.63 0 -9 2 11.96 1.94 0 9 2 7.92 1.93 0 9 -2 8.51 1.85 0 9 3 507.22 13.16 0 -9 3 502.28 15.42 0 -9 -3 485.98 14.59 0 -9 3 517.09 13.40 0 -9 3 493.87 13.59 0 9 3 489.20 12.65 0 9 -3 484.37 13.28 0 9 4 94.62 5.31 0 9 4 93.86 5.59 0 9 -4 96.18 5.57 0 -9 4 90.42 6.39 0 -9 4 90.45 5.17 0 -9 4 95.69 6.35 0 9 4 84.55 5.38 0 -9 5 687.36 19.04 0 9 5 665.02 18.41 0 9 5 719.92 17.77 0 9 -5 702.60 17.11 0 9 -5 746.07 18.10 0 -9 5 751.42 18.89 0 9 5 685.34 17.90 0 -9 5 725.58 17.16 0 9 6 94.15 5.41 0 9 6 93.83 5.95 0 9 6 93.36 4.93 0 -9 6 95.84 5.09 0 -9 6 106.04 5.93 0 9 -6 107.73 5.43 0 9 -6 102.05 4.75 0 -9 6 96.96 6.16 0 -9 7 9.16 2.20 0 9 7 7.76 2.59 0 -9 7 8.69 2.01 0 -9 7 8.32 2.50 0 9 -7 9.28 1.70 0 9 -7 10.14 1.84 0 9 8 11.72 1.76 0 -9 -8 14.13 1.72 0 -9 8 10.61 1.18 0 9 8 12.88 1.95 0 -10 0 1659.06 33.70 0 10 0 1627.14 33.36 0 10 0 1638.02 34.01 0 10 1 80.92 3.97 0 -10 1 67.04 4.34 0 10 -1 68.06 4.40 0 10 1 73.85 4.17 0 10 -2 6.61 1.91 0 -10 2 7.20 2.30 0 -10 -2 8.90 2.40 0 -10 2 3.53 1.92 0 10 2 7.42 1.65 0 10 -2 6.75 1.88 0 10 2 5.63 1.56 0 10 -3 167.50 7.21 0 10 3 157.97 7.92 0 -10 3 165.32 8.58 0 -10 -3 158.00 7.96 0 10 -3 174.80 7.75 0 10 3 171.94 6.83 0 -10 3 166.31 7.34 0 10 3 161.54 6.66 0 -10 3 183.51 7.39 0 -10 4 1431.62 29.33 0 10 4 1338.43 29.66 0 10 4 1368.57 29.75 0 -10 -4 1232.80 29.60 0 10 4 1328.04 29.24 0 -10 4 1387.75 30.28 0 10 -4 1485.60 29.86 0 10 4 1256.37 31.67 0 -10 5 79.07 5.84 0 10 5 75.02 5.40 0 10 5 81.61 5.05 0 -10 5 73.30 4.30 0 -10 5 81.81 4.71 0 10 5 76.16 5.07 0 10 -5 76.08 4.51 0 10 -5 85.04 5.02 0 -10 5 81.59 5.54 0 -10 6 46.23 4.21 0 -10 -6 48.26 4.58 0 10 6 49.90 4.38 0 10 6 46.18 3.60 0 10 -6 51.22 3.70 0 10 -6 43.52 3.16 0 10 6 44.19 3.86 0 -10 6 41.93 3.95 0 10 -7 402.51 9.57 0 10 7 358.05 10.30 0 -10 7 389.33 10.16 0 -10 7 392.73 10.10 0 10 -7 392.78 9.17 0 -10 -7 395.26 10.68 0 10 8 160.96 4.11 0 10 8 157.97 4.27 0 11 0 2.60 1.52 0 -11 0 2.55 2.09 0 -11 1 134.90 5.84 0 11 1 153.75 6.18 0 11 1 157.30 6.56 0 -11 -1 162.17 8.40 0 11 -1 151.43 6.97 0 11 2 2148.35 41.52 0 11 -2 2229.06 43.68 0 -11 -2 2018.97 45.37 0 -11 2 2130.47 45.70 0 11 2 2078.64 42.50 0 -11 2 1985.49 42.68 0 11 -2 2204.26 42.48 0 11 2 2118.32 41.92 0 -11 -2 2025.88 41.79 0 -11 2 2160.86 43.04 0 -11 -3 -0.29 1.82 0 11 3 2.63 1.99 0 11 3 1.76 2.39 0 11 -3 2.04 2.16 0 -11 3 1.37 3.36 0 -11 3 3.45 2.42 0 -11 3 0.95 2.59 0 -11 -3 1.80 3.32 0 11 4 1010.23 23.85 0 11 -4 1051.68 23.51 0 -11 4 985.29 23.76 0 11 4 976.51 23.16 0 -11 -4 924.50 23.61 0 -11 4 988.97 23.56 0 -11 4 1076.99 23.40 0 11 5 132.05 6.40 0 11 -5 140.38 6.38 0 -11 5 125.90 6.57 0 -11 -5 122.24 7.00 0 11 -5 134.17 5.83 0 -11 5 128.72 5.80 0 11 5 122.10 6.29 0 -11 5 126.98 7.10 0 -11 6 1280.98 26.60 0 -11 -6 1227.54 27.27 0 11 7 22.58 2.78 0 11 7 25.46 2.65 0 -11 -7 26.27 2.84 0 -11 7 23.59 2.61 0 -11 -7 25.52 2.94 0 11 -7 23.47 2.06 0 -12 0 687.80 17.36 0 12 0 660.69 16.90 0 12 0 634.29 17.41 0 12 1 453.24 12.58 0 -12 -1 457.72 16.32 0 12 -1 391.73 13.22 0 12 1 437.87 12.93 0 -12 -1 439.39 12.82 0 -12 -1 435.54 12.76 0 -12 1 450.09 13.46 0 12 1 437.74 12.97 0 -12 -2 60.04 4.41 0 12 2 61.40 4.20 0 -12 2 49.78 4.82 0 12 2 57.45 4.60 0 -12 2 57.85 5.01 0 -12 -2 54.88 4.29 0 -12 2 62.90 4.95 0 -12 -2 58.63 5.79 0 -12 3 1295.68 29.31 