#------------------------------------------------------------------------------ #$Date: 2019-10-09 07:03:03 +0300 (Wed, 09 Oct 2019) $ #$Revision: 219178 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021794.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_2021794 loop_ _publ_author_name 'Shorunov, Sergey V.' 'Bermeshev, Maxim V.' 'Demchuk, Dmitry V.' 'Nelyubina, Yulia V.' _publ_section_title ; Synthesis and structure of 2,4,6-tricyclobutyl-1,3,5-trioxane ; _journal_coeditor_code KQ2025 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_page_first 1578 _journal_paper_doi 10.1107/S205698901900896X _journal_volume 75 _journal_year 2019 _chemical_formula_iupac 'C15 H24 O3' _chemical_formula_moiety 'C15 H24 O3' _chemical_formula_sum 'C15 H24 O3' _chemical_formula_weight 252.34 _chemical_name_systematic ; 2,4,6-Tricyclobutyl-1,3,5-trioxane ; _space_group_crystal_system hexagonal _space_group_IT_number 185 _space_group_name_Hall 'P 6c -2' _space_group_name_H-M_alt 'P 63 c m' _symmetry_space_group_name_Hall 'P 6c -2' _symmetry_space_group_name_H-M 'P 63 c m' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/6 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 2 _cell_length_a 9.9966(12) _cell_length_b 9.9966(12) _cell_length_c 7.9461(10) _cell_measurement_reflns_used 7859 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 30 _cell_measurement_theta_min 3 _cell_volume 687.68(15) _computing_cell_refinement ; SAINT (Bruker, 2008) ; _computing_data_collection ; APEX2 (Bruker, 2008) ; _computing_data_reduction ; SAINT (Bruker, 2008) ; _computing_molecular_graphics ; SHELXL2014/6 (Sheldrick, 2015b) ; _computing_publication_material ; SHELXL2014/6 (Sheldrick, 2015b) ; _computing_structure_refinement ; SHELXL2014/6 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEXII DUO CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_unetI/netI 0.0113 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 7859 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.961 _diffrn_reflns_theta_min 2.353 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.7005 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2008) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.219 _exptl_crystal_description prism _exptl_crystal_F_000 276 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.363 _refine_diff_density_min -0.223 _refine_ls_abs_structure_details 'Refined as an inversion twin' _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 35 _refine_ls_number_reflns 671 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0406 _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^)+(0.0819P)^2^+0.1148P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1070 _refine_ls_wR_factor_ref 0.1083 _reflns_number_gt 645 _reflns_number_total 671 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file kq2025sup1.cif _cod_data_source_block Trioxane _cod_original_cell_volume 687.68(19) _cod_database_code 2021794 _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 0.976 _shelx_estimated_absorpt_t_max 0.984 _shelx_hkl_file ; 0 1 0 717.83 10.50 -1 0 0 733.33 10.50 0 -1 0 729.33 10.80 0 1 0 774.62 10.60 1 -1 0 744.33 10.50 0 1 0 760.22 10.70 1 0 0 756.02 10.70 -1 1 0 749.13 10.00 -1 1 0 739.83 10.70 -1 0 0 707.73 10.50 1 -2 0 21.70 0.60 2 -1 0 21.90 0.60 -2 1 0 21.80 0.50 -1 2 0 22.60 0.50 1 1 0 22.50 0.70 -1 -1 0 23.00 0.60 -2 1 0 22.10 0.70 -1 -1 0 21.50 0.50 -1 2 0 