#------------------------------------------------------------------------------ #$Date: 2024-06-01 05:25:10 +0300 (Sat, 01 Jun 2024) $ #$Revision: 292162 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/17/1571764.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_1571764 loop_ _publ_author_name 'Bationo, Valentin' 'Ziki, Eric' 'Sombi\'e, Charles Bavouma' 'Semd\'e, Rasman\'e' 'Djand\'e, Abdoulaye' _publ_section_title ; 2-Oxo-2H-chromen-4-yl 3,3-dimethylbutanoate ; _journal_coeditor_code HB4474 _journal_issue 5 _journal_name_full IUCrData _journal_paper_doi 10.1107/S2414314624004942 _journal_volume 9 _journal_year 2024 _chemical_formula_iupac 'C15 H16 O4' _chemical_formula_moiety 'C15 H16 O4' _chemical_formula_sum 'C15 H16 O4' _chemical_formula_weight 260.28 _chemical_melting_point 430 _chemical_name_systematic ; 2-Oxo-2H-chromen-4-yl 3,3-dimethylbutanoate ; _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.6769(3) _cell_length_b 17.9611(5) _cell_length_c 7.0266(2) _cell_measurement_reflns_used 6044 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 72.4 _cell_measurement_theta_min 4.8 _cell_volume 1347.48(7) _computing_cell_refinement ; CrysAlisPro 1.171.42.102a (Rigaku OD, 2023) ; _computing_data_collection ; CrysAlisPro 1.171.42.102a (Rigaku OD, 2023) ; _computing_data_reduction ; CrysAlisPro 1.171.42.102a (Rigaku OD, 2023) ; _computing_molecular_graphics ; Ortep-3 fro Windows (Farrugia, 2012) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2013 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2015 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2' _diffrn_measurement_method '\w scan' _diffrn_radiation_monochromator Mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_unetI/netI 0.0145 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 9694 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.359 _diffrn_reflns_theta_min 4.818 _diffrn_source 'micro-focus sealed X-ray tube; SuperNova (Cu) X-ray Source' _diffrn_standards_interval_time 25 _diffrn_standards_number 2249 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.82874 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2023) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.283 _exptl_crystal_description Prism _exptl_crystal_F_000 552 _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.160 _refine_diff_density_max 0.109 _refine_diff_density_min -0.129 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.5(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 176 _refine_ls_number_reflns 2249 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0305 _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^)+(0.0490P)^2^+0.0768P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0823 _refine_ls_wR_factor_ref 0.0841 _reflns_number_gt 2133 _reflns_number_total 2249 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb4474.cif _cod_data_source_block I _cod_database_code 1571764 _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 0.792 _shelx_estimated_absorpt_t_max 0.887 _shelx_hkl_file ; 0 -2 0 4029.62 14.51 0 -2 0 3966.02 12.68 0 -3 0 0.49 0.24 0 -3 0 0.23 0.27 0 -3 0 -0.38 0.26 0 -4 0 1.70 0.48 0 -4 0 2.67 0.66 0 -5 0 -0.14 0.36 0 -5 0 0.93 0.52 0 -6 0 3902.28 25.87 0 -6 0 3940.93 22.29 0 -7 0 -0.60 0.54 0 -7 0 -0.52 0.55 0 -8 0 2291.39 23.71 0 -8 0 2274.23 19.89 0 8 0 2320.10 23.86 0 -9 0 -0.31 1.08 0 9 0 -2.90 1.13 0 -10 0 784.38 16.00 0 10 0 816.14 16.58 0 -11 0 1.47 0.99 0 11 0 4.14 1.42 0 -12 0 11.40 1.91 0 12 0 24.62 3.40 0 -13 0 0.25 0.57 0 13 0 1.45 0.63 0 -13 0 0.60 0.47 0 -14 0 35.60 4.67 0 14 0 29.67 4.37 0 -14 0 29.95 2.84 0 -14 0 32.43 2.43 0 15 0 -2.87 2.53 0 -15 0 -0.61 0.63 0 -15 0 -0.28 0.78 0 -16 0 685.18 11.67 0 -16 0 675.11 13.76 0 -17 0 0.71 0.73 0 -18 0 1.40 0.77 0 -19 0 0.54 0.73 0 -20 0 11.93 1.46 0 -21 0 -0.21 0.48 0 -22 0 