#------------------------------------------------------------------------------ #$Date: 2024-07-02 05:18:23 +0300 (Tue, 02 Jul 2024) $ #$Revision: 292684 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572026.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_1572026 loop_ _publ_author_name 'Weare, Benjamin L.' 'Hoggett, Sean' 'Cull, William J.' 'Argent, Stephen P.' 'Khlobystov, Andrei N.' 'Brown, Paul D.' _publ_section_title ; Benzene-1,2,4,5-tetrol ; _journal_coeditor_code BX4030 _journal_issue 6 _journal_name_full IUCrData _journal_paper_doi 10.1107/S2414314624006126 _journal_volume 9 _journal_year 2024 _chemical_formula_iupac 'C6 H6 O4' _chemical_formula_moiety 'C6 H6 O4' _chemical_formula_sum 'C6 H6 O4' _chemical_formula_weight 142.11 _chemical_name_common ; 1,2,4,5-Tetrahydroxybenzene ; _chemical_name_systematic ; Benzene-1,2,4,5-tetrol ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _cell_angle_alpha 68.407(5) _cell_angle_beta 85.779(4) _cell_angle_gamma 89.843(4) _cell_formula_units_Z 4 _cell_length_a 3.7474(2) _cell_length_b 11.6254(6) _cell_length_c 13.7771(8) _cell_measurement_reflns_used 4683 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 75.5450 _cell_measurement_theta_min 3.4310 _cell_volume 556.37(6) _computing_cell_refinement ; CrysAlisPro 1.171.43.63a (Rigaku OD, 2023) ; _computing_data_collection ; CrysAlisPro system (CCD 42.102a 64-bit; release 15-09-2023)(Rigaku OD, 2023) ; _computing_data_reduction ; CrysAlisPro 1.171.43.63a (Rigaku OD, 2023) ; _computing_molecular_graphics ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018/2 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 120(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 5.8140 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.934 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'XtalLAB PRO MM007, PILATUS3 R 200K' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _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 0.0631 _diffrn_reflns_av_unetI/netI 0.0480 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 8096 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.156 _diffrn_reflns_theta_min 3.461 _diffrn_source 'rotating anode' _exptl_absorpt_coefficient_mu 1.265 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.927 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2023) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.697 _exptl_crystal_description block _exptl_crystal_F_000 296 _exptl_crystal_size_max 0.067 _exptl_crystal_size_mid 0.048 _exptl_crystal_size_min 0.016 _refine_diff_density_max 0.277 _refine_diff_density_min -0.335 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 205 _refine_ls_number_reflns 2185 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 1.086 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0445 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+0.1541P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1263 _refine_ls_wR_factor_ref 0.1327 _reflns_number_gt 1842 _reflns_number_total 2185 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file bx4030.cif _cod_data_source_block I _cod_database_code 1572026 _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 0.917 _shelx_estimated_absorpt_t_max 0.975 _shelx_hkl_file ; 0 0 1 25.62 1.58 0 0 -1 22.70 2.03 0 0 -1 21.25 1.57 0 0 1 19.33 1.94 0 0 -2 41.52 3.34 0 0 -2 48.17 4.10 0 0 2 47.74 3.16 0 0 2 45.43 3.23 0 0 -3 24.73 3.68 0 0 -3 20.86 2.29 0 0 -4 614.33 36.87 0 0 -4 680.65 38.29 0 0 -4 582.30 36.81 0 0 4 582.50 37.99 0 0 -4 626.31 37.12 0 0 5 164.28 11.35 0 0 -5 173.79 11.80 0 0 -5 168.71 11.32 0 0 5 201.67 11.80 0 0 -5 181.03 11.42 0 0 -5 179.58 13.18 0 0 6 11.90 1.65 0 0 6 13.93 2.49 0 0 -6 18.41 4.39 0 0 -6 10.89 1.70 0 0 -6 11.20 1.56 0 0 -6 9.65 2.72 0 0 -7 1.69 2.72 0 0 -7 1.74 1.19 0 0 -7 0.67 2.16 0 0 -7 2.20 3.66 0 0 -7 1.62 1.47 0 0 -7 3.88 4.80 0 0 7 1.74 1.41 0 0 7 0.86 1.79 0 0 -8 465.75 22.33 0 0 -8 305.94 19.95 0 0 -8 310.36 19.59 0 0 -8 211.92 19.92 0 0 -8 398.70 23.23 0 0 8 317.78 19.52 0 0 8 246.66 20.20 0 0 8 320.39 19.33 0 0 -8 263.58 19.16 0 0 8 309.27 21.35 0 0 -8 349.97 20.36 0 0 -9 0.83 1.84 0 0 -9 0.47 1.48 0 0 9 0.10 3.30 0 0 -9 0.57 2.71 0 0 -9 0.64 2.35 0 0 -9 0.83 3.91 0 0 9 0.65 2.11 0 0 -10 321.67 22.52 0 0 10 311.48 23.08 0 0 -10 362.08 23.00 0 0 -10 392.25 23.46 0 0 -10 339.55 22.35 0 0 10 340.46 22.53 0 0 11 8.94 2.59 0 0 -11 8.36 3.35 0 0 -11 8.54 3.34 0 0 -11 8.75 2.80 0 0 -11 10.57 2.21 0 0 -11 10.58 1.87 0 0 12 36.63 19.05 0 0 -12 54.37 5.14 0 0 -12 51.38 5.48 0 0 -12 49.41 5.28 0 0 -12 50.98 4.40 0 0 12 47.97 4.64 0 0 13 8.97 4.21 0 0 -13 11.32 2.19 0 0 -13 7.95 2.68 0 0 -13 10.12 3.17 0 0 13 3.96 5.62 0 0 13 11.90 2.38 0 0 -14 1.83 1.51 0 0 14 1.17 3.08 0 0 -15 -0.39 1.04 0 0 15 1.93 1.94 0 1 -15 4.01 1.33 0 1 -15 3.29 1.45 0 1 -14 2.67 1.40 0 -1 14 4.15 2.31 0 1 -14 0.06 1.84 0 -1 13 5.84 3.33 0 -1 13 3.41 5.73 0 1 -13 6.71 1.87 0 1 -13 9.86 2.87 0 -1 12 154.09 11.18 0 1 -12 169.07 11.94 0 -1 12 166.88 23.67 0 -1 12 135.19 12.28 0 1 -12 172.72 11.79 0 1 -12 165.92 11.19 0 1 -11 1017.23 65.65 0 1 -11 1007.45 65.46 0 -1 11 772.60 73.45 0 1 -11 1022.79 64.77 0 1 -11 1047.42 65.04 0 -1 11 983.18 64.96 0 1 -10 7.39 2.98 0 1 -10 10.38 1.89 0 1 -10 6.27 2.81 0 1 -10 5.28 3.34 0 1 -10 6.26 2.08 0 -1 10 10.31 2.62 0 1 -9 5.58 2.82 0 1 -9 1.60 3.12 0 1 -9 4.08 1.70 0 1 -9 4.89 2.18 0 -1 9 2.04 2.25 0 1 -9 3.83 1.53 0 1 -8 