#------------------------------------------------------------------------------ #$Date: 2024-05-18 04:51:48 +0300 (Sat, 18 May 2024) $ #$Revision: 291951 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023131.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_2023131 loop_ _publ_author_name 'Sadikhova, Nurlana D.' 'Akkurt, Mehmet' 'Ismayilov, Valeh M.' 'Yusubov, Niftali N.' 'Hasanov, Khudayar I.' 'Bhattarai, Ajaya' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of 3,3′-[ethane-1,2-diylbis(oxy)]bis(5,5-dimethylcyclohex-2-en-1-one) including an unknown solvate ; _journal_coeditor_code NX2010 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989024004286 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C18 H26 O4' _chemical_formula_moiety 'C18 H26 O4' _chemical_formula_sum 'C18 H26 O4' _chemical_formula_weight 306.39 _chemical_name_systematic ; 3,3'-[Ethane-1,2-diylbis(oxy)]bis(5,5-dimethylcyclohex-2-en-1-one) ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2019/3 _cell_angle_alpha 90 _cell_angle_beta 111.822(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.9184(13) _cell_length_b 6.5230(5) _cell_length_c 17.2645(11) _cell_measurement_reflns_used 2235 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.71 _cell_measurement_theta_min 2.54 _cell_volume 1768.8(2) _computing_cell_refinement ; SAINT (Bruker, 2018) ; _computing_data_collection ; APEX4 (Bruker, 2018) ; _computing_data_reduction ; SAINT (Bruker, 2018) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_unetI/netI 0.0380 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 10346 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.910 _diffrn_reflns_theta_min 2.542 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_correction_T_min 0.966 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.151 _exptl_crystal_description prism _exptl_crystal_F_000 664 _exptl_crystal_size_max 0.330 _exptl_crystal_size_mid 0.290 _exptl_crystal_size_min 0.180 _refine_diff_density_max 0.263 _refine_diff_density_min -0.200 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 102 _refine_ls_number_reflns 2111 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0452 _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^)+(0.0456P)^2^+1.1303P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1066 _refine_ls_wR_factor_ref 0.1180 _reflns_number_gt 1559 _reflns_number_total 2111 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file nx2010.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2023131 _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 0.974 _shelx_estimated_absorpt_t_max 0.986 _shelx_hkl_file ; 2 0 0 358.66 16.00 -2 0 0 361.56 16.00 -2 0 0 368.16 16.00 -4 0 0 6.60 1.40 4 0 0 8.00 1.50 -4 0 0 5.00 1.10 4 0 0 7.20 1.30 6 0 0 2392.66 103.89 -6 0 0 2456.55 103.99 6 0 0 2372.96 103.99 -6 0 0 2346.37 103.89 -8 0 0 242.58 12.20 8 0 0 248.08 12.20 -8 0 0 243.58 12.20 8 0 0 247.08 12.30 -10 0 0 6.40 2.10 10 0 0 8.80 2.40 -12 0 0 123.79 7.50 12 0 0 117.39 7.90 -14 0 0 220.58 12.60 14 0 0 227.68 13.00 