22.40 0.60 -2 0 0 680.03 9.70 0 2 0 671.03 10.10 0 2 0 670.73 9.20 -2 0 0 665.03 9.10 2 -2 0 674.03 9.60 2 -2 0 678.93 9.90 2 -2 0 681.03 9.80 2 0 0 679.43 10.10 -2 2 0 676.13 9.30 0 -2 0 684.13 9.60 -2 3 0 0.60 0.10 -2 3 0 0.40 0.10 -1 -2 0 1.00 0.10 -3 1 0 0.40 0.20 3 -1 0 0.20 0.10 2 -3 0 0.40 0.20 -1 -2 0 0.50 0.10 1 2 0 0.30 0.20 -3 1 0 0.90 0.20 2 1 0 1.60 0.30 -2 -1 0 0.40 0.10 3 -2 0 0.40 0.10 -3 2 0 0.20 0.20 1 -3 0 0.50 0.10 -3 2 0 0.30 0.10 -1 3 0 0.50 0.10 -1 3 0 0.30 0.10 -2 -1 0 0.50 0.10 -3 3 0 58.89 1.30 3 0 0 59.99 1.60 0 3 0 59.69 1.50 3 -3 0 61.59 1.00 0 3 0 56.09 1.30 0 -3 0 58.39 1.20 -3 0 0 58.19 1.20 -3 0 0 58.69 1.40 3 -3 0 57.79 1.50 -4 1 0 357.16 5.80 -3 4 0 354.06 5.10 -4 1 0 350.36 5.20 3 -4 0 352.66 5.90 1 3 0 355.16 6.10 -1 -3 0 357.36 5.20 4 -1 0 344.97 5.90 -3 4 0 338.37 5.40 -1 -3 0 343.57 5.30 -2 4 0 236.98 3.90 2 2 0 241.08 4.60 -4 2 0 238.28 4.30 4 -2 0 234.48 4.00 -2 -2 0 240.48 3.70 -4 2 0 244.38 3.80 -2 4 0 237.08 3.90 -2 -2 0 242.08 3.70 2 -4 0 238.28 4.10 3 1 0 352.06 6.20 1 -4 0 349.87 5.50 -1 4 0 350.96 5.80 -1 4 0 343.67 5.40 -3 -1 0 354.76 5.20 4 -3 0 356.86 5.40 -4 3 0 358.26 5.40 -3 -1 0 357.16 5.50 -4 4 0 112.99 2.30 -4 0 0 115.79 2.10 0 4 0 113.09 2.60 4 -4 0 116.89 1.80 4 0 0 110.29 2.70 0 4 0 112.49 2.30 0 -4 0 113.09 2.10 4 -4 0 114.39 2.60 -4 0 0 116.69 2.40 1 4 0 -0.10 0.20 -4 5 0 0.30 0.10 -1 -4 0 -0.10 0.10 -4 5 0 0.10 0.20 -5 1 0 -0.10 0.10 4 -5 0 0.20 0.20 -1 -4 0 -0.30 0.10 5 -1 0 0.30 0.20 -5 1 0 0.30 0.20 5 -2 0 533.65 8.70 -3 5 0 528.65 8.20 -5 2 0 556.44 8.00 3 -5 0 539.95 8.60 2 3 0 539.15 9.20 -2 -3 0 549.74 8.00 -2 -3 0 555.74 8.00 -3 5 0 550.94 8.10 -5 2 0 546.65 8.80 -3 -2 0 550.24 8.10 -2 5 0 536.95 8.40 -2 5 0 553.94 8.20 3 2 0 532.75 9.20 -3 -2 0 547.85 7.90 5 -3 0 540.85 8.30 -5 3 0 533.95 8.80 2 -5 0 533.65 8.40 -5 3 0 549.15 8.00 -1 5 0 0.30 0.20 1 -5 0 0.30 0.20 5 -4 0 0.10 0.20 4 1 0 0.20 0.20 -4 -1 0 0.30 0.20 -5 4 0 0.00 0.20 -1 5 0 0.00 0.20 -4 -1 0 0.00 0.10 5 -4 0 0.20 0.10 -5 5 0 112.39 2.50 0 5 0 108.99 2.40 0 5 0 111.99 2.80 5 0 0 108.99 2.80 5 -5 0 107.09 2.80 -5 0 0 110.59 2.50 -5 0 0 116.39 2.20 5 -5 0 110.39 1.80 0 -5 0 109.19 2.10 5 -6 0 31.80 0.70 -1 -5 0 33.70 1.20 -6 1 0 32.40 1.10 -5 6 0 30.20 1.20 6 -1 0 31.50 1.40 -6 1 0 30.30 1.30 -1 -5 0 32.00 0.90 5 -6 0 32.50 1.40 1 5 0 29.00 1.40 2 4 0 41.60 1.70 6 -2 0 43.40 1.50 -2 -4 0 43.50 1.30 -4 6 0 42.90 1.50 -6 2 0 42.50 1.30 -6 2 0 45.50 1.60 -4 6 0 42.80 0.90 4 -6 0 43.30 1.60 -2 -4 0 44.60 1.10 -3 -3 0 482.35 7.20 6 -3 0 466.45 7.70 -3 -3 0 484.75 7.20 -6 3 0 468.45 8.20 -3 6 0 476.55 7.50 -6 3 0 494.35 7.40 3 -6 0 474.25 7.80 -3 6 0 478.25 7.40 3 3 0 467.25 8.50 2 -6 0 43.80 1.40 -6 4 0 43.80 1.40 6 -4 0 42.70 1.20 -2 6 0 43.70 1.40 -4 -2 0 45.00 1.30 -4 -2 0 45.60 1.20 -2 6 0 43.80 1.40 6 -4 0 43.60 1.70 4 2 0 44.90 1.80 5 1 0 32.20 1.50 -5 -1 0 28.60 1.10 -5 -1 0 31.60 1.00 1 -6 0 29.10 1.00 -6 5 0 29.70 1.20 6 -5 0 30.40 0.80 -1 6 0 30.00 1.20 -1 6 0 30.90 1.30 6 -5 0 30.90 1.40 6 -6 0 287.57 5.80 0 6 0 300.67 5.80 -6 0 0 300.57 4.90 6 0 0 287.77 5.90 0 6 0 295.97 5.10 0 -6 0 292.47 4.90 -6 0 0 301.47 5.40 -6 6 0 299.27 5.30 -1 -6 0 110.29 2.20 -7 1 0 102.99 2.80 -6 7 0 108.29 2.70 7 -1 0 100.19 3.00 1 6 0 102.49 3.10 -7 1 0 104.89 2.40 6 -7 0 103.29 2.90 -1 -6 0 106.69 2.50 -5 7 0 23.70 0.60 -5 7 0 23.90 1.20 5 -7 0 25.80 1.30 -2 -5 0 24.60 0.80 7 -2 0 26.30 1.30 -7 2 0 24.30 1.00 -7 2 0 24.40 1.30 2 5 0 