0 12 3 1137.80 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1421.10 29.56 -8 6 5 1379.48 28.99 -8 -6 5 1338.76 28.35 -8 6 5 1417.09 29.20 -8 -6 5 1408.02 29.44 -8 6 5 1388.68 28.91 -8 6 5 1414.60 29.79 -8 -6 5 1444.75 29.96 -8 -6 4 217.89 8.45 -8 6 4 200.44 7.14 -8 -6 4 205.21 8.16 -8 -6 4 208.80 8.04 -8 -6 4 210.14 8.06 -8 -6 4 220.15 8.52 -8 6 4 196.96 7.06 -8 -6 4 196.20 7.03 -8 6 4 200.50 7.61 -8 6 4 212.77 7.83 -8 -6 4 214.33 8.37 -8 6 4 210.81 8.12 -8 6 4 201.81 8.05 -8 -6 3 45.71 4.15 -8 6 3 44.23 3.52 -8 -6 3 48.40 4.06 -8 -6 3 49.22 4.01 -8 -6 3 50.01 4.26 -8 -6 3 40.84 3.99 -8 -6 3 48.96 4.37 -8 6 3 53.53 4.23 -8 -6 3 42.49 3.94 -8 6 3 58.03 4.41 -8 6 3 63.20 4.16 -8 6 3 49.93 4.30 -8 6 3 46.79 3.69 -8 6 3 49.10 3.80 -8 6 3 54.61 4.00 -8 6 3 45.75 3.91 -8 6 3 49.76 4.17 -8 6 2 220.37 8.70 -8 6 2 216.67 7.71 -8 -6 2 228.12 8.25 -8 -6 2 227.83 8.53 -8 -6 2 207.57 7.91 -8 6 2 225.61 7.91 -8 6 2 237.18 8.72 -8 -6 2 219.82 8.51 -8 6 2 227.98 8.23 -8 -6 2 232.26 8.64 -8 6 2 220.07 7.98 -8 6 2 216.95 8.31 -8 -6 1 1368.15 29.41 -8 -6 1 1332.92 28.92 -8 6 1 1328.72 27.89 -8 6 1 1402.91 28.59 -8 6 1 1408.17 29.81 -8 -6 1 1403.42 30.25 -8 6 1 1408.60 28.79 -8 6 1 1404.46 30.18 -8 -6 1 1437.75 30.65 -8 6 1 1393.94 29.61 -8 6 1 1370.95 28.97 -8 -6 0 22.54 3.06 -8 -6 0 23.10 2.73 -8 6 0 18.78 2.47 -8 -6 0 18.17 3.08 -8 6 0 20.77 3.02 -8 6 0 19.54 2.71 -8 6 0 18.87 2.74 -8 -6 0 20.68 2.60 -8 6 0 17.78 2.58 -8 6 -1 826.67 18.70 -8 -6 -1 805.39 18.40 -8 -6 -1 859.29 20.06 -8 6 -1 848.45 19.71 -8 6 -1 833.00 19.25 -8 -6 -1 824.80 19.57 -8 6 -2 107.69 5.18 -8 6 -2 93.33 4.92 -8 6 -2 112.30 4.96 -8 -6 -2 101.08 4.62 8 -6 2 95.79 5.52 -8 6 -3 402.30 10.38 8 -6 3 387.17 11.81 -8 6 -3 405.22 10.55 8 -6 4 18.10 2.71 8 -6 4 20.28 2.81 8 6 4 17.13 2.51 -8 6 -5 1099.78 21.06 8 -6 5 1140.67 21.80 -8 -6 -5 1125.17 21.44 8 -6 5 1148.09 21.92 -8 7 7 52.73 2.84 -8 -7 7 52.57 2.92 -8 7 7 58.44 3.06 -8 -7 6 633.47 14.75 -8 -7 6 616.31 14.02 -8 7 6 610.36 14.30 -8 7 6 625.59 14.53 -8 7 6 589.76 13.99 -8 -7 6 618.66 14.11 -8 7 6 623.46 14.85 -8 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115.89 6.01 -8 -7 1 111.92 5.87 -8 -7 1 126.51 6.55 -8 -7 1 111.15 5.81 -8 -7 1 109.58 5.89 -8 -7 1 112.15 5.38 -8 -7 1 108.33 6.28 -8 7 1 122.54 6.27 -8 -7 1 106.91 6.29 -8 7 1 119.24 5.67 -8 7 1 113.14 5.39 -8 -7 0 1539.39 32.66 -8 -7 0 1543.73 32.44 -8 7 0 1584.31 31.60 -8 -7 0 1564.50 33.17 -8 7 0 1576.11 32.36 -8 -7 0 1513.39 32.85 -8 7 0 1528.99 32.04 -8 7 0 1621.30 31.90 -8 -7 -1 48.21 4.13 -8 7 -1 49.13 4.00 -8 -7 -1 49.40 4.55 -8 -7 -1 44.34 3.73 -8 7 -1 45.29 3.73 8 -7 2 319.23 10.46 -8 7 -2 322.65 9.72 -8 7 -2 332.93 9.72 8 7 3 193.03 6.99 -8 7 -3 179.52 6.12 8 -7 4 1205.78 25.15 8 7 4 1289.12 25.09 8 -7 4 1230.06 25.17 8 -7 5 9.76 1.55 8 7 5 12.38 1.71 -8 7 -5 11.01 1.31 -8 -7 -5 11.66 1.45 -8 8 7 88.16 3.15 -8 -8 7 87.31 3.19 -8 8 7 84.23 3.23 -8 -8 6 37.65 2.65 -8 8 6 38.53 3.12 -8 -8 6 35.37 2.68 -8 8 6 40.54 2.80 -8 8 6 35.94 2.70 -8 -8 6 40.54 3.17 -8 8 5 431.46 11.62 -8 -8 5 418.66 11.41 -8 -8 5 386.34 10.89 -8 -8 5 404.76 11.19 -8 8 5 425.74 11.33 -8 8 5 432.29 11.59 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1932.25 38.44 -8 -9 3 1966.64 39.12 -8 -9 3 1994.46 39.60 -8 9 3 1927.35 38.19 -8 9 