16 0 0 50.09 6.20 -16 0 0 50.19 6.00 18 0 0 4.10 3.80 -18 0 0 2.10 3.00 20 0 0 1.90 4.00 -20 0 0 7.70 4.00 -1 -1 0 469.95 21.20 1 -1 0 469.45 21.20 1 -1 0 497.55 21.20 -1 -1 0 477.65 20.90 -1 -1 0 478.25 21.10 1 -1 0 507.35 21.30 1 -1 0 476.55 21.30 1 1 0 469.85 20.90 -1 1 0 494.65 21.20 1 1 0 476.65 21.10 -1 1 0 472.55 21.20 -1 1 0 501.75 21.30 3 -1 0 2030.30 87.59 3 -1 0 2060.99 87.49 -3 -1 0 1882.51 87.59 -3 -1 0 2016.10 87.39 -3 -1 0 2026.70 87.59 3 -1 0 2061.49 87.59 3 1 0 2126.99 87.69 -3 1 0 1978.30 87.49 3 1 0 1994.80 87.59 3 1 0 2066.19 87.39 -3 1 0 2002.20 87.59 5 -1 0 215.78 10.20 5 -1 0 210.48 10.40 -5 -1 0 202.28 10.30 5 -1 0 203.08 10.30 -5 -1 0 203.58 10.30 5 1 0 219.28 10.40 -5 1 0 219.98 10.50 -5 1 0 221.28 10.30 5 1 0 225.78 10.40 5 1 0 221.38 10.10 -7 -1 0 86.49 5.00 7 -1 0 90.19 5.10 7 -1 0 79.19 5.10 -7 -1 0 65.29 4.60 -7 1 0 89.99 5.20 7 1 0 75.19 4.80 -7 1 0 59.89 4.70 7 1 0 77.69 4.80 -9 -1 0 167.08 9.60 9 -1 0 197.38 10.10 -9 1 0 187.68 10.00 -11 -1 0 18.70 3.00 11 -1 0 19.40 3.30 11 1 0 22.00 3.40 -11 1 0 18.30 3.20 -13 -1 0 35.80 4.40 13 -1 0 33.80 4.60 13 -1 0 43.50 4.30 13 1 0 33.20 4.60 -13 1 0 43.70 4.80 15 -1 0 88.29 6.10 15 -1 0 100.39 7.50 -15 -1 0 73.19 7.10 -15 1 0 75.29 7.30 15 1 0 73.89 6.80 15 1 0 88.69 7.30 -17 -1 0 43.50 5.70 17 -1 0 46.10 6.30 17 -1 0 39.00 4.70 17 1 0 44.80 5.50 -17 1 0 38.10 5.60 17 1 0 41.30 5.90 19 -1 0 -2.20 3.20 -19 -1 0 2.20 3.50 -19 1 0 6.20 3.80 19 1 0 -1.70 3.60 19 1 0 0.00 2.90 0 -2 0 1024.40 44.00 0 -2 0 984.70 44.00 0 -2 0 998.90 43.50 0 2 0 946.41 43.90 0 2 0 1002.80 44.00 0 2 0 1092.89 44.00 0 2 0 976.80 44.00 2 -2 0 1176.98 50.89 2 -2 0 1169.78 50.89 -2 -2 0 1165.78 50.69 -2 -2 0 1279.17 50.99 2 -2 0 1118.99 50.79 2 2 0 1203.48 50.89 2 2 0 1132.89 50.59 2 2 0 1159.18 50.19 -2 2 0 1039.30 50.69 -4 -2 0 457.15 20.10 4 -2 0 432.96 20.00 4 -2 0 424.46 20.00 -4 -2 0 435.96 20.00 -4 -2 0 442.46 19.70 4 -2 0 443.66 20.10 -4 2 0 444.96 20.00 4 2 0 428.56 20.10 4 2 0 438.46 19.50 -4 2 0 436.66 19.90 4 2 0 429.96 19.80 -6 -2 0 2134.39 95.19 6 -2 0 2202.78 95.19 6 -2 0 2169.18 95.29 6 -2 0 2274.17 95.49 -6 -2 0 2140.19 95.39 -6 2 0 2109.79 95.39 6 2 0 2132.89 95.19 6 2 0 2262.17 94.99 -6 2 0 2113.79 95.19 6 2 0 2303.87 95.49 8 -2 0 149.88 8.80 8 -2 0 157.48 8.50 -8 -2 0 172.08 8.80 -8 2 0 154.28 8.90 8 2 0 158.98 8.40 8 2 0 171.18 9.40 -10 -2 0 0.80 1.80 10 -2 0 3.10 1.70 10 -2 0 1.20 1.60 -10 2 0 2.10 2.00 10 2 0 0.00 1.50 10 2 0 -2.00 1.70 12 -2 0 144.89 8.50 12 -2 0 132.79 8.90 -12 -2 0 136.89 8.60 -12 2 0 143.59 9.00 12 2 0 137.39 8.20 12 2 0 147.89 9.10 14 -2 0 0.80 2.50 -14 -2 0 2.70 2.40 14 -2 0 6.60 2.60 -14 2 0 -2.10 2.30 14 2 0 1.00 2.50 14 2 0 1.20 2.00 16 -2 0 -4.20 2.60 -16 -2 0 3.90 2.90 16 -2 0 1.70 2.40 16 2 0 -0.10 2.60 -16 2 0 5.10 3.30 16 2 0 0.80 3.30 18 -2 0 59.49 7.20 -18 -2 0 52.29 6.50 18 -2 0 60.69 6.10 18 2 0 23.70 5.50 18 2 0 42.90 5.70 -18 2 0 62.69 7.10 -20 -2 0 4.50 4.10 20 -2 0 4.70 4.20 -20 2 0 -0.30 3.80 20 2 0 2.90 4.20 20 2 0 0.30 3.60 1 -3 0 132.59 6.90 1 -3 0 117.69 6.10 1 -3 0 109.79 