22.80 1.40 -2 -5 0 27.30 1.10 4 -7 0 17.20 1.00 -7 3 0 17.60 1.10 -4 7 0 19.40 0.70 -7 3 0 18.30 0.90 -3 -4 0 19.10 0.90 3 4 0 19.00 1.30 -4 7 0 18.80 1.00 -3 -4 0 18.10 0.70 7 -3 0 17.30 1.00 -3 7 0 19.40 1.00 -7 4 0 19.00 1.00 3 -7 0 17.30 0.90 -3 7 0 18.90 0.80 -4 -3 0 18.40 0.80 7 -4 0 18.60 0.90 -4 -3 0 18.70 0.90 4 3 0 17.00 1.20 -5 -2 0 25.40 1.00 -2 7 0 27.10 1.10 7 -5 0 25.20 1.40 -5 -2 0 24.30 1.00 5 2 0 24.40 1.50 -7 5 0 22.50 1.10 7 -5 0 24.60 0.90 2 -7 0 23.70 1.00 -2 7 0 26.60 1.20 7 -6 0 106.49 3.10 1 -7 0 107.79 2.40 -7 6 0 107.59 2.70 -1 7 0 106.39 2.60 -6 -1 0 108.19 2.40 6 1 0 105.79 3.20 -1 7 0 105.29 2.80 -6 -1 0 104.79 2.60 7 0 0 962.60 16.00 0 7 0 944.21 15.60 0 7 0 971.30 14.20 -7 7 0 969.70 14.50 7 -7 0 948.61 15.50 -7 0 0 971.90 15.00 0 -7 0 959.70 14.20 -7 0 0 993.00 13.90 -1 -7 0 107.19 2.70 -1 -7 0 101.49 2.20 7 -8 0 102.49 3.10 -7 8 0 100.19 2.80 1 7 0 102.19 3.20 -8 1 0 102.39 2.50 8 -1 0 100.49 3.20 -8 1 0 103.29 2.90 -8 2 0 54.69 1.70 2 6 0 58.29 2.40 8 -2 0 53.49 2.10 -2 -6 0 55.19 1.80 -2 -6 0 53.29 1.40 -6 8 0 55.99 2.00 -8 2 0 54.19 2.10 6 -8 0 57.19 2.10 -8 3 0 2.60 0.50 3 5 0 2.80 0.70 -3 -5 0 3.20 0.50 -5 8 0 2.80 0.60 8 -3 0 2.70 0.50 -5 8 0 3.20 0.30 -3 -5 0 4.00 0.40 -8 3 0 2.60 0.60 5 -8 0 3.00 0.60 -4 -4 0 70.59 1.90 -4 8 0 69.69 1.70 4 -8 0 67.29 2.10 4 4 0 65.89 2.60 -4 -4 0 73.69 1.70 8 -4 0 69.59 2.00 -4 8 0 66.49 2.10 -8 4 0 69.79 2.00 3 -8 0 2.30 0.50 5 3 0 3.50 0.70 -8 5 0 2.30 0.50 -3 8 0 3.40 0.50 -5 -3 0 2.40 0.40 -3 8 0 3.10 0.60 -5 -3 0 2.50 0.40 8 -5 0 3.00 0.60 8 -5 0 2.70 0.40 -2 8 0 54.49 1.80 8 -6 0 54.39 2.20 -2 8 0 54.49 1.90 6 2 0 57.39 2.40 -6 -2 0 54.19 1.60 -8 6 0 55.19 1.90 8 -6 0 59.39 1.80 2 -8 0 55.49 1.70 -6 -2 0 53.99 1.70 -7 -1 0 98.99 2.70 -8 7 0 101.79 2.80 1 -8 0 99.39 2.30 -7 -1 0 102.99 2.40 7 1 0 103.79 3.40 -1 8 0 100.19 2.90 -1 8 0 102.09 2.70 8 -7 0 98.59 3.20 0 -8 0 286.37 5.00 8 -8 0 284.57 6.20 -8 8 0 288.67 5.70 -8 0 0 290.57 5.10 -8 0 0 285.17 5.70 8 0 0 285.07 6.40 0 8 0 288.67 6.10 -8 9 0 4.90 0.80 1 8 0 3.90 0.80 9 -1 0 4.00 0.90 8 -9 0 3.50 0.80 -9 1 0 4.70 0.80 -1 -8 0 4.90 0.70 -9 1 0 5.50 0.70 -2 -7 0 14.20 1.00 -9 2 0 16.60 1.20 2 7 0 14.00 1.30 -2 -7 0 14.30 1.10 -7 9 0 15.90 1.20 -9 2 0 14.20 1.00 7 -9 0 13.80 1.20 9 -2 0 16.20 1.30 3 6 0 8.10 1.10 -6 9 0 8.80 1.00 -3 -6 0 7.50 0.60 -9 3 0 7.40 1.00 -3 -6 0 6.60 0.80 -9 3 0 6.90 0.80 6 -9 0 8.40 1.00 9 -3 0 8.50 1.00 -4 -5 0 146.59 3.20 -4 -5 0 142.59 2.80 9 -4 0 138.49 3.90 9 -4 0 139.59 3.40 4 5 0 134.99 4.20 -5 9 0 141.29 3.50 -9 4 0 142.89 3.30 5 -9 0 143.69 3.60 -5 9 0 143.09 2.60 -9 5 0 145.39 3.40 5 4 0 148.49 4.30 -4 9 0 140.09 3.50 -5 -4 0 145.49 3.10 9 -5 0 139.19 3.10 4 -9 0 136.39 3.40 9 -5 0 139.09 3.90 -5 -4 0 142.09 2.90 -4 9 0 141.39 2.90 -3 9 0 7.40 0.70 9 -6 0 5.30 0.90 -9 6 0 6.70 0.80 3 -9 0 7.80 0.70 -6 -3 0 8.50 0.80 6 3 0 6.70 1.00 -6 -3 0 6.80 0.60 -3 9 0 8.00 0.90 2 -9 0 14.40 0.90 -2 9 0 14.10 1.10 -2 9 0 14.90 1.00 -7 -2 0 15.70 1.00 7 2 0 13.60 1.40 -7 -2 0 16.00 1.00 -9 7 0 15.10 1.10 9 -7 0 15.40 1.40 -8 -1 0 5.90 0.80 9 -8 0 5.30 0.90 8 1 0 7.40 1.10 -8 -1 0 4.30 0.60 -9 8 0 3.00 0.60 1 -9 0 4.50 0.60 -1 9 0 4.10 0.70 -1 9 0 4.30 0.70 -9 0 0 88.59 2.80 0 9 0 95.19 3.10 -9 9 0 89.29 2.90 0 -9 0 87.59 2.70 -9 0 0 87.79 2.50 9 0 0 95.59 3.40 9 -9 0 85.39 3.20 -9 10 0 3.90 0.80 1 9 0 3.10 0.80 -10 1 0 3.80 0.70 10 -1 0 3.40 0.90 9 -10 0 4.90 0.90 -10 1 0 4.10 0.80 -1 -9 0 3.60 0.70 -2 -8 0 14.70 1.10 2 8 0 11.70 1.30 8 -10 0 10.70 1.20 10 -2 0 13.40 1.30 -8 10 0 13.10 1.20 -10 2 0 11.20 1.00 -10 2 0 10.40 1.20 3 7 0 0.10 0.50 -3 -7 0 0.70 0.40 -7 10 0 -0.30 0.40 10 -3 0 0.40 0.50 -10 3 0 1.10 0.50 7 -10 0 0.20 0.40 6 -10 0 15.50 1.20 -4 -6 0 16.10 1.10 10 -4 0 15.70 1.20 4 6 0 16.30 1.50 10 -4 0 14.80 1.30 -10 4 0 16.60 1.10 -6 10 0 16.40 1.20 -5 10 0 56.09 2.20 -5 -5 0 50.49 1.80 5 -10 0 54.29 2.10 -10 5 0 51.29 2.00 5 5 0 53.99 2.70 10 -5 0 51.59 2.40 4 -10 0 14.70 1.10 -4 10 0 17.50 1.30 -6 -4 0 17.20 1.10 6 4 0 16.00 1.50 -10 6 0 15.90 1.20 -4 10 0 17.50 1.00 10 -6 0 19.70 1.60 -10 7 0 0.70 0.50 10 -7 0 0.50 0.50 7 3 0 0.10 0.60 -3 10 0 0.40 0.40 -7 -3 0 0.10 0.30 3 -10 0 0.20 0.30 -3 10 0 0.20 0.40 -2 10 0 12.90 1.10 10 -8 0 11.60 1.40 8 2 0 10.50 1.40 -8 -2 0 15.10 1.60 -2 10 0 11.80 1.10 -8 -2 0 10.10 0.90 2 -10 0 12.00 0.90 -10 8 0 11.70 1.20 -1 10 0 3.70 0.80 -10 9 0 4.50 0.90 10 -9 0 4.90 1.00 9 1 0 3.30 0.90 -1 10 0 3.90 0.80 -9 -1 0 4.30 0.80 -9 -1 0 4.90 0.70 0 10 0 17.30 1.50 10 0 0 15.70 1.60 10 -10 0 16.40 1.60 -10 0 0 18.40 1.40 -10 10 0 16.10 1.40 0 -10 0 16.60 1.30 -10 0 0 16.10 1.20 1 10 0 16.20 1.60 11 -1 0 18.90 1.70 -1 -10 0 17.60 1.40 10 -11 0 17.30 1.60 -10 11 0 17.90 1.50 -11 1 0 18.20 1.30 -2 -9 0 49.30 2.10 11 -2 0 50.69 2.50 -11 2 0 52.09 2.00 -9 11 0 53.49 2.40 2 9 0 49.00 2.60 11 -2 0 51.49 2.40 9 -11 0 50.49 2.50 -11 3 0 0.80 0.50 11 -3 0 -0.60 0.50 11 -3 0 -0.30 0.50 -3 -8 0 -0.20 0.40 -8 11 0 0.40 0.50 8 -11 0 0.00 0.50 3 8 0 0.20 0.60 -7 11 0 9.10 1.20 -11 4 0 10.10 1.10 -4 -7 0 9.40 1.00 7 -11 0 11.30 1.30 4 7 0 9.60 1.40 11 -4 0 12.10 1.20 11 -4 0 9.00 1.20 11 -5 0 0.20 0.60 6 -11 0 0.70 0.50 -11 5 0 -0.20 0.40 5 6 0 0.20 0.60 -5 -6 0 -0.40 0.40 -6 11 0 0.30 0.50 -6 -5 0 0.60 0.40 11 -6 0 0.60 0.60 6 5 0 0.90 0.60 5 -11 0 -0.10 0.40 -5 11 0 0.80 0.50 -11 6 0 -0.30 0.40 4 -11 0 10.60 1.00 11 -7 0 10.40 1.40 -11 7 0 9.20 1.10 -7 -4 0 9.80 1.00 7 4 0 10.50 1.40 -4 11 0 8.90 1.10 -3 11 0 0.00 0.40 8 3 0 0.00 0.60 11 -8 0 0.50 0.70 -3 11 0 0.20 0.50 3 -11 0 0.10 0.40 -8 -3 0 0.00 0.40 -11 8 0 0.80 0.50 -9 -2 0 53.49 1.90 -2 11 0 52.39 2.10 9 2 0 48.80 2.80 -11 9 0 54.59 2.40 11 -9 0 50.59 2.60 -2 11 0 50.79 2.20 -10 -1 0 17.90 1.30 10 1 0 16.40 1.80 -11 10 0 17.80 1.50 -1 11 0 20.10 1.50 11 -10 0 19.20 1.80 1 -11 0 20.10 1.50 -11 0 0 4.50 0.80 0 -11 0 5.30 1.00 11 -11 0 5.20 1.20 11 0 0 5.60 1.20 -11 11 0 4.00 0.90 0 11 0 4.00 1.00 -11 12 0 0.70 0.70 12 -1 0 0.40 0.70 -1 -11 0 1.10 0.70 -12 1 0 -0.20 0.50 1 11 0 0.70 0.70 11 -12 0 -0.60 0.70 12 -2 0 3.80 1.00 -2 -10 0 3.60 0.80 12 -2 0 2.40 0.90 10 -12 0 3.10 1.00 2 10 0 4.70 1.10 -12 2 0 3.10 0.80 -10 12 0 4.80 1.00 12 -3 0 51.09 2.50 9 -12 0 52.39 2.60 -9 12 0 56.89 2.60 -3 -9 0 52.69 2.20 3 9 0 48.70 2.80 12 -3 0 55.19 2.70 -12 3 0 54.29 2.20 12 -4 0 13.90 1.60 -4 -8 0 12.20 1.20 8 -12 0 13.20 1.50 4 8 0 15.30 1.80 -8 12 0 12.50 1.40 -12 4 0 14.50 1.20 -12 5 0 28.30 1.60 5 7 0 32.80 2.30 -7 12 0 29.20 1.80 -5 -7 0 28.60 1.60 7 -12 0 28.80 1.80 12 -5 0 29.60 2.00 6 6 0 2.70 0.90 12 -6 0 5.10 1.10 -6 12 0 5.20 1.00 6 -12 0 4.40 0.90 -6 -6 0 3.90 0.80 -12 6 0 5.50 0.90 5 -12 0 30.80 1.70 7 5 0 29.40 2.30 -12 7 0 30.30 1.80 12 -7 0 31.20 2.10 -7 -5 0 29.50 1.50 -5 12 0 28.00 1.80 -8 -4 0 13.80 1.10 4 -12 0 12.90 1.10 -12 8 0 15.80 1.50 -4 12 0 14.40 1.50 12 -8 0 14.80 1.80 8 4 0 15.00 1.90 -12 9 0 53.09 2.40 12 -9 0 55.09 2.90 -3 12 0 51.79 2.40 -9 -3 0 53.39 2.00 9 3 0 48.00 2.90 12 -10 0 4.10 1.10 10 2 0 4.60 1.20 -10 -2 0 4.20 0.80 -2 12 0 3.80 0.80 -12 10 0 4.40 1.00 12 -11 0 0.10 0.70 -1 12 0 0.20 0.60 1 -12 0 1.00 0.70 -11 -1 0 0.20 0.60 -12 11 0 0.20 0.60 11 1 0 1.20 0.90 -12 0 0 0.60 0.60 0 -12 0 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5.20 0.90 -1 -5 -9 4.70 0.80 5 -6 -9 4.80 1.00 1 5 -9 5.90 1.20 -1 -5 9 4.40 1.00 6 -1 9 3.20 0.80 -5 6 9 5.60 1.10 -6 1 9 5.50 1.20 5 -6 9 6.10 1.10 1 5 9 4.70 0.90 6 -2 -9 11.80 1.60 -2 -4 -9 14.60 1.20 4 -6 -9 15.50 1.40 -6 2 -9 16.00 1.30 2 4 -9 17.20 2.00 4 -6 9 14.00 1.60 -2 -4 9 15.00 1.70 2 4 9 17.50 1.50 -4 6 9 13.80 1.50 6 -2 9 15.90 1.30 -6 2 9 15.10 1.80 3 3 -9 19.80 1.90 6 -3 -9 19.10 1.70 -3 -3 -9 20.30 1.40 -3 6 -9 16.70 1.50 -6 3 -9 18.90 1.40 -3 6 9 20.20 1.70 6 -3 9 18.60 1.40 -3 -3 9 19.00 1.80 -6 3 9 17.80 1.90 3 3 9 22.30 1.70 6 -3 9 21.90 1.60 3 -6 9 19.00 1.80 4 2 -9 15.80 1.90 -2 6 -9 16.20 1.50 6 -4 -9 15.50 1.70 -6 4 -9 14.50 1.20 -4 -2 -9 15.60 1.20 -4 -2 9 12.50 1.50 4 2 9 12.80 1.30 6 -4 9 16.20 1.50 -6 4 9 12.60 1.60 -2 6 9 15.10 1.60 2 -6 9 12.20 1.50 1 -6 -9 4.90 0.80 6 -5 -9 6.30 1.10 -6 5 -9 6.20 0.90 5 1 -9 8.30 1.50 -1 6 -9 6.50 1.20 -5 -1 -9 5.40 0.90 6 -5 9 7.80 1.20 -5 -1 9 5.70 1.10 -1 6 9 5.30 1.00 -6 5 9 5.30 1.10 1 -6 9 3.40 1.00 5 1 9 4.30 0.90 -6 6 -9 0.50 0.50 0 6 -9 0.30 0.60 0 -6 -9 0.40 0.50 6 -6 -9 0.30 0.50 -6 0 -9 -0.20 0.50 6 0 -9 0.20 0.70 -6 6 9 -1.00 0.60 6 0 9 0.10 0.60 0 -6 9 -0.10 0.70 6 -6 9 0.40 0.70 0 6 9 -0.10 0.60 -6 0 9 0.50 0.80 -1 -6 -9 5.60 0.90 6 -7 -9 5.10 1.00 7 -1 -9 6.40 1.40 1 6 -9 7.00 1.40 -7 1 -9 5.80 1.00 -6 7 -9 4.40 1.00 -6 7 9 4.30 1.10 6 -7 9 4.60 1.10 7 -1 9 4.50 0.90 -7 1 9 4.60 1.20 1 6 9 6.00 1.00 -1 -6 9 3.60 1.00 5 -7 -9 2.80 0.80 -2 -5 -9 1.10 0.60 -7 2 -9 2.30 0.70 7 -2 -9 2.70 0.90 2 5 -9 2.40 1.00 5 -7 9 0.30 0.70 7 -2 9 2.30 0.70 -5 7 9 1.80 0.80 -2 -5 9 1.90 0.90 -7 2 9 1.50 0.90 2 5 9 2.20 0.80 -7 3 -9 1.80 0.70 7 -3 -9 2.50 0.90 -3 -4 -9 2.00 0.70 3 4 -9 1.90 1.00 3 4 9 1.90 0.80 -7 3 9 1.10 0.90 4 -7 9 1.50 0.90 -3 -4 9 2.50 0.90 -4 7 9 1.60 0.80 4 3 -9 2.40 1.00 7 -4 -9 1.60 0.80 -7 4 -9 2.90 0.70 -4 -3 -9 0.80 0.50 7 -4 9 1.70 0.80 3 -7 9 2.40 1.00 -3 7 9 2.30 0.80 -7 4 9 1.50 0.90 4 3 9 2.40 0.80 -4 -3 9 3.00 1.00 -5 -2 -9 1.30 0.60 7 -5 -9 2.10 0.80 2 -7 -9 2.30 0.80 -2 7 -9 2.30 0.80 5 2 -9 1.60 0.90 -7 5 -9 2.60 0.70 2 -7 9 2.00 0.90 5 2 9 2.10 0.80 7 -5 9 3.50 0.90 -7 5 9 2.40 1.00 -5 -2 9 2.30 0.90 -2 7 9 3.40 0.90 -6 -1 -9 5.70 1.00 7 -6 -9 3.00 0.80 -1 7 -9 5.90 1.20 6 1 -9 6.90 1.50 1 -7 -9 5.40 0.90 -7 6 -9 6.10 1.00 6 1 9 5.10 1.00 -1 7 9 4.70 1.00 1 -7 9 4.70 1.10 -6 -1 9 4.10 1.10 7 -6 9 5.60 1.10 -7 6 9 5.20 1.30 0 7 -9 0.50 0.70 7 0 -9 0.60 0.80 0 -7 -9 -0.60 0.50 7 -7 -9 0.40 0.50 -7 0 -9 -0.40 0.50 -7 7 -9 0.00 0.50 -7 7 9 0.40 0.80 7 0 9 0.20 0.60 0 -7 9 -1.80 0.60 -7 0 9 -1.40 0.70 7 -7 9 -0.50 0.70 0 7 9 0.40 0.60 -8 2 -9 2.20 0.80 -2 -6 -9 2.50 0.80 2 6 -9 4.50 1.30 6 -8 -9 2.50 0.80 8 -2 -9 2.00 0.90 6 -8 9 3.00 1.00 -8 2 9 1.90 1.00 2 6 9 2.50 0.90 -2 -6 9 0.90 0.90 -3 -5 -9 1.90 0.60 8 -3 -9 1.50 0.80 3 5 -9 0.60 0.80 -8 3 -9 1.60 0.70 -8 3 9 0.50 0.90 5 -8 9 2.00 0.90 3 5 9 2.00 0.90 -3 -5 9 1.10 0.90 -8 4 -9 5.90 1.00 -4 -4 -9 6.60 1.00 8 -4 -9 6.20 1.30 4 4 -9 5.40 1.40 -4 8 9 6.10 1.20 4 -8 9 3.40 1.10 -8 4 9 7.70 1.50 -4 -4 9 5.00 1.20 4 4 9 5.10 1.10 -8 5 -9 1.50 0.70 8 -5 -9 0.90 0.70 -5 -3 -9 1.70 0.70 5 3 -9 0.70 0.90 -3 8 9 1.90 0.80 8 -5 9 0.50 0.80 -5 -3 9 1.90 1.00 3 -8 9 -0.30 0.80 -8 5 9 1.60 1.00 5 3 9 1.70 0.80 6 2 -9 2.50 1.10 2 -8 -9 1.60 0.70 8 -6 -9 3.00 0.90 -6 -2 -9 2.20 0.70 -8 6 -9 2.60 0.80 -2 8 9 2.30 0.90 2 -8 9 2.40 0.90 -8 6 9 2.00 1.00 8 -6 9 2.80 1.00 -6 -2 9 2.40 1.00 6 2 9 0.60 0.70 0 0 -10 28.60 1.80 0 0 10 29.70 1.90 0 1 -10 8.30 1.20 1 0 -10 10.30 1.30 -1 0 -10 9.50 1.20 1 -1 -10 9.80 1.30 0 -1 -10 9.20 1.20 -1 1 -10 12.60 1.20 1 -1 10 8.10 1.20 -1 1 10 11.50 1.40 1 0 10 10.00 1.20 0 -1 10 10.40 1.30 -1 0 10 10.10 1.30 0 1 10 8.60 1.20 -1 2 -10 0.80 0.50 1 1 -10 1.50 0.70 -2 1 -10 0.80 0.50 1 -2 -10 0.20 0.50 2 -1 -10 1.40 0.70 -2 1 10 2.00 0.80 -1 2 10 1.30 0.70 1 -2 10 0.80 0.70 1 1 10 0.80 0.70 -1 -1 10 2.40 0.90 2 -1 10 0.80 0.70 2 -2 -10 7.30 1.10 2 0 -10 6.10 1.20 -2 2 -10 4.90 0.90 0 2 -10 7.10 1.20 0 -2 10 6.10 1.10 -2 0 10 6.50 1.20 -2 2 10 7.90 1.20 0 2 10 7.50 1.10 2 -2 10 6.10 1.10 2 0 10 5.90 1.00 1 2 -10 3.00 0.90 2 -3 -10 1.20 0.60 3 -1 -10 2.20 0.80 -3 1 -10 1.40 0.60 -2 3 -10 1.50 0.60 2 -3 10 0.20 0.70 -2 3 10 1.80 0.80 -3 1 10 0.50 0.70 -1 -2 10 1.20 0.70 1 2 10 1.30 0.80 3 -1 10 1.90 0.70 -3 2 -10 1.70 0.60 -1 3 -10 2.40 0.70 2 1 -10 2.20 0.80 3 -2 -10 2.10 0.70 -1 3 10 1.80 0.80 2 1 10 0.80 0.70 3 -2 10 -0.40 0.70 1 -3 10 2.20 0.90 -2 -1 10 0.70 0.80 -3 2 10 2.40 0.80 0 3 -10 4.70 1.00 3 0 -10 4.90 1.10 -3 3 -10 4.30 0.80 3 -3 -10 5.10 1.00 0 -3 10 2.70 0.90 0 3 10 5.70 1.10 -3 0 10 5.30 1.20 -3 3 10 6.40 1.10 3 0 10 4.70 0.90 3 -3 10 3.60 0.90 1 3 -10 3.00 0.90 -4 1 -10 2.10 0.80 3 -4 -10 4.00 0.90 4 -1 -10 3.40 1.00 -3 4 -10 1.80 0.70 3 -4 10 2.70 0.90 -4 1 10 2.60 0.90 4 -1 10 2.50 0.80 -3 4 10 3.00 0.90 1 3 10 1.90 0.80 -1 -3 10 4.30 1.10 2 -4 -10 4.90 1.00 4 -2 -10 4.80 1.00 -4 2 -10 4.90 0.90 -2 4 -10 3.70 0.90 2 2 -10 3.60 1.00 2 2 10 4.20 1.00 -4 2 10 4.10 1.10 2 -4 10 3.80 1.00 -2 -2 10 3.30 1.00 4 -2 10 3.30 0.90 4 -3 -10 1.30 0.70 -1 4 -10 2.70 0.80 -3 -1 -10 1.80 0.70 3 1 -10 3.90 1.10 -4 3 -10 2.10 0.60 1 -4 10 0.80 0.90 -1 4 10 3.10 0.90 -4 3 10 4.00 1.00 3 1 10 1.80 0.80 4 -3 10 1.10 0.70 -3 -1 10 3.50 1.00 0 4 -10 2.80 0.90 -4 4 -10 5.40 0.90 4 0 -10 3.40 1.00 4 -4 -10 4.60 1.00 -4 0 -10 4.30 0.80 4 0 10 1.80 0.80 0 -4 10 3.90 1.10 4 -4 10 3.70 1.00 0 4 10 3.80 0.90 -4 4 10 4.10 1.00 -4 0 10 3.10 1.00 4 -5 -10 2.80 0.90 -5 1 -10 2.80 0.70 5 -1 -10 4.70 1.30 1 4 -10 3.20 1.00 1 4 10 2.90 0.90 -1 -4 10 2.80 1.00 4 -5 10 3.30 1.00 -4 5 10 3.80 1.00 5 -1 10 2.80 0.80 -5 1 10 4.20 1.10 -2 -3 -10 2.40 0.70 2 3 -10 3.00 1.00 3 -5 -10 2.70 0.80 -5 2 -10 3.60 0.80 -3 5 -10 3.20 0.80 5 -2 -10 1.60 0.90 3 -5 10 3.20 1.00 2 3 10 3.90 1.00 -5 2 10 3.00 1.00 -2 -3 10 3.40 1.10 -3 -2 -10 2.50 0.70 -5 3 -10 2.00 0.60 3 2 -10 0.90 0.80 -2 5 -10 3.10 0.90 5 -3 -10 3.00 0.90 2 -5 10 3.90 1.10 -2 5 10 2.40 0.90 -5 3 10 2.60 0.90 -3 -2 10 3.10 1.00 5 -3 10 3.10 0.90 3 2 10 3.20 0.90 4 1 -10 4.10 1.20 -4 -1 -10 1.60 0.60 -1 5 -10 4.70 1.10 5 -4 -10 2.50 0.90 1 -5 10 2.20 1.00 -5 4 10 3.40 1.00 -4 -1 10 3.00 1.10 4 1 10 2.20 0.80 5 -4 10 3.00 0.90 -1 5 10 3.90 1.00 0 5 -10 2.00 0.90 5 -5 -10 2.60 0.80 5 0 -10 5.20 1.30 -5 0 -10 2.70 0.70 5 -5 10 3.10 1.00 -5 0 10 1.30 0.90 -5 5 10 3.10 1.10 0 -5 10 1.90 0.90 0 5 10 3.40 1.00 5 0 10 1.70 0.80 -6 1 -10 0.70 0.60 -1 -5 -10 1.10 0.60 5 -6 -10 1.50 0.70 1 5 -10 1.00 0.80 6 -1 -10 0.80 0.80 1 5 10 -0.40 0.70 -6 1 10 1.60 1.00 5 -6 10 0.70 0.90 -5 6 10 0.30 0.80 -1 -5 10 0.30 0.90 6 -1 10 0.60 0.70 4 -6 -10 13.60 1.60 2 4 -10 14.20 1.90 -6 2 -10 13.50 1.40 -2 -4 -10 12.80 1.20 6 -2 -10 16.80 2.10 -2 -4 10 12.50 1.70 -6 2 10 14.80 1.80 4 -6 10 13.70 1.60 2 4 10 11.40 1.40 6 -2 10 17.00 1.50 3 3 -10 4.70 1.30 6 -3 -10 3.80 1.10 -6 3 -10 5.70 1.00 -3 -3 -10 5.00 0.90 -3 -3 10 5.20 1.20 3 -6 10 4.10 1.10 -3 6 10 3.60 0.90 -6 3 10 2.60 1.00 3 3 10 4.50 1.00 -6 4 -10 14.00 1.50 4 2 -10 16.00 2.10 6 -4 -10 15.00 1.90 -2 6 -10 13.20 1.70 -4 -2 -10 11.50 1.20 2 -6 10 16.10 1.70 4 2 10 12.10 1.40 -2 6 10 11.20 1.40 -6 4 10 11.80 1.70 -4 -2 10 10.80 1.60 6 -4 10 13.00 1.50 5 1 -10 1.70 0.90 -5 -1 -10 1.20 0.60 6 -5 -10 0.60 0.70 -1 6 -10 1.10 0.80 -1 6 10 -0.30 0.60 1 -6 10 0.80 0.80 6 -5 10 0.90 0.80 -6 5 10 0.40 0.90 -5 -1 10 1.00 0.80 5 1 10 0.70 0.70 0 0 -11 -0.40 0.50 0 0 11 -0.20 0.70 0 1 -11 -0.10 0.50 -1 1 -11 -0.10 0.50 1 0 -11 0.50 0.60 0 -1 -11 0.20 0.50 -1 0 -11 -0.20 0.50 1 -1 -11 -0.30 0.50 1 0 11 -0.90 0.60 0 -1 11 0.00 0.80 0 1 11 0.30 0.70 1 -1 11 0.30 0.80 -1 1 11 0.40 0.70 -1 0 11 -0.40 0.70 1 -2 -11 8.80 1.30 2 -1 -11 9.40 1.50 1 1 -11 9.80 1.50 -1 2 -11 8.60 1.30 -1 -1 -11 8.30 1.30 -2 1 -11 9.30 1.30 -1 2 11 5.90 1.20 -1 -1 11 9.60 1.40 -2 1 11 10.10 1.40 2 -1 11 8.60 1.30 1 -2 11 8.50 1.40 2 -2 -11 0.10 0.60 -2 0 -11 0.20 0.50 2 0 -11 -0.50 0.50 0 2 -11 0.00 0.60 -2 2 -11 0.10 0.50 0 -2 -11 -0.30 0.50 0 -2 11 -0.40 0.70 2 -2 11 0.00 0.80 -2 2 11 -0.30 0.70 -2 0 11 0.50 0.80 2 -3 -11 2.80 0.90 -2 3 -11 3.60 0.90 3 -1 -11 2.80 1.00 1 2 -11 2.80 1.00 -3 1 11 2.00 1.00 2 -3 11 2.30 1.00 -2 3 11 2.60 1.00 -1 -2 11 0.30 0.90 2 1 -11 2.30 0.90 -3 2 -11 1.90 0.70 -1 3 -11 3.90 1.00 1 -3 -11 2.70 0.90 3 -2 -11 2.80 1.00 -3 2 11 1.90 0.90 3 -2 11 1.60 0.90 1 -3 11 1.20 0.90 -2 -1 11 3.60 1.10 ; _shelx_hkl_checksum 89775 _shelx_res_file ; TITL a_a.res in P6(3)cm CELL 0.71073 9.9966 9.9966 7.9461 90.000 90.000 120.000 ZERR 2.000 0.0012 0.0012 0.0010 0.000 0.000 0.000 LATT -1 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SYMM -X, -Y, 1/2+Z SYMM Y, -X+Y, 1/2+Z SYMM X-Y, X, 1/2+Z SYMM -Y, -X, 1/2+Z SYMM -X+Y, Y, 1/2+Z SYMM X, X-Y, 1/2+Z SYMM Y, X, Z SYMM X-Y, -Y, Z SYMM -X, -X+Y, Z SFAC C H O UNIT 30 48 6 TEMP -153.000 size 0.20 0.25 0.30 L.S. 10 acta BOND $H htab conf omit -4 58 FMAP 2 PLAN 20 WGHT 0.081900 0.114800 FVAR 0.63200 O1 3 0.000000 0.134667 0.477370 10.50000 0.01007 0.01218 = 0.01699 0.00171 0.00000 0.00503 C1 1 0.134824 0.134824 0.535092 10.50000 0.01126 0.01126 = 0.01353 -0.00162 -0.00162 0.00566 AFIX 13 H1A 2 0.138407 0.138407 0.660859 10.50000 -1.20000 AFIX 0 C2 1 0.274517 0.274517 0.464533 10.50000 0.01232 0.01232 = 0.01928 0.00024 0.00024 0.00557 AFIX 13 H2A 2 0.271606 0.271605 0.338739 10.50000 -1.20000 AFIX 0 C3 1 0.435218 0.310602 0.528115 11.00000 0.01184 0.01416 = 0.03387 -0.00080 -0.00216 0.00684 AFIX 23 H3A 2 0.493819 0.285175 0.446226 11.00000 -1.20000 H3B 2 0.433425 0.266688 0.640319 11.00000 -1.20000 AFIX 0 C4 1 0.483872 0.483872 0.531863 10.50000 0.01236 0.01236 = 0.03035 -0.00143 -0.00143 0.00437 AFIX 23 H4A 2 0.542047 0.542046 0.431036 10.50000 -1.20000 H4B 2 0.537662 0.537662 0.636473 10.50000 -1.20000 AFIX 0 HKLF 4 REM a_a.res in P6(3)cm REM R1 = 0.0406 for 645 Fo > 4sig(Fo) and 0.0417 for all 671 data REM 34 parameters refined using 0 restraints END WGHT 0.0749 0.0983 REM Instructions for potential hydrogen bonds EQIV $1 y, -x+y, z+1/2 HTAB C1 O1_$1 REM Highest difference peak 0.363, deepest