3 2012.80 39.85 -8 9 3 1894.15 38.09 -8 9 3 1920.55 37.87 -8 9 3 1975.19 38.94 -8 9 3 2037.17 39.05 -8 -9 2 70.16 4.47 -8 -9 2 65.52 4.68 -8 -9 2 63.72 4.41 -8 9 2 64.72 4.67 -8 -9 2 67.45 4.99 -8 9 2 61.73 4.10 -8 9 2 61.81 4.12 -8 9 2 60.68 4.82 -8 -9 2 64.76 4.65 -8 9 2 66.66 4.48 -8 9 1 189.31 6.58 -8 9 1 200.62 7.34 -8 9 1 182.65 7.48 -8 -9 1 180.56 7.12 -8 -9 1 188.84 7.73 -8 -9 1 195.89 7.43 -8 -9 1 189.22 8.15 -8 9 1 191.57 7.65 -8 -9 1 192.01 8.17 -8 9 1 191.30 7.19 -8 -9 0 34.44 4.02 -8 9 0 27.95 3.15 -8 -9 0 31.07 3.09 -8 -9 0 31.28 3.43 -8 -9 0 37.61 3.80 -8 -9 0 29.97 3.98 -8 9 0 36.49 3.37 -8 9 0 29.95 3.01 -8 9 -1 1367.00 27.48 -8 -9 -1 1366.52 28.69 -8 -9 -1 1344.07 29.34 -8 -9 -1 1329.24 27.93 -8 -9 -1 1345.77 28.33 -8 9 -1 1355.67 27.95 8 9 2 2.44 1.76 -8 9 -2 3.70 2.00 -8 9 -2 1.66 1.78 8 -9 2 3.26 2.00 -8 -9 -2 1.59 1.90 -8 -9 -2 1.83 1.93 8 9 2 1.71 1.91 8 9 3 757.49 17.62 -8 9 -3 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-10 -8 2 471.89 11.76 -10 8 2 462.55 11.22 -10 8 2 469.76 11.36 -10 8 2 430.77 10.61 -10 -8 2 439.83 11.03 -10 -8 1 22.45 2.65 -10 -8 1 19.60 2.29 -10 8 1 30.02 2.47 -10 8 1 22.08 2.20 -10 8 1 23.94 2.59 -10 -8 1 22.82 2.64 -10 -8 1 31.69 2.85 -10 -8 0 1009.16 20.41 -10 8 0 1023.84 20.64 -10 8 0 1030.78 20.84 -10 8 0 999.95 20.81 -10 -8 0 1022.15 21.16 -10 -8 0 1029.22 21.15 -10 -8 -1 190.62 5.31 -10 8 -1 215.84 6.16 -10 8 -1 202.69 5.85 -10 -8 -1 209.61 6.39 -10 -8 -1 209.64 6.47 -10 8 -1 215.36 6.23 -10 -8 -2 9.99 1.78 -10 -8 -2 9.17 1.54 -10 8 -2 8.61 1.31 -10 9 5 996.15 18.93 -10 9 5 1058.79 19.16 -10 -9 4 6.18 1.76 -10 9 4 6.49 1.49 -10 9 4 5.16 1.60 -10 -9 4 5.32 1.68 -10 -9 3 147.97 5.42 -10 9 3 151.14 5.28 -10 9 3 147.96 4.87 -10 -9 3 143.67 5.30 -10 -9 3 152.03 5.43 -10 9 3 143.38 5.03 -10 -9 3 151.57 5.32 -10 -9 2 8.89 2.07 -10 -9 2 9.80 2.37 -10 9 2 8.83 2.13 -10 9 2 9.32 2.08 -10 -9 2 8.83 2.02 -10 9 2 7.41 1.50 -10 -9 1 770.64 16.42 -10 -9 1 839.28 17.27 -10 -9 1 858.28 17.53 -10 9 1 792.16 17.02 -10 9 1 789.86 16.44 -10 9 1 842.21 17.23 -10 -9 1 813.48 17.12 -10 -9 0 4.44 1.42 -10 9 0 4.73 2.13 -10 9 0 5.30 2.02 -10 -9 0 5.61 2.13 -10 -9 0 6.74 2.15 -10 9 -1 761.10 15.44 -10 9 -1 840.71 16.11 -10 -9 -1 793.07 16.09 -10 -9 -1 826.48 16.27 -10 9 -1 802.93 15.86 -10 -9 -2 25.08 1.56 -10 9 -2 21.45 1.33 -10 10 4 391.50 8.53 -10 -10 4 406.03 8.65 -10 -10 3 232.08 6.24 -10 -10 3 224.93 6.15 -10 -10 3 230.89 6.13 -10 10 3 221.32 5.76 -10 10 3 242.88 6.18 -10 -10 3 224.39 6.07 -10 -10 2 192.52 5.57 -10 -10 2 166.42 4.93 -10 -10 2 199.38 5.61 -10 10 2 197.74 5.42 -10 10 2 186.29 5.40 -10 10 2 168.39 4.63 -10 -10 2 182.75 5.30 -10 -10 1 531.85 11.73 -10 -10 1 524.59 11.68 -10 -10 1 518.15 11.27 -10 10 1 522.49 10.98 -10 -10 0 434.21 9.70 -10 10 0 440.69 9.56 -10 -10 0 419.21 9.37 -10 -10 -1 116.76 3.50 -10 -10 -1 113.23 3.42 -10 -11 3 10.24 1.28 -10 -11 3 9.67 1.27 -10 11 3 9.62 1.18 -10 -11 2 824.16 15.25 -10 -11 2 799.54 15.33 -10 11 2 814.71 14.97 -10 11 2 797.17 15.05 -10 -11 1 8.53 1.30 -10 -11 1 10.03 1.56 -10 11 1 11.91 1.53 -10 -11 1 10.01 1.54 -10 11 0 57.34 2.11 -11 0 3 2.31 1.93 -11 0 3 0.09 1.87 -11 0 3 3.18 2.02 -11 0 2 962.94 21.02 -11 0 2 1012.93 21.09 -11 0 2 965.48 20.99 -11 0 2 973.29 20.63 -11 0 2 975.78 21.11 -11 0 1 1.75 