6.70 -1 -3 0 121.89 5.90 1 -3 0 122.29 6.90 -1 -3 0 124.79 6.70 -1 -3 0 123.09 6.90 -1 3 0 111.69 6.60 1 3 0 130.99 6.80 -1 3 0 128.29 6.80 -1 3 0 124.99 6.90 -1 3 0 132.99 6.70 1 3 0 150.58 7.00 1 3 0 114.79 6.70 -3 -3 0 297.87 14.00 3 -3 0 261.67 13.80 -3 -3 0 288.07 13.60 3 3 0 291.87 13.00 3 3 0 289.17 13.90 -3 3 0 276.57 13.90 -3 3 0 307.67 14.00 -3 3 0 284.17 13.80 3 3 0 290.87 13.70 -5 -3 0 282.47 13.50 5 -3 0 244.98 13.70 -5 -3 0 285.37 13.90 5 -3 0 277.67 13.90 5 3 0 277.37 13.50 -5 3 0 264.67 13.60 5 3 0 283.27 13.00 5 3 0 289.67 14.00 -5 3 0 345.77 14.20 7 -3 0 169.28 9.80 -7 -3 0 168.58 9.60 7 -3 0 191.48 9.70 -7 -3 0 184.68 9.30 7 3 0 187.98 9.00 7 3 0 186.18 9.40 7 3 0 170.58 9.80 9 -3 0 92.59 6.20 9 -3 0 99.49 6.60 -9 -3 0 98.39 6.40 9 3 0 70.79 6.20 9 3 0 100.69 6.10 -11 -3 0 0.10 2.00 11 -3 0 -0.60 2.10 11 -3 0 0.80 2.00 11 3 0 -0.80 2.10 11 3 0 -1.40 1.60 13 -3 0 18.10 3.90 -13 -3 0 15.40 3.40 13 -3 0 23.20 3.60 13 3 0 11.50 2.90 13 3 0 25.90 4.40 15 -3 0 48.20 6.20 15 -3 0 36.20 4.80 -15 -3 0 43.20 5.70 15 3 0 42.40 4.90 15 3 0 32.20 5.40 17 -3 0 -2.20 2.40 17 -3 0 -2.30 3.00 -17 -3 0 -3.30 2.90 17 3 0 -4.80 2.40 17 3 0 3.00 3.80 19 -3 0 -1.50 3.60 19 -3 0 -2.00 2.90 -19 -3 0 -1.40 3.40 19 3 0 -1.10 3.60 0 -4 0 9.70 2.20 0 -4 0 9.70 1.40 0 4 0 14.60 2.30 0 4 0 15.70 2.50 0 4 0 8.70 2.00 2 -4 0 163.68 9.30 -2 -4 0 173.08 8.00 2 -4 0 169.58 8.40 -2 4 0 186.78 9.10 2 4 0 157.08 8.90 2 4 0 167.18 9.00 -2 4 0 162.78 9.10 2 4 0 162.48 9.00 4 -4 0 31.00 3.70 4 4 0 38.50 3.80 4 4 0 34.00 3.40 4 4 0 34.00 2.40 -4 4 0 26.40 3.30 -4 4 0 27.20 3.20 -6 -4 0 1.00 1.90 6 -4 0 4.60 2.10 6 4 0 -1.60 1.50 6 4 0 0.30 2.00 -6 4 0 0.60 1.90 6 4 0 2.30 1.20 8 -4 0 2.40 2.10 8 -4 0 0.40 1.90 -8 -4 0 -2.80 1.90 8 4 0 2.90 2.20 8 4 0 -3.20 1.60 -8 4 0 -0.60 1.70 8 4 0 0.00 1.40 10 -4 0 30.30 4.10 10 -4 0 39.00 4.80 -10 -4 0 29.70 4.30 10 4 0 34.10 3.90 10 4 0 25.70 4.20 12 -4 0 37.50 5.00 -12 -4 0 45.70 5.30 12 -4 0 57.19 6.30 12 4 0 39.80 5.30 12 4 0 47.60 4.80 14 -4 0 1.70 2.70 -14 -4 0 0.80 2.70 14 -4 0 -1.90 2.80 14 4 0 6.50 2.80 14 4 0 -1.50 3.10 16 -4 0 -2.10 3.20 -16 -4 0 -2.80 2.70 16 -4 0 7.90 3.60 16 4 0 2.30 3.00 16 4 0 -3.00 3.00 18 -4 0 2.50 3.50 -18 -4 0 -1.80 4.00 18 -4 0 -0.60 3.90 18 4 0 0.20 4.40 -1 -5 0 20.00 2.00 1 -5 0 27.20 2.50 1 -5 0 31.00 3.90 1 5 0 22.80 3.30 -1 5 0 29.70 3.80 1 5 0 24.70 3.40 3 -5 0 23.00 2.50 3 -5 0 21.20 3.40 3 5 0 21.90 3.30 -3 5 0 16.40 2.90 3 5 0 20.80 3.10 5 -5 0 2.10 2.10 -5 -5 0 -1.20 2.00 5 5 0 -0.80 1.00 -5 5 0 -0.90 1.70 5 5 0 -3.40 1.70 5 5 0 -1.00 1.70 7 -5 0 2.30 2.40 -7 -5 0 1.00 2.30 7 5 0 -0.10 2.30 -7 5 0 2.20 2.30 7 5 0 1.40 1.40 7 5 0 -1.30 1.70 -9 -5 0 14.50 3.40 9 -5 0 18.30 3.70 -9 5 0 19.10 3.50 9 5 0 14.50 3.10 9 5 0 17.20 3.60 11 -5 0 -1.00 2.70 -11 -5 0 2.60 3.00 11 5 0 2.20 2.40 11 5 0 2.40 3.10 -11 5 0 1.30 2.70 13 -5 0 1.10 3.00 13 -5 0 5.10 3.10 -13 -5 0 3.90 3.40 -13 5 0 3.30 3.00 13 5 0 2.40 3.10 13 5 0 1.60 2.50 15 -5 0 8.30 3.50 15 -5 0 10.10 4.30 -15 -5 0 13.80 4.30 15 5 0 13.70 4.90 -15 5 0 7.10 3.50 0 -6 0 