33.78 4.19 0 1 -8 26.55 2.69 0 1 -8 27.45 3.43 0 -1 8 28.29 7.21 0 -1 8 28.63 3.02 0 1 -8 29.37 2.89 0 1 -7 23.05 2.96 0 1 -7 27.83 5.24 0 -1 7 24.26 2.66 0 1 -7 23.94 2.32 0 1 -7 19.84 2.37 0 1 -7 25.02 3.57 0 1 -6 594.43 34.44 0 1 -6 476.70 31.66 0 1 -6 479.82 31.82 0 -1 6 523.13 32.01 0 1 -6 497.40 32.08 0 -1 5 2394.61 142.23 0 1 -5 2124.44 141.99 0 1 -5 2474.83 144.02 0 1 -4 248.02 19.17 0 -1 4 227.83 19.92 0 -1 4 266.74 19.03 0 1 -4 287.65 20.46 0 1 -3 328.48 24.77 0 1 -3 288.64 23.95 0 -1 3 349.43 23.86 0 -1 2 1.80 2.05 0 -1 2 4.00 1.42 0 1 -2 3.47 2.66 0 1 -2 3.37 1.04 0 -1 1 272.72 18.92 0 1 -1 292.83 18.46 0 1 0 8.60 1.38 0 -1 0 13.10 1.39 0 -1 -1 124.24 8.16 0 -1 -1 123.96 8.54 0 1 1 145.10 8.56 0 1 2 3.44 1.82 0 -1 -2 1.70 1.44 0 -1 -3 525.59 33.58 0 -1 -3 452.58 32.88 0 1 3 549.86 32.77 0 1 4 2.64 1.44 0 -1 -4 1.59 1.88 0 -1 -4 5.42 3.25 0 1 4 2.58 1.81 0 -1 -5 700.35 43.24 0 1 5 659.74 41.79 0 1 5 638.31 41.74 0 -1 -5 660.34 42.01 0 -1 -6 668.77 43.25 0 1 6 661.84 42.88 0 1 6 718.58 42.96 0 -1 -6 633.57 42.87 0 -1 -6 741.66 44.82 0 -1 -7 6.00 1.48 0 -1 -7 3.93 1.49 0 1 7 5.46 2.09 0 -1 -7 5.41 2.20 0 1 7 4.82 1.68 0 -1 -7 8.93 3.72 0 -1 -7 4.19 2.38 0 -1 -7 7.00 2.77 0 1 8 96.24 6.41 0 -1 -8 103.04 6.42 0 1 8 92.34 6.77 0 -1 -8 91.00 6.62 0 -1 -8 81.26 7.05 0 -1 -8 82.11 6.21 0 -1 -8 111.38 9.63 0 -1 -8 88.60 7.31 0 1 8 85.24 6.58 0 -1 -9 1.31 3.72 0 1 9 2.05 4.08 0 1 9 2.01 1.49 0 -1 -9 1.86 1.75 0 -1 -9 2.49 2.87 0 -1 -9 4.43 2.26 0 1 9 2.19 1.98 0 -1 -10 30.97 3.69 0 1 10 32.52 2.98 0 -1 -10 35.54 4.74 0 1 10 31.48 3.40 0 -1 -10 28.96 5.94 0 -1 -10 27.68 3.21 0 1 10 28.85 4.74 0 -1 -10 33.34 4.40 0 -1 -11 45.55 4.97 0 1 11 49.65 4.68 0 1 11 45.90 5.72 0 -1 -11 54.37 4.60 0 -1 -11 64.62 5.80 0 -1 -11 53.23 4.29 0 1 12 1190.79 78.58 0 -1 -12 1238.69 78.34 0 1 12 1097.56 86.31 0 -1 -12 1331.45 79.37 0 -1 -12 1211.73 79.07 0 -1 -12 1220.83 78.62 0 1 12 1202.82 79.13 0 1 13 74.39 17.53 0 -1 -13 69.36 5.29 0 -1 -13 64.82 6.06 0 1 13 61.89 5.48 0 -1 -13 69.59 6.18 0 -1 -13 67.90 5.85 0 1 14 43.42 5.50 0 -1 -14 49.02 4.49 0 -1 -14 49.92 4.62 0 -1 -14 43.37 3.84 0 -1 -15 1.15 1.16 0 1 15 2.42 2.57 0 1 16 4.00 1.50 0 2 -15 -1.32 1.70 0 2 -14 12.44 1.57 0 2 -14 10.94 1.87 0 -2 13 2.02 2.33 0 2 -13 4.46 2.18 0 2 -13 3.05 1.61 0 -2 13 2.13 5.40 0 2 -12 8.51 2.97 0 -2 12 1.06 15.93 0 -2 12 9.81 7.70 0 2 -12 10.87 2.16 0 -2 12 10.76 3.48 0 2 -11 108.01 8.42 0 -2 11 87.32 22.12 0 -2 11 102.55 7.69 0 -2 11 84.17 8.73 0 2 -11 116.14 7.81 0 2 -10 243.31 16.46 0 -2 10 227.44 16.36 0 2 -10 249.19 16.37 0 2 -10 234.11 17.13 0 2 -10 260.46 16.28 0 2 -10 242.97 16.97 0 2 -9 110.04 7.62 0 -2 9 102.44 7.76 0 2 -9 103.06 7.77 0 2 -9 105.89 8.21 0 2 -9 116.72 8.60 0 2 -8 158.90 11.47 0 2 -8 163.43 11.88 0 2 -8 173.49 11.39 0 2 -8 171.14 12.17 0 2 -8 167.98 12.35 0 -2 8 172.77 11.52 0 2 -7 20.52 3.53 0 2 -7 21.03 2.27 0 2 -7 21.40 3.40 0 2 -7 20.64 2.43 0 2 -7 23.48 2.80 0 -2 7 22.77 2.68 0 2 -6 1943.29 120.59 0 -2 6 1904.34 120.02 0 2 -6 1912.81 120.42 0 2 -6 1775.80 120.06 0 2 -6 1923.22 120.04 0 2 -6 1895.29 120.31 0 2 -5 0.64 1.28 0 2 -5 0.35 1.62 0 -2 5 -0.33 1.84 0 2 -5 -1.63 2.25 0 -2 4 0.80 1.89 0 2 -4 -0.65 1.68 0 -2 3 31.87 2.97 0 -2 3 38.78 3.56 0 2 -3 28.02 2.99 0 -2 2 46.58 5.20 0 2 -2 57.83 4.43 0 -2 2 53.01 4.94 0 -2 1 38.73 2.76 0 2 -1 29.54 3.77 0 2 -1 33.17 2.79 0 -2 1 27.33 3.15 0 -2 0 3568.18 229.93 0 2 0 3362.19 229.91 0 -2 0 3698.76 229.40 0 -2 -1 30.42 3.43 0 2 1 35.28 2.30 0 -2 -1 38.84 2.70 0 -2 -2 1039.88 69.30 0 -2 -2 1096.91 68.71 0 2 2 1218.43 69.33 0 -2 -2 1052.37 68.58 0 -2 -3 83.29 5.19 0 2 3 92.79 6.34 0 2 4 270.35 17.22 0 2 4 268.62 15.69 0 2 4 262.52 15.76 0 -2 -4 288.02 17.26 0 -2 -5 10.67 2.52 0 2 5 11.83 1.46 0 2 5 10.78 1.70 0 -2 -5 9.82 3.86 0 -2 -6 28.67 4.57 0 -2 -6 22.39 3.18 0 2 6 26.48 2.46 0 -2 -6 23.35 2.54 0 -2 -7 139.39 9.54 0 2 7 127.88 8.91 0 -2 -7 137.67 11.18 0 2 8 1036.80 63.30 0 2 8 1017.32 63.47 0 -2 -8 1015.61 63.84 0 2 8 974.79 63.32 0 -2 -8 1016.29 63.77 0 -2 -8 1159.15 66.16 0 -2 -8 1018.01 63.25 0 2 9 14.33 2.06 0 -2 -9 11.15 1.71 0 -2 -9 16.07 4.37 0 2 9 9.51 2.47 0 -2 -9 12.42 2.95 0 -2 -9 12.95 2.80 0 -2 -9 12.81 1.93 0 2 9 12.78 2.39 0 -2 -9 13.41 2.24 0 -2 -9 13.24 3.10 0 2 10 433.08 27.86 0 2 10 447.39 27.72 0 -2 -10 499.11 31.72 0 -2 -10 417.49 28.40 0 -2 -10 461.78 27.94 0 -2 -10 498.13 28.75 0 -2 -10 390.31 27.60 0 2 11 151.62 10.35 0 -2 -11 136.11 10.85 0 -2 -11 152.66 10.37 0 -2 -11 147.89 11.28 0 2 11 150.10 10.12 0 2 11 115.96 11.44 0 -2 -11 164.03 13.99 0 -2 -12 0.97 1.53 0 -2 -12 0.65 3.01 0 -2 -12 0.97 2.71 0 -2 -12 0.07 1.95 0 2 12 2.77 3.81 0 2 12 2.10 15.57 0 2 12 2.60 1.79 0 2 12 0.88 2.21 0 2 13 3.96 3.24 0 2 13 11.82 15.70 0 -2 -13 5.06 3.00 0 -2 -13 3.92 2.06 0 -2 -13 3.72 2.72 0 2 13 3.37 2.29 0 -2 -14 1.69 2.26 0 2 14 -0.97 3.84 0 -2 -14 -0.35 2.59 0 2 14 3.95 2.06 0 -2 -14 3.52 1.71 0 2 14 1.65 2.25 0 2 15 16.68 3.37 0 -2 -15 15.85 2.59 0 -2 -15 17.56 1.99 0 2 16 -1.71 1.86 0 -2 -16 -0.02 0.91 0 3 -14 1.14 1.39 0 3 -13 22.97 2.38 0 3 -13 23.55 2.84 0 -3 13 21.81 5.68 0 3 -12 2.49 1.80 0 3 -12 3.55 2.36 0 -3 12 -0.82 7.21 0 3 -11 76.17 6.84 0 -3 11 90.93 20.83 0 -3 11 87.49 6.97 0 3 -11 76.79 6.13 0 3 -10 218.45 13.70 0 -3 10 190.48 27.89 0 3 -10 228.31 14.46 0 3 -10 224.02 13.64 0 -3 10 190.07 14.39 0 3 -9 696.93 46.30 0 3 -9 727.38 45.73 0 3 -9 723.53 45.74 0 -3 9 681.24 45.54 0 3 -8 19.11 4.54 0 -3 8 24.42 2.92 0 