128.00 3.39 0 0 1 0.18 0.19 0 0 -1 0.43 0.22 0 0 -1 0.33 0.16 0 1 1 350.71 3.54 0 1 -1 350.00 2.97 0 -1 -1 349.18 4.73 0 1 -1 355.12 4.94 0 1 -1 355.26 3.65 0 2 -1 0.10 0.26 0 2 -1 1.92 0.52 0 -2 -1 1.42 0.54 0 2 1 0.21 0.17 0 -2 1 0.79 0.30 0 -3 -1 3363.05 19.99 0 3 -1 3263.57 16.82 0 4 -1 0.22 0.49 0 -4 -1 0.02 0.53 0 -4 1 0.37 0.46 0 -5 -1 1966.36 18.59 0 -5 -1 1996.84 17.50 0 5 -1 1999.74 17.10 0 5 1 1957.07 10.39 0 -5 1 1985.11 10.36 0 -5 1 2015.09 17.16 0 -6 -1 -0.25 0.70 0 6 -1 -0.30 0.65 0 6 1 -0.33 0.14 0 -6 1 0.70 0.26 0 -6 1 -1.00 0.65 0 -7 1 1074.83 14.52 0 7 -1 1054.49 15.02 0 -7 -1 1037.61 15.69 0 -7 -1 1071.39 14.82 0 -7 1 1036.88 14.44 0 8 -1 0.38 0.72 0 -8 -1 -0.09 0.74 0 -8 1 0.89 0.84 0 -8 -1 0.41 0.84 0 -8 1 0.79 0.99 0 -9 -1 306.35 9.02 0 -9 -1 305.17 9.89 0 -9 1 299.03 9.16 0 9 1 308.92 9.60 0 9 -1 311.75 9.66 0 -10 -1 0.92 0.53 0 -10 1 0.90 0.79 0 -10 -1 1.34 1.36 0 10 1 -0.26 1.08 0 10 -1 -0.02 0.95 0 -11 1 139.42 7.18 0 -11 -1 144.64 7.73 0 11 -1 149.84 7.71 0 11 1 153.66 7.89 0 -12 -1 -0.12 0.59 0 12 -1 0.19 1.29 0 12 1 1.93 0.97 0 -12 -1 -0.09 0.45 0 -12 -1 1.13 0.91 0 -13 1 57.53 5.16 0 -13 -1 69.08 6.20 0 13 1 60.71 5.59 0 13 -1 72.17 6.21 0 -13 -1 69.49 4.30 0 -13 -1 71.79 3.51 0 -14 -1 -0.34 0.83 0 14 -1 -0.01 1.55 0 14 1 1.33 1.41 0 -14 -1 0.18 0.52 0 -14 -1 2.00 1.45 0 -15 -1 305.90 13.79 0 -15 1 312.55 13.16 0 -15 -1 328.94 9.98 0 -15 -1 317.74 7.96 0 -15 1 335.64 7.99 0 15 -1 347.09 14.65 0 15 1 332.42 14.34 0 15 -1 341.24 13.83 0 -16 -1 0.39 1.02 0 -16 -1 0.65 0.68 0 -16 1 0.54 0.69 0 -17 1 37.44 2.79 0 -17 -1 33.36 2.71 0 -17 -1 29.75 3.05 0 -18 -1 -0.11 0.63 0 -18 1 -0.21 0.56 0 -19 1 3.12 0.91 0 -19 -1 3.24 0.99 0 -20 1 -0.14 0.52 0 -20 -1 -0.09 0.52 0 -21 1 62.26 2.72 0 -21 -1 62.76 2.80 0 -22 -1 0.10 0.33 0 -22 1 -0.34 0.33 0 -1 2 0.37 0.49 0 1 2 -0.12 0.53 0 1 -2 -0.20 0.43 0 1 -2 0.22 0.36 0 1 -2 1.21 0.74 0 2 -2 6511.03 16.91 0 -2 -2 6622.18 30.01 0 2 -2 6483.03 30.85 0 2 -2 6537.84 22.29 0 2 2 6441.55 21.50 0 -2 2 6465.57 30.13 0 -2 -2 6559.88 31.92 0 -3 -2 0.38 0.53 0 3 -2 -0.06 0.43 0 3 -2 -0.15 0.60 0 -3 2 0.96 0.49 0 3 2 0.87 0.34 0 -3 -2 -0.16 0.65 0 -4 -2 332.82 8.30 0 -4 -2 315.82 7.62 0 4 -2 311.28 6.34 0 4 -2 320.48 7.75 0 -4 2 311.24 7.53 0 4 2 315.52 4.19 0 5 2 0.90 0.22 0 -5 2 0.82 0.67 0 -5 -2 0.36 0.63 0 5 -2 0.03 0.65 0 5 2 -0.72 0.37 0 -5 -2 -0.08 0.92 0 -6 -2 74.78 4.22 0 -6 -2 79.63 4.60 0 6 -2 86.35 4.11 0 6 -2 77.83 4.30 0 -6 2 77.33 4.25 0 6 2 74.50 3.08 0 -6 2 75.35 3.08 0 -7 2 0.24 0.77 0 -7 -2 0.16 0.73 0 7 -2 0.03 0.74 0 7 -2 1.99 1.04 0 7 2 3.31 0.62 0 -7 2 2.04 0.75 0 -7 -2 -0.97 1.59 0 -8 2 136.23 6.30 0 8 -2 133.87 6.39 0 8 -2 129.30 5.93 0 -8 -2 127.05 6.52 0 -8 -2 146.79 6.60 0 9 -2 0.64 0.99 0 9 -2 -1.79 1.03 0 9 2 -1.51 0.90 0 -9 -2 0.78 0.72 0 -9 2 2.76 1.21 0 -9 2 -0.49 0.59 0 -9 -2 -0.32 0.98 0 -10 -2 234.43 10.00 0 -10 2 258.23 9.36 0 -10 -2 248.68 9.64 0 10 -2 263.00 10.08 0 10 2 260.90 9.71 0 10 -2 259.98 9.69 0 -11 -2 -0.28 0.73 0 11 -2 0.94 1.29 0 11 -2 -0.16 0.59 0 11 2 4.49 1.25 0 -11 -2 -4.91 1.41 0 -11 -2 -0.30 0.53 0 -11 -2 -0.46 0.75 0 -11 2 0.50 0.62 0 -12 -2 6.44 1.18 0 -12 -2 9.24 1.63 0 -12 -2 6.23 1.31 0 12 2 7.07 1.43 0 12 -2 4.69 1.36 0 12 -2 10.62 2.51 0 -12 -2 6.91 1.19 0 -12 2 10.77 2.11 0 -12 -2 7.28 1.94 0 -13 -2 -0.07 0.59 0 -13 -2 -0.07 0.65 0 -13 -2 0.48 0.59 0 13 -2 1.95 1.66 0 13 -2 -0.03 0.73 0 -13 -2 0.30 0.84 0 -13 2 -1.54 0.88 0 -13 -2 0.07 0.55 0 14 2 0.62 0.67 0 14 -2 1.38 2.43 0 -14 -2 0.88 0.63 0 -14 -2 0.40 0.92 0 -14 -2 0.67 1.15 0 -15 -2 0.75 0.88 0 -15 -2 1.39 0.93 0 -16 -2 160.28 5.92 0 -16 -2 159.38 7.13 0 -17 -2 -0.33 0.69 0 -17 2 0.81 0.78 0 -17 -2 1.18 1.04 0 -18 2 7.31 1.27 0 -18 -2 5.48 1.21 0 -18 -2 4.64 1.39 0 -19 -2 0.04 0.55 0 -19 2 -0.33 0.52 0 -20 2 8.81 1.14 0 -20 -2 9.42 1.23 0 -21 -2 0.54 0.47 0 -21 2 -0.14 0.39 0 0 -3 3.33 0.94 0 0 3 0.47 0.53 0 1 -3 3147.03 19.07 0 -1 -3 3169.47 22.96 0 -1 3 3140.63 23.84 0 1 3 3209.45 21.19 0 -2 -3 1.24 0.89 0 2 -3 2.06 0.59 0 2 3 0.12 0.38 0 -2 3 0.54 0.66 0 -3 -3 2817.05 24.65 0 3 -3 2727.44 25.73 0 3 -3 2803.41 17.67 0 3 3 2784.76 16.99 0 -3 3 2795.29 25.24 0 -4 -3 0.50 0.81 0 4 -3 -0.79 1.13 0 4 -3 0.67 0.75 0 -4 -3 0.34 0.92 0 -4 3 1.45 0.78 0 -5 3 273.02 7.65 0 5 3 261.49 7.40 0 -5 -3 287.65 8.88 0 5 -3 281.67 8.97 0 5 -3 281.19 6.99 0 -5 -3 273.00 9.23 0 -5 3 278.79 8.81 0 -6 3 0.57 0.65 0 6 3 0.75 0.64 0 -6 -3 -0.95 1.19 0 6 -3 1.31 1.36 0 -6 -3 0.18 0.88 0 -6 3 -0.28 1.12 0 -7 -3 88.25 5.96 0 -7 -3 80.95 5.26 0 7 -3 85.19 5.52 0 7 -3 79.23 4.41 0 7 3 81.83 4.07 0 -7 3 87.10 4.22 0 -7 3 83.89 5.37 0 8 -3 0.41 0.97 0 8 3 -2.76 0.94 0 8 -3 1.23 0.93 0 -8 -3 -0.85 1.31 0 -8 -3 0.17 1.24 0 -8 3 -1.13 0.88 0 -9 -3 40.30 4.41 0 -9 -3 33.09 3.65 0 9 -3 37.67 4.15 0 9 3 35.05 3.31 0 9 -3 37.06 3.49 0 -9 3 37.70 3.92 0 -10 -3 -0.34 0.62 0 -10 -3 -0.20 0.60 0 -10 -3 1.73 0.82 0 10 -3 -1.11 1.60 0 10 3 6.13 1.55 0 10 -3 -4.12 1.47 0 -10 -3 -5.02 1.49 0 -10 3 0.23 1.23 0 -10 -3 0.25 0.51 0 -10 -3 3.04 1.48 0 -10 3 -1.58 0.84 0 -11 -3 161.89 5.66 0 -11 -3 158.44 5.36 0 -11 -3 163.79 6.44 0 11 -3 157.08 8.99 0 11 -3 157.78 8.22 0 -11 -3 160.09 9.51 0 -11 -3 142.31 8.29 0 -11 -3 160.85 6.09 0 -11 -3 162.16 5.32 0 -12 -3 1.78 0.96 0 -12 -3 0.38 0.53 0 -12 -3 0.35 0.72 0 12 -3 -3.13 1.55 0 12 -3 1.82 1.33 0 -12 -3 1.95 2.37 0 -12 -3 0.51 0.67 0 -12 -3 0.15 0.63 0 -13 -3 188.46 6.18 0 -13 -3 188.81 7.46 0 13 -3 186.39 9.86 0 13 -3 189.28 10.73 0 -13 -3 196.40 11.21 0 -13 -3 192.01 6.82 0 -13 -3 191.33 6.53 0 -14 -3 0.10 0.70 0 -14 -3 0.44 0.79 0 -14 -3 -0.19 0.74 0 -14 -3 0.71 0.99 0 -15 -3 334.64 8.69 0 -15 -3 304.27 8.31 0 -15 -3 318.82 9.90 0 -16 -3 -0.12 1.03 0 -16 -3 0.72 0.88 0 -17 -3 36.73 2.78 0 -17 -3 37.37 3.28 0 -18 3 -0.16 0.55 0 -18 -3 -0.38 0.72 0 -19 -3 6.68 1.12 0 -19 3 7.58 1.06 0 -20 -3 0.14 0.39 0 -20 3 0.36 0.38 0 0 4 9815.39 54.32 0 0 -4 9999.00 43.84 0 -1 4 2.55 1.60 0 1 4 2.58 1.52 0 1 4 1.35 0.93 0 -1 4 0.57 0.67 0 -1 -4 0.65 1.00 0 2 4 2082.69 25.19 0 -2 4 2091.46 25.13 0 -2 4 2101.87 24.06 0 -2 -4 2126.01 23.22 0 3 4 0.47 0.90 0 -3 4 0.08 0.83 0 -3 4 -1.34 0.86 0 -3 -4 0.54 0.87 0 4 4 287.33 9.44 0 -4 4 288.22 9.49 0 -4 4 314.14 10.22 0 -4 -4 297.91 9.75 0 5 4 -0.74 0.87 0 -5 4 -2.15 1.33 0 -5 -4 -0.64 1.00 0 -6 -4 232.77 9.53 0 -6 4 240.81 8.66 0 6 4 231.01 8.35 0 -6 4 239.58 9.76 0 6 -4 225.58 9.76 0 -7 -4 0.57 0.72 0 -7 4 -0.21 1.31 0 7 4 -0.97 0.74 0 -7 -4 -0.03 0.63 0 7 -4 0.74 1.63 0 -7 4 0.40 0.60 0 -7 -4 0.06 0.50 0 -8 -4 2.92 1.65 0 -8 -4 3.26 0.87 0 -8 -4 3.49 1.06 0 -8 -4 5.18 1.05 0 -8 -4 5.33 1.16 0 8 -4 1.85 1.79 0 -8 -4 1.83 1.28 0 -8 -4 2.66 0.87 0 -8 4 7.23 1.86 0 -9 -4 2.78 1.79 0 -9 -4 -0.26 0.61 0 -9 -4 -0.42 0.64 0 -9 -4 -0.32 0.70 0 -9 -4 -0.39 0.64 0 -9 -4 -2.30 1.59 0 -9 4 1.07 0.95 0 -9 -4 -0.16 0.59 0 10 -4 52.94 5.60 0 -10 -4 54.11 3.14 0 -10 -4 48.31 3.47 0 -10 -4 50.31 3.63 0 -10 -4 49.76 3.06 0 -10 -4 45.00 5.27 0 -10 -4 44.72 3.21 0 -11 -4 -0.43 0.64 0 11 -4 0.25 1.80 0 -11 -4 0.23 0.62 0 -11 -4 0.14 0.70 0 -11 -4 0.35 0.71 0 -11 -4 -0.44 1.89 0 -11 -4 0.02 0.81 0 -12 -4 21.29 2.09 0 -12 -4 22.59 2.52 0 -12 -4 23.56 2.60 0 -12 -4 22.24 2.40 0 -12 -4 22.73 2.19 0 -13 -4 0.03 0.68 0 -13 -4 -0.50 0.74 0 -13 -4 0.86 0.88 0 -13 -4 -0.14 0.90 0 -14 -4 182.18 7.13 0 -14 -4 184.22 6.56 0 -14 -4 185.60 5.90 0 -15 -4 -0.44 0.87 0 -15 -4 0.94 0.98 0 -16 -4 126.24 5.65 0 -16 -4 121.37 4.96 0 -17 -4 -0.24 0.65 0 -18 4 1.35 0.58 0 -18 -4 1.12 0.62 0 -19 4 0.30 0.38 0 -19 -4 -0.13 0.37 0 0 -5 0.68 0.76 0 0 5 1.03 1.24 0 0 -5 -0.54 0.67 0 0 -5 0.56 0.69 0 -1 -5 149.58 4.99 0 1 -5 144.72 5.02 0 1 5 140.67 7.69 0 -1 5 148.92 7.97 0 -1 -5 153.97 5.58 0 1 -5 148.36 5.54 0 -1 -5 148.18 4.73 0 -2 -5 -0.34 0.56 0 -2 5 -2.37 1.12 0 2 -5 -0.22 0.68 0 -2 -5 -0.52 0.77 0 -2 5 -0.92 1.25 0 2 5 -3.00 1.33 0 2 -5 -0.32 0.64 0 -2 -5 0.50 0.70 0 -3 -5 542.18 9.10 0 3 -5 531.88 9.86 0 -3 -5 536.80 9.47 0 -3 5 504.38 14.10 0 3 5 507.27 14.74 0 -3 5 509.73 14.63 0 -3 -5 519.23 10.13 0 3 -5 510.94 10.27 0 4 -5 0.87 0.75 0 -4 -5 0.54 0.66 0 -4 -5 0.50 0.66 0 -4 5 0.46 0.59 0 -4 5 1.03 1.40 0 4 5 1.48 0.91 0 4 -5 0.50 0.61 0 -4 -5 0.24 0.64 0 -5 -5 73.41 3.43 0 -5 -5 75.87 3.69 0 5 -5 72.56 3.80 0 -5 5 63.02 5.41 0 5 -5 75.34 3.92 0 -5 -5 69.38 3.68 0 -5 -5 71.74 4.01 0 5 5 71.35 5.54 0 -5 5 72.75 5.62 0 -6 -5 0.04 0.46 0 -6 -5 0.51 0.56 0 6 -5 0.33 0.55 0 -6 -5 0.25 0.47 0 -6 -5 -0.12 0.69 0 -6 5 -0.61 1.47 0 7 -5 52.95 3.20 0 -7 -5 55.61 3.16 0 -7 -5 54.23 3.06 0 -7 5 54.85 5.46 0 -7 -5 52.51 3.15 0 -7 -5 46.56 3.35 0 -7 5 52.64 4.64 0 -8 -5 0.36 0.75 0 -8 -5 0.54 0.61 0 -8 -5 -0.23 0.65 0 -9 -5 17.62 2.17 0 -9 -5 17.70 1.86 0 -9 -5 19.96 2.05 0 -10 -5 0.27 0.70 0 -10 -5 0.09 0.74 0 -11 -5 20.85 2.27 0 -11 -5 18.98 2.00 0 -11 -5 19.84 2.32 0 -12 -5 -0.30 0.64 0 -12 -5 0.09 0.78 0 -12 -5 0.01 0.73 0 -13 -5 39.04 3.04 0 -13 -5 38.45 3.02 0 -14 -5 0.62 0.77 0 -14 -5 -0.15 0.72 0 -15 -5 31.03 2.46 0 -16 -5 0.83 0.61 0 -17 -5 23.67 1.79 0 18 -5 -0.19 0.41 0 -18 5 -0.17 0.27 0 0 -6 1001.49 13.98 0 0 -6 979.33 15.39 0 0 -6 1000.31 13.21 0 -1 -6 1.02 1.18 0 -1 -6 -0.35 0.81 0 1 -6 -0.97 0.93 0 1 -6 3.17 1.30 0 1 -6 3.65 1.42 0 -1 -6 2.25 1.26 0 2 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-11 -8 0 2.85 0.75 11 8 0 2.77 0.98 -11 -8 0 2.42 0.76 11 -8 0 1.90 0.78 -11 -9 0 9.17 1.16 11 9 0 8.63 1.43 -11 -9 0 8.33 1.21 11 -9 0 9.25 1.42 -11 -10 0 6.67 0.95 11 -10 0 7.05 1.16 11 10 0 6.94 1.19 -11 -10 0 6.15 1.04 11 11 0 10.62 1.33 -11 -11 0 10.63 1.10 -11 -11 0 11.67 1.29 -11 -12 0 3.85 0.72 11 12 0 4.57 0.79 11 0 1 -0.34 0.72 11 0 -1 0.14 0.74 11 -1 1 13.10 1.94 11 -1 -1 11.64 1.85 11 1 1 10.53 1.76 11 1 -1 12.63 1.89 11 -2 -1 22.01 2.31 -11 -2 1 24.18 2.11 11 -2 1 22.66 2.49 11 -2 -1 23.32 2.51 11 2 1 24.60 2.59 11 2 -1 24.40 2.58 11 -3 1 14.15 1.98 11 -3 -1 13.94 1.94 11 3 1 13.60 1.95 11 3 -1 8.72 1.59 -11 -3 1 13.64 1.65 11 -3 -1 13.27 1.80 11 4 1 11.63 1.81 11 4 -1 12.85 1.89 -11 -4 1 11.98 1.60 11 -4 -1 11.02 1.63 11 -4 -1 14.81 1.97 11 -4 1 11.59 1.81 11 5 1 6.02 1.40 11 5 -1 6.87 1.46 11 -5 1 4.77 1.18 11 -5 -1 6.54 1.40 -11 -5 1 5.23 1.11 11 -5 -1 4.20 1.09 -11 -6 -1 37.89 2.54 -11 -6 1 36.28 2.66 11 -6 -1 36.75 2.73 11 -6 1 36.41 2.90 11 -6 -1 38.63 2.95 11 6 1 37.52 3.01 11 6 -1 39.98 3.03 11 -7 -1 6.84 1.17 11 7 1 7.68 1.45 11 7 -1 8.07 1.44 -11 -7 -1 6.10 1.12 -11 -7 1 6.88 1.22 11 -7 1 8.10 1.41 11 -7 -1 8.47 1.46 11 -8 -1 2.95 0.88 11 8 1 2.19 0.83 11 8 -1 2.38 0.85 -11 -8 -1 3.25 0.71 -11 -8 1 1.75 0.61 11 -8 1 3.39 1.00 11 -8 -1 3.39 1.01 -11 -8 -1 1.74 0.66 -11 -8 1 2.88 0.85 -11 -9 1 12.61 1.49 -11 -9 -1 13.08 1.45 11 9 1 11.97 1.57 11 9 -1 13.44 1.63 11 -9 1 12.80 1.55 11 -9 -1 12.28 1.53 -11 -9 -1 12.38 1.30 -11 -9 1 12.11 1.24 11 -9 -1 11.38 1.33 -11 -10 -1 12.59 1.38 -11 -10 1 14.71 1.50 11 10 1 14.99 1.57 11 10 -1 16.84 1.67 11 -10 1 15.40 1.61 11 -10 -1 15.61 1.58 -11 -10 1 14.98 1.32 -11 -10 -1 15.41 1.37 11 -10 -1 14.06 1.32 -11 -11 -1 0.81 0.39 -11 -11 1 1.38 0.49 -11 -11 -1 1.65 0.58 -11 -11 1 1.73 0.63 11 11 1 0.53 0.53 11 11 -1 1.55 0.57 -11 -12 1 3.19 0.67 11 0 -2 0.30 0.54 11 0 2 -0.40 0.74 11 0 -2 -0.40 0.76 11 -1 -2 20.81 2.00 11 1 -2 19.53 1.95 11 -1 -2 22.84 2.39 11 -1 2 19.62 2.17 11 -1 -2 16.68 1.97 11 1 2 18.35 2.11 11 1 -2 17.49 2.05 11 -2 -2 15.93 1.99 11 -2 2 16.53 2.00 11 2 2 15.68 1.97 11 2 -2 16.63 1.94 11 -2 -2 17.30 1.80 11 2 -2 15.48 1.74 11 -2 -2 13.34 1.75 11 -3 -2 5.97 1.27 11 -3 -2 5.34 1.06 11 3 -2 6.76 1.24 11 3 2 3.83 1.03 11 3 -2 4.78 1.14 11 -3 2 4.63 1.14 11 -3 -2 4.97 1.20 11 -4 -2 15.01 1.86 11 -4 2 13.30 