0.10 1.10 0 6 0 -1.00 1.90 2 -6 0 116.09 8.20 2 -6 0 118.29 6.40 2 6 0 117.99 7.80 -2 6 0 110.09 7.50 2 6 0 107.29 7.40 4 -6 0 6.10 2.00 4 -6 0 5.30 2.80 4 6 0 2.00 2.50 4 6 0 3.40 2.50 -4 6 0 5.00 2.60 -6 -6 0 3.10 2.80 6 -6 0 10.40 3.20 6 6 0 4.80 2.90 6 6 0 1.40 2.50 -6 6 0 8.10 2.80 8 -6 0 33.70 5.10 -8 -6 0 34.60 5.10 -8 6 0 23.30 4.00 8 6 0 34.90 4.90 8 6 0 36.70 4.60 10 -6 0 2.70 3.10 -10 -6 0 3.20 3.10 -10 6 0 -0.80 2.20 10 6 0 2.20 2.40 10 6 0 1.70 3.10 -12 -6 0 6.20 4.00 12 -6 0 5.00 3.90 12 6 0 4.40 3.30 12 6 0 5.30 3.50 -12 6 0 6.20 3.30 14 -6 0 39.80 6.60 -14 -6 0 33.10 5.90 -14 6 0 27.50 5.10 14 6 0 31.40 6.00 1 7 0 1.50 2.60 -1 7 0 3.70 2.70 3 -7 0 2.90 3.00 3 7 0 -2.00 2.50 3 7 0 5.00 2.70 -3 7 0 0.10 2.30 -5 -7 0 0.80 3.00 5 -7 0 -1.10 2.80 -5 7 0 -0.80 2.50 5 7 0 2.10 2.90 5 7 0 2.70 2.90 7 -7 0 29.50 5.40 -7 -7 0 27.80 5.10 7 7 0 29.10 4.90 -7 7 0 24.90 4.30 7 7 0 31.50 4.60 9 -7 0 11.70 4.60 -9 -7 0 14.70 4.70 9 7 0 20.00 4.70 -9 7 0 17.30 4.10 9 7 0 16.20 4.00 11 -7 0 7.50 4.40 -11 -7 0 0.40 4.10 11 7 0 11.70 4.10 -11 7 0 8.40 3.70 0 8 0 7.10 3.30 2 8 0 1.40 2.80 -2 8 0 3.10 3.10 -4 -8 0 18.90 5.50 4 -8 0 15.20 4.60 -4 8 0 9.00 3.60 4 8 0 15.10 3.90 -6 -8 0 22.20 5.40 6 -8 0 9.90 4.60 6 8 0 18.60 4.10 6 8 0 17.70 4.50 -6 8 0 12.50 3.90 -20 0 1 -2.10 3.30 20 0 -1 -2.10 3.50 18 0 -1 0.80 3.20 -18 0 1 -2.80 2.70 -16 0 1 -2.40 2.30 16 0 -1 1.20 2.80 14 0 -1 -1.10 2.10 -14 0 1 -1.60 2.10 -12 0 1 -0.70 1.80 12 0 -1 -1.80 2.00 -10 0 1 0.60 1.50 10 0 -1 -0.30 1.30 -8 0 1 0.80 1.40 -8 0 1 0.70 1.40 8 0 -1 0.80 1.30 8 0 -1 -1.30 1.10 6 0 -1 -0.10 1.00 6 0 -1 -0.30 1.20 -6 0 1 -0.60 1.10 -6 0 1 -0.60 1.20 -4 0 1 0.20 0.90 4 0 -1 1.20 0.90 -4 0 1 -0.70 0.90 4 0 -1 2.00 0.90 2 0 -1 1.60 0.50 2 0 -1 1.10 0.40 -2 0 1 2.00 0.50 -2 0 1 1.10 0.40 0 0 -1 -0.20 0.10 0 0 1 0.40 0.20 0 0 1 0.00 0.10 0 0 -1 0.10 0.20 0 0 1 0.20 0.20 0 0 -1 0.00 0.20 0 0 1 0.00 0.20 0 0 -1 0.00 0.20 -2 0 -1 5.10 0.90 -2 0 -1 2.50 0.80 2 0 1 2.20 0.80 2 0 1 3.00 0.80 -4 0 -1 1.20 0.90 4 0 1 0.50 1.20 4 0 1 0.40 1.10 -4 0 -1 0.00 1.20 -6 0 -1 -1.20 1.20 6 0 1 -0.80 1.40 -6 0 -1 -0.20 1.40 6 0 1 1.60 1.40 8 0 1 2.70 1.70 -8 0 -1 1.80 1.70 10 0 1 1.50 2.00 -10 0 -1 0.60 1.90 -12 0 -1 1.50 2.00 12 0 1 -2.70 1.90 -14 0 -1 -0.90 2.30 14 0 1 2.20 2.80 16 0 1 -3.10 2.50 -16 0 -1 -1.40 2.60 -18 0 -1 -1.40 2.90 18 0 1 -4.00 3.00 -20 0 -1 0.80 3.50 20 0 1 -7.40 3.00 19 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45.30 6.40 4 6 -9 61.09 6.80 -2 -6 9 12.50 3.30 2 6 -9 16.60 4.30 2 6 -9 9.20 3.90 0 -6 -9 1.10 3.30 0 -6 9 1.00 2.60 0 6 -9 1.00 3.20 0 6 -9 3.30 3.40 2 -6 9 16.70 4.40 -2 -6 -9 17.10 4.90 2 -6 9 17.40 3.70 -2 6 -9 14.20 4.20 -4 -6 -9 20.80 4.60 4 -6 9 14.00 4.50 4 -6 9 20.40 4.60 -4 6 -9 10.90 4.10 -6 -6 -9 1.10 4.10 6 -6 9 1.30 3.10 6 -6 9 6.50 4.00 -6 6 -9 5.20 4.00 -8 -6 -9 1.00 3.30 8 -6 9 0.30 3.60 8 -6 9 1.60 3.80 -8 6 -9 -9.20 2.80 11 -7 -9 19.30 5.20 11 7 -9 11.30 4.80 11 7 -9 11.40 4.40 9 7 -9 73.79 8.40 9 7 -9 57.59 7.60 -7 -7 9 -0.20 2.60 7 7 -9 9.20 4.50 7 7 -9 9.40 4.40 -5 -7 9 -0.20 