3 -8 30.91 3.02 0 3 -8 23.67 2.79 0 3 -8 30.49 6.74 0 3 -8 27.45 2.74 0 3 -8 21.36 3.81 0 3 -7 51.73 3.99 0 3 -7 42.03 4.76 0 3 -7 55.63 7.47 0 3 -7 41.07 3.85 0 3 -7 44.19 3.74 0 -3 7 44.73 3.91 0 -3 6 11.68 2.01 0 3 -6 13.33 4.58 0 3 -6 13.75 2.81 0 3 -6 13.93 1.86 0 3 -6 13.15 2.24 0 3 -5 30.36 3.03 0 3 -5 28.31 3.28 0 3 -5 29.23 2.63 0 -3 5 28.58 2.76 0 3 -5 32.50 5.65 0 -3 4 1425.64 93.95 0 -3 4 1598.21 94.40 0 3 -4 1497.61 94.24 0 3 -4 1412.84 94.28 0 3 -4 1695.71 96.54 0 3 -3 983.03 55.29 0 -3 3 790.08 53.10 0 3 -3 814.15 53.41 0 -3 3 955.02 53.58 0 -3 2 688.80 40.50 0 -3 2 609.16 40.27 0 3 -2 692.73 42.05 0 3 -2 626.26 40.52 0 3 -2 630.70 40.59 0 -3 1 656.95 35.52 0 3 -1 703.50 36.87 0 3 0 6.47 1.48 0 -3 0 4.35 2.47 0 -3 0 5.07 1.80 0 3 0 8.17 3.06 0 -3 -1 10.30 2.47 0 -3 -1 9.72 1.84 0 3 1 10.02 1.81 0 -3 -2 1.10 1.54 0 3 2 1.62 1.99 0 3 2 -0.16 0.68 0 -3 -2 0.07 2.19 0 -3 -3 14.24 2.42 0 3 3 14.81 2.80 0 -3 -3 9.49 3.27 0 -3 -4 48.80 3.96 0 3 4 52.60 5.11 0 -3 -4 38.41 3.95 0 -3 -5 218.15 16.20 0 -3 -5 263.33 17.50 0 3 5 254.84 15.88 0 -3 -6 830.67 53.70 0 -3 -6 801.87 53.36 0 -3 -6 937.81 55.25 0 3 6 853.58 53.36 0 -3 -7 1369.86 86.55 0 -3 -7 1321.56 86.22 0 3 7 1374.26 86.19 0 -3 -7 1556.90 88.45 0 -3 -7 1291.57 86.51 0 -3 -8 91.83 6.93 0 3 8 86.02 6.55 0 3 8 87.26 6.25 0 -3 -8 90.97 8.58 0 -3 -8 87.58 6.37 0 -3 -9 107.72 9.83 0 3 9 108.63 7.30 0 -3 -9 101.17 7.74 0 -3 -9 90.15 6.83 0 3 9 93.36 6.95 0 -3 -9 100.94 7.62 0 -3 -10 -0.72 2.61 0 -3 -10 -1.84 2.37 0 -3 -10 0.24 1.42 0 3 10 0.05 1.72 0 -3 -10 2.63 3.63 0 -3 -10 -2.46 2.80 0 3 10 0.06 2.23 0 3 11 299.89 25.30 0 -3 -11 342.38 23.83 0 -3 -11 311.63 24.57 0 -3 -11 449.11 25.20 0 -3 -11 421.68 28.08 0 -3 -11 399.01 24.25 0 3 11 387.56 24.04 0 -3 -12 33.49 4.40 0 3 12 32.73 3.17 0 3 12 21.09 5.26 0 -3 -12 31.31 3.39 0 -3 -12 26.58 4.08 0 -3 -13 481.61 28.84 0 -3 -13 437.67 28.08 0 3 13 404.53 27.95 0 3 13 445.71 27.88 0 -3 -13 357.48 28.35 0 3 13 440.50 29.04 0 -3 -13 428.83 27.79 0 3 13 491.20 35.90 0 -3 -14 8.53 2.91 0 3 14 7.26 2.23 0 -3 -14 10.71 2.02 0 3 14 9.53 3.07 0 3 15 9.14 2.13 0 -3 -15 8.10 1.67 0 3 15 4.11 3.17 0 3 16 7.35 2.38 0 -3 -16 3.03 0.99 0 3 17 1.71 1.95 0 -4 13 -2.18 4.03 0 4 -13 0.62 1.58 0 4 -12 1.03 1.51 0 4 -12 -1.06 2.03 0 -4 12 4.22 6.01 0 4 -11 18.58 3.13 0 4 -11 18.06 2.52 0 -4 11 13.83 3.15 0 -4 11 17.33 8.66 0 4 -10 294.26 19.90 0 -4 10 327.78 31.67 0 4 -10 299.74 20.29 0 4 -9 193.65 13.36 0 4 -9 185.18 12.87 0 4 -9 182.08 12.90 0 -4 9 206.35 27.13 0 -4 8 541.74 47.08 0 4 -8 544.12 36.30 0 4 -8 577.30 36.90 0 4 -8 530.41 36.99 0 4 -8 579.49 36.44 0 4 -7 64.03 5.27 0 4 -7 66.17 6.40 0 4 -7 77.14 8.97 0 4 -7 57.02 5.86 0 4 -6 40.04 4.46 0 4 -6 49.48 7.19 0 4 -6 44.75 3.91 0 4 -6 44.09 4.99 0 4 -5 22.69 3.66 0 -4 5 21.19 2.23 0 4 -5 25.03 5.42 0 4 -5 21.22 3.22 0 4 -5 22.17 2.55 0 -4 4 1315.71 88.75 0 4 -4 1388.57 89.29 0 4 -4 1517.63 89.16 0 4 -4 1463.68 89.50 0 4 -4 1545.44 91.88 0 -4 3 48.88 4.38 0 4 -3 44.86 3.77 0 4 -3 49.63 3.82 0 4 -3 45.20 4.07 0 -4 3 42.83 3.26 0 4 -3 51.65 6.29 0 4 -2 9.74 3.62 0 -4 2 5.23 2.44 0 4 -1 91.16 7.95 0 -4 1 91.23 6.51 0 4 0 1881.60 119.68 0 -4 -1 127.10 9.31 0 -4 -1 111.21 8.21 0 4 1 132.33 8.22 0 -4 -2 1989.09 119.46 0 -4 -2 1810.50 118.29 0 4 2 1889.46 118.47 0 4 3 199.92 12.57 0 -4 -3 194.76 12.88 0 -4 -3 216.34 13.24 0 -4 -4 37.74 3.58 0 4 4 36.62 2.71 0 4 4 37.21 2.93 0 -4 -4 31.48 4.78 0 -4 -4 35.29 3.49 0 4 5 0.09 1.36 0 -4 -5 -0.09 2.11 0 -4 -6 507.79 33.43 0 4 6 518.09 33.03 0 4 6 507.39 32.92 0 -4 -6 556.33 34.95 0 -4 -7 13.26 3.87 0 -4 -7 11.31 1.91 0 -4 -7 10.05 2.46 0 4 7 12.94 1.93 0 4 7 10.80 1.80 0 -4 -7 11.75 2.78 0 4 8 1240.59 85.51 0 -4 -8 1369.88 85.49 0 -4 -8 1419.27 85.94 0 4 8 1389.86 85.44 0 4 8 1322.27 85.36 0 -4 -8 1319.52 85.85 0 4 9 16.75 2.35 0 -4 -9 15.09 2.38 0 4 9 15.71 2.16 0 -4 -9 16.75 2.99 0 -4 -9 20.00 3.44 0 -4 -9 24.19 4.75 0 4 9 19.58 2.85 0 -4 -10 362.05 25.39 0 4 10 381.13 25.53 0 4 10 389.30 25.53 0 -4 -10 372.00 26.08 0 4 10 452.67 25.84 0 -4 -10 409.77 26.27 0 -4 -10 422.21 28.67 0 -4 -11 130.54 9.39 0 -4 -11 130.50 11.83 0 4 11 115.61 8.85 0 4 11 118.61 8.66 0 -4 -11 128.30 8.46 0 4 11 118.85 8.61 0 -4 -11 133.55 9.67 0 4 12 128.23 17.50 0 -4 -12 146.59 10.07 0 4 12 113.58 11.52 0 4 12 142.38 10.00 0 -4 -12 159.16 11.00 0 4 12 139.31 9.92 0 -4 -13 7.29 2.23 0 4 13 11.76 11.28 0 4 13 5.85 2.27 0 4 13 8.21 2.04 0 4 13 8.83 4.34 0 -4 -13 10.26 3.33 0 4 14 66.27 6.36 0 4 14 61.89 4.99 0 4 14 67.84 5.29 0 -4 -14 67.96 5.84 0 -4 -14 61.57 5.09 0 -4 -15 15.51 2.13 0 4 15 19.27 2.96 0 -4 -16 0.52 0.92 0 4 16 0.04 1.46 0 -5 12 9.73 4.93 0 5 -12 8.33 2.16 0 5 -11 8.70 2.46 0 -5 11 5.64 7.49 0 -5 11 5.17 2.44 0 5 -11 5.29 1.88 0 -5 10 11.79 3.49 0 5 -10 13.75 3.05 0 5 -10 14.22 2.52 0 5 -9 1.94 2.55 0 5 -9 1.92 2.10 0 5 -9 -0.14 2.09 0 -5 8 198.14 24.60 0 5 -8 156.01 11.76 0 5 -8 181.23 12.25 0 5 -7 159.68 10.87 0 -5 7 135.60 10.60 0 -5 7 154.70 24.22 0 5 -7 148.30 11.33 0 5 -7 147.78 10.52 0 5 -6 128.88 9.70 0 5 -6 126.54 12.45 0 5 -6 119.37 8.85 0 -5 6 120.97 21.02 0 5 -6 116.66 8.96 0 5 -5 124.31 11.68 0 5 -5 118.28 9.31 0 5 -5 115.84 8.56 0 5 -5 120.88 8.62 0 5 -4 350.29 23.44 0 5 -4 350.65 23.00 0 5 -4 344.96 23.00 0 5 -4 348.84 25.81 0 -5 4 353.83 26.27 0 5 -3 651.03 39.87 0 5 -3 652.46 40.22 0 5 -3 590.18 39.68 0 5 -3 623.09 39.86 0 5 -3 672.06 42.49 0 5 -2 1423.42 89.19 0 5 -2 1482.50 91.44 0 5 -2 1327.80 89.05 