1.91 -11 0 1 1.40 1.83 -11 0 0 441.75 10.97 -11 0 0 445.05 10.93 -11 0 0 433.38 11.14 -11 0 -1 3.54 1.61 -11 0 -1 2.54 1.46 -11 0 -1 4.15 1.80 -11 0 -2 187.48 5.39 -11 0 -2 179.54 5.50 -11 0 -3 1.78 0.74 -11 1 4 172.15 5.75 -11 1 3 348.16 9.59 -11 -1 3 354.98 9.86 -11 -1 3 353.54 9.73 -11 1 3 339.93 9.69 -11 1 3 335.73 9.44 -11 -1 3 338.09 9.19 -11 1 2 446.40 11.33 -11 -1 2 440.13 11.41 -11 -1 2 410.08 11.03 -11 1 2 439.37 11.39 -11 1 2 425.41 11.26 -11 -1 2 425.68 11.29 -11 -1 2 418.77 10.98 -11 1 2 409.55 10.54 -11 1 1 912.09 19.91 -11 -1 1 920.12 20.03 -11 -1 1 936.32 19.74 -11 1 1 905.34 19.84 -11 -1 1 928.36 20.02 -11 1 1 921.03 19.90 -11 -1 1 925.75 19.86 -11 1 0 65.48 3.61 -11 -1 0 60.05 3.57 -11 -1 0 60.19 3.32 -11 1 0 58.46 3.46 -11 -1 -1 4.18 1.86 -11 -1 -1 4.45 1.38 -11 1 -1 5.17 1.57 -11 1 -1 2.03 1.57 -11 -1 -1 4.47 1.74 -11 -1 -2 259.58 6.47 -11 1 -2 261.98 6.54 -11 1 -3 855.92 15.93 -11 2 4 3.26 1.88 -11 2 4 2.17 1.67 -11 -2 4 1.60 1.57 -11 2 3 1439.65 29.03 -11 -2 3 1471.95 29.64 -11 -2 3 1448.61 29.10 -11 -2 3 1524.10 29.60 -11 2 3 1447.07 28.90 -11 -2 3 1474.95 29.02 -11 2 2 61.91 3.76 -11 -2 2 60.87 3.71 -11 2 2 64.05 3.93 -11 -2 2 64.70 3.95 -11 2 2 62.97 3.67 -11 -2 2 63.36 4.01 -11 -2 2 63.88 3.75 -11 2 1 14.08 2.35 -11 -2 1 16.70 2.49 -11 -2 1 18.37 2.59 -11 2 1 19.91 2.44 -11 -2 1 16.98 2.23 -11 2 1 18.33 2.56 -11 2 0 2.52 1.76 -11 -2 0 8.05 1.91 -11 -2 0 4.13 1.74 -11 2 0 3.44 1.77 -11 -2 0 2.17 1.38 -11 2 0 4.99 1.87 -11 -2 -1 1893.60 35.59 -11 -2 -1 1961.44 36.03 -11 2 -1 1991.24 36.06 -11 2 -1 2008.57 35.84 -11 -2 -2 17.06 1.70 -11 -2 -2 18.07 1.86 -11 2 -2 17.74 1.60 -11 2 -3 39.85 1.59 -11 3 4 414.37 10.19 -11 3 4 402.73 9.78 -11 3 3 173.21 5.91 -11 3 3 174.55 6.02 -11 -3 3 167.58 5.79 -11 3 3 179.59 6.22 -11 -3 3 170.57 6.47 -11 -3 3 177.19 6.29 -11 -3 3 173.67 6.08 -11 3 2 283.97 8.47 -11 -3 2 286.66 8.26 -11 -3 2 293.60 8.26 -11 -3 2 312.31 8.87 -11 3 2 292.48 8.27 -11 -3 2 309.48 9.01 -11 -3 2 300.65 8.67 -11 -3 1 453.72 11.00 -11 3 1 466.35 11.75 -11 -3 1 467.06 11.30 -11 -3 1 470.65 11.76 -11 3 1 475.69 11.52 -11 -3 1 488.84 12.04 -11 3 1 470.85 11.69 -11 3 0 212.19 6.60 -11 -3 0 197.69 6.26 -11 -3 0 210.38 6.56 -11 3 0 201.89 6.38 -11 -3 0 209.25 6.68 -11 3 0 200.01 6.37 -11 3 -1 0.85 1.87 -11 -3 -1 3.63 1.85 -11 3 -1 3.12 1.85 -11 -3 -1 3.06 1.80 -11 3 -1 1.14 1.30 -11 3 -2 732.57 14.44 -11 -3 -2 735.75 14.74 -11 -3 -2 721.37 14.36 -11 3 -2 756.41 14.80 -11 4 4 176.39 5.56 -11 -4 4 170.41 5.62 -11 -4 3 87.03 4.20 -11 -4 3 79.75 3.93 -11 4 3 94.63 4.27 -11 4 3 87.29 4.00 -11 4 3 83.65 3.99 -11 -4 3 84.90 4.11 -11 4 2 623.71 13.95 -11 4 2 606.57 14.36 -11 -4 2 641.83 14.47 -11 4 2 639.44 14.59 -11 -4 2 653.05 14.66 -11 4 1 35.91 2.88 -11 -4 1 34.96 2.70 -11 -4 1 33.85 2.80 -11 -4 1 33.88 3.03 -11 -4 1 34.55 2.84 -11 4 0 572.96 12.96 -11 -4 0 562.71 13.01 -11 -4 0 579.27 12.97 -11 4 0 575.51 12.85 -11 -4 0 579.13 13.37 -11 4 0 587.71 13.21 -11 4 -1 157.15 5.11 -11 -4 -1 157.26 5.17 -11 -4 -1 152.72 4.80 -11 4 -1 156.04 5.01 -11 -4 -1 164.14 5.27 -11 4 -2 181.21 4.76 -11 -4 -2 177.46 4.99 -11 4 -2 174.23 4.76 -11 -5 4 35.82 2.90 -11 5 4 35.69 2.84 -11 -5 3 167.78 5.79 -11 5 3 171.55 5.62 -11 -5 3 180.37 6.27 -11 5 3 172.33 5.63 -11 5 3 169.75 5.63 -11 -5 3 173.79 