2.40 5 7 -9 -0.90 3.60 5 7 -9 -0.90 3.30 -3 -7 9 -5.10 2.70 3 7 -9 -5.10 3.10 3 7 -9 1.20 3.60 -1 -7 9 7.10 3.50 1 -7 -9 10.00 4.80 1 7 -9 10.40 4.30 1 7 -9 8.50 4.10 -1 -7 -9 11.20 4.70 1 -7 9 4.00 3.50 -1 7 -9 4.00 3.80 -3 -7 -9 1.20 4.40 3 -7 9 3.60 3.70 -3 7 -9 11.40 4.60 -5 -7 -9 9.10 5.20 5 -7 9 4.60 3.80 5 -7 9 5.00 4.50 -5 7 -9 6.00 4.30 22 0 -10 7.70 4.50 22 0 -10 6.00 4.30 20 0 -10 107.19 8.50 20 0 -10 76.19 8.50 18 0 -10 31.90 5.40 18 0 -10 27.00 4.80 16 0 -10 66.59 6.70 16 0 -10 64.39 6.40 -14 0 10 21.40 2.80 14 0 -10 13.20 3.40 14 0 -10 14.40 2.90 -12 0 10 84.79 4.80 12 0 -10 88.29 4.90 12 0 -10 72.99 6.00 12 0 -10 82.49 5.60 10 0 -10 34.90 2.60 10 0 -10 34.70 3.30 10 0 -10 31.10 3.90 8 0 -10 120.79 6.50 8 0 -10 116.39 7.20 -6 0 10 380.86 17.80 6 0 -10 362.06 17.70 6 0 -10 383.66 17.00 6 0 -10 364.66 17.00 4 0 -10 203.38 9.80 4 0 -10 195.48 10.20 -4 0 10 207.68 10.40 -4 0 10 198.08 10.10 -2 0 10 255.47 12.70 2 0 -10 251.07 12.40 -2 0 10 247.68 12.20 -2 0 10 268.77 12.50 2 0 -10 263.37 12.40 2 0 -10 249.97 12.00 0 0 -10 63.99 4.50 0 0 10 60.09 4.50 0 0 10 67.39 5.10 0 0 10 59.69 3.90 0 0 -10 59.09 4.10 0 0 -10 57.79 3.90 2 0 10 89.29 5.90 -2 0 -10 82.69 5.90 2 0 10 84.89 4.90 2 0 10 84.69 5.00 -4 0 -10 123.79 7.60 4 0 10 106.09 6.60 4 0 10 114.89 7.20 4 0 10 113.09 6.30 -6 0 -10 95.59 7.10 6 0 10 97.19 5.80 6 0 10 92.99 6.40 8 0 10 6.60 2.50 -8 0 -10 0.30 2.80 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1.80 5 1 -10 7.20 2.00 5 1 -10 11.70 2.00 5 1 -10 8.60 1.00 -5 1 10 9.60 1.90 3 -1 -10 0.30 1.00 3 -1 -10 0.60 1.40 -3 -1 10 1.80 1.70 -3 -1 10 0.10 1.00 3 -1 -10 1.00 0.60 3 -1 -10 -0.10 1.20 3 1 -10 0.10 1.30 3 1 -10 0.80 0.90 -3 1 10 -1.40 1.20 3 1 -10 -1.20 1.20 1 -1 -10 198.38 9.10 1 -1 -10 189.28 10.10 1 -1 -10 172.88 9.00 -1 -1 10 201.08 10.20 -1 -1 10 198.38 9.70 -1 1 10 190.78 9.80 1 1 -10 200.08 9.70 1 1 -10 181.98 9.90 -1 -1 -10 55.79 3.90 -1 -1 -10 54.29 5.00 1 -1 10 57.69 4.90 1 -1 10 61.49 4.20 -1 -1 -10 58.59 3.20 -1 1 -10 56.69 4.30 1 1 10 56.89 3.20 -1 1 -10 58.79 4.50 1 1 10 55.59 4.20 -3 -1 -10 86.59 6.60 3 -1 10 96.69 6.60 3 -1 10 98.99 6.10 3 1 10 95.09 6.00 3 1 10 96.69 5.10 -3 1 -10 99.09 5.00 -3 1 -10 100.09 6.50 3 1 10 91.89 4.70 -5 -1 -10 37.40 4.60 5 -1 10 37.90 4.20 -5 1 -10 32.90 4.20 5 1 10 37.60 3.50 5 1 10 32.00 2.40 7 -1 10 99.69 7.10 -7 -1 -10 104.49 7.90 7 1 10 91.39 6.60 -7 1 -10 119.99 8.00 9 -1 10 -2.40 2.30 -9 -1 -10 2.30 3.00 -9 1 -10 1.50 2.30 9 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-2 -2 10 4.20 1.50 2 -2 -10 4.40 1.00 -2 -2 10 6.20 1.90 -2 2 10 3.70 1.40 2 2 -10 1.80 1.90 2 2 -10 4.80 1.30 2 2 -10 2.50 1.80 0 -2 10 50.49 4.80 0 -2 -10 51.29 3.50 0 -2 10 55.79 4.40 0 -2 -10 52.89 5.10 0 -2 -10 50.09 3.50 0 -2 10 52.19 4.10 0 2 10 57.19 3.80 0 2 -10 50.39 3.90 0 2 -10 58.79 4.60 -2 -2 -10 6.70 2.60 2 -2 10 7.60 2.50 2 -2 10 9.40 2.60 2 2 10 7.70 1.80 -2 2 -10 9.70 2.40 -2 2 -10 10.40 2.30 -4 -2 -10 4.30 2.60 4 -2 10 14.90 3.20 4 -2 10 11.00 2.70 -4 2 -10 12.40 2.00 4 2 10 10.90 1.50 4 2 10 9.70 2.20 -4 2 -10 