1.73 11 -4 -2 13.76 1.75 11 4 2 14.94 1.83 11 4 -2 15.37 1.68 11 -4 -2 13.89 1.56 11 4 -2 12.34 1.69 11 -5 -2 4.08 1.10 11 -5 2 3.44 0.98 11 -5 -2 2.92 0.97 11 5 2 4.32 1.04 11 5 -2 2.76 0.90 11 5 -2 3.85 0.90 11 -6 -2 3.35 0.94 -11 -6 2 3.38 0.96 11 -6 2 4.99 1.07 11 -6 -2 4.96 1.06 11 6 -2 2.88 0.85 11 6 2 4.57 1.07 11 6 -2 4.77 1.03 11 -7 -2 4.83 1.04 -11 -7 2 5.45 1.04 11 -7 2 4.10 0.92 11 -7 -2 5.54 1.04 11 7 2 4.30 0.96 11 7 -2 7.73 1.25 11 7 -2 5.81 0.97 11 8 -2 2.48 0.71 11 -8 -2 2.04 0.75 11 8 2 2.28 0.71 11 8 -2 2.53 0.76 -11 -8 -2 2.61 0.74 -11 -8 2 2.76 0.77 -11 -8 2 1.70 0.53 11 -8 2 1.53 0.62 11 -8 -2 2.44 0.73 11 -9 -2 17.18 1.62 11 9 2 17.01 1.54 11 9 -2 18.65 1.66 11 -9 -2 18.77 1.59 11 9 -2 17.26 1.40 -11 -9 2 19.17 1.43 -11 -9 2 19.17 1.73 -11 -9 -2 16.40 1.42 11 10 2 1.05 0.49 11 10 -2 1.42 0.56 -11 -10 2 1.26 0.50 -11 -10 2 0.82 0.54 11 -10 -2 0.30 0.44 -11 -11 2 15.61 1.34 11 0 -3 -0.19 0.66 11 0 -3 -0.74 0.73 11 1 -3 2.12 0.74 11 -1 -3 2.10 0.77 11 -1 -3 2.21 0.91 11 1 -3 2.48 0.89 11 -2 -3 1.64 0.69 11 2 -3 1.33 0.75 11 -2 -3 2.43 0.93 11 2 -3 0.76 0.60 11 -3 -3 1.47 0.72 11 3 -3 1.54 0.63 11 -3 -3 1.94 0.83 11 4 -3 10.94 1.36 11 -4 -3 12.49 1.46 11 -4 -3 11.18 1.50 11 5 -3 4.06 0.91 11 -5 -3 1.50 0.72 11 6 -3 5.40 0.99 11 -6 -3 4.47 0.95 11 7 -3 7.99 1.09 -11 -7 3 8.41 1.17 11 -7 -3 7.92 1.18 11 8 -3 1.14 0.49 -11 -8 3 0.77 0.50 11 -8 -3 0.02 0.43 -11 -9 3 0.64 0.46 11 -9 -3 1.43 0.52 11 0 -4 -1.01 0.56 11 0 -4 0.17 0.47 11 -1 -4 3.54 0.78 11 1 -4 4.73 0.89 11 -1 -4 4.71 0.90 11 1 -4 3.99 0.87 11 -2 -4 21.38 1.73 11 2 -4 20.34 1.70 11 -2 -4 23.19 1.86 11 2 -4 23.17 1.78 11 -3 -4 4.06 0.79 11 3 -4 3.85 0.82 11 3 -4 4.60 0.82 11 -3 -4 4.39 0.86 11 4 -4 8.50 1.08 11 -4 -4 9.35 1.17 11 4 -4 9.65 1.08 11 5 -4 1.93 0.59 11 -5 -4 1.97 0.56 11 6 -4 2.61 0.57 -11 -6 4 4.07 0.78 11 -6 -4 2.93 0.70 12 0 0 -0.77 0.51 12 0 0 0.05 0.56 12 -1 0 -0.02 0.53 12 -1 0 0.71 0.70 12 1 0 0.35 0.67 12 -2 0 8.52 1.24 12 -2 0 8.53 1.36 12 2 0 8.34 1.41 12 -3 0 21.89 2.12 12 3 0 22.28 2.17 12 -3 0 21.94 1.83 12 4 0 0.17 0.59 12 -4 0 0.67 0.66 12 -5 0 26.72 2.21 12 5 0 27.64 2.29 12 6 0 0.47 0.60 12 -6 0 -0.38 0.50 12 7 0 1.92 0.72 12 -7 0 1.23 0.64 -12 -7 0 0.93 0.47 12 8 0 1.28 0.57 12 -8 0 0.87 0.46 12 9 0 0.25 0.38 12 -9 0 0.84 0.49 12 0 1 2.23 0.87 12 0 -1 2.91 0.90 12 0 -1 4.06 0.96 12 -1 1 2.77 0.90 12 -1 -1 3.39 0.97 12 1 1 3.51 0.99 12 1 -1 3.85 0.99 12 -1 -1 3.71 0.94 12 -2 -1 4.74 1.00 12 -2 1 5.96 1.17 12 2 1 5.60 1.13 12 2 -1 4.12 1.06 12 -2 -1 6.34 1.14 12 -3 1 1.42 0.76 12 -3 -1 1.45 0.65 12 3 1 0.90 0.71 12 3 -1 1.34 0.83 12 -3 -1 2.10 0.75 12 -4 1 2.37 0.80 12 -4 -1 1.24 0.63 12 -4 -1 2.35 0.79 12 4 1 1.17 0.69 12 4 -1 2.34 0.76 12 5 1 1.52 0.61 12 5 -1 1.43 0.58 -12 -5 1 0.40 0.44 12 -5 1 1.94 0.74 12 -5 -1 0.17 0.50 12 -5 -1 0.93 0.52 12 6 1 0.42 0.51 12 6 -1 0.90 0.59 -12 -6 1 0.88 0.43 12 -6 1 0.88 0.53 12 -6 -1 0.76 0.54 12 -6 -1 1.09 0.57 -12 -7 1 8.88 1.02 12 7 1 11.84 1.34 12 7 -1 10.12 1.25 12 -7 1 10.81 1.28 12 -7 -1 9.94 1.20 12 -7 -1 9.49 1.06 12 8 1 4.53 0.80 12 8 -1 5.42 0.89 -12 -8 1 5.17 0.79 12 -8 1 3.97 0.77 12 -8 -1 3.56 0.70 12 0 -2 1.91 0.72 12 0 2 0.83 0.54 12 0 -2 1.48 0.64 12 -1 -2 4.69 0.99 12 1 -2 3.98 0.96 12 -1 2 3.13 0.77 12 -1 -2 2.86 0.74 12 1 2 2.59 0.72 12 1 -2 3.21 0.81 12 -2 -2 9.51 1.30 12 2 -2 7.63 1.21 12 -2 2 7.30 1.13 12 -2 -2 7.98 1.16 12 2 2 8.53 1.21 12 2 -2 7.42 1.09 12 3 2 9.76 1.26 12 3 -2 7.82 1.10 -12 -3 2 8.72 1.05 12 -3 -2 9.58 1.30 12 -3 2 10.18 1.29 12 -3 -2 9.12 1.19 12 4 2 2.15 0.66 12 4 -2 1.29 0.54 12 -4 2 1.22 0.54 12 -4 -2 1.67 0.59 -12 -4 2 0.93 0.47 12 -4 -2 1.76 0.64 12 5 2 6.65 0.97 12 5 -2 3.77 0.77 -12 -5 2 4.92 0.80 12 -5 2 5.04 0.92 12 -5 -2 4.57 0.82 12 -5 -2 3.83 0.80 12 6 -2 1.42 0.54 12 -6 -2 1.20 0.60 12 -6 -2 1.10 0.53 -12 -6 2 0.78 0.46 12 0 -3 0.11 0.41 12 0 -3 -0.15 0.41 12 -1 -3 0.30 0.46 12 1 -3 0.75 0.46 12 -1 -3 0.01 0.35 12 1 -3 0.42 0.46 12 -2 -3 0.73 0.51 12 2 -3 0.60 0.49 12 3 -3 4.84 0.83 12 -3 -3 3.40 0.75 12 4 -3 4.01 0.75 12 -4 -3 3.76 0.73 12 -5 -3 0.91 0.42 13 0 0 0.63 0.48 13 1 0 5.33 0.89 13 -1 0 7.64 1.06 13 2 0 -0.38 0.43 13 -2 0 0.26 0.37 13 3 0 1.35 0.52 13 -3 0 1.26 0.52 13 0 1 0.49 0.41 13 0 -1 -0.65 0.49 13 1 1 0.46 0.34 13 -1 -1 0.19 0.43 13 1 -1 -0.06 0.44 13 2 -1 0.92 0.49 13 -2 -1 1.45 0.53 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 41149 _shelx_res_file ; TITL bv2_auto_a.res in Pna2(1) CELL 1.54184 10.6769 17.9611 7.0266 90 90 90 ZERR 4 0.0003 0.0005 0.0002 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,+Z SYMM 0.5-X,0.5+Y,0.5+Z SFAC C H O UNIT 60 64 16 EQIV $1 -0.5+X,0.5-Y,+Z L.S. 4 PLAN 10 SIZE 0.16 0.18 0.32 TEMP 21.85 CONF HTAB C5 O1_$1 HTAB C2 O4 MORE -1 BOND $H fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.049000 0.076800 BASF 0.52665 FVAR 1.08228 O1 3 0.813140 0.291933 0.456779 11.00000 0.11164 0.04846 = 0.10302 -0.00575 -0.00044 0.02539 O2 3 0.624602 0.339441 0.489700 11.00000 0.08188 0.03436 = 0.07316 0.00233 -0.00183 -0.00706 O3 3 0.765061 0.552949 0.541635 11.00000 0.05227 0.03867 = 0.08243 0.00432 -0.00644 -0.00794 O4 3 0.935420 0.529151 0.720901 11.00000 0.09240 0.06341 = 0.12144 0.02318 -0.04733 -0.01848 C1 1 0.727070 0.479954 0.525494 11.00000 0.05380 0.03643 = 0.05032 0.00393 0.00009 -0.00528 C2 1 0.802844 0.421789 0.501292 11.00000 0.05696 0.04825 = 0.06541 0.00188 0.00144 0.00319 AFIX 43 H2 2 0.889064 0.428993 0.497448 11.00000 -1.20000 AFIX 0 C3 1 0.752175 0.347546 0.480948 11.00000 0.08115 0.04341 = 0.05984 0.00171 -0.00116 0.00921 C4 1 0.546034 0.399579 0.509229 11.00000 0.06559 0.04207 = 0.04361 0.00453 -0.00076 -0.00995 C5 1 0.418284 0.385809 0.510501 11.00000 0.07376 0.06367 = 0.05744 0.00923 -0.00381 -0.03016 AFIX 43 H5 2 0.388194 0.337348 0.501419 11.00000 -1.20000 AFIX 0 C6 1 0.337028 0.444437 0.525290 11.00000 0.05327 0.09226 = 0.05633 0.00940 0.00051 -0.01530 AFIX 43 H6 2 0.251198 0.435621 0.526199 11.00000 -1.20000 AFIX 0 C7 1 0.381282 0.516998 0.538968 11.00000 0.05454 0.07617 = 0.05621 0.00330 0.00098 0.00647 AFIX 43 H7 2 0.325182 0.556481 0.547034 11.00000 -1.20000 AFIX 0 C8 1 0.508081 0.530372 0.540566 11.00000 0.05794 0.04678 = 0.04979 0.00142 -0.00094 0.00027 AFIX 43 H8 2 0.537523 0.578934 0.550915 11.00000 -1.20000 AFIX 0 C9 1 0.592672 0.471579 0.526769 11.00000 0.05268 0.03809 = 0.03972 0.00389 0.00009 -0.00646 C10 1 0.870006 0.573156 0.643674 11.00000 0.05748 0.05141 = 0.06596 0.00289 -0.00168 -0.01366 C11 1 0.886657 0.655929 0.642476 11.00000 0.05972 0.04974 = 0.07161 -0.00990 0.00734 -0.01167 AFIX 23 H11A 2 0.927453 0.670687 0.759912 11.00000 -1.20000 H11B 2 0.804650 0.679152 0.640128 11.00000 -1.20000 AFIX 0 C12 1 0.963672 0.685729 0.473935 11.00000 0.05253 0.03983 = 0.06256 -0.00191 -0.00345 -0.00862 C13 1 0.902386 0.668537 0.284038 11.00000 0.09133 0.07466 = 0.07332 0.01087 -0.02364 -0.01821 AFIX 137 H13A 2 0.895842 0.615580 0.268435 11.00000 -1.50000 H13B 2 0.952290 0.688895 0.183003 11.00000 -1.50000 H13C 2 0.820266 0.690261 0.280572 11.00000 -1.50000 AFIX 0 C14 1 0.974455 0.770045 0.502331 11.00000 0.10122 0.04408 = 0.11515 -0.00451 0.00603 -0.01920 AFIX 137 H14A 2 0.892192 0.791544 0.506977 11.00000 -1.50000 H14B 2 1.020427 0.791351 0.398310 11.00000 -1.50000 H14C 2 1.017503 0.780082 0.619503 11.00000 -1.50000 AFIX 0 C15 1 1.094730 0.652016 0.476527 11.00000 0.05757 0.08474 = 0.07935 -0.00324 0.00180 -0.00153 AFIX 137 H15A 2 1.134828 0.663632 0.595153 11.00000 -1.50000 H15B 2 1.142988 0.672232 0.373479 11.00000 -1.50000 H15C 2 1.088885 0.598960 0.462582 11.00000 -1.50000 AFIX 0 HKLF 4 REM bv2_auto_a.res in Pna2(1) REM R1 = 0.0305 for 2133 Fo > 4sig(Fo) and 0.0320 for all 2249 data REM 176 parameters refined