5.79 -11 5 2 66.54 3.33 -11 -5 2 72.15 3.79 -11 5 2 67.79 3.64 -11 -5 2 69.48 3.58 -11 -5 2 65.43 3.86 -11 -5 2 75.39 3.83 -11 5 1 1211.48 24.45 -11 -5 1 1231.15 24.44 -11 -5 1 1209.22 24.20 -11 -5 1 1261.92 24.73 -11 5 0 10.49 1.99 -11 5 0 13.40 2.39 -11 -5 0 6.25 1.63 -11 -5 0 13.20 2.44 -11 -5 0 9.89 2.14 -11 -5 0 9.94 2.19 -11 5 -1 4.62 1.42 -11 5 -1 3.06 1.46 -11 -5 -1 3.11 1.31 -11 -5 -1 2.27 1.60 -11 -5 -1 4.47 1.55 -11 -5 -1 3.68 1.57 -11 5 -2 30.73 1.76 -11 -5 -2 24.35 1.43 -11 -6 4 24.13 2.18 -11 6 4 23.33 2.10 -11 -6 3 1098.88 21.58 -11 -6 3 1073.40 21.59 -11 -6 3 1066.77 21.85 -11 6 3 1056.52 21.25 -11 6 3 1065.86 21.19 -11 -6 3 1083.61 21.47 -11 -6 2 100.40 4.57 -11 -6 2 98.97 4.31 -11 -6 2 98.09 4.37 -11 6 2 98.55 4.10 -11 6 2 94.24 3.81 -11 -6 2 100.95 4.17 -11 6 1 141.14 5.13 -11 -6 1 148.99 5.33 -11 6 1 143.83 5.11 -11 -6 1 139.85 5.12 -11 -6 1 135.29 4.54 -11 -6 1 143.44 5.46 -11 -6 1 151.57 5.22 -11 6 0 75.25 3.48 -11 -6 0 78.84 3.59 -11 -6 0 66.78 2.78 -11 -6 0 77.13 3.48 -11 6 -1 1066.49 20.34 -11 -6 -1 1082.85 20.52 -11 -6 -1 1026.83 19.91 -11 -6 -2 24.32 1.31 -11 6 -2 23.06 1.22 -11 7 4 700.61 14.07 -11 7 3 117.90 4.08 -11 7 3 110.82 3.96 -11 -7 2 510.59 11.28 -11 7 2 485.00 10.79 -11 -7 2 513.21 11.65 -11 -7 2 502.12 11.18 -11 -7 1 69.66 3.48 -11 -7 1 66.19 3.18 -11 7 1 67.70 3.18 -11 7 1 66.88 3.19 -11 7 0 435.57 9.75 -11 7 0 463.55 10.04 -11 -7 0 471.27 10.35 -11 -7 0 443.44 9.67 -11 -7 -1 9.96 1.43 -11 -8 3 312.36 7.78 -11 8 3 347.89 7.60 -11 8 2 230.14 5.71 -11 -8 2 246.87 6.39 -11 -8 2 241.87 6.31 -11 -8 2 241.56 6.12 -11 8 1 72.15 3.07 -11 -8 1 73.29 3.21 -11 -8 1 76.97 3.22 -11 8 0 119.68 3.55 -11 -8 0 131.87 4.00 -11 -8 0 124.04 4.00 -11 8 0 122.69 3.62 -11 9 3 60.59 2.08 -11 -9 2 14.19 1.50 -11 9 2 17.98 1.50 -11 -9 2 17.84 1.49 -11 9 1 1496.81 24.45 -11 -9 1 1367.87 24.42 -12 0 3 0.98 1.51 -12 0 2 1249.68 23.86 -12 0 2 1218.95 23.98 -12 0 1 1.11 1.53 -12 0 0 19.23 1.49 -12 0 0 23.71 1.91 -12 0 0 21.40 1.76 -12 0 -1 3.21 1.00 -12 0 -1 1.02 0.89 -12 1 3 306.55 7.56 -12 1 2 39.66 2.67 -12 1 2 40.42 2.72 -12 -1 2 40.28 2.49 -12 1 1 267.48 6.73 -12 -1 1 264.99 6.90 -12 1 1 263.41 6.81 -12 -1 1 246.61 6.60 -12 -1 0 739.28 14.56 -12 -1 0 730.28 14.47 -12 -1 -1 63.93 2.32 -12 2 2 59.91 3.03 -12 2 2 58.52 3.06 -12 -2 2 60.16 3.04 -12 2 2 59.04 2.92 -12 -2 2 56.98 2.88 -12 2 1 391.64 8.91 -12 2 1 379.18 8.97 -12 -2 1 386.61 9.05 -12 2 1 384.92 8.91 -12 -2 1 388.91 8.95 -12 2 0 3.04 1.32 -12 -2 0 5.36 1.43 -12 2 0 5.63 1.33 -12 2 -1 442.64 8.65 -12 -2 -1 455.90 8.77 -12 3 3 117.42 4.01 -12 3 3 121.62 3.98 -12 3 2 3.47 1.45 -12 3 2 3.17 1.50 -12 -3 2 3.73 1.49 -12 -3 2 2.77 1.46 -12 -3 2 4.92 1.41 -12 3 1 94.98 3.46 -12 3 1 97.38 3.64 -12 -3 1 95.29 3.57 -12 3 0 1227.42 22.65 -12 -3 0 1175.34 22.47 -12 -3 0 1247.07 22.83 -12 -3 -1 41.43 1.61 -12 4 3 40.18 2.24 -12 -4 2 1394.46 26.69 -12 4 2 1440.63 26.50 -12 4 1 59.96 2.57 -12 4 1 57.43 2.74 -12 -4 1 50.05 2.43 -12 -4 1 58.81 2.78 -12 -4 1 55.68 2.65 -12 4 0 5.95 1.28 -12 -4 0 5.59 1.23 -12 5 3 249.92 5.82 -12 5 2 3.81 1.30 -12 5 2 5.68 1.41 -12 -5 2 2.56 1.26 -12 -5 1 198.29 5.24 -12 -5 1 201.58 5.13 -12 5 1 206.69 5.03 -12 -5 0 362.00 7.53 -12 5 0 387.50 7.75 -12 6 2 299.29 6.52 -12 6 1 115.89 3.01 -12 6 1 109.28 2.99 