#------------------------------------------------------------------------------ #$Date: 2024-06-22 04:50:10 +0300 (Sat, 22 Jun 2024) $ #$Revision: 292526 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023175.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_2023175 loop_ _publ_author_name 'Bationo, Valentin' 'Kambo, Konan Ren\'e' 'Sombi\'e, Charles Bavouma' 'Semd\'e, Rasman\'e' 'Francotte, Pierre' 'Djand\'e, Abdoulaye' _publ_section_title ; Synthesis, structure and Hirshfeld surface analysis of 2-oxo-2H-chromen-4-yl pentanoate ; _journal_coeditor_code OX2005 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S205698902400584X _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C14 H14 O4' _chemical_formula_moiety 'C14 H14 O4' _chemical_formula_sum 'C14 H14 O4' _chemical_formula_weight 246.25 _chemical_name_systematic ; 2-Oxo-2H-chromen-4-yl pentanoate ; _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 geom _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 100.9517(14) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.57455(13) _cell_length_b 9.29660(17) _cell_length_c 14.5761(2) _cell_measurement_reflns_used 5988 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 72.2840 _cell_measurement_theta_min 6.1740 _cell_volume 1273.80(3) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2023) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2023) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2023) ; _computing_molecular_graphics ; PLATON (Spek, 2020), ORTEP-III Burnett & Johnson, 1996) ; _computing_publication_material ; publCIF (Westrip, 2010) and WinGX (Farrugia, 2012) ; _computing_structure_refinement ; SHELXL2013 (Sheldrick, 2015b18) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 295(2) _diffrn_detector_area_resol_mean 5.3045 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Rigaku Oxford Diffraction SuperNova, Dual, Atlas 2' _diffrn_measurement_method '\w scan' _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_unetI/netI 0.0134 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 13663 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.418 _diffrn_reflns_theta_min 4.704 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.86857 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2023) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.284 _exptl_crystal_description prism _exptl_crystal_F_000 520 _exptl_crystal_size_max 0.260 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.180 _refine_diff_density_max 0.295 _refine_diff_density_min -0.273 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 164 _refine_ls_number_reflns 2492 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.078 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0560 _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^)+(0.0899P)^2^+0.3573P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1665 _refine_ls_wR_factor_ref 0.1749 _reflns_number_gt 2107 _reflns_number_total 2492 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ox2005.