0 5 -2 1460.33 89.50 0 5 -1 129.99 8.89 0 5 -1 127.88 8.75 0 -5 0 1.05 2.19 0 -5 0 -2.42 6.12 0 5 0 0.58 1.87 0 5 1 1129.95 67.40 0 -5 -1 986.71 67.30 0 -5 -2 1683.39 106.43 0 5 2 1655.12 106.62 0 5 3 2940.27 192.68 0 -5 -3 3097.11 192.31 0 -5 -3 2762.38 192.58 0 5 3 3110.58 192.11 0 5 4 1504.41 92.12 0 -5 -4 1613.44 92.59 0 5 4 1395.10 91.93 0 5 5 1115.46 68.10 0 5 5 1013.67 67.60 0 -5 -5 1120.06 68.18 0 5 5 1068.92 67.78 0 -5 -5 1118.76 68.22 0 5 6 128.38 8.42 0 5 6 121.16 8.27 0 5 6 119.94 8.88 0 -5 -6 128.48 9.09 0 -5 -7 295.79 20.03 0 -5 -7 356.57 22.22 0 -5 -7 253.16 19.84 0 5 7 322.50 19.41 0 -5 -7 291.45 19.54 0 5 8 33.19 3.02 0 -5 -8 34.51 3.28 0 5 8 37.98 3.12 0 -5 -8 33.77 3.86 0 -5 -8 39.20 4.28 0 -5 -8 36.99 5.68 0 5 8 32.39 3.57 0 -5 -9 14.03 4.26 0 -5 -9 18.63 3.07 0 5 9 14.37 2.76 0 -5 -9 17.03 3.41 0 5 9 15.66 2.27 0 -5 -9 15.32 2.30 0 5 9 16.43 2.19 0 -5 -10 3.87 3.51 0 -5 -10 3.44 1.96 0 5 10 3.49 1.89 0 5 10 4.75 2.02 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388.49 26.90 0 -6 5 31.82 14.56 0 6 -5 21.84 4.34 0 6 -5 22.36 5.75 0 6 -5 19.40 3.37 0 -6 5 21.00 3.58 0 6 -5 22.69 3.10 0 6 -4 99.33 7.53 0 6 -4 97.24 7.50 0 6 -4 83.03 7.11 0 6 -4 110.77 10.75 0 -6 4 104.83 7.89 0 6 -4 114.87 8.29 0 6 -3 190.37 12.39 0 6 -3 150.22 11.43 0 -6 3 179.91 12.09 0 6 -3 169.47 11.71 0 6 -3 166.60 11.73 0 6 -2 247.24 17.17 0 6 -2 260.14 17.41 0 6 -2 219.79 18.09 0 6 -2 280.18 17.95 0 -6 2 294.83 17.72 0 6 -1 257.84 21.49 0 6 -1 353.35 20.95 0 6 -1 292.32 20.87 0 6 -1 352.14 21.39 0 6 0 311.22 19.37 0 6 0 278.64 19.02 0 -6 0 265.37 18.96 0 6 0 317.93 18.99 0 6 0 262.35 18.92 0 6 1 59.88 5.47 0 -6 -1 62.25 6.92 0 6 1 74.64 5.65 0 -6 -1 76.94 5.55 0 -6 -2 187.39 14.81 0 6 2 155.30 13.15 0 6 2 201.31 13.49 0 6 2 217.40 13.31 0 6 2 202.90 13.39 0 -6 -2 202.93 13.12 0 6 3 45.95 3.44 0 6 3 52.36 4.54 0 -6 -3 54.69 4.17 0 6 3 42.31 4.67 0 6 3 49.95 4.63 0 -6 -3 46.82 4.74 0 -6 -3 48.95 5.74 0 6 4 160.24 12.71 0 -6 -4 170.92 12.56 0 6 4 180.13 11.88 0 6 5 55.37 3.71 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131.41 9.41 0 6 15 142.58 10.23 0 6 15 135.85 10.12 0 -6 -15 150.46 10.35 0 6 15 136.56 9.44 0 6 16 8.89 2.13 0 -6 -16 4.85 1.11 0 6 16 5.49 1.97 0 6 16 7.63 1.46 0 6 17 100.91 6.30 0 -6 -17 82.98 6.36 0 7 -11 8.90 2.32 0 -7 11 8.88 5.10 0 -7 10 1.82 2.02 0 7 -10 0.58 1.97 0 -7 10 -3.34 5.41 0 -7 9 16.04 7.92 0 7 -9 7.09 2.84 0 -7 9 11.49 3.28 0 -7 8 60.34 10.61 0 -7 8 59.38 6.10 0 7 -8 50.06 5.09 0 7 -8 56.63 5.48 0 7 -8 56.23 4.66 0 7 -7 144.62 10.24 0 7 -7 146.78 10.79 0 -7 7 125.08 15.79 0 7 -7 136.69 10.56 0 7 -6 0.29 2.58 0 7 -6 -1.71 2.32 0 -7 6 0.82 2.83 0 7 -6 2.62 3.35 0 -7 6 7.06 11.17 0 7 -5 493.91 34.06 0 7 -5 491.55 34.12 0 7 -5 518.92 34.46 0 -7 5 553.28 34.12 0 7 -5 519.13 33.96 0 7 -4 454.19 30.02 0 7 -4 448.14 29.93 0 7 -4 508.47 30.51 0 7 -4 490.25 29.92 0 -7 4 497.75 30.08 0 7 -3 163.71 12.99 0 7 -3 192.61 13.03 0 7 -3 191.03 13.66 0 7 -3 179.58 13.13 0 -7 3 201.75 13.31 0 7 -2 18.17 3.37 0 -7 2 30.66 3.78 0 7 -2 31.91 4.55 0 7 -2 24.08 3.24 0 7 -1 22.41 3.56 0 7 -1 35.45 3.44 0 7 -1 31.02 4.33 0 7 0 25.48 3.45 0 -7 0 24.73 4.59 0 7 0 22.21 3.45 0 7 0 31.99 3.34 0 -7 -1 16.59 3.99 0 7 1 12.49 3.01 0 7 1 23.06 3.45 0 -7 -1 19.80 2.89 0 -7 -2 40.90 4.02 0 7 2 37.59 4.55 0 -7 -2 41.20 4.17 0 7 2 42.43 4.22 0 -7 -2 46.00 5.78 0 -7 -3 5.62 2.88 0 -7 -3 10.11 2.55 0 7 3 7.33 3.10 0 7 3 10.30 2.61 0 -7 -3 8.98 2.37 0 -7 -3 7.80 3.70 0 7 4 1.43 1.14 0 -7 -4 0.63 3.05 0 7 4 3.05 2.61 0 -7 -4 1.63 2.64 0 7 4 1.82 2.92 0 7 5 13.72 4.00 0 7 5 16.10 1.89 0 -7 -5 16.27 4.48 0 7 5 19.58 3.04 0 -7 -5 12.60 2.75 0 -7 -5 18.81 3.32 0 7 6 125.67 8.47 0 7 6 122.97 11.07 0 -7 -6 138.79 9.55 0 -7 -6 113.29 8.97 0 7 7 3.60 3.05 0 7 7 12.20 1.91 0 -7 -7 10.69 2.38 0 7 7 9.88 6.00 0 -7 -7 11.22 3.17 0 -7 -8 39.83 4.63 0 -7 -8 48.39 6.48 0 -7 -8 42.04 3.81 0 7 8 46.11 3.87 0 -7 -8 55.41 5.02 0 7 8 45.97 3.47 0 -7 -9 104.49 7.71 0 -7 -9 129.69 8.81 0 7 9 100.48 7.97 0 -7 -9 92.14 8.18 0 7 9 105.33 7.63 0 -7 -9 124.69 11.06 0 7 9 110.37 7.40 0 -7 -10 43.30 4.87 0 7 10 34.12 3.15 0 7 10 32.50 3.86 0 -7 -10 35.54 4.34 0 -7 -10 35.20 3.53 0 -7 -11 291.03 18.61 0 7 11 273.07 17.47 0 7 11 266.54 17.65 0 -7 -11 263.67 17.75 0 -7 -11 273.37 18.39 0 -7 -12 220.63 15.46 0 7 12 202.06 14.79 0 7 12 226.02 14.68 0 -7 -12 235.64 15.80 0 -7 -13 2.89 2.49 0 7 13 0.66 4.30 0 -7 -13 0.61 3.00 0 7 13 4.01 1.93 0 7 13 1.65 1.79 0 -7 -14 27.26 2.93 0 7 14 25.51 2.83 0 7 14 24.71 4.48 0 7 14 27.92 3.72 0 -7 -14 30.65 3.97 0 7 15 2.32 2.17 0 -7 -15 1.90 1.36 0 7 15 3.75 1.52 0 7 15 3.19 2.79 0 -7 -16 6.75 1.74 0 7 16 7.82 1.47 0 -7 -16 6.10 1.15 0 7 16 8.23 1.70 0 7 16 9.17 2.06 0 7 17 -0.10 1.13 0 -7 -17 -0.58 1.38 0 -8 9 4.61 4.90 0 8 -9 1.57 2.09 0 -8 9 0.40 2.27 0 -8 8 1.52 3.11 0 -8 8 4.62 6.88 0 8 -8 0.16 2.66 0 8 -7 0.27 1.86 0 -8 7 3.77 4.05 0 -8 7 4.89 8.66 0 8 -7 0.09 2.66 0 8 -7 1.21 3.05 0 8 -6 157.06 11.52 0 8 -6 138.74 11.30 0 -8 6 151.18 16.24 0 8 -6 160.69 11.10 0 -8 5 -0.60 2.93 0 8 -5 0.33 2.90 0 8 -5 0.54 3.12 0 8 -5 0.46 2.57 0 -8 5 10.48 9.44 0 8 -4 424.66 30.01 0 -8 4 405.90 33.34 0 -8 4 493.49 30.00 0 8 -4 472.33 29.84 0 8 -4 410.97 29.92 0 8 -3 13.18 3.72 0 8 -3 12.83 3.26 0 -8 3 17.06 9.23 0 8 -3 17.32 3.08 0 -8 3 12.83 3.32 0 8 -2 321.25 20.21 0 8 -2 289.19 20.23 0 8 -2 263.67 20.19 0 -8 2 253.74 22.66 0 -8 2 258.93 22.72 0 -8 2 333.69 20.33 0 8 -1 213.11 15.68 0 -8 1 