TITL stock36_auto in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 10.030958 14.675493 7.676547 90.0000 102.3543 90.0000 ZERR 4.00 0.000082 0.000127 0.000072 0.0000 0.0009 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O Ce UNIT 4.00 28.00 28.00 32.00 4.00 REM CrysAlisPro recorded range (K): Min=99.9; max=100.0; aver:100.0 TEMP -173 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 65416 _shelx_res_file ; TITL stock36_auto in P21/c #14 stock36.res created by SHELXL-2016/6 at 13:32:22 on 04-Sep-2023 REM reset to P21/c #14 CELL 1.54184 10.030958 14.675493 7.676547 90 102.3543 90 ZERR 4 0.000082 0.000127 0.000072 0 0.0009 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Ce O S UNIT 32 28 4 28 4 DFIX 0.87 O7 H7a O7 H7b DANG 1.38 H7a H7b L.S. 10 PLAN 10 TEMP -173 BOND $H HTAB fmap 2 acta REM REM REM WGHT 0.050800 2.381800 EXTI 0.000967 FVAR 0.34628 CE1 3 0.397766 0.611974 0.393220 11.00000 0.00288 0.00494 = 0.00770 0.00042 -0.00018 0.00049 S1 5 0.978230 0.624558 0.897642 11.00000 0.00467 0.00732 = 0.01422 0.00084 -0.00134 -0.00070 C1 1 0.833541 0.669313 0.763984 11.00000 0.00398 0.01361 = 0.00872 -0.00012 -0.00057 -0.00031 C2 1 0.838488 0.762806 0.755095 11.00000 0.00612 0.01296 = 0.01491 0.00170 -0.00211 0.00051 AFIX 43 H2 2 0.766359 0.799189 0.690202 11.00000 -1.20000 AFIX 0 C3 1 0.962559 0.798733 0.853029 11.00000 0.00880 0.00729 = 0.01823 0.00226 -0.00255 0.00067 AFIX 43 H3 2 0.984488 0.861789 0.859212 11.00000 -1.20000 AFIX 0 C4 1 1.048088 0.731620 0.938568 11.00000 0.00497 0.00974 = 0.00858 0.00061 -0.00080 -0.00224 C5 1 0.722739 0.608257 0.670260 11.00000 0.00758 0.01004 = 0.01290 -0.00069 0.00190 -0.00262 O1 4 0.622469 0.646142 0.570219 11.00000 0.00872 0.01221 = 0.01766 0.00270 -0.00410 -0.00277 O2 4 0.738662 0.523567 0.696038 11.00000 0.00949 0.01165 = 0.01729 0.00211 -0.00511 -0.00126 C6 1 1.184834 0.741745 1.056076 11.00000 0.00379 0.01122 = 0.00520 -0.00109 0.00061 -0.00048 O3 4 1.235692 0.672969 1.143427 11.00000 0.00709 0.01213 = 0.00915 0.00180 -0.00297 0.00011 O4 4 1.243556 0.819273 1.062856 11.00000 0.00708 0.00821 = 0.01225 -0.00071 0.00002 -0.00247 O5 4 0.565923 0.484007 0.337060 11.00000 0.01056 0.01260 = 0.01069 0.00303 0.00386 0.00204 O6 4 0.534728 0.598797 0.150075 11.00000 0.01232 0.01009 = 0.01484 0.00326 0.00456 0.00264 C7 1 0.602777 0.530222 0.213261 11.00000 0.00741 0.00649 = 0.00861 0.00229 0.00059 -0.00102 C8 1 0.728237 0.501650 0.152925 11.00000 0.01256 0.01148 = 0.01952 -0.00164 0.00930 -0.00049 AFIX 137 H8A 2 0.743427 0.542620 0.058242 11.00000 -1.20000 H8B 2 0.716894 0.439144 0.107223 11.00000 -1.20000 H8C 2 0.806844 0.504409 0.253655 11.00000 -1.20000 AFIX 0 O7 4 0.445286 0.778509 0.371112 11.00000 0.01311 0.01055 = 0.01022 -0.00060 -0.00300 -0.00240 H7A 2 0.386828 0.806563 0.290568 11.00000 -1.50000 H7B 2 0.483858 0.815594 0.452144 11.00000 -1.50000 HKLF 4 REM stock36_auto in P21/c #14 REM R1 = 0.0265 for 2349 Fo > 4sig(Fo) and 0.0266 for all 2360 data REM 162 parameters refined using 3 restraints END WGHT 0.0508 2.3821 REM Instructions for potential hydrogen bonds EQIV $6 -x+2, -y+1, -z+1 HTAB C8 O3_$6 EQIV $4 x-1, y, z-1 HTAB O7 O4_$4 EQIV $7 x, -y+3/2, z+1/2 HTAB O7 O6_$7 REM Highest difference peak 1.429, deepest hole -1.304, 1-sigma level 