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2023175 _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 0.823 _shelx_estimated_absorpt_t_max 0.872 _shelx_hkl_file ; 0 0 -2 1137.59 8.63 0 0 2 1141.94 7.42 0 0 3 -0.19 0.25 0 0 3 3.15 0.50 0 0 -4 4240.66 23.79 0 0 4 4228.25 20.66 0 0 5 0.38 0.41 0 0 -5 0.44 0.36 0 0 -5 0.02 0.45 0 0 5 0.38 0.35 0 0 5 0.38 0.45 0 0 -6 570.07 11.21 0 0 -6 584.18 11.17 0 0 6 583.69 11.35 0 0 6 567.86 11.20 0 0 6 564.81 9.64 0 0 -7 -0.78 0.57 0 0 7 0.22 0.51 0 0 7 0.05 0.39 0 0 -8 92.22 5.46 0 0 8 91.71 5.52 0 0 8 97.57 4.83 0 0 -9 0.03 0.67 0 0 9 0.68 0.74 0 0 10 369.85 8.15 0 0 -10 377.21 9.40 0 0 10 348.89 8.34 0 0 -10 350.08 12.66 0 0 10 371.33 8.97 0 0 10 348.66 10.79 0 0 11 0.79 0.55 0 0 11 -0.38 0.55 0 0 11 -0.29 0.71 0 0 -11 0.31 0.63 0 0 -11 1.82 1.09 0 0 11 0.17 0.46 0 0 12 30.97 2.92 0 0 12 26.89 2.62 0 0 -12 30.40 2.98 0 0 12 30.60 2.61 0 0 -12 32.65 4.40 0 0 12 31.47 3.92 0 0 12 34.18 2.65 0 0 13 -0.35 0.60 0 0 13 -0.60 0.55 0 0 13 -0.32 0.70 0 0 -13 0.60 0.52 0 0 14 -0.27 0.77 0 0 14 0.89 0.60 0 0 -14 0.28 0.56 0 0 15 0.41 0.65 0 0 -15 -0.83 0.86 0 0 -16 21.89 2.20 0 0 16 21.48 2.08 0 0 17 0.29 0.48 0 0 -17 -0.12 0.33 0 -1 0 0.07 0.16 0 -1 -1 9205.46 21.78 0 1 1 9120.22 20.11 0 1 -1 9318.97 20.86 0 1 -1 9464.91 17.84 0 1 2 302.60 4.57 0 -1 2 307.63 2.98 0 1 -2 293.19 4.43 0 1 2 298.20 4.47 0 -1 2 318.92 4.64 0 -1 -2 324.21 4.63 0 -1 2 300.83 4.63 0 -1 -2 302.61 2.93 0 1 3 222.39 4.72 0 -1 3 233.79 3.55 0 -1 3 239.35 4.53 0 -1 -3 253.42 5.13 0 1 3 227.60 4.85 0 -1 3 241.56 4.99 0 1 -3 249.37 4.98 0 -1 -3 236.25 2.18 0 -1 4 814.92 10.56 0 1 -4 810.54 10.47 0 -1 -4 855.10 10.67 0 1 -4 799.63 10.44 0 -1 -4 811.93 10.43 0 1 4 781.96 10.39 0 -1 4 749.31 7.88 0 -1 4 809.81 8.92 0 1 4 808.65 10.63 0 1 -5 214.09 6.13 0 -1 -5 229.57 6.33 0 -1 -5 224.54 6.29 0 -1 5 225.56 6.36 0 1 -5 215.28 6.14 0 1 5 216.46 6.25 0 -1 5 221.76 4.88 0 1 5 217.41 5.87 0 -1 5 224.21 6.55 0 1 5 233.39 6.41 0 1 -6 888.03 13.96 0 1 -6 900.06 14.03 0 -1 -6 930.94 14.23 0 -1 -6 934.73 14.31 0 1 6 931.30 13.40 0 -1 6 872.08 10.96 0 1 6 921.10 14.16 0 -1 -7 600.33 12.68 0 1 -7 588.09 12.64 0 1 7 595.68 11.72 0 -1 7 578.56 9.96 0 1 7 573.32 12.47 0 1 -8 50.38 4.08 0 -1 -8 60.60 4.45 0 1 8 64.45 4.24 0 -1 8 57.28 3.47 0 1 8 59.15 4.43 0 1 -9 0.91 1.13 0 -1 -9 1.06 1.03 0 1 9 0.42 0.59 0 1 9 -0.51 0.78 0 -1 9 -0.49 0.81 0 -1 10 87.44 4.15 0 1 10 87.77 4.29 0 -1 -10 91.46 4.60 0 1 -10 91.83 4.69 0 1 10 85.77 4.28 0 1 10 85.06 4.29 0 1 10 89.24 4.41 0 -1 10 78.71 4.23 0 -1 -10 89.72 6.47 0 1 -10 87.33 6.36 0 -1 10 81.17 4.03 0 1 10 90.75 4.19 0 1 10 85.19 5.63 0 -1 11 2.58 0.88 0 1 11 4.35 1.12 0 1 11 3.36 1.00 0 -1 -11 2.19 0.80 0 1 -11 3.04 0.98 0 1 -11 1.70 0.75 0 1 11 1.22 1.09 0 1 11 2.23 0.84 0 -1 11 3.35 1.06 0 -1 12 1.25 0.52 0 1 12 2.65 1.02 0 1 12 2.35 0.84 0 1 12 1.32 0.67 0 1 -12 2.33 1.06 0 -1 -12 1.48 0.71 0 1 12 0.31 0.46 0 1 12 1.70 0.71 0 -1 -12 1.52 1.57 0 -1 12 1.74 0.85 0 1 12 1.57 1.43 0 1 12 2.32 1.36 0 -1 -13 1.72 1.02 0 1 -13 0.42 0.69 0 1 13 1.24 0.76 0 -1 13 0.75 0.72 0 1 13 1.79 0.67 0 1 13 1.09 0.49 0 1 13 0.68 0.69 0 1 13 0.80 0.57 0 1 14 0.93 0.53 0 1 14 0.72 0.73 0 -1 14 0.36 0.59 0 1 14 0.15 0.65 0 1 14 1.07 0.83 0 1 -14 1.35 0.88 0 -1 -14 0.75 0.66 0 1 -15 6.92 1.38 0 -1 -15 7.55 1.49 0 -1 15 6.48 1.32 0 1 15 6.61 1.33 0 1 15 8.48 1.26 0 -1 -16 0.00 0.42 0 1 -16 -0.09 0.52 0 1 16 0.08 0.51 0 -1 16 -0.05 0.48 0 -1 -17 11.32 1.24 0 1 -17 9.26 1.19 0 1 17 8.22 1.02 0 -1 17 10.95 1.24 0 -2 0 4773.29 21.79 0 2 0 4870.82 10.65 0 -2 -1 492.81 6.54 0 2 1 493.06 4.98 0 -2 -1 469.39 7.07 0 2 1 474.43 5.60 0 2 -1 506.05 3.80 0 -2 -1 496.73 3.68 0 -2 -2 574.42 6.58 0 2 2 573.42 7.00 0 -2 -2 561.07 7.75 0 2 -2 557.18 7.45 0 2 2 564.78 7.42 0 2 2 566.36 7.25 0 2 -2 573.23 6.14 0 -2 -2 578.63 6.06 0 -2 -3 33.18 1.44 0 2 3 31.10 1.91 0 -2 -3 31.69 1.89 0 -2 3 33.50 2.14 0 2 3 31.82 2.01 0 -2 -3 33.53 1.88 0 2 -3 31.46 1.80 0 2 -3 33.86 1.86 0 -2 -3 32.17 1.79 0 -2 -4 33.53 1.22 0 2 -4 32.94 2.14 0 -2 -4 37.24 2.28 0 2 -4 32.04 2.16 0 -2 -4 34.14 1.97 0 2 4 37.72 2.36 0 2 -4 31.96 2.32 0 -2 4 