184.77 17.60 0 8 -1 247.71 15.79 0 -8 1 242.58 15.77 0 -8 1 193.14 17.89 0 8 0 3.90 3.16 0 -8 0 0.84 3.41 0 8 0 3.97 3.40 0 8 0 3.47 2.60 0 -8 -1 372.07 22.93 0 8 1 327.73 23.26 0 8 1 298.41 22.89 0 -8 -1 361.72 25.59 0 -8 -1 362.15 23.10 0 -8 -2 6.17 3.63 0 8 2 2.90 3.23 0 -8 -2 3.77 2.88 0 8 2 8.93 3.16 0 -8 -2 5.27 2.65 0 -8 -3 137.71 9.56 0 8 3 107.92 10.24 0 8 3 132.21 10.13 0 8 3 153.64 10.02 0 -8 -3 121.34 10.10 0 -8 -3 134.17 11.83 0 -8 -3 129.28 9.49 0 -8 -4 1.78 3.22 0 8 4 2.01 2.80 0 8 4 4.25 3.23 0 -8 -4 0.28 3.24 0 -8 -5 28.99 3.86 0 8 5 27.98 3.64 0 8 5 20.98 2.12 0 8 5 16.96 4.20 0 -8 -5 22.82 4.61 0 8 6 19.38 2.08 0 8 6 14.26 5.51 0 -8 -6 15.57 3.05 0 8 6 20.35 3.32 0 -8 -6 15.22 3.50 0 8 7 7.84 2.89 0 8 7 5.70 1.59 0 -8 -7 6.17 2.52 0 8 7 9.01 5.91 0 8 8 425.96 25.46 0 -8 -8 333.50 25.28 0 -8 -8 345.01 25.19 0 8 8 391.40 24.56 0 -8 -9 394.48 26.45 0 8 9 373.16 22.67 0 -8 -9 330.42 23.28 0 -8 -9 358.44 22.77 0 8 10 270.31 17.29 0 -8 -10 251.01 17.74 0 -8 -10 262.11 17.08 0 8 10 257.94 17.00 0 -8 -10 264.68 17.92 0 -8 -11 437.31 27.40 0 -8 -11 443.98 28.08 0 -8 -11 466.32 28.22 0 8 12 35.15 5.85 0 -8 -12 60.92 5.54 0 -8 -13 11.45 2.68 0 8 13 12.22 2.15 0 8 13 14.30 2.70 0 8 13 11.55 4.06 0 -8 -13 9.99 3.18 0 -8 -14 2.26 2.67 0 8 14 1.79 1.83 0 8 14 0.10 1.69 0 -8 -14 0.29 1.60 0 -8 -14 1.57 2.23 0 -8 -15 2.51 1.27 0 8 15 1.65 1.46 0 -8 -15 1.95 1.92 0 -8 -16 2.80 0.98 0 -8 -16 2.19 1.38 0 8 16 5.06 1.67 0 9 -8 4.87 2.15 0 -9 8 8.73 2.57 0 -9 7 137.30 10.76 0 9 -7 93.89 7.87 0 9 -6 7.41 3.41 0 -9 6 13.43 7.03 0 9 -6 8.86 3.24 0 9 -6 11.68 2.63 0 -9 5 235.63 18.07 0 -9 5 253.25 15.71 0 9 -5 211.90 15.17 0 9 -5 175.29 14.93 0 9 -5 204.39 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-11 58.64 4.49 -3 -6 -12 1.23 1.57 -3 -6 -13 3.96 1.25 3 7 0 34.00 4.32 3 7 1 39.58 4.42 3 7 2 61.79 6.18 3 7 2 90.32 6.49 3 7 3 213.59 14.38 3 7 3 162.13 14.12 3 7 4 92.44 7.94 3 7 4 107.33 7.73 3 7 5 32.68 4.33 3 7 5 32.97 3.66 3 7 6 14.10 3.69 3 7 6 10.07 2.53 3 7 7 67.30 5.43 -3 -7 -7 56.52 4.62 -3 -7 -7 58.11 4.95 3 7 8 87.23 7.04 -3 -7 -8 75.51 6.32 -3 -7 -8 82.01 6.69 3 7 9 6.83 3.25 -3 -7 -9 9.33 2.34 -3 -7 -9 7.08 2.67 3 7 10 97.69 7.41 -3 -7 -10 93.28 7.05 3 7 11 153.96 10.84 -3 -7 -12 0.65 1.26 3 7 12 -0.14 1.85 -3 -7 -13 2.85 0.98 3 8 1 1.44 2.66 3 8 2 0.96 2.48 3 8 3 170.91 10.66 3 8 3 129.12 10.47 3 8 4 139.73 8.81 3 8 4 96.36 8.28 3 8 5 -0.29 2.95 3 8 6 4.98 3.07 3 8 7 34.42 4.28 3 8 8 3.23 3.05 -3 -8 -8 5.93 2.20 3 8 9 97.27 7.57 -3 -8 -9 97.96 7.17 3 8 10 57.59 5.04 3 8 11 3.11 1.98 3 8 12 1.30 1.87 3 9 -2 -0.30 2.73 3 9 -1 31.11 3.19 3 9 0 3.23 2.05 3 9 1 8.12 2.34 3 9 2 0.77 2.17 3 9 4 197.25 10.17 3 9 4 103.83 9.71 3 9 5 0.23 2.56 3 9 6 72.60 5.98 3 9 7 -1.64 2.61 3 9 8 2.72 2.49 3 9 9 5.32 2.39 3 9 10 6.48 2.08 3 9 11 -0.57 1.98 3 10 1 6.94 2.57 3 10 2 0.39 1.85 3 10 3 21.44 2.49 3 10 5 41.73 3.67 3 10 6 13.45 2.42 3 10 7 179.43 12.14 3 10 8 12.67 2.29 3 10 9 54.54 4.50 3 10 10 -1.76 2.45 -4 7 5 18.43 7.12 4 -7 -5 36.61 3.35 -4 7 3 43.02 8.06 4 -7 -3 70.46 5.29 -4 7 2 90.24 12.76 4 -7 -2 174.22 10.76 4 -7 -1 203.93 13.74 -4 6 6 7.83 5.39 4 -6 -6 21.79 2.39 4 -6 -5 0.45 1.68 -4 6 3 39.44 7.16 4 -6 -3 65.87 4.99 4 -6 -2 18.82 2.74 -4 6 2 19.47 5.21 -4 6 1 66.77 7.58 4 -6 -1 64.65 5.25 -4 6 0 565.27 35.72 4 -6 0 513.46 34.03 -4 6 -1 119.44 10.15 4 -6 1 115.72 8.16 4 -5 -6 13.95 1.58 4 -5 -6 17.66 2.16 -4 5 5 0.97 4.85 4 -5 -5 1.22 1.29 4 -5 -4 21.44 2.90 -4 5 4 13.70 5.34 4 -5 -4 20.76 2.35 -4 5 3 57.38 7.90 -4 5 3 63.04 4.91 4 -5 -3 64.51 4.97 4 -5 -3 69.20 5.50 4 -5 -2 2.65 2.34 -4 5 2 0.33 1.60 4 -5 -2 0.57 1.71 -4 5 1 64.53 5.24 4 -5 -1 70.44 5.39 4 -5 -1 76.49 5.80 -4 5 0 63.34 5.25 4 -5 0 74.46 5.48 4 -5 0 75.81 5.76 4 -5 1 24.23 2.85 4 -5 1 25.23 2.90 -4 5 -2 1.25 3.49 4 -5 2 6.47 1.87 -4 5 -3 2.30 3.28 4 -5 3 5.75 1.66 4 -5 4 57.37 4.60 4 -5 4 44.13 3.28 4 -4 -6 38.56 3.08 4 -4 -6 34.34 3.31 -4 4 5 -3.49 4.88 4 -4 -5 0.13 1.50 -4 4 4 32.96 6.64 -4 4 4 32.88 3.08 4 -4 -4 33.27 3.20 4 -4 -4 35.85 3.60 -4 4 3 114.02 10.23 -4 4 3 87.18 6.86 4 -4 -3 99.97 7.04 4 -4 -3 95.52 7.29 4 -4 -2 70.25 5.60 4 -4 -2 73.63 5.98 -4 4 1 276.78 18.96 4 -4 -1 279.34 19.05 4 -4 -1 306.58 19.30 -4 4 0 208.04 14.69 4 -4 0 219.87 14.83 4 -4 0 230.46 14.97 -4 4 -1 288.74 19.90 4 -4 1 297.87 20.05 4 -4 1 306.94 19.98 -4 4 -1 311.79 20.10 -4 4 -2 381.71 25.50 4 -4 2 401.97 25.71 4 -4 3 411.63 22.86 4 -4 3 345.62 21.80 4 -4 4 93.17 7.22 -4 4 -4 73.70 7.13 4 -4 4 86.58 6.39 4 -4 5 11.39 2.84 -4 4 -5 7.74 2.85 4 -4 5 11.48 2.09 -4 4 -6 1.84 2.21 4 -4 6 1.34 1.26 4 -3 -6 9.92 1.85 4 -3 -5 13.92 2.31 -4 3 5 11.07 1.79 4 -3 -5 12.62 2.04 -4 3 4 98.17 9.52 -4 3 4 84.64 6.64 4 -3 -4 110.39 7.77 4 -3 -4 91.94 6.81 4 -3 -4 92.33 7.03 4 -3 -3 17.53 2.84 -4 3 3 18.15 5.83 -4 3 3 13.33 2.20 4 -3 -3 10.95 3.33 4 -3 -3 15.11 2.47 -4 3 2 109.71 8.55 4 -3 -2 133.87 9.29 4 -3 -2 120.41 8.71 4 -3 -2 123.30 8.89 -4 3 1 58.42 5.16 4 -3 -1 68.19 5.88 4 -3 -1 70.54 5.48 4 -3 -1 63.76 5.53 4 -3 0 26.92 3.65 4 -3 0 23.79 3.23 4 -3 0 26.74 3.28 -4 3 0 24.09 2.98 4 -3 1 -0.06 2.04 -4 3 -1 0.47 1.96 -4 3 -1 1.06 1.80 4 -3 1 -0.40 2.52 4 -3 1 2.46 2.41 -4 3 -2 47.14 4.11 4 -3 2 53.81 4.44 -4 3 -3 11.62 2.30 -4 3 -3 9.91 2.13 -4 3 -3 4.18 2.90 4 -3 3 11.28 2.60 4 -3 4 2.33 3.14 -4 3 -4 2.08 1.78 -4 3 -4 1.43 2.87 4 -3 4 1.49 2.23 4 -3 5 4.86 2.74 -4 3 -5 2.52 2.69 4 -3 5 2.73 2.08 -4 3 -6 31.81 4.01 4 -3 6 40.61 3.54 -4 3 -7 