0.170 Q1 1 0.3957 0.5598 0.3949 11.00000 0.05 1.43 Q2 1 0.4069 0.6629 0.4041 11.00000 0.05 1.28 Q3 1 0.3471 0.6171 0.2250 11.00000 0.05 1.03 Q4 1 0.4521 0.6115 0.5575 11.00000 0.05 0.96 Q5 1 0.4912 0.6128 0.5170 11.00000 0.05 0.76 Q6 1 1.2620 0.6217 1.1329 11.00000 0.05 0.72 Q7 1 0.5536 0.6165 0.6323 11.00000 0.05 0.70 Q8 1 0.5989 0.6445 0.1104 11.00000 0.05 0.65 Q9 1 0.4567 0.6713 0.3351 11.00000 0.05 0.64 Q10 1 0.4721 0.5579 0.3252 11.00000 0.05 0.62 ; _shelx_res_checksum 27435 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 Ce Ce1 0.39777(2) 0.61197(2) 0.39322(2) 0.00537(11) Uani d 1 . . S S1 0.97823(9) 0.62456(6) 0.89764(12) 0.00924(18) Uani d 1 . . C C1 0.8335(3) 0.6693(2) 0.7640(5) 0.0091(7) Uani d 1 . . C C2 0.8385(4) 0.7628(3) 0.7551(5) 0.0120(7) Uani d 1 . . H H2 0.766359 0.799189 0.690202 0.014 Uiso calc 1 . . C C3 0.9626(4) 0.7987(2) 0.8530(5) 0.0123(7) Uani d 1 . . H H3 0.984488 0.861789 0.859212 0.015 Uiso calc 1 . . C C4 1.0481(3) 0.7316(2) 0.9386(5) 0.0081(6) Uani d 1 . . C C5 0.7227(4) 0.6083(2) 0.6703(5) 0.0102(7) Uani d 1 . . O O1 0.6225(3) 0.64614(19) 0.5702(4) 0.0139(5) Uani d 1 . . O O2 0.7387(3) 0.52357(18) 0.6960(4) 0.0140(5) Uani d 1 . . C C6 1.1848(3) 0.7417(2) 1.0561(4) 0.0068(6) Uani d 1 . . O O3 1.2357(2) 0.67297(17) 1.1434(3) 0.0102(5) Uani d 1 . . O O4 1.2436(2) 0.81927(17) 1.0629(3) 0.0095(5) Uani d 1 . . O O5 0.5659(3) 0.48401(17) 0.3371(3) 0.0110(5) Uani d 1 . . O O6 0.5347(3) 0.59880(18) 0.1501(4) 0.0122(5) Uani d 1 . . C C7 0.6028(3) 0.5302(2) 0.2133(5) 0.0077(6) Uani d 1 . . C C8 0.7282(4) 0.5017(3) 0.1529(5) 0.0136(7) Uani d 1 . . H H8A 0.743427 0.542620 0.058242 0.016 Uiso calc 1 . . H H8B 0.716894 0.439144 0.107223 0.016 Uiso calc 1 . . H H8C 0.806844 0.504409 0.253655 0.016 Uiso calc 1 . . O O7 0.4453(3) 0.77851(18) 0.3711(3) 0.0121(5) Uani d 1 . . H H7A 0.387(4) 0.807(3) 0.291(5) 0.018 Uiso d 1 . . H H7B 0.484(5) 0.816(3) 0.452(5) 0.018 Uiso d 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 Ce1 0.00288(14) 0.00494(15) 0.00770(14) 0.00049(5) -0.00018(9) 0.00042(5) S1 0.0047(4) 0.0073(4) 0.0142(4) -0.0007(3) -0.0013(3) 0.0008(3) C1 0.0040(15) 0.0136(17) 0.0087(15) -0.0003(12) -0.0006(12) -0.0001(12) C2 0.0061(16) 0.0130(18) 0.0149(18) 0.0005(12) -0.0021(13) 0.0017(13) C3 0.0088(15) 0.0073(16) 0.0182(17) 0.0007(12) -0.0025(13) 0.0023(13) C4 0.0050(15) 0.0097(16) 0.0086(15) -0.0022(12) -0.0008(12) 0.0006(12) C5 0.0076(17) 0.0100(18) 0.0129(18) -0.0026(11) 0.0019(14) -0.0007(12) O1 0.0087(11) 0.0122(13) 0.0177(13) -0.0028(10) -0.0041(10) 0.0027(11) O2 0.0095(12) 0.0116(13) 0.0173(13) -0.0013(9) -0.0051(10) 0.0021(10) C6 0.0038(15) 0.0112(16) 0.0052(15) -0.0005(12) 0.0006(12) -0.0011(12) O3 0.0071(11) 0.0121(12) 0.0091(11) 0.0001(9) -0.0030(9) 0.0018(9) O4 0.0071(11) 0.0082(12) 0.0122(11) -0.0025(9) 0.0000(9) -0.0007(9) O5 0.0106(12) 0.0126(12) 0.0107(11) 0.0020(9) 0.0039(9) 0.0030(9) O6 0.0123(13) 0.0101(11) 0.0148(13) 0.0026(10) 0.0046(10) 0.0033(10) C7 0.0074(15) 0.0065(15) 0.0086(14) -0.0010(12) 0.0006(12) 0.0023(12) C8 0.0126(17) 0.0115(17) 0.0195(17) -0.0005(13) 0.0093(14) -0.0016(14) O7 0.0131(13) 0.0106(12) 0.0102(12) -0.0024(10) -0.0030(10) -0.0006(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Ce Ce -1.8482 9.6596 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 O1 Ce1 Ce1 . 