33.35 2.27 0 2 4 34.83 2.32 0 2 -5 237.26 6.51 0 -2 -5 244.05 6.56 0 2 5 244.68 6.78 0 -2 -5 246.28 5.45 0 2 5 246.94 6.77 0 -2 5 233.36 6.31 0 2 -6 262.62 7.68 0 -2 -6 267.78 7.72 0 -2 -6 274.02 5.80 0 2 6 287.80 8.13 0 2 6 284.17 8.02 0 2 -7 205.73 7.57 0 -2 -7 214.66 7.64 0 2 7 205.91 7.59 0 2 7 213.80 7.58 0 -2 -8 0.52 0.48 0 2 -8 1.23 0.89 0 2 8 1.60 0.81 0 2 8 0.59 0.69 0 -2 -9 3.86 1.26 0 2 -9 3.18 1.31 0 2 9 4.98 1.42 0 2 9 3.47 1.13 0 2 10 52.05 4.72 0 -2 -10 47.01 4.65 0 2 -10 46.22 4.70 0 2 10 49.42 3.30 0 -2 -10 48.72 3.37 0 2 -10 52.03 3.63 0 2 10 46.26 3.16 0 2 10 51.63 3.41 0 2 10 43.61 4.45 0 2 10 45.95 3.20 0 -2 10 50.70 3.48 0 -2 11 0.10 0.56 0 2 11 0.90 0.55 0 2 11 0.35 0.51 0 2 11 0.58 0.66 0 -2 -11 0.31 0.62 0 2 11 0.13 0.55 0 2 -11 1.56 0.85 0 2 11 -1.00 1.29 0 -2 -11 -0.66 0.66 0 2 -11 0.24 1.02 0 -2 11 0.03 0.43 0 2 11 1.12 0.95 0 2 12 33.45 2.98 0 -2 -12 26.62 2.71 0 2 -12 28.74 2.95 0 -2 12 27.22 2.82 0 2 12 26.14 2.67 0 2 12 29.51 2.71 0 -2 12 25.62 2.60 0 2 -13 13.68 2.09 0 -2 -13 15.77 2.14 0 2 13 15.18 2.05 0 2 13 13.74 1.83 0 2 13 13.75 1.83 0 -2 13 15.33 2.14 0 2 13 13.66 1.91 0 2 13 15.15 1.94 0 2 -14 10.01 1.82 0 -2 -14 8.44 1.57 0 2 14 7.64 1.25 0 2 14 8.76 1.42 0 2 14 10.74 1.67 0 2 14 9.93 1.62 0 -2 14 11.03 1.86 0 2 14 10.34 1.61 0 -2 -15 37.67 2.90 0 2 -15 43.97 3.33 0 2 15 39.22 2.68 0 -2 15 45.97 3.32 0 2 15 39.14 2.89 0 2 15 34.33 2.30 0 -2 -16 24.12 2.04 0 2 -16 26.38 2.35 0 2 16 21.55 1.72 0 2 16 27.56 2.07 0 -2 16 28.22 2.33 0 -2 17 2.31 0.64 0 2 -17 1.49 0.53 0 3 0 0.24 0.20 0 -3 0 0.25 0.34 0 3 0 0.29 0.14 0 3 -1 178.91 2.36 0 3 1 186.03 4.18 0 3 1 187.12 4.28 0 -3 -1 193.47 5.13 0 -3 1 185.16 5.42 0 3 1 186.26 3.44 0 3 -2 199.29 5.32 0 3 2 202.44 5.20 0 3 2 204.06 4.95 0 3 -2 196.29 3.06 0 -3 -2 198.82 3.32 0 3 -2 201.06 3.41 0 3 2 189.71 4.67 0 -3 -2 192.79 5.73 0 -3 -2 202.93 5.06 0 -3 2 206.79 6.05 0 3 -3 276.49 7.09 0 3 -3 268.22 6.56 0 -3 3 280.58 7.37 0 3 3 276.23 6.44 0 3 -3 272.95 5.17 0 -3 -3 273.58 5.13 0 -3 -3 278.58 6.77 0 3 3 268.92 6.04 0 -3 -3 274.27 5.55 0 3 4 445.34 9.05 0 3 -4 469.48 9.94 0 -3 4 447.95 9.70 0 3 -4 432.86 7.80 0 -3 -4 455.74 7.84 0 3 4 460.07 8.71 0 -3 -4 451.82 8.70 0 -3 -4 453.29 6.58 0 3 5 12.71 1.69 0 3 -5 16.53 1.75 0 -3 -5 15.38 1.69 0 3 5 14.88 1.79 0 -3 -5 15.54 1.66 0 -3 5 12.98 1.77 0 3 6 4.15 1.21 0 3 6 2.87 1.01 0 3 -6 3.14 0.90 0 -3 -6 3.45 0.94 0 -3 -6 2.85 0.65 0 -3 6 2.54 0.87 0 3 7 2.33 0.94 0 3 7 0.88 0.68 0 3 -7 2.05 0.97 0 -3 -7 2.23 0.96 0 3 -8 186.42 7.97 0 -3 -8 184.77 7.86 0 3 8 189.19 8.13 0 3 8 189.83 8.27 0 -3 9 66.91 3.86 0 3 9 70.79 3.77 0 3 9 66.84 3.73 0 -3 -9 78.85 5.60 0 3 -9 61.83 5.04 0 3 9 73.83 5.54 0 -3 9 74.72 4.24 0 3 9 70.92 5.35 0 3 10 22.47 3.27 0 3 10 28.22 3.69 0 3 -10 21.21 2.41 0 -3 -10 20.41 2.23 0 3 10 23.85 2.40 0 3 10 24.75 2.40 0 3 -10 27.36 3.69 0 -3 -10 23.51 3.36 0 3 10 22.92 3.29 0 -3 10 23.97 2.50 0 -3 10 27.24 2.62 0 3 10 24.22 2.30 0 3 11 28.86 3.98 0 3 11 26.73 2.62 0 3 11 24.91 2.53 0 3 -11 22.68 2.56 0 -3 -11 21.98 2.37 0 3 11 23.08 2.48 0 3 11 22.00 2.37 0 3 -11 19.98 3.20 0 -3 -11 26.56 3.84 0 3 11 20.87 3.44 0 -3 11 24.79 2.62 0 3 11 24.99 2.45 0 -3 11 21.08 2.46 0 3 12 16.19 2.11 0 -3 -12 13.83 1.96 0 3 12 11.35 1.81 0 3 -12 8.54 1.78 0 3 12 12.43 1.89 0 -3 12 13.37 2.03 0 3 12 11.20 1.72 0 -3 12 10.45 1.74 0 3 13 161.85 6.44 0 3 13 162.05 5.98 0 -3 13 173.39 6.88 0 3 13 161.63 6.18 0 3 -13 162.39 6.92 0 -3 -13 145.59 6.06 0 3 13 157.27 6.18 0 -3 13 154.87 6.31 0 3 13 159.56 6.13 0 3 14 68.06 4.05 0 3 14 72.90 3.92 0 -3 14 73.61 4.33 0 3 14 70.06 3.73 