12.10 2.70 6 -2 10 13.20 3.10 -6 -2 -10 16.90 3.80 -6 2 -10 19.00 3.50 6 2 10 13.40 2.30 -8 -2 -10 141.49 9.80 8 -2 10 142.39 9.40 -8 2 -10 120.59 9.00 8 2 10 126.79 7.90 10 -2 10 10.00 3.50 -10 -2 -10 3.30 3.40 10 2 10 11.00 3.30 -10 2 -10 8.80 3.60 12 -2 10 5.80 3.60 -12 -2 -10 6.10 3.90 12 2 10 13.80 3.80 -12 2 -10 9.00 4.10 14 -2 10 8.30 4.10 -14 -2 -10 3.20 3.30 -14 2 -10 2.90 4.10 14 2 10 2.70 3.60 19 -3 -10 -0.70 3.10 19 -3 -10 2.90 3.10 19 3 -10 3.60 3.60 19 3 -10 1.70 3.70 17 -3 -10 21.60 4.20 17 -3 -10 17.50 4.30 17 3 -10 16.30 4.30 17 3 -10 23.40 4.80 15 -3 -10 24.40 4.40 15 -3 -10 21.90 3.60 15 3 -10 20.40 4.40 15 3 -10 17.30 4.00 13 -3 -10 4.00 2.60 13 -3 -10 0.80 1.90 13 3 -10 -0.10 2.70 13 3 -10 0.70 2.50 11 -3 -10 256.57 14.20 11 -3 -10 270.97 12.80 11 3 -10 268.07 14.40 11 3 -10 236.78 14.00 9 -3 -10 230.28 12.30 -9 -3 10 222.78 12.00 9 -3 -10 225.28 10.50 9 3 -10 221.08 12.30 9 3 -10 183.68 11.80 -7 -3 10 135.79 8.20 7 -3 -10 140.59 7.40 7 -3 -10 142.79 8.60 7 -3 -10 136.09 6.70 7 3 -10 139.59 8.60 7 3 -10 138.99 8.90 5 -3 -10 5.30 0.80 5 -3 -10 8.10 2.40 -5 -3 10 4.30 1.00 5 -3 -10 7.20 1.50 -5 -3 10 0.70 1.90 5 -3 -10 5.50 0.80 5 3 -10 3.90 2.50 5 3 -10 4.10 2.00 3 -3 -10 127.99 7.10 -3 -3 10 126.19 7.60 3 -3 -10 111.89 5.60 -3 -3 10 113.49 6.20 3 -3 -10 120.19 6.10 3 -3 -10 126.19 8.00 3 3 -10 122.29 7.80 3 3 -10 105.99 7.50 -1 -3 10 40.20 4.30 1 -3 -10 38.90 3.60 -1 -3 10 40.90 3.60 1 -3 -10 34.90 2.80 1 -3 -10 46.60 5.00 1 -3 -10 41.20 2.10 1 -3 -10 39.70 2.10 1 3 -10 39.00 4.40 -1 3 10 36.50 2.80 1 3 -10 46.50 4.60 1 -3 10 21.10 3.40 1 -3 10 21.80 3.50 -1 -3 -10 12.50 3.30 -1 3 -10 16.10 3.10 1 3 10 18.50 2.00 -1 3 -10 12.80 2.60 3 -3 10 38.10 4.80 3 -3 10 44.80 4.90 -3 -3 -10 30.00 4.50 3 3 10 33.60 3.00 -3 3 -10 35.00 4.10 5 -3 10 181.18 11.10 5 -3 10 177.18 11.00 -5 -3 -10 181.48 11.30 5 3 10 187.38 9.60 5 3 10 190.28 8.70 -5 3 -10 172.98 10.70 -7 -3 -10 1.10 3.00 7 -3 10 9.40 3.30 7 3 10 8.00 2.10 -7 3 -10 4.70 3.00 9 -3 10 4.90 3.30 -9 -3 -10 5.00 3.40 9 3 10 1.40 2.20 -9 3 -10 1.30 3.00 -11 -3 -10 12.20 4.50 11 -3 10 3.10 3.70 11 3 10 5.40 3.00 -11 3 -10 7.60 4.00 13 -3 10 -3.10 3.50 -13 -3 -10 -0.90 3.80 -13 3 -10 6.30 4.10 13 3 10 -1.90 3.10 18 -4 -10 95.59 9.30 18 4 -10 77.29 8.90 18 4 -10 100.49 9.80 16 -4 -10 50.39 6.60 16 -4 -10 54.79 6.80 16 4 -10 57.99 7.10 16 4 -10 55.59 7.00 14 -4 -10 9.60 3.50 14 -4 -10 7.70 2.70 14 4 -10 7.40 3.40 14 4 -10 8.00 3.60 12 -4 -10 83.59 5.80 12 -4 -10 69.19 7.00 12 4 -10 73.39 7.30 12 4 -10 67.49 7.00 10 -4 -10 40.50 5.20 10 -4 -10 42.80 4.00 10 4 -10 32.70 4.80 10 4 -10 40.80 5.30 -8 -4 10 37.40 4.50 8 -4 -10 44.80 3.50 -8 -4 10 45.00 2.40 8 -4 -10 49.90 5.30 -8 -4 10 43.00 2.40 8 4 -10 44.60 5.40 8 4 -10 44.90 5.50 -6 -4 10 357.96 16.20 6 -4 -10 355.26 18.10 -6 -4 10 345.87 17.90 6 -4 -10 350.66 16.50 6 -4 -10 370.76 16.50 6 -4 -10 370.86 16.50 6 4 -10 331.27 18.40 6 4 -10 356.46 18.60 4 -4 -10 46.70 3.30 -4 -4 10 45.60 3.60 4 -4 -10 49.80 4.00 4 -4 -10 41.00 4.50 4 -4 -10 45.90 3.30 -4 -4 10 48.90 4.90 4 -4 -10 