88.28 6.73 4 -3 7 85.35 6.22 -4 2 6 0.48 3.73 4 -2 -6 2.97 1.44 -4 2 5 1.22 4.63 -4 2 5 1.06 1.32 4 -2 -5 1.49 1.53 -4 2 4 72.23 8.17 -4 2 4 74.62 5.66 4 -2 -4 72.39 6.79 4 -2 -4 80.87 5.91 4 -2 -4 78.17 6.06 -4 2 3 163.03 12.35 -4 2 3 126.01 9.35 4 -2 -3 146.35 10.36 4 -2 -3 132.87 9.59 4 -2 -3 133.70 9.69 -4 2 2 41.03 3.86 4 -2 -2 42.89 4.91 4 -2 -2 46.09 4.26 4 -2 -2 47.91 4.35 -4 2 1 35.66 3.68 4 -2 -1 34.99 4.58 4 -2 -1 40.31 4.08 4 -2 -1 39.59 4.00 -4 2 1 41.22 3.76 -4 2 0 34.19 3.58 -4 2 0 35.84 3.57 4 -2 0 32.36 4.39 4 -2 0 37.94 3.98 4 -2 0 33.61 3.62 -4 2 -1 173.73 11.81 -4 2 -1 144.73 11.65 4 -2 1 178.52 12.34 4 -2 1 189.05 12.07 4 -2 1 167.30 11.60 -4 2 -2 5.43 2.11 4 -2 2 8.10 2.93 4 -2 2 7.85 2.74 -4 2 -3 1.55 2.03 4 -2 3 1.35 2.55 4 -2 3 1.77 2.48 -4 2 -4 6.57 2.28 -4 2 -4 9.52 2.19 4 -2 4 4.35 2.59 -4 2 -4 10.63 2.82 4 -2 4 8.37 2.51 -4 2 -5 23.20 2.64 -4 2 -5 30.40 3.52 4 -2 5 29.90 3.19 -4 2 -6 54.34 4.04 4 -2 6 47.93 3.43 -4 2 -7 15.41 2.72 4 -2 7 13.55 2.21 -4 2 -8 24.94 2.86 4 -2 8 18.84 2.59 4 -1 -6 69.87 5.14 4 -1 -5 29.97 2.97 -4 1 4 72.13 8.30 -4 1 4 80.80 5.92 4 -1 -4 74.65 7.12 4 -1 -4 88.87 6.24 -4 1 3 30.10 3.13 4 -1 -3 25.95 4.19 4 -1 -3 36.00 3.53 4 -1 -3 35.30 3.56 4 -1 -2 18.77 2.75 -4 1 2 15.68 2.35 4 -1 -2 11.66 3.47 4 -1 -2 17.01 2.76 -4 1 1 72.86 5.52 4 -1 -1 62.13 6.31 4 -1 -1 75.29 5.77 4 -1 -1 68.12 5.61 -4 1 1 65.49 5.44 4 -1 0 6.64 2.17 -4 1 0 5.19 2.13 -4 1 0 7.85 2.03 4 -1 0 4.15 3.02 4 -1 0 6.69 2.59 4 -1 1 4.27 1.76 -4 1 -1 8.65 2.33 -4 1 -1 5.02 2.21 4 -1 1 5.02 3.28 4 -1 1 5.91 2.64 -4 1 -2 57.42 5.21 -4 1 -2 63.13 5.24 4 -1 2 68.19 5.91 4 -1 2 60.67 5.39 -4 1 -3 12.58 2.46 4 -1 3 15.39 3.31 4 -1 3 15.60 2.98 -4 1 -4 55.76 5.18 -4 1 -4 63.25 5.10 4 -1 4 64.96 5.93 4 -1 4 63.18 5.47 -4 1 -5 9.71 2.33 4 -1 5 8.07 2.93 -4 1 -5 10.37 2.64 4 -1 5 11.17 2.65 -4 1 -6 36.09 3.18 -4 1 -6 43.02 3.75 4 -1 6 36.02 3.49 4 -1 7 1.28 2.08 -4 1 -7 0.63 2.12 4 -1 8 -0.81 1.58 -4 1 -8 39.24 2.73 4 0 -5 16.37 2.14 4 0 -4 35.98 4.77 -4 0 3 9.86 4.57 -4 0 3 7.47 1.64 4 0 -3 6.60 3.52 -4 0 2 78.59 5.80 4 0 -2 71.39 7.07 -4 0 1 31.03 3.08 4 0 -1 25.02 4.20 -4 0 1 26.48 2.91 -4 0 0 47.68 4.21 -4 0 0 48.51 4.26 4 0 0 47.06 5.30 -4 0 -1 18.37 2.75 -4 0 -1 21.45 2.78 4 0 1 20.97 3.93 -4 0 -2 141.78 10.30 -4 0 -2 142.15 10.30 4 0 2 155.05 11.06 -4 0 -3 8.29 2.41 4 0 3 9.77 3.17 4 0 3 5.38 2.50 -4 0 -4 19.67 2.83 4 0 4 19.17 3.82 4 0 4 21.71 3.17 -4 0 -5 33.41 3.51 4 0 5 32.07 3.52 -4 0 -6 60.85 4.94 4 0 6 51.08 4.77 -4 0 -7 20.89 2.72 4 0 7 11.29 2.40 -4 0 -8 1.06 1.89 4 0 8 0.41 1.60 4 0 9 1.17 2.29 4 0 9 79.76 3.45 4 1 -4 42.51 5.37 4 1 -4 52.09 4.09 4 1 -3 84.21 8.28 4 1 -3 103.33 7.27 -4 -1 3 104.01 7.29 -4 -1 2 53.14 4.22 4 1 -2 49.32 5.59 4 1 -2 55.28 4.58 -4 -1 1 47.62 3.94 4 1 -1 42.10 5.23 4 1 -1 45.28 4.21 -4 -1 0 5.48 1.82 -4 -1 0 6.99 1.96 4 1 0 6.14 3.29 4 1 0 8.02 2.28 -4 -1 -1 6.30 1.97 -4 -1 -1 7.09 2.02 4 1 1 5.42 3.42 4 1 1 5.23 2.23 -4 -1 -2 50.52 4.72 -4 -1 -2 55.39 4.74 4 1 2 64.83 5.89 4 1 2 60.59 4.99 -4 -1 -3 89.35 7.12 4 1 3 102.07 7.93 4 1 3 94.53 7.25 -4 -1 -4 16.50 2.75 4 1 4 11.83 3.38 4 1 4 16.36 2.70 -4 -1 -5 27.46 3.28 4 1 5 34.16 4.35 4 1 5 26.44 3.29 -4 -1 -6 107.03 8.18 4 1 6 115.21 8.15 -4 -1 -7 88.90 6.37 4 1 7 77.14 6.25 -4 -1 -8 49.87 3.99 4 1 8 40.79 3.77 -4 -1 -9 12.28 1.82 4 1 9 3.54 2.19 4 2 -4 38.75 3.17 4 2 -3 10.98 3.65 4 2 -3 11.78 1.92 4 2 -2 8.18 3.47 4 2 -2 8.55 1.99 4 2 -1 8.43 3.38 4 2 -1 10.99 2.13 -4 -2 0 16.23 2.23 4 2 0 18.97 3.86 4 2 0 17.17 2.60 -4 -2 -1 23.14 2.79 4 2 1 23.25 4.01 4 2 1 26.40 3.01 -4 -2 -2 29.74 3.08 -4 -2 -2 26.96 3.12 4 2 2 27.21 4.18 4 2 2 31.84 3.39 -4 -2 -3 21.01 2.80 4 2 3 30.01 3.98 4 2 3 22.17 3.00 -4 -2 -4 147.23 11.15 4 2 4 179.17 11.94 4 2 4 160.84 11.15 -4 -2 -5 2.60 2.00 4 2 5 3.07 2.95 4 2 5 3.26 2.05 -4 -2 -6 0.89 1.93 4 2 6 0.22 1.86 4 2 7 192.69 13.02 -4 -2 -8 68.90 4.98 4 2 8 60.15 4.79 -4 -2 -9 223.11 11.35 4 2 9 132.60 11.04 4 3 -3 0.52 2.82 4 3 -2 120.58 12.00 4 3 -2 192.66 11.37 4 3 -1 -1.46 3.19 4 3 -1 -1.11 1.56 4 3 0 34.83 3.20 -4 -3 -1 1.79 1.53 4 3 1 1.98 1.80 -4 -3 -2 0.59 1.59 4 3 2 -0.45 1.70 -4 -3 -3 115.09 8.77 4 3 3 135.98 8.84 -4 -3 -4 7.26 2.00 4 3 4 5.26 1.97 -4 -3 -5 7.79 2.08 4 3 5 8.30 1.89 4 3 6 -0.17 1.62 4 3 7 20.18 2.20 4 3 8 -0.43 0.79 4 4 -2 135.37 9.97 4 4 -1 5.60 2.87 4 4 0 2.22 2.75 4 4 1 8.28 2.88 4 4 2 67.21 5.96 -4 -4 -3 41.07 3.72 4 4 3 56.49 4.88 4 4 4 2.78 2.55 4 4 5 8.50 2.74 4 4 6 3.05 2.22 4 4 7 0.07 2.14 4 4 8 27.29 3.07 4 4 9 -1.10 2.09 4 5 0 14.30 2.91 4 5 1 9.39 2.77 4 5 2 276.82 18.71 4 5 3 -0.36 2.30 4 5 4 110.20 8.24 4 5 5 7.39 2.32 4 5 6 2.63 1.99 4 5 7 0.11 1.74 4 5 8 35.15 3.54 4 6 2 32.98 3.21 4 6 3 17.45 2.50 4 6 4 47.16 4.05 4 6 5 -0.72 1.77 4 6 6 1.44 1.90 0 0 0 0.00 0.00 TITL BWPBCA in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 3.747434 11.625393 13.777123 68.4074 85.7794 89.8430 ZERR 3.00 0.000190 0.000610 0.000810 0.0052 0.0044 0.0042 LATT 1 SFAC C H O UNIT 18.00 18.00 12.00 REM CrysAlisPro recorded range (K): Min=119.9; max=120.0; aver:120.0 TEMP -153 SIZE 0.02 0.05 0.07 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 45301 _shelx_res_file ; TITL bwpbca_a.res in P-1 bwpbca.res created by SHELXL-2018/3 at 11:27:29 on 15-Dec-2023 REM Old TITL BWPBCA in P-1 REM SHELXT solution in P-1: R1 0.125, Rweak 0.004, Alpha 0.022 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C12 O8 CELL 1.54184 3.7474 11.6254 