0 -3 -14 68.95 3.98 0 3 -14 73.80 4.51 0 3 14 75.86 4.13 0 3 14 77.16 4.10 0 3 15 28.47 2.46 0 -3 -15 31.33 2.38 0 3 -15 30.60 2.71 0 3 15 28.76 2.28 0 3 15 27.06 2.09 0 -3 15 28.52 2.49 0 3 15 26.73 2.12 0 3 15 28.15 2.30 0 3 16 8.94 1.12 0 3 16 8.97 0.99 0 -3 16 10.08 1.37 0 3 -16 9.35 1.36 0 -3 17 4.30 0.70 0 3 -17 2.32 0.59 0 4 0 280.09 4.82 0 -4 0 277.83 7.68 0 4 1 2.17 0.53 0 4 -1 2.06 0.51 0 4 1 1.59 0.50 0 4 1 1.92 0.39 0 4 1 2.01 0.50 0 -4 1 1.53 0.76 0 -4 -1 1.84 0.74 0 4 -2 0.57 0.44 0 4 2 1.53 0.62 0 4 -2 2.77 0.46 0 4 2 1.63 0.56 0 4 2 1.16 0.45 0 -4 -2 2.30 0.76 0 -4 2 1.97 0.89 0 4 -3 606.15 11.30 0 4 3 619.78 10.73 0 4 3 586.32 10.92 0 -4 3 628.87 12.70 0 4 3 603.85 9.37 0 -4 -3 603.08 10.11 0 4 3 605.22 9.98 0 4 4 38.72 2.96 0 4 -4 37.71 3.22 0 -4 4 38.69 3.30 0 -4 -4 37.30 2.40 0 4 4 37.91 2.79 0 4 4 42.84 2.80 0 4 -5 301.59 9.60 0 4 5 303.97 8.94 0 -4 5 295.81 9.52 0 -4 -5 313.09 7.39 0 4 5 296.79 8.29 0 4 5 308.01 8.28 0 4 6 123.54 6.16 0 -4 6 116.30 6.14 0 4 -6 112.40 5.10 0 -4 -6 118.17 5.17 0 4 6 121.75 5.72 0 4 6 110.24 5.42 0 4 7 1079.28 19.51 0 4 7 1033.50 18.06 0 4 7 1064.48 18.37 0 4 8 136.08 5.04 0 -4 8 143.98 5.52 0 4 8 138.60 7.51 0 -4 8 141.64 5.95 0 4 8 135.11 7.05 0 -4 -9 138.20 5.52 0 4 9 142.58 5.59 0 4 9 138.34 5.39 0 -4 9 145.36 5.87 0 4 9 144.20 8.13 0 -4 9 148.77 6.37 0 4 9 134.79 7.55 0 4 -10 152.09 6.49 0 -4 -10 155.42 6.02 0 4 10 144.05 5.77 0 4 10 146.15 5.95 0 -4 10 150.07 6.22 0 4 10 154.57 8.82 0 -4 10 150.07 6.58 0 4 10 137.35 8.05 0 4 11 116.35 5.47 0 4 11 119.88 5.40 0 4 -11 120.82 5.96 0 -4 -11 117.93 5.36 0 -4 11 125.82 5.81 0 -4 11 119.33 5.94 0 4 11 124.38 5.66 0 4 12 32.77 2.95 0 4 12 26.84 2.68 0 -4 12 32.63 3.02 0 -4 12 28.07 2.85 0 -4 -12 28.05 2.59 0 4 -12 32.07 3.07 0 4 12 33.17 2.95 0 4 13 25.33 2.48 0 -4 -13 25.79 2.38 0 4 -13 26.86 2.75 0 -4 13 29.74 2.80 0 -4 13 27.15 2.67 0 4 13 30.49 2.78 0 4 13 30.39 2.78 0 4 -14 3.40 1.02 0 4 14 3.53 1.01 0 -4 14 5.17 1.21 0 4 14 4.09 1.07 0 4 14 2.92 0.95 0 -4 14 4.56 1.03 0 4 14 3.38 0.97 0 4 15 35.42 2.51 0 4 -15 36.89 2.76 0 4 15 37.59 2.52 0 4 15 36.33 2.45 0 -4 15 33.68 2.51 0 4 15 30.11 2.12 0 -4 16 0.45 0.41 0 4 16 -0.33 0.35 0 4 16 0.07 0.32 0 4 -16 0.77 0.55 0 5 0 0.10 0.39 0 -5 0 -0.82 0.95 0 5 1 1.99 0.75 0 5 1 4.44 0.94 0 5 -1 3.03 0.69 0 -5 -1 2.67 0.98 0 -5 1 2.78 1.06 0 5 -2 33.65 2.98 0 5 2 34.64 2.95 0 -5 2 42.21 3.64 0 -5 -2 31.83 2.86 0 5 2 33.70 2.47 0 5 -2 39.15 3.27 0 -5 3 705.78 15.38 0 5 -3 723.81 15.02 0 -5 -3 668.47 12.51 0 5 -3 674.78 13.65 0 5 3 725.67 12.55 0 5 3 668.72 13.18 0 5 -4 12.11 1.99 0 5 -4 8.54 1.75 0 5 4 6.83 1.39 0 -5 4 8.32 1.75 0 5 5 1.40 0.73 0 -5 5 0.20 0.67 0 5 5 0.84 0.66 0 -5 6 77.73 5.63 0 5 6 82.65 5.41 0 -5 6 75.68 4.28 0 -5 6 83.19 4.10 0 5 6 82.40 4.89 0 -5 7 187.86 6.20 0 5 7 195.22 8.84 0 -5 7 187.02 6.29 0 5 7 190.18 8.01 0 -5 7 185.52 6.97 0 5 8 19.65 2.95 0 5 8 19.84 3.06 0 -5 8 15.83 1.95 0 -5 8 18.41 2.32 0 5 9 275.19 7.98 0 5 9 282.05 7.76 0 5 9 276.34 11.11 0 5 9 267.92 11.60 0 -5 9 266.75 8.04 0 -5 9 275.31 9.09 0 -5 10 306.48 9.68 0 -5 10 305.88 8.85 0 5 10 304.07 8.26 0 5 10 311.88 8.67 0 5 -10 318.18 9.40 0 5 -11 74.34 4.64 0 5 11 76.23 4.39 0 5 11 71.25 4.07 0 5 11 69.29 4.20 0 -5 11 71.16 4.35 0 -5 11 70.41 4.64 0 5 12 7.26 1.41 0 5 12 7.98 1.55 0 5 -12 8.12 1.60 0 5 12 7.19 1.49 0 -5 12 7.86 1.55 0 -5 12 8.53 1.70 0 5 13 14.78 1.86 0 5 13 16.90 2.00 0 5 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172.47 8.70 -2 4 -8 22.65 2.23 2 -4 8 23.89 2.70 2 4 8 21.41 3.22 2 4 8 22.76 3.42 2 4 8 19.60 2.16 2 -4 8 20.57 2.12 -2 4 -8 23.43 2.43 -2 4 -9 293.94 8.23 2 4 9 302.07 8.63 2 -4 9 305.59 9.77 2 4 9 286.01 12.11 2 -4 9 289.86 8.19 2 4 9 296.36 8.41 2 4 9 298.88 12.72 -2 4 -9 296.16 8.80 2 4 10 85.12 4.72 2 4 10 87.77 4.83 -2 4 -10 91.09 4.66 2 -4 10 95.46 5.57 -2 4 -10 87.94 4.93 2 4 10 92.11 4.84 2 -4 10 84.22 4.56 2 4 11 81.83 4.70 2 4 11 80.16 4.65 2 -4 11 73.28 4.28 2 4 11 80.85 4.55 2 -4 11 89.52 5.36 -2 4 -11 79.67 4.67 -2 4 -11 83.30 5.03 2 4 12 81.46 4.54 2 4 12 84.09 4.68 2 4 12 91.31 4.76 2 4 12 91.53 4.60 2 -4 12 86.40 5.06 2 4 12 82.07 4.42 2 -4 12 88.18 4.58 -2 4 -12 89.99 5.07 -2 4 -13 44.31 3.44 2 4 13 37.90 2.98 2 -4 13 37.75 3.11 2 4 13 38.83 2.87 2 -4 13 39.18 2.89 2 4 13 40.27 2.89 2 4 13 39.74 3.01 2 4 14 19.22 1.88 2 -4 14 16.04 1.85 2 4 14 17.66 1.70 -2 4 -14 17.87 1.99 2 4 14 21.21 1.88 2 4 14 21.09 1.90 2 4 14 18.35 1.60 2 -4 14 17.49 1.75 2 -4 15 8.01 1.02 2 4 15 11.66 1.15 -2 4 -15 12.81 1.47 2 -4 15 8.06 1.00 2 4 15 10.36 1.23 2 4 15 9.40 1.06 -2 -5 16 6.10 0.90 -2 5 16 6.72 0.84 -2 5 15 6.17 1.02 -2 5 15 6.80 1.07 2 -5 -15 6.11 0.95 2 5 -15 6.47 1.00 -2 5 15 5.94 0.98 2 5 -14 23.11 2.08 2 -5 -14 24.88 2.17 -2 5 14 27.80 2.33 -2 5 14 26.11 2.28 -2 -5 14 25.28 2.33 -2 5 14 27.31 2.27 -2 5 13 12.10 1.70 -2 -5 13 10.84 1.64 -2 5 13 12.27 1.72 -2 5 13 10.74 1.64 -2 5 13 10.27 1.48 2 5 -13 13.29 1.75 2 -5 -13 11.37 1.64 -2 5 12 39.97 2.99 -2 5 12 41.52 3.17 -2 -5 12 41.72 3.26 2 -5 -12 39.62 3.17 2 5 -12 40.65 3.16 -2 5 12 38.57 3.08 -2 -5 12 40.95 3.30 -2 5 12 37.36 3.05 -2 5 11 122.14 5.22 2 5 -11 120.21 5.48 2 -5 -11 110.49 5.40 -2 -5 11 112.29 5.55 -2 5 11 125.95 5.59 -2 5 11 115.34 5.35 -2 -5 11 129.55 5.93 -2 5 10 1.03 0.71 2 -5 -10 0.91 0.85 -2 -5 10 1.37 0.70 -2 -5 10 -0.50 0.57 -2 5 10 2.48 1.08 2 -5 -9 41.89 3.34 -2 -5 9 43.05 3.51 -2 5 9 41.17 4.55 -2 5 9 44.10 4.43 -2 -5 9 40.75 3.26 -2 5 9 44.06 3.20 -2 5 9 45.93 3.04 -2 -5 8 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3.71 1.51 -4 -4 -5 7.24 1.29 4 -4 5 4.40 1.08 -4 4 -5 4.19 1.04 -4 4 -6 2.92 0.80 -4 -4 -6 2.31 0.84 4 4 6 0.37 0.84 -4 4 -6 3.79 1.01 4 -4 6 2.10 0.76 4 -4 6 3.55 1.01 4 4 6 4.13 0.99 4 -4 7 249.55 7.74 4 4 7 254.58 7.34 4 4 7 242.81 11.90 4 4 7 239.44 10.96 4 4 7 253.58 7.99 -4 4 -7 242.46 7.29 4 -4 7 227.86 7.38 -4 4 -7 243.91 8.03 4 4 8 1.76 0.71 4 -4 8 2.26 1.05 -4 4 -8 2.02 0.90 -4 4 -8 1.92 0.93 4 4 9 73.94 4.49 4 4 9 73.00 4.43 4 -4 9 72.16 4.37 -4 4 -9 65.81 4.28 -4 4 -9 67.63 4.53 4 4 10 10.42 1.72 4 4 10 11.02 1.78 4 4 10 11.42 1.84 4 -4 10 10.67 1.99 -4 4 -10 10.14 1.67 -4 4 -10 6.90 1.47 4 4 11 36.93 3.01 4 4 11 34.14 2.85 4 4 11 34.93 2.92 4 -4 11 36.72 3.32 -4 4 -11 31.58 2.93 -4 4 -11 37.42 3.17 -4 4 -12 27.94 2.53 4 4 12 25.78 2.31 4 4 12 31.80 2.56 4 -4 12 27.51 2.66 4 4 12 31.38 2.53 4 4 12 32.31 2.49 4 4 12 31.33 2.28 4 4 13 20.85 1.59 4 4 13 20.31 1.57 4 -4 13 21.45 2.05 -4 4 -13 24.24 2.12 4 4 13 23.02 1.95 4 4 13 23.94 1.92 4 -4 14 9.37 1.13 4 4 14 11.79 1.16 4 4 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2 1.72 0.59 11 -2 -1 4.11 0.80 11 2 -1 2.81 0.64 -11 -2 1 3.85 0.74 -11 2 1 5.36 0.88 11 2 -1 4.27 0.72 -11 2 1 6.02 0.97 -11 -2 0 2.75 0.67 -11 2 0 1.85 0.49 11 2 0 2.95 0.62 -11 2 -1 3.81 0.69 11 -2 1 5.63 0.93 11 2 1 4.02 0.68 -11 2 -1 5.29 0.85 11 -2 2 2.03 0.53 -11 2 -2 1.48 0.43 -11 3 7 16.20 1.28 -11 3 6 1.04 0.44 11 3 -5 0.85 0.47 -11 3 5 1.60 0.50 -11 3 5 0.57 0.26 11 3 -4 1.91 0.50 11 -3 -4 1.37 0.45 11 3 -4 1.05 0.43 -11 3 4 1.90 0.57 11 -3 -4 1.42 0.40 -11 3 4 1.39 0.49 11 3 -3 -0.18 0.33 11 -3 -3 0.11 0.32 11 3 -3 -0.03 0.43 -11 3 3 -0.11 0.29 11 -3 -3 0.31 0.33 -11 3 3 0.58 0.38 -11 3 2 2.68 0.64 11 3 -2 3.59 0.65 11 -3 -2 3.03 0.67 -11 3 2 3.76 0.74 -11 3 1 0.26 0.32 11 3 -1 0.61 0.41 11 -3 -1 0.62 0.39 -11 3 1 0.48 0.32 -11 3 0 2.39 0.53 11 3 0 1.74 0.48 -11 3 0 1.73 0.50 11 -3 0 2.28 0.61 -11 3 -1 -0.02 0.33 11 -3 1 -0.04 0.30 -11 4 5 7.77 0.86 -11 4 4 -0.31 0.27 -11 4 4 -0.17 0.30 -11 4 3 0.83 0.38 -11 4 3 1.23 0.44 -11 4 2 0.68 0.37 -11 4 1 1.48 0.39 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 75609 _shelx_res_file ; TITL bv1_auto_a.res in P2(1)/c CELL 1.54184 9.574547 9.296602 14.576117 90 100.9517 90 ZERR 4 0.000132 0.000167 0.000204 0 0.0014 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H O UNIT 56 56 16 L.S. 4 PLAN 13 SIZE 0.18 0.22 0.26 TEMP 21.85 CONF MORE -1 BOND $H HTAB C2 O4 EQIV $1 -x+2, y+1/2, -z+1/2 HTAB C5 O1_$1 EQIV $2 x, -y+1/2, z+1/2 HTAB C11 O1_$2 fmap 2 acta WGHT 0.089900 0.357300 FVAR 1.03777 O1 3 0.853079 0.189818 0.348628 11.00000 0.11244 0.06738 = 0.09447 -0.02305 0.04704 -0.00794 O2 3 0.898420 0.420278 0.338528 11.00000 0.07724 0.06693 = 0.06063 -0.00663 0.03270 -0.00333 O3 3 0.735478 0.514873 0.574134 11.00000 0.06657 0.06548 = 0.05927 -0.00602 0.03211 -0.01209 O4 3 0.556236 0.355465 0.563758 11.00000 0.09942 0.11662 = 0.08549 -0.03195 0.05118 -0.04835 C1 1 0.780278 0.474125 0.493944 11.00000 0.04978 0.05937 = 0.05115 0.00022 0.01968 -0.00230 C2 1 0.782935 0.339578 0.462052 11.00000 0.06765 0.05385 = 0.06452 0.00053 0.02743 -0.00585 AFIX 43 H2 2 0.744661 0.265441 0.492287 11.00000 -1.20000 AFIX 0 C3 1 0.844160 0.307981 0.381657 11.00000 0.06847 0.06096 = 0.06606 -0.00523 0.02375 -0.00342 C4 1 0.893588 0.559643 0.369738 11.00000 0.05462 0.06141 = 0.05234 0.00413 0.01737 0.00021 C5 1 0.949188 0.665341 0.320286 11.00000 0.07264 0.07830 = 0.06052 0.01156 0.02685 -0.00484 AFIX 43 H5 2 0.989087 0.641700 0.268861 11.00000 -1.20000 AFIX 0 C6 1 0.944327 0.805547 0.348550 11.00000 0.08290 0.07211 = 0.08118 0.02425 0.02862 -0.00460 AFIX 43 H6 2 0.980663 0.877591 0.315530 11.00000 -1.20000 AFIX 0 C7 1 0.886204 0.841653 0.425456 11.00000 0.08764 0.05132 = 0.09670 0.00879 0.03018 -0.00105 AFIX 43 H7 2 0.883732 0.937254 0.443867 11.00000 -1.20000 AFIX 0 C8 1 0.832077 0.735602 0.474591 11.00000 0.06660 0.05820 = 0.07276 0.00105 0.02760 0.00169 AFIX 43 H8 2 0.793042 0.759960 0.526251 11.00000 -1.20000 AFIX 0 C9 1 0.835267 0.592764 0.447708 11.00000 0.04791 0.05494 = 0.05453 0.00361 0.01747 0.00029 C10 1 0.626285 0.447146 0.606266 11.00000 0.05851 0.06565 = 0.05679 0.00352 0.02237 -0.00639 C11 1 0.610422 0.511700 0.696394 11.00000 0.09031 0.08337 = 0.06523 -0.00786 0.04017 -0.01965 AFIX 23 H11A 2 0.590474 0.613362 0.686233 11.00000 -1.20000 H11B 2 0.701026 0.503887 0.739159 11.00000 -1.20000 AFIX 0 C12 1 0.499421 0.449915 0.742656 11.00000 0.07396 0.10443 = 0.06141 -0.00625 0.03038 -0.01905 AFIX 23 H12A 2 0.409093 0.456876 0.699517 11.00000 -1.20000 H12B 2 0.519944 0.348417 0.753133 11.00000 -1.20000 AFIX 0 C13 1 0.481813 0.513208 0.831055 11.00000 0.13080 0.11576 = 0.08458 -0.02612 0.06635 -0.04187 AFIX 23 H13A 2 0.463585 0.615047 0.820320 11.00000 -1.20000 H13B 2 0.572278 0.505046 0.873931 11.00000 -1.20000 AFIX 0 C14 1 0.371970 0.457398 0.878977 11.00000 0.11695 0.16679 = 0.07800 -0.02136 0.05787 -0.04296 AFIX 137 H14A 2 0.283279 0.450848 0.835525 11.00000 -1.50000 H14B 2 0.361434 0.521057 0.929073 11.00000 -1.50000 H14C 2 0.399152 0.363683 0.903766 11.00000 -1.50000 AFIX 0 HKLF 4 REM bv1_auto_a.res in P2(1)/c REM R1 = 0.0560 for 2107 Fo > 4sig(Fo) and 0.0628 for all 2492 data REM 164 parameters refined using 0 restraints