3_666 67.00(6) ? O1 Ce1 O2 . 3_666 136.75(9) ? O1 Ce1 O4 . 4_475 103.58(9) ? O1 Ce1 O5 . . 71.71(9) ? O1 Ce1 O5 . 3_666 72.22(9) ? O1 Ce1 O6 . . 81.02(10) ? O1 Ce1 C7 . . 71.95(10) ? O1 Ce1 O7 . . 70.61(9) ? O2 Ce1 Ce1 3_666 3_666 69.76(6) ? O2 Ce1 O4 3_666 4_475 96.07(9) ? O2 Ce1 O5 3_666 3_666 75.06(9) ? O2 Ce1 O5 3_666 . 73.16(8) ? O2 Ce1 O6 3_666 . 95.20(9) ? O2 Ce1 C7 3_666 . 86.69(9) ? O2 Ce1 O7 3_666 . 152.22(8) ? O3 Ce1 Ce1 1_454 3_666 145.65(6) ? O3 Ce1 O1 1_454 . 139.39(9) ? O3 Ce1 O2 1_454 3_666 80.56(8) ? O3 Ce1 O4 1_454 4_475 82.77(8) ? O3 Ce1 O5 1_454 3_666 146.62(8) ? O3 Ce1 O5 1_454 . 118.98(8) ? O3 Ce1 O6 1_454 . 79.80(9) ? O3 Ce1 C7 1_454 . 101.36(9) ? O3 Ce1 O7 1_454 . 71.86(8) ? O4 Ce1 Ce1 4_475 3_666 116.42(6) ? O4 Ce1 O5 4_475 . 152.47(8) ? O4 Ce1 O5 4_475 3_666 77.58(8) ? O4 Ce1 O6 4_475 . 157.36(8) ? O4 Ce1 C7 4_475 . 175.38(9) ? O4 Ce1 O7 4_475 . 77.54(9) ? O5 Ce1 Ce1 3_666 3_666 38.93(6) ? O5 Ce1 Ce1 . 3_666 36.25(5) ? O5 Ce1 O5 3_666 . 75.18(9) ? O5 Ce1 O6 3_666 . 124.42(8) ? O5 Ce1 C7 . . 25.65(9) ? O5 Ce1 C7 3_666 . 99.64(9) ? O5 Ce1 O7 3_666 . 128.22(8) ? O6 Ce1 Ce1 . 3_666 85.93(6) ? O6 Ce1 O5 . . 50.13(8) ? O6 Ce1 C7 . . 24.85(9) ? C7 Ce1 Ce1 . 3_666 61.08(6) ? O7 Ce1 Ce1 . 3_666 137.38(6) ? O7 Ce1 O5 . . 123.36(8) ? O7 Ce1 O6 . . 83.35(9) ? O7 Ce1 C7 . . 101.68(9) ? C1 S1 C4 . . 91.09(17) ? C2 C1 S1 . . 112.1(3) ? C2 C1 C5 . . 127.4(3) ? C5 C1 S1 . . 120.4(3) ? C1 C2 H2 . . 123.7 ? C1 C2 C3 . . 112.5(3) ? C3 C2 H2 . . 123.7 ? C2 C3 H3 . . 124.0 ? C4 C3 C2 . . 112.0(3) ? C4 C3 H3 . . 124.0 ? C3 C4 S1 . . 112.2(3) ? C3 C4 C6 . . 128.4(3) ? C6 C4 S1 . . 119.4(3) ? O1 C5 C1 . . 116.5(3) ? O1 C5 O2 . . 126.1(3) ? O2 C5 C1 . . 117.4(3) ? C5 O1 Ce1 . . 141.1(2) ? C5 O2 Ce1 . 3_666 135.8(2) ? O3 C6 C4 . . 117.5(3) ? O3 C6 O4 . . 124.2(3) ? O4 C6 C4 . . 118.3(3) ? C6 O3 Ce1 . 1_656 148.4(2) ? C6 O4 Ce1 . 4_676 133.3(2) ? Ce1 O5 Ce1 3_666 . 104.82(9) ? C7 O5 Ce1 . 3_666 155.3(2) ? C7 O5 Ce1 . . 92.3(2) ? C7 O6 Ce1 . . 96.4(2) ? O5 C7 Ce1 . . 62.02(18) ? O5 C7 C8 . . 118.5(3) ? O6 C7 Ce1 . . 58.74(19) ? O6 C7 O5 . . 119.4(3) ? O6 C7 C8 . . 122.1(3) ? C8 C7 Ce1 . . 166.9(2) ? C7 C8 H8A . . 109.5 ? C7 C8 H8B . . 109.5 ? C7 C8 H8C . . 109.5 ? H8A C8 H8B . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? Ce1 O7 H7A . . 114(3) ? Ce1 O7 H7B . . 129(3) ? H7A O7 H7B . . 111(4) ? 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 Ce1 Ce1 3_666 4.0320(3) ? Ce1 O1 . 2.422(3) y Ce1 O2 3_666 2.428(3) y Ce1 O3 1_454 2.406(2) y Ce1 O4 4_475 2.443(2) y Ce1 O5 . 2.621(2) y Ce1 O5 3_666 2.466(2) y Ce1 O6 . 2.551(3) y Ce1 C7 . 2.965(4) ? Ce1 O7 . 2.503(3) y S1 C1 . 1.719(3) ? S1 C4 . 1.722(4) ? C1 C2 . 1.375(5) ? C1 C5 . 1.488(5) ? C2 H2 . 0.9500 ? C2 C3 . 1.411(5) ? C3 H3 . 0.9500 ? C3 C4 . 1.377(5) ? C4 C6 . 1.479(4) ? C5 O1 . 1.257(5) ? C5 O2 . 1.263(4) ? C6 O3 . 1.258(4) ? C6 O4 . 1.277(4) ? O5 C7 . 1.285(4) ? O6 C7 . 1.254(4) ? C7 C8 . 1.491(5) ? C8 H8A . 0.9800 ? C8 H8B . 0.9800 ? C8 H8C . 0.9800 ? O7 H7A . 0.861(19) ? O7 H7B . 0.854(19) ? 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 C8 H8B O3 3_766 0.98 2.65 3.497(5) 144.7 O7 H7A O4 1_454 0.861(19) 2.02(2) 2.829(4) 156(4) O7 H7B O6 4_576 0.854(19) 1.95(2) 2.795(4) 168(5)