13.7771 68.407 85.779 89.843 ZERR 4 0.0002 0.0006 0.0008 0.005 0.004 0.004 LATT 1 SFAC C H O UNIT 24 24 16 DFIX 0.84 O4A H4A O5A H5A O5B H5B O4B H4B O4D H4D O4C H4C O5C H5C O5D H5D L.S. 8 PLAN 5 SIZE 0.02 0.05 0.07 TEMP -153 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 ACTA OMIT -3 6 11 OMIT 4 3 8 OMIT 4 4 8 OMIT 4 5 8 REM REM REM WGHT 0.079900 0.154100 FVAR 1.00652 C1A 1 -0.146821 1.095677 0.025976 11.00000 0.01210 0.01637 = 0.01926 -0.00519 -0.00462 0.00510 AFIX 43 H1A 2 -0.249116 1.160936 0.043654 11.00000 -1.20000 AFIX 0 C2A 1 -0.056087 0.986951 0.104285 11.00000 0.01059 0.02008 = 0.01560 -0.00386 -0.00362 0.00366 C3A 1 0.087592 0.891141 0.078473 11.00000 0.01258 0.01589 = 0.01531 -0.00034 -0.00486 0.00367 O4A 3 -0.101148 0.968120 0.209102 11.00000 0.02378 0.02167 = 0.01456 -0.00463 -0.00510 0.00961 H4A 2 -0.224328 1.024194 0.220470 11.00000 -1.50000 O5A 3 0.186487 0.783691 0.155237 11.00000 0.02669 0.01854 = 0.01529 0.00122 -0.00234 0.01201 H5A 2 0.054564 0.767432 0.210440 11.00000 -1.50000 C1B 1 0.370182 0.380744 0.021758 11.00000 0.01422 0.01538 = 0.02147 -0.00364 -0.00724 0.00672 AFIX 43 H1B 2 0.280395 0.299234 0.036481 11.00000 -1.20000 AFIX 0 C2B 1 0.385054 0.425020 0.102089 11.00000 0.01276 0.01659 = 0.01618 -0.00088 -0.00553 0.00560 C3B 1 0.513609 0.544649 0.080353 11.00000 0.01365 0.01908 = 0.01829 -0.00645 -0.00961 0.00925 O4B 3 0.272031 0.347463 0.202604 11.00000 0.03018 0.01816 = 0.01710 -0.00223 -0.00100 0.00734 H4B 2 0.192009 0.388178 0.240291 11.00000 -1.50000 O5B 3 0.533712 0.583936 0.162330 11.00000 0.03093 0.01961 = 0.01948 -0.00834 -0.01283 0.01358 H5B 2 0.434269 0.652146 0.151744 11.00000 -1.50000 C1C 1 0.582529 0.126160 0.451452 11.00000 0.01425 0.01623 = 0.01715 -0.00242 -0.00355 0.00630 AFIX 43 H1C 2 0.639580 0.212043 0.418210 11.00000 -1.20000 AFIX 0 C2C 1 0.484713 0.057908 0.392764 11.00000 0.01299 0.01942 = 0.01331 -0.00046 -0.00387 0.00723 C3C 1 0.403763 -0.067641 0.440629 11.00000 0.01194 0.01762 = 0.01713 -0.00413 -0.00405 0.00581 O4C 3 0.471322 0.109544 0.285105 11.00000 0.02637 0.01568 = 0.01381 -0.00134 -0.00685 0.00741 H4C 2 0.420963 0.186779 0.266755 11.00000 -1.50000 O5C 3 0.311210 -0.137538 0.383830 11.00000 0.02101 0.01755 = 0.01540 -0.00317 -0.00797 0.00515 H5C 2 0.226338 -0.093238 0.328602 11.00000 -1.50000 C1D 1 1.090751 0.387868 0.492708 11.00000 0.01226 0.01454 = 0.01833 -0.00260 -0.00356 0.00430 AFIX 43 H1D 2 1.153969 0.310947 0.487689 11.00000 -1.20000 AFIX 0 C2D 1 0.945459 0.478692 0.408860 11.00000 0.01029 0.01798 = 0.01479 -0.00369 -0.00335 0.00258 C3D 1 0.856162 0.591394 0.416828 11.00000 0.01195 0.01438 = 0.01504 -0.00003 -0.00453 0.00413 O4D 3 0.890592 0.450664 0.322857 11.00000 0.02374 0.02105 = 0.01643 -0.00620 -0.00940 0.01072 H4D 2 0.772698 0.509196 0.281219 11.00000 -1.50000 O5D 3 0.719806 0.680818 0.330761 11.00000 0.01940 0.01706 = 0.01482 -0.00153 -0.00749 0.00924 H5D 2 0.610768 0.735796 0.347664 11.00000 -1.50000 HKLF 4 REM bwpbca_a.res in P-1 REM wR2 = 0.1327, GooF = S = 1.087, Restrained GooF = 1.086 for all data REM R1 = 0.0445 for 1842 Fo > 4sig(Fo) and 0.0521 for all 2185 data REM 205 parameters refined using 8 restraints END WGHT 0.0798 0.1539 REM Highest difference peak 0.277, deepest hole -0.335, 1-sigma level 0.076 Q1 1 0.8602 0.5353 0.4176 11.00000 0.05 0.28 Q2 1 0.9502 0.5420 0.4019 11.00000 0.05 0.26 Q3 1 0.3914 0.0730 0.2391 11.00000 0.05 0.26 Q4 1 0.4416 -0.1995 0.3759 11.00000 0.05 0.25 Q5 1 -0.3173 1.0840 0.2211 11.00000 0.05 0.24 ; _shelx_res_checksum 23597 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 C C1A -0.1468(5) 1.09568(17) 0.02598(13) 0.0161(4) Uani d 1 . . H H1A -0.249116 1.160936 0.043654 0.019 Uiso calc 1 . . C C2A -0.0561(4) 0.98695(17) 0.10428(13) 0.0161(4) Uani d 1 . . C C3A 0.0876(5) 0.89114(17) 0.07847(13) 0.0159(4) Uani d 1 . . O O4A -0.1011(3) 0.96812(13) 0.20910(9) 0.0204(3) Uani d 1 . . H H4A -0.224(6) 1.024(2) 0.2205(19) 0.031 Uiso d 1 . . O O5A 0.1865(4) 0.78369(12) 0.15524(10) 0.0223(3) Uani d 1 . . H H5A 0.055(6) 0.767(2) 0.2104(15) 0.033 Uiso d 1 . . C C1B 0.3702(5) 0.38074(17) 0.02176(14) 0.0176(4) Uani d 1 . . H H1B 0.280395 0.299234 0.036481 0.021 Uiso calc 1 . . C C2B 0.3851(5) 0.42502(17) 0.10209(13) 0.0164(4) Uani d 1 . . C C3B 0.5136(5) 0.54465(17) 0.08035(14) 0.0167(4) Uani d 1 . . O O4B 0.2720(4) 0.34746(13) 0.20260(10) 0.0231(3) Uani d 1 . . H H4B 0.192(7) 0.388(2) 0.2403(18) 0.035 Uiso d 1 . . O O5B 0.5337(4) 0.58394(13) 0.16233(10) 0.0225(3) Uani d 1 . . H H5B 0.434(7) 0.6521(18) 0.1517(19) 0.034 Uiso d 1 . . C C1C 0.5825(5) 0.12616(17) 0.45145(13) 0.0168(4) Uani d 1 . . H H1C 0.639580 0.212043 0.418210 0.020 Uiso calc 1 . . C C2C 0.4847(5) 0.05791(17) 0.39276(13) 0.0167(4) Uani d 1 . . C C3C 0.4038(5) -0.06764(17) 0.44063(13) 0.0161(4) Uani d 1 . . O O4C 0.4713(4) 0.10954(12) 0.28510(9) 0.0195(3) Uani d 1 . . H H4C 0.421(6) 0.1868(16) 0.2668(18) 0.029 Uiso d 1 . . O O5C 0.3112(3) -0.13754(12) 0.38383(9) 0.0185(3) Uani d 1 . . H H5C 0.226(6) -0.093(2) 0.3286(14) 0.028 Uiso d 1 . . C C1D 1.0908(4) 0.38787(17) 0.49271(13) 0.0159(4) Uani d 1 . . H H1D 1.153969 0.310947 0.487689 0.019 Uiso calc 1 . . C C2D 0.9455(4) 0.47869(17) 0.40886(13) 0.0149(4) Uani d 1 . . C C3D 0.8562(4) 0.59139(17) 0.41683(13) 0.0151(4) Uani d 1 . . O O4D 0.8906(4) 0.45066(13) 0.32286(9) 0.0202(3) Uani d 1 . . H H4D 0.773(6) 0.509(2) 0.2812(17) 0.030 Uiso d 1 . . O O5D 0.7198(3) 