END WGHT 0.0899 0.3573 REM Highest difference peak 0.295, deepest hole -0.273, 1-sigma level 0.040 Q1 1 0.6460 0.3035 0.6093 11.00000 0.05 0.30 Q2 1 0.4296 0.3698 0.7044 11.00000 0.05 0.29 Q3 1 0.5447 0.6002 0.8596 11.00000 0.05 0.27 Q4 1 0.6752 0.5979 0.7219 11.00000 0.05 0.21 Q5 1 0.8723 0.5706 0.4240 11.00000 0.05 0.21 Q6 1 0.2995 0.3771 0.8430 11.00000 0.05 0.21 Q7 1 0.8048 0.5450 0.4648 11.00000 0.05 0.14 Q8 1 0.5590 0.3771 0.8638 11.00000 0.05 0.13 Q9 1 0.9315 0.8210 0.3998 11.00000 0.05 0.13 Q10 1 0.4975 0.6138 0.6423 11.00000 0.05 0.13 Q11 1 0.3258 0.5651 0.8425 11.00000 0.05 0.13 Q12 1 0.3641 0.4769 0.9396 11.00000 0.05 0.12 Q13 1 0.4093 0.5703 0.7092 11.00000 0.05 0.12 ; _shelx_res_checksum 72228 _shelxl_version_number .2013 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 O O1 0.8531(2) 0.18982(18) 0.34863(13) 0.0878(6) Uani d 1 . . O O2 0.89842(16) 0.42028(16) 0.33853(10) 0.0657(4) Uani d 1 . . O O3 0.73548(14) 0.51487(15) 0.57413(9) 0.0611(4) Uani d 1 . . O O4 0.5562(2) 0.3555(2) 0.56376(12) 0.0961(7) Uani d 1 . . C C1 0.78028(18) 0.4741(2) 0.49394(12) 0.0521(4) Uani d 1 . . C C2 0.7829(2) 0.3396(2) 0.46205(14) 0.0601(5) Uani d 1 . . H H2 0.7447 0.2654 0.4923 0.072 Uiso calc 1 . . C C3 0.8442(2) 0.3080(2) 0.38166(15) 0.0637(5) Uani d 1 . . C C4 0.89359(19) 0.5596(2) 0.36974(13) 0.0552(5) Uani d 1 . . C C5 0.9492(2) 0.6653(3) 0.32029(15) 0.0686(6) Uani d 1 . . H H5 0.9891 0.6417 0.2689 0.082 Uiso calc 1 . . C C6 0.9443(3) 0.8055(3) 0.34855(18) 0.0770(7) Uani d 1 . . H H6 0.9807 0.8776 0.3155 0.092 Uiso calc 1 . . C C7 0.8862(3) 0.8417(2) 0.42546(19) 0.0769(6) Uani d 1 . . H H7 0.8837 0.9373 0.4439 0.092 Uiso calc 1 . . C C8 0.8321(2) 0.7356(2) 0.47459(15) 0.0640(5) Uani d 1 . . H H8 0.7930 0.7600 0.5263 0.077 Uiso calc 1 . . C C9 0.83527(18) 0.5928(2) 0.44771(13) 0.0514(4) Uani d 1 . . C C10 0.6263(2) 0.4471(2) 0.60627(13) 0.0588(5) Uani d 1 . . C C11 0.6104(3) 0.5117(3) 0.69639(16) 0.0763(7) Uani d 1 . . H H11A 0.5905 0.6134 0.6862 0.092 Uiso calc 1 . . H H11B 0.7010 0.5039 0.7392 0.092 Uiso calc 1 . . C C12 0.4994(3) 0.4499(3) 0.74266(16) 0.0776(7) Uani d 1 . . H H12A 0.4091 0.4569 0.6995 0.093 Uiso calc 1 . . H H12B 0.5199 0.3484 0.7531 0.093 Uiso calc 1 . . C C13 0.4818(4) 0.5132(4) 0.8311(2) 0.1043(11) Uani d 1 . . H H13A 0.4636 0.6150 0.8203 0.125 Uiso calc 1 . . H H13B 0.5723 0.5050 0.8739 0.125 Uiso calc 1 . . C C14 0.3720(4) 0.4574(4) 0.8790(2) 0.1154(12) Uani d 1 . . H H14A 0.2833 0.4508 0.8355 0.173 Uiso calc 1 . . H H14B 0.3614 0.5211 0.9291 0.173 Uiso calc 1 . . H H14C 0.3992 0.3637 0.9038 0.173 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 0.1124(13) 0.0674(10) 0.0945(12) -0.0079(9) 0.0470(10) -0.0231(9) O2 0.0772(9) 0.0669(9) 0.0606(8) -0.0033(7) 0.0327(7) -0.0066(6) O3 0.0666(8) 0.0655(9) 0.0593(8) -0.0121(6) 0.0321(6) -0.0060(6) O4 0.0994(12) 0.1166(15) 0.0855(11) -0.0483(11) 0.0512(10) -0.0319(10) C1 0.0498(8) 0.0594(11) 0.0511(9) -0.0023(7) 0.0197(7) 0.0002(8) C2 0.0676(11) 0.0539(11) 0.0645(11) -0.0058(9) 0.0274(9) 0.0005(9) C3 0.0685(11) 0.0610(12) 0.0661(12) -0.0034(9) 0.0237(9) -0.0052(9) C4 0.0546(9) 0.0614(11) 0.0523(9) 0.0002(8) 0.0174(7) 0.0041(8) C5 0.0726(12) 0.0783(14) 0.0605(11) -0.0048(10) 0.0269(10) 0.0116(10) C6 0.0829(15) 0.0721(15) 0.0812(15) -0.0046(11) 0.0286(12) 0.0243(12) C7 0.0876(15) 0.0513(12) 0.0967(17) -0.0010(10) 0.0302(13) 0.0088(11) C8 0.0666(11) 0.0582(12) 0.0728(12) 0.0017(9) 0.0276(10) 0.0010(10) C9 0.0479(8) 0.0549(11) 0.0545(9) 0.0003(7) 0.0175(7) 0.0036(8) C10 0.0585(10) 0.0657(12) 0.0568(10) -0.0064(9) 0.0224(8) 0.0035(9) C11 0.0903(15) 0.0834(16) 0.0652(12) -0.0196(12) 0.0402(11) -0.0079(11) C12 0.0740(13) 0.1044(18) 0.0614(12) -0.0191(13) 0.0304(10) -0.0062(12) C13 0.131(2) 0.116(2) 0.0846(17) -0.0419(19) 0.0664(17) -0.0261(16) C14 0.117(2) 0.167(3) 0.0780(17) -0.043(2) 0.0579(17) -0.0214(19) 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 . . 