hole -0.223, 1-sigma level 0.054 Q1 1 0.0000 0.1401 0.5893 10.50000 0.05 0.36 Q2 1 0.0000 0.1289 0.3552 10.50000 0.05 0.21 Q3 1 0.2735 0.2735 0.6018 10.50000 0.05 0.21 Q4 1 0.2124 0.2124 0.5036 10.50000 0.05 0.20 Q5 1 0.4772 0.4317 0.5280 11.00000 0.05 0.19 Q6 1 0.3577 0.2774 0.5026 11.00000 0.05 0.17 Q7 1 0.1552 0.1552 0.4121 10.50000 0.05 0.16 Q8 1 0.0699 0.1332 0.5075 11.00000 0.05 0.14 Q9 1 0.7034 0.7034 0.4147 10.50000 0.05 0.13 Q10 1 0.4175 0.2845 0.3918 11.00000 0.05 0.13 Q11 1 0.2341 0.2341 0.8119 10.50000 0.05 0.10 Q12 1 0.4803 0.2696 0.5195 11.00000 0.05 0.10 Q13 1 0.5382 0.5382 0.5035 10.50000 0.05 0.10 Q14 1 0.5577 0.5577 0.3520 10.50000 0.05 0.10 Q15 1 0.4011 0.2980 0.6947 11.00000 0.05 0.09 Q16 1 0.1381 0.0000 0.7107 10.50000 0.05 0.09 Q17 1 0.2494 0.1939 0.2712 11.00000 0.05 0.09 Q18 1 0.5425 0.2990 0.2993 11.00000 0.05 0.09 Q19 1 0.1090 0.1801 0.7627 11.00000 0.05 0.08 Q20 1 0.3168 0.2544 0.7035 11.00000 0.05 0.08 ; _shelx_res_checksum 95057 _shelxl_version_number 2014/6 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'y, x, z' 'x-y, -y, z' '-x, -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 O O1 0.0000 0.13467(13) 0.4774(2) 0.0133(4) Uani d 1 C C1 0.13482(17) 0.13482(17) 0.5351(3) 0.0120(5) Uani d 1 H H1A 0.1384 0.1384 0.6609 0.014 Uiso calc 1 C C2 0.2745(2) 0.2745(2) 0.4645(3) 0.0149(4) Uani d 1 H H2A 0.2716 0.2716 0.3387 0.018 Uiso calc 1 C C3 0.43522(17) 0.31060(18) 0.5281(3) 0.0198(4) Uani d 1 H H3A 0.4938 0.2852 0.4462 0.024 Uiso calc 1 H H3B 0.4334 0.2667 0.6403 0.024 Uiso calc 1 C C4 0.4839(2) 0.4839(2) 0.5319(4) 0.0192(5) Uani d 1 H H4A 0.5420 0.5420 0.4310 0.023 Uiso calc 1 H H4B 0.5377 0.5377 0.6365 0.023 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 0.0101(7) 0.0122(6) 0.0170(7) 0.0050(3) 0.000 0.0017(5) C1 0.0113(7) 0.0113(7) 0.0135(9) 0.0057(6) -0.0016(7) -0.0016(7) C2 0.0123(7) 0.0123(7) 0.0193(8) 0.0056(7) 0.0002(7) 0.0002(7) C3 0.0118(6) 0.0142(7) 0.0339(8) 0.0068(6) -0.0022(7) -0.0008(8) C4 0.0124(7) 0.0124(7) 0.0304(9) 0.0044(7) -0.0014(10) -0.0014(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 C1 O1 C1 . 2 110.23(18) y O1 C1 O1 3 . 110.03(17) y O1 C1 C2 3 . 108.66(11) ? O1 C1 C2 . . 108.66(11) ? O1 C1 H1A 3 . 109.8 ? O1 C1 H1A . . 109.8 ? C2 C1 H1A . . 109.8 ? C1 C2 C3 . . 117.97(13) ? C1 C2 C3 . 10 117.97(13) ? C3 C2 C3 . 10 88.59(16) y C1 C2 H2A . . 110.2 ? C3 C2 H2A . . 110.2 ? C3 C2 H2A 10 . 110.2 ? C2 C3 C4 . . 88.62(11) y C2 C3 H3A . . 113.9 ? C4 C3 H3A . . 113.9 ? C2 C3 H3B . . 113.9 ? C4 C3 H3B . . 113.9 ? H3A C3 H3B . . 111.1 ? C3 C4 C3 . 10 88.39(15) ? C3 C4 H4A . . 113.9 ? C3 C4 H4A 10 . 113.9 ? C3 C4 H4B . . 113.9 ? C3 C4 H4B 10 . 113.9 ? H4A C4 H4B . . 111.1 ? 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 C1 . 1.4229(13) y O1 C1 2 1.4230(13) ? C1 O1 3 1.4229(13) n C1 C2 . 1.505(3) y C1 H1A . 1.0000 ? C2 C3 . 1.545(2) y C2 C3 10 1.545(2) ? C2 H2A . 1.0000 ? C3 C4 . 1.548(2) y C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C4 C3 10 1.548(2) ? C4 H4A . 0.9900 ? C4 H4B . 0.9900 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C1 H1A O1 5 1.00 2.52 3.514(3) 177.1 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_4 _geom_torsion C1 O1 C1 O1 2 3 58.4(3) C1 O1 C1 C2 2 . 177.20(10) O1 C1 C2 C3 3 . -67.9(2) O1 C1 C2 C3 . . 172.39(15) O1 C1 C2 C3 3 10 -172.39(15) O1 C1 C2 C3 . 10 67.9(2) C1 C2 C3 C4 . . -139.29(18) C3 C2 C3 C4 10 . -18.09(19) C2 C3 C4 C3 . 10 18.05(19)