0.68082(12) 0.33076(9) 0.0180(3) Uani d 1 . . H H5D 0.611(6) 0.7358(19) 0.3477(18) 0.027 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 C1A 0.0121(8) 0.0164(9) 0.0193(9) 0.0051(7) -0.0046(7) -0.0052(7) C2A 0.0106(8) 0.0201(10) 0.0156(8) 0.0037(7) -0.0036(6) -0.0039(7) C3A 0.0126(8) 0.0159(9) 0.0153(8) 0.0037(7) -0.0049(6) -0.0003(7) O4A 0.0238(7) 0.0217(7) 0.0146(6) 0.0096(6) -0.0051(5) -0.0046(5) O5A 0.0267(7) 0.0185(7) 0.0153(6) 0.0120(6) -0.0023(5) 0.0012(5) C1B 0.0142(8) 0.0154(9) 0.0215(9) 0.0067(7) -0.0072(7) -0.0036(7) C2B 0.0128(8) 0.0166(9) 0.0162(8) 0.0056(7) -0.0055(7) -0.0009(7) C3B 0.0136(8) 0.0191(9) 0.0183(8) 0.0092(7) -0.0096(7) -0.0065(7) O4B 0.0302(8) 0.0182(7) 0.0171(6) 0.0073(6) -0.0010(5) -0.0022(5) O5B 0.0309(8) 0.0196(7) 0.0195(7) 0.0136(6) -0.0128(6) -0.0083(6) C1C 0.0143(8) 0.0162(9) 0.0172(8) 0.0063(7) -0.0036(7) -0.0024(7) C2C 0.0130(8) 0.0194(10) 0.0133(8) 0.0072(7) -0.0039(6) -0.0005(7) C3C 0.0119(8) 0.0176(9) 0.0171(8) 0.0058(7) -0.0040(6) -0.0041(7) O4C 0.0264(7) 0.0157(7) 0.0138(6) 0.0074(6) -0.0068(5) -0.0013(5) O5C 0.0210(7) 0.0175(7) 0.0154(6) 0.0051(6) -0.0080(5) -0.0032(5) C1D 0.0123(8) 0.0145(9) 0.0183(8) 0.0043(7) -0.0036(7) -0.0026(7) C2D 0.0103(8) 0.0180(9) 0.0148(8) 0.0026(7) -0.0033(6) -0.0037(7) C3D 0.0120(8) 0.0144(9) 0.0150(8) 0.0041(7) -0.0045(6) 0.0000(7) O4D 0.0237(7) 0.0210(7) 0.0164(6) 0.0107(6) -0.0094(5) -0.0062(5) O5D 0.0194(6) 0.0171(7) 0.0148(6) 0.0092(5) -0.0075(5) -0.0015(5) 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 7 4 0.0194 -1 -7 -3 0.0250 2 4 5 0.0217 0 0 -8 0.0010 -2 -4 3 0.0285 0 0 8 0.0150 2 -2 5 0.0355 1 5 -1 0.0145 2 1 0 0.0275 -1 1 5 0.0282 -2 4 1 0.0234 1 -5 -3 0.0344 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 C2A C1A H1A . . 120.1 ? C2A C1A C3A . 2_575 119.82(17) ? C3A C1A H1A 2_575 . 120.1 ? C3A C2A C1A . . 120.03(16) ? O4A C2A C1A . . 123.07(16) ? O4A C2A C3A . . 116.90(15) ? C2A C3A C1A . 2_575 120.14(16) ? O5A C3A C1A . 2_575 119.11(16) ? O5A C3A C2A . . 120.70(15) ? C2A O4A H4A . . 112.3(16) ? C3A O5A H5A . . 111.3(17) ? C2B C1B H1B . . 119.9 ? C2B C1B C3B . 2_665 120.17(18) ? C3B C1B H1B 2_665 . 119.9 ? C1B C2B C3B . . 119.88(17) ? O4B C2B C1B . . 118.40(17) ? O4B C2B C3B . . 121.71(16) ? C2B C3B C1B . 2_665 119.95(17) ? O5B C3B C1B . 2_665 121.84(18) ? O5B C3B C2B . . 118.17(16) ? C2B O4B H4B . . 111.8(18) ? C3B O5B H5B . . 112.5(16) ? C2C C1C H1C . . 120.2 ? C2C C1C C3C . 2_656 119.53(18) ? C3C C1C H1C 2_656 . 120.2 ? C3C C2C C1C . . 120.55(16) ? O4C C2C C1C . . 122.61(17) ? O4C C2C C3C . . 116.82(16) ? C2C C3C C1C . 2_656 119.92(17) ? O5C C3C C1C . 2_656 118.51(17) ? O5C C3C C2C . . 121.57(15) ? C2C O4C H4C . . 109.5(15) ? C3C O5C H5C . . 110.6(17) ? C2D C1D H1D . . 119.7 ? C3D C1D H1D 2_766 . 119.7 ? C3D C1D C2D 2_766 . 120.58(17) ? C1D C2D C3D . . 119.20(16) ? O4D C2D C1D . . 117.50(16) ? O4D C2D C3D . . 123.28(15) ? C1D C3D C2D 2_766 . 120.22(15) ? C1D C3D O5D 2_766 . 122.17(16) ? O5D C3D C2D . . 117.60(15) ? C2D O4D H4D . . 108.3(17) ? C3D O5D H5D . . 111.5(16) ? 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 C1A H1A . 0.9500 ? C1A C2A . 1.388(2) ? C1A C3A 2_575 1.391(2) ? C2A C3A . 1.385(3) ? C2A O4A . 1.376(2) ? C3A O5A . 1.378(2) ? O4A H4A . 0.852(17) ? O5A H5A . 0.835(17) ? C1B H1B . 0.9500 ? C1B C2B . 1.386(2) ? C1B C3B 2_665 1.391(3) ? C2B C3B . 1.390(3) ? C2B O4B . 1.381(2) ? C3B O5B . 1.372(2) ? O4B H4B . 0.861(16) ? O5B H5B . 0.843(17) ? C1C H1C . 0.9500 ? C1C C2C . 1.391(3) ? C1C C3C 2_656 1.394(2) ? C2C C3C . 1.386(3) ? C2C O4C . 1.385(2) ? C3C O5C . 1.379(2) ? O4C H4C . 0.863(17) ? O5C H5C . 0.832(16) ? C1D H1D . 0.9500 ? C1D C2D . 1.392(2) ? C1D C3D 2_766 1.382(2) ? C2D C3D . 1.392(3) ? C2D O4D . 1.368(2) ? C3D O5D . 1.3881(19) ? O4D H4D . 0.858(16) ? O5D H5D . 0.851(16) ? 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 O4A H4A O4C 1_465 0.85(2) 1.89(2) 2.715(2) 163(2) O4B H4B O4D 1_455 0.86(2) 1.88(2) 2.708(2) 163(3) O4B H4B O5B . 0.86(2) 2.45(2) 2.764(2) 102.4(18) O4C H4C O4B . 0.86(2) 1.85(2) 2.702(2) 167(2) O4D H4D O5B . 0.86(2) 1.85(2) 2.6425(19) 154(2) O4D H4D O5D . 0.86(2) 2.34(2) 2.789(2) 113.0(18) O5A H5A O4A . 0.83(2) 2.40(2) 2.711(2) 102.7(18) O5A H5A O5D 1_455 0.83(2) 1.95(2) 2.7562(18) 162(2) O5B H5B O5A . 0.84(2) 1.80(2) 2.633(2) 169(2) O5C H5C O4A 1_545 0.833(19) 2.04(2) 2.8376(16) 161(2) O5C H5C O4C . 0.833(19) 2.38(2) 2.734(2) 106.8(18) O5D H5D O5C 1_565 0.85(2) 2.03(2) 2.8796(19) 175(2) 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 C1A C2A C3A C1A . . . 2_575 1.1(3) ? C1A C2A C3A O5A . . . . 178.53(16) ? C3A C1A C2A C3A 2_575 . . . -1.0(3) ? C3A C1A C2A O4A 2_575 . . . 178.86(16) ? O4A C2A C3A C1A . . . 2_575 -178.86(16) ? O4A C2A C3A O5A . . . . -1.4(3) ? C1B C2B C3B C1B . . . 2_665 -0.5(3) ? C1B C2B C3B O5B . . . . -178.19(14) ? C3B C1B C2B C3B 2_665 . . . 0.5(3) ? C3B C1B C2B O4B 2_665 . . . -179.07(15) ? O4B C2B C3B C1B . . . 2_665 179.06(15) ? O4B C2B C3B O5B . . . . 1.4(2) ? C1C C2C C3C C1C . . . 2_656 0.5(3) ? C1C C2C C3C O5C . . . . -179.04(15) ? C3C C1C C2C C3C 2_656 . . . -0.5(3) ? C3C C1C C2C O4C 2_656 . . . -178.89(15) ? O4C C2C C3C C1C . . . 2_656 178.98(15) ? O4C C2C C3C O5C . . . . -0.6(2) ? C1D C2D C3D C1D . . . 2_766 -0.4(3) ? C1D C2D C3D O5D . . . . 178.51(15) ? C3D C1D C2D C3D 2_766 . . . 0.4(3) ? C3D C1D C2D O4D 2_766 . . . -178.16(16) ? O4D C2D C3D C1D . . . 2_766 178.07(17) ? O4D C2D C3D O5D . . . . -3.0(3) ?