121.71(15) ? C1 O3 C10 . . 122.95(15) ? C2 C1 O3 . . 125.75(17) ? C2 C1 C9 . . 121.34(17) ? O3 C1 C9 . . 112.80(16) ? C1 C2 C3 . . 120.85(18) ? C1 C2 H2 . . 119.6 ? C3 C2 H2 . . 119.6 ? O1 C3 O2 . . 116.60(19) ? O1 C3 C2 . . 125.5(2) ? O2 C3 C2 . . 117.86(18) ? O2 C4 C5 . . 117.11(17) ? O2 C4 C9 . . 121.44(17) ? C5 C4 C9 . . 121.45(19) ? C6 C5 C4 . . 118.7(2) ? C6 C5 H5 . . 120.6 ? C4 C5 H5 . . 120.6 ? C5 C6 C7 . . 121.1(2) ? C5 C6 H6 . . 119.5 ? C7 C6 H6 . . 119.5 ? C8 C7 C6 . . 119.8(2) ? C8 C7 H7 . . 120.1 ? C6 C7 H7 . . 120.1 ? C7 C8 C9 . . 120.5(2) ? C7 C8 H8 . . 119.7 ? C9 C8 H8 . . 119.7 ? C8 C9 C4 . . 118.44(17) ? C8 C9 C1 . . 124.78(17) ? C4 C9 C1 . . 116.78(17) ? O4 C10 O3 . . 122.85(18) ? O4 C10 C11 . . 127.85(18) ? O3 C10 C11 . . 109.25(17) ? C10 C11 C12 . . 116.9(2) ? C10 C11 H11A . . 108.1 ? C12 C11 H11A . . 108.1 ? C10 C11 H11B . . 108.1 ? C12 C11 H11B . . 108.1 ? H11A C11 H11B . . 107.3 ? C13 C12 C11 . . 117.4(2) ? C13 C12 H12A . . 107.9 ? C11 C12 H12A . . 107.9 ? C13 C12 H12B . . 107.9 ? C11 C12 H12B . . 107.9 ? H12A C12 H12B . . 107.2 ? C12 C13 C14 . . 119.6(3) ? C12 C13 H13A . . 107.4 ? C14 C13 H13A . . 107.4 ? C12 C13 H13B . . 107.4 ? C14 C13 H13B . . 107.4 ? H13A C13 H13B . . 107.0 ? C13 C14 H14A . . 109.5 ? C13 C14 H14B . . 109.5 ? H14A C14 H14B . . 109.5 ? C13 C14 H14C . . 109.5 ? H14A C14 H14C . . 109.5 ? H14B C14 H14C . . 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 . 1.209(3) ? O2 C3 . 1.371(2) ? O2 C4 . 1.377(2) ? O3 C1 . 1.373(2) ? O3 C10 . 1.377(2) ? O4 C10 . 1.184(3) ? C1 C2 . 1.336(3) ? C1 C9 . 1.443(2) ? C2 C3 . 1.437(3) ? C2 H2 . 0.9300 ? C4 C5 . 1.384(3) ? C4 C9 . 1.393(3) ? C5 C6 . 1.370(3) ? C5 H5 . 0.9300 ? C6 C7 . 1.384(4) ? C6 H6 . 0.9300 ? C7 C8 . 1.376(3) ? C7 H7 . 0.9300 ? C8 C9 . 1.387(3) ? C8 H8 . 0.9300 ? C10 C11 . 1.478(3) ? C11 C12 . 1.479(3) ? C11 H11A . 0.9700 ? C11 H11B . 0.9700 ? C12 C13 . 1.455(3) ? C12 H12A . 0.9700 ? C12 H12B . 0.9700 ? C13 C14 . 1.464(3) ? C13 H13A . 0.9700 ? C13 H13B . 0.9700 ? C14 H14A . 0.9600 ? C14 H14B . 0.9600 ? C14 H14C . 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 2.40 2.855(3) 110.1 C5 H5 O1 2_755 0.93 2.53 3.387(3) 153.3 C11 H11B O1 4_566 0.97 2.65 3.446(3) 139.4 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 . . . . -34.4(3) ? C10 O3 C1 C9 . . . . 149.38(17) ? O3 C1 C2 C3 . . . . -174.29(19) ? C9 C1 C2 C3 . . . . 1.6(3) ? C4 O2 C3 O1 . . . . 179.69(19) ? C4 O2 C3 C2 . . . . -0.8(3) ? C1 C2 C3 O1 . . . . 178.9(2) ? C1 C2 C3 O2 . . . . -0.5(3) ? C3 O2 C4 C5 . . . . -178.94(18) ? C3 O2 C4 C9 . . . . 1.1(3) ? O2 C4 C5 C6 . . . . 179.07(19) ? C9 C4 C5 C6 . . . . -0.9(3) ? C4 C5 C6 C7 . . . . 0.5(4) ? C5 C6 C7 C8 . . . . -0.1(4) ? C6 C7 C8 C9 . . . . 0.0(4) ? C7 C8 C9 C4 . . . . -0.4(3) ? C7 C8 C9 C1 . . . . -179.4(2) ? O2 C4 C9 C8 . . . . -179.15(17) ? C5 C4 C9 C8 . . . . 0.9(3) ? O2 C4 C9 C1 . . . . 0.0(3) ? C5 C4 C9 C1 . . . . 179.97(17) ? C2 C1 C9 C8 . . . . 177.8(2) ? O3 C1 C9 C8 . . . . -5.9(3) ? C2 C1 C9 C4 . . . . -1.3(3) ? O3 C1 C9 C4 . . . . 175.07(16) ? C1 O3 C10 O4 . . . . -5.5(3) ? C1 O3 C10 C11 . . . . 176.86(19) ? O4 C10 C11 C12 . . . . 3.8(4) ? O3 C10 C11 C12 . . . . -178.7(2) ? C10 C11 C12 C13 . . . . -179.5(3) ? C11 C12 C13 C14 . . . . 179.1(3) ?