using 1 restraints END WGHT 0.0490 0.0768 REM Highest difference peak 0.109, deepest hole -0.129, 1-sigma level 0.026 Q1 1 0.5724 0.4404 0.5074 11.00000 0.05 0.11 Q2 1 0.3768 0.4755 0.5206 11.00000 0.05 0.09 Q3 1 1.1019 0.5978 0.6093 11.00000 0.05 0.08 Q4 1 0.5635 0.5890 0.5705 11.00000 0.05 0.08 Q5 1 0.4268 0.3165 0.4283 11.00000 0.05 0.08 Q6 1 0.9697 0.7229 0.4767 11.00000 0.05 0.07 Q7 1 0.7725 0.3901 0.5135 11.00000 0.05 0.07 Q8 1 0.9011 0.4093 0.5233 11.00000 0.05 0.07 Q9 1 0.9148 0.6084 0.2388 11.00000 0.05 0.07 Q10 1 1.1213 0.7816 0.6900 11.00000 0.05 0.07 ; _shelx_res_checksum 77023 _shelxl_version_number .2013 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, 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 O O1 0.81314(18) 0.29193(8) 0.4568(3) 0.0877(6) Uani d 1 . . O O2 0.62460(14) 0.33944(6) 0.4897(2) 0.0631(4) Uani d 1 . . O O3 0.76506(11) 0.55295(6) 0.5416(2) 0.0578(4) Uani d 1 . . O O4 0.93542(18) 0.52915(9) 0.7209(4) 0.0924(7) Uani d 1 . . C C1 0.72707(16) 0.47995(8) 0.5255(3) 0.0468(4) Uani d 1 . . C C2 0.80284(18) 0.42179(10) 0.5013(4) 0.0569(4) Uani d 1 . . H H2 0.8891 0.4290 0.4974 0.068 Uiso calc 1 . . C C3 0.7522(2) 0.34755(10) 0.4809(3) 0.0615(5) Uani d 1 . . C C4 0.54603(17) 0.39958(9) 0.5092(3) 0.0504(4) Uani d 1 . . C C5 0.4183(2) 0.38581(12) 0.5105(3) 0.0650(5) Uani d 1 . . H H5 0.3882 0.3373 0.5014 0.078 Uiso calc 1 . . C C6 0.33703(19) 0.44444(14) 0.5253(3) 0.0673(6) Uani d 1 . . H H6 0.2512 0.4356 0.5262 0.081 Uiso calc 1 . . C C7 0.38128(18) 0.51700(12) 0.5390(3) 0.0623(5) Uani d 1 . . H H7 0.3252 0.5565 0.5470 0.075 Uiso calc 1 . . C C8 0.50808(17) 0.53037(10) 0.5406(3) 0.0515(4) Uani d 1 . . H H8 0.5375 0.5789 0.5509 0.062 Uiso calc 1 . . C C9 0.59267(16) 0.47158(8) 0.5268(3) 0.0435(4) Uani d 1 . . C C10 0.87001(19) 0.57316(12) 0.6437(4) 0.0583(5) Uani d 1 . . C C11 0.8867(2) 0.65593(11) 0.6425(4) 0.0604(5) Uani d 1 . . H H11A 0.9275 0.6707 0.7599 0.072 Uiso calc 1 . . H H11B 0.8046 0.6792 0.6401 0.072 Uiso calc 1 . . C C12 0.96367(16) 0.68573(9) 0.4739(3) 0.0516(4) Uani d 1 . . C C13 0.9024(3) 0.66854(15) 0.2840(4) 0.0798(7) Uani d 1 . . H H13A 0.8958 0.6156 0.2684 0.120 Uiso calc 1 . . H H13B 0.9523 0.6889 0.1830 0.120 Uiso calc 1 . . H H13C 0.8203 0.6903 0.2806 0.120 Uiso calc 1 . . C C14 0.9745(3) 0.77005(12) 0.5023(6) 0.0868(8) Uani d 1 . . H H14A 0.8922 0.7915 0.5070 0.130 Uiso calc 1 . . H H14B 1.0204 0.7914 0.3983 0.130 Uiso calc 1 . . H H14C 1.0175 0.7801 0.6195 0.130 Uiso calc 1 . . C C15 1.0947(2) 0.65202(14) 0.4765(5) 0.0739(6) Uani d 1 . . H H15A 1.1348 0.6636 0.5952 0.111 Uiso calc 1 . . H H15B 1.1430 0.6722 0.3735 0.111 Uiso calc 1 . . H H15C 1.0889 0.5990 0.4626 0.111 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 O1 0.1116(13) 0.0485(8) 0.1030(14) 0.0254(8) -0.0004(12) -0.0058(9) O2 0.0819(9) 0.0344(6) 0.0732(10) -0.0071(5) -0.0018(9) 0.0023(7) O3 0.0523(6) 0.0387(6) 0.0824(10) -0.0079(5) -0.0064(7) 0.0043(6) O4 0.0924(12) 0.0634(9) 0.1214(18) -0.0185(9) -0.0473(12) 0.0232(10) C1 0.0538(9) 0.0364(8) 0.0503(10) -0.0053(6) 0.0001(9) 0.0039(8) C2 0.0570(9) 0.0482(9) 0.0654(12) 0.0032(7) 0.0014(10) 0.0019(10) C3 0.0812(13) 0.0434(9) 0.0598(13) 0.0092(9) -0.0012(12) 0.0017(9) C4 0.0656(10) 0.0421(8) 0.0436(9) -0.0100(7) -0.0008(9) 0.0045(8) C5 0.0738(12) 0.0637(11) 0.0574(12) -0.0302(10) -0.0038(11) 0.0092(11) C6 0.0533(10) 0.0923(15) 0.0563(12) -0.0153(10) 0.0005(11) 0.0094(13) C7 0.0545(10) 0.0762(13) 0.0562(11) 0.0065(9) 0.0010(10) 0.0033(11) C8 0.0579(9) 0.0468(9) 0.0498(10) 0.0003(7) -0.0009(9) 0.0014(8) C9 0.0527(8) 0.0381(7) 0.0397(8) -0.0065(6) 0.0001(8) 0.0039(7) C10 0.0575(10) 0.0514(10) 0.0660(12) -0.0137(9) -0.0017(10) 0.0029(10) C11 0.0597(11) 0.0497(10) 0.0716(13) -0.0117(8) 0.0073(10) -0.0099(10) C12 0.0525(9) 0.0398(8) 0.0626(12) -0.0086(7) -0.0034(9) -0.0019(8) C13 0.0913(17) 0.0747(16) 0.0733(16) -0.0182(13) -0.0236(13) 0.0109(13) C14 0.1012(16) 0.0441(10) 0.115(2) -0.0192(10) 0.0060(19) -0.0045(14) C15 0.0576(11) 0.0847(14) 0.0793(16) -0.0015(10) 0.0018(12) -0.0032(13) 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_ _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 C3 O2 C4 . . 