45.40 2.90 4 4 -10 34.40 4.80 4 4 -10 47.10 5.50 2 -4 -10 17.70 3.90 2 -4 -10 27.10 2.40 2 -4 -10 30.00 3.60 -2 -4 10 24.10 3.70 2 4 -10 20.00 3.90 2 4 -10 28.20 4.20 0 -4 10 167.08 10.10 0 -4 -10 174.38 10.60 0 4 -10 175.88 10.70 0 4 -10 159.58 10.40 -2 -4 -10 81.79 7.60 2 -4 10 73.59 6.80 2 -4 10 84.89 7.40 -2 4 -10 65.89 6.90 -2 4 -10 83.79 6.70 2 4 10 77.49 4.00 4 -4 10 9.10 2.80 -4 -4 -10 9.70 3.60 4 -4 10 13.50 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-21 -1.90 3.20 -6 -2 21 31.90 5.90 -6 2 21 27.90 4.70 6 2 -21 32.90 5.60 4 -2 -21 1.30 3.10 -4 -2 21 -2.30 3.30 -4 2 21 8.20 3.40 4 2 -21 -0.50 3.90 -2 -2 21 -1.00 3.80 2 -2 -21 3.20 3.60 -9 -3 21 -5.90 3.00 9 3 -21 -1.70 3.50 -7 -3 21 7.70 4.20 7 -3 -21 2.20 3.40 7 3 -21 -3.20 3.30 5 -3 -21 14.40 5.00 -5 -3 21 22.60 5.50 5 3 -21 21.60 6.40 5 3 -21 9.90 4.50 12 0 -22 121.29 9.70 -10 0 22 31.70 5.50 -8 0 22 56.49 6.90 -6 0 22 128.19 9.80 -4 0 22 47.50 6.60 -11 -1 22 8.50 4.10 11 1 -22 6.40 4.30 -9 -1 22 7.10 3.80 -9 1 22 14.10 4.40 9 1 -22 15.20 4.30 -7 -1 22 -6.80 2.90 -7 1 22 -5.20 3.10 -5 -1 22 -1.50 3.70 -5 1 22 4.00 3.30 -8 -2 22 24.80 5.40 8 2 -22 23.30 5.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 17748 _shelx_res_file ; TITL n1e_a_a.res in C2/c shelx.res created by SHELXL-2019/3 at 20:19:01 on 01-Apr-2024 CELL 0.71073 16.9184 6.5230 17.2645 90.000 111.822 90.000 ZERR 4.00 0.0013 0.0005 0.0011 0.000 0.004 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H O UNIT 72 104 16 MERG 2 ABIN MORE -1 FMAP 2 PLAN 2 SIZE 0.180 0.290 0.330 ACTA BOND $H CONF L.S. 5 0 2 TEMP -123.00 WGHT 0.045600 1.130300 FVAR 0.43885 O1 3 0.441504 0.326314 0.289858 11.00000 0.03178 0.04809 = 0.02797 0.01097 0.02024 0.01144 O2 3 0.420538 0.157245 0.548055 11.00000 0.07158 0.06898 = 0.03665 0.02803 0.03617 0.04416 C6 1 0.305147 0.539629 0.392185 11.00000 0.02893 0.02468 = 0.02383 0.00067 0.01208 0.00613 C2 1 0.417316 0.353409 0.355424 11.00000 0.02058 0.03740 = 0.02509 0.00310 0.01303 0.00234 C3 1 0.435584 0.226069 0.421086 11.00000 0.02552 0.03518 = 0.02589 0.00585 0.01409 0.01014 AFIX 43 H3 2 0.468878 0.106836 0.424213 11.00000 -1.20000 AFIX 0 C7 1 0.367727 0.547668 0.346834 11.00000 0.03408 0.03094 = 0.03193 0.00819 0.01633 0.00352 AFIX 23 H7A 2 0.335662 0.575102 0.286885 11.00000 -1.20000 H7B 2 0.407869 0.662711 0.369541 11.00000 -1.20000 AFIX 0 C5 1 0.353602 0.464032 0.481476 11.00000 0.03421 0.03234 = 0.02440 -0.00165 0.01343 0.00651 AFIX 23 H5A 2 0.392750 0.573764 0.513085 11.00000 -1.20000 H5B 2 0.312185 0.439501 0.508610 11.00000 -1.20000 AFIX 0 C4 1 0.404468 0.270574 0.487289 11.00000 0.02913 0.03925 = 0.02366 0.00564 0.01237 0.01068 C1 1 0.492928 0.149468 0.290540 11.00000 0.02587 0.04676 = 0.02741 0.00365 0.01598 0.00668 AFIX 23 H1A 2 0.463346 0.022376 0.295832 11.00000 -1.20000 H1B 2 0.548105 0.157036 0.338214 11.00000 -1.20000 AFIX 0 C8 1 0.231734 0.392988 0.347028 11.00000 0.02473 0.04415 = 0.03555 -0.00368 0.01059 0.00490 AFIX 137 H8A 2 0.201336 0.441546 0.289903 11.00000 -1.50000 H8B 2 0.192439 0.388104 0.376769 