121.82(13) ? C1 O3 C10 . . 122.19(15) ? C2 C1 O3 . . 125.33(16) ? C2 C1 C9 . . 121.53(15) ? O3 C1 C9 . . 113.06(14) ? C1 C2 C3 . . 120.57(18) ? C1 C2 H2 . . 119.7 ? C3 C2 H2 . . 119.7 ? O1 C3 O2 . . 117.08(19) ? O1 C3 C2 . . 125.2(2) ? O2 C3 C2 . . 117.71(16) ? O2 C4 C5 . . 117.45(16) ? O2 C4 C9 . . 121.39(16) ? C5 C4 C9 . . 121.16(18) ? C6 C5 C4 . . 119.15(18) ? C6 C5 H5 . . 120.4 ? C4 C5 H5 . . 120.4 ? C5 C6 C7 . . 120.76(18) ? C5 C6 H6 . . 119.6 ? C7 C6 H6 . . 119.6 ? C8 C7 C6 . . 119.95(19) ? C8 C7 H7 . . 120.0 ? C6 C7 H7 . . 120.0 ? C7 C8 C9 . . 120.36(17) ? C7 C8 H8 . . 119.8 ? C9 C8 H8 . . 119.8 ? C4 C9 C8 . . 118.61(16) ? C4 C9 C1 . . 116.89(15) ? C8 C9 C1 . . 124.49(15) ? O4 C10 O3 . . 122.75(19) ? O4 C10 C11 . . 126.5(2) ? O3 C10 C11 . . 110.79(18) ? C10 C11 C12 . . 114.42(18) ? C10 C11 H11A . . 108.7 ? C12 C11 H11A . . 108.7 ? C10 C11 H11B . . 108.7 ? C12 C11 H11B . . 108.7 ? H11A C11 H11B . . 107.6 ? C13 C12 C15 . . 109.0(2) ? C13 C12 C14 . . 110.4(2) ? C15 C12 C14 . . 108.79(17) ? C13 C12 C11 . . 112.06(17) ? C15 C12 C11 . . 110.08(19) ? C14 C12 C11 . . 106.50(19) ? C12 C13 H13A . . 109.5 ? C12 C13 H13B . . 109.5 ? H13A C13 H13B . . 109.5 ? C12 C13 H13C . . 109.5 ? H13A C13 H13C . . 109.5 ? H13B C13 H13C . . 109.5 ? C12 C14 H14A . . 109.5 ? C12 C14 H14B . . 109.5 ? H14A C14 H14B . . 109.5 ? C12 C14 H14C . . 109.5 ? H14A C14 H14C . . 109.5 ? H14B C14 H14C . . 109.5 ? C12 C15 H15A . . 109.5 ? C12 C15 H15B . . 109.5 ? H15A C15 H15B . . 109.5 ? C12 C15 H15C . . 109.5 ? H15A C15 H15C . . 109.5 ? H15B C15 H15C . . 109.5 ? 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 O1 C3 . 1.204(2) ? O2 C3 . 1.371(3) ? O2 C4 . 1.374(2) ? O3 C1 . 1.3771(19) ? O3 C10 . 1.379(2) ? O4 C10 . 1.186(3) ? C1 C2 . 1.332(2) ? C1 C9 . 1.443(2) ? C2 C3 . 1.446(3) ? C2 H2 . 0.9300 ? C4 C5 . 1.386(3) ? C4 C9 . 1.391(2) ? C5 C6 . 1.368(3) ? C5 H5 . 0.9300 ? C6 C7 . 1.390(3) ? C6 H6 . 0.9300 ? C7 C8 . 1.375(3) ? C7 H7 . 0.9300 ? C8 C9 . 1.393(2) ? C8 H8 . 0.9300 ? C10 C11 . 1.497(3) ? C11 C12 . 1.538(3) ? C11 H11A . 0.9700 ? C11 H11B . 0.9700 ? C12 C13 . 1.518(3) ? C12 C15 . 1.525(3) ? C12 C14 . 1.532(3) ? C13 H13A . 0.9600 ? C13 H13B . 0.9600 ? C13 H13C . 0.9600 ? C14 H14A . 0.9600 ? C14 H14B . 0.9600 ? C14 H14C . 0.9600 ? C15 H15A . 0.9600 ? C15 H15B . 0.9600 ? C15 H15C . 0.9600 ? 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 C2 H2 O4 . 0.93 2.44 2.847(3) 107 C5 H5 O1 3_455 0.93 2.48 3.405(2) 176 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 C10 O3 C1 C2 . . . . -40.0(3) ? C10 O3 C1 C9 . . . . 143.23(18) ? O3 C1 C2 C3 . . . . -178.33(19) ? C9 C1 C2 C3 . . . . -1.8(3) ? C4 O2 C3 O1 . . . . -177.4(2) ? C4 O2 C3 C2 . . . . 2.6(3) ? C1 C2 C3 O1 . . . . 179.2(2) ? C1 C2 C3 O2 . . . . -0.7(3) ? C3 O2 C4 C5 . . . . 178.0(2) ? C3 O2 C4 C9 . . . . -1.9(3) ? O2 C4 C5 C6 . . . . -178.5(2) ? C9 C4 C5 C6 . . . . 1.4(3) ? C4 C5 C6 C7 . . . . 0.0(4) ? C5 C6 C7 C8 . . . . -1.0(4) ? C6 C7 C8 C9 . . . . 0.6(3) ? O2 C4 C9 C8 . . . . 178.16(18) ? C5 C4 C9 C8 . . . . -1.7(3) ? O2 C4 C9 C1 . . . . -0.6(3) ? C5 C4 C9 C1 . . . . 179.5(2) ? C7 C8 C9 C4 . . . . 0.7(3) ? C7 C8 C9 C1 . . . . 179.4(2) ? C2 C1 C9 C4 . . . . 2.5(3) ? O3 C1 C9 C4 . . . . 179.41(17) ? C2 C1 C9 C8 . . . . -176.2(2) ? O3 C1 C9 C8 . . . . 0.7(3) ? C1 O3 C10 O4 . . . . 1.4(4) ? C1 O3 C10 C11 . . . . -178.15(18) ? O4 C10 C11 C12 . . . . 91.9(3) ? O3 C10 C11 C12 . . . . -88.6(2) ? C10 C11 C12 C13 . . . . 61.4(2) ? C10 C11 C12 C15 . . . . -60.0(2) ? C10 C11 C12 C14 . . . . -177.8(2) ?