11.00000 -1.50000 H8C 2 0.254452 0.255480 0.345518 11.00000 -1.50000 AFIX 0 C9 1 0.268253 0.752688 0.393433 11.00000 0.05836 0.03321 = 0.04062 0.00449 0.02228 0.01731 AFIX 137 H9A 2 0.314317 0.847356 0.423877 11.00000 -1.50000 H9B 2 0.227197 0.745890 0.421145 11.00000 -1.50000 H9C 2 0.239567 0.801562 0.336078 11.00000 -1.50000 AFIX 0 HKLF 4 REM n1e_a_a.res in C2/c REM wR2 = 0.1180, GooF = S = 1.036, Restrained GooF = 1.036 for all data REM R1 = 0.0452 for 1559 Fo > 4sig(Fo) and 0.0672 for all 2111 data REM 102 parameters refined using 0 restraints END WGHT 0.0455 1.1377 REM Highest difference peak 0.263, deepest hole -0.200, 1-sigma level 0.040 Q1 1 0.4188 0.2512 0.4485 11.00000 0.05 0.26 Q2 1 0.5000 0.1345 0.2500 10.50000 0.05 0.25 ; _shelx_res_checksum 58977 _shelx_fab_file ; 2 0 0 8.83 0.00 4 0 0 3.52 0.00 6 0 0 0.01 0.00 8 0 0 -0.70 0.00 10 0 0 -0.63 0.00 12 0 0 -0.88 0.00 14 0 0 -0.73 0.00 16 0 0 0.04 0.00 18 0 0 0.50 0.00 20 0 0 0.20 0.00 1 1 0 2.89 0.00 3 1 0 1.62 0.00 5 1 0 0.34 0.00 7 1 0 -0.12 0.00 9 1 0 -0.08 0.00 11 1 0 -0.10 0.00 13 1 0 -0.10 0.00 15 1 0 0.10 0.00 17 1 0 0.30 0.00 19 1 0 0.22 0.00 0 2 0 -6.84 0.00 2 2 0 -5.24 0.00 4 2 0 -2.04 0.00 6 2 0 0.06 0.00 8 2 0 0.48 0.00 10 2 0 0.50 0.00 12 2 0 0.78 0.00 14 2 0 0.83 0.00 16 2 0 0.41 0.00 18 2 0 0.05 0.00 20 2 0 0.06 0.00 1 3 0 -3.49 0.00 3 3 0 -1.81 0.00 5 3 0 -0.18 0.00 7 3 0 0.29 0.00 9 3 0 0.20 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-0.26 0.00 6 0 16 -0.17 0.00 8 0 16 -0.09 0.00 -19 1 16 0.09 0.00 -17 1 16 0.14 0.00 -15 1 16 0.22 0.00 -13 1 16 0.35 0.00 -11 1 16 0.44 0.00 -9 1 16 0.32 0.00 -7 1 16 -0.01 0.00 -5 1 16 -0.32 0.00 -3 1 16 -0.37 0.00 -1 1 16 -0.19 0.00 1 1 16 -0.02 0.00 3 1 16 0.05 0.00 5 1 16 0.06 0.00 7 1 16 0.05 0.00 -18 2 16 -0.05 0.00 -16 2 16 -0.20 0.00 -14 2 16 -0.46 0.00 -12 2 16 -0.82 0.00 -10 2 16 -1.05 0.00 -8 2 16 -0.80 0.00 -6 2 16 -0.02 0.00 -4 2 16 0.80 0.00 -2 2 16 1.13 0.00 0 2 16 0.96 0.00 2 2 16 0.66 0.00 4 2 16 0.48 0.00 6 2 16 0.33 0.00 8 2 16 0.15 0.00 -17 3 16 0.02 0.00 -15 3 16 -0.10 0.00 -13 3 16 -0.39 0.00 -11 3 16 -0.72 0.00 -9 3 16 -0.69 0.00 -7 3 16 -0.11 0.00 -5 3 16 0.59 0.00 -3 3 16 0.86 0.00 -1 3 16 0.65 0.00 1 3 16 0.37 0.00 3 3 16 0.24 0.00 5 3 16 0.15 0.00 -16 4 16 0.04 0.00 -14 4 16 0.10 0.00 -12 4 16 0.21 0.00 -10 4 16 0.35 0.00 -8 4 16 0.36 0.00 -6 4 16 0.14 0.00 -4 4 16 -0.21 0.00 -2 4 16 -0.41 0.00 0 4 16 -0.39 0.00 2 4 16 -0.30 0.00 4 4 16 -0.29 0.00 -13 5 16 -0.08 0.00 -11 5 16 0.21 0.00 -9 5 16 0.38 0.00 -7 5 16 0.17 0.00 -5 5 16 -0.23 0.00 -3 5 16 -0.37 0.00 -1 5 16 -0.21 0.00 1 5 16 -0.08 0.00 -8 6 16 -0.08 0.00 -6 6 16 0.02 0.00 -4 6 16 0.15 0.00 -19 1 17 -0.20 0.00 -17 1 17 -0.38 0.00 -15 1 17 -0.64 0.00 -13 1 17 -0.94 0.00 -11 1 17 -1.12 0.00 -9 1 17 -0.85 0.00 -7 1 17 -0.02 0.00 -5 1 17 0.89 0.00 -3 1 17 1.24 0.00 -1 1 17 0.94 0.00 1 1 17 0.47 0.00 3 1 17 0.21 0.00 5 1 17 0.15 0.00 7 1 17 0.10 0.00 -18 2 17 -0.14 0.00 -16 2 17 -0.25 0.00 -14 2 17 -0.44 0.00 -12 2 17 -0.61 0.00 -10 2 17 -0.53 0.00 -8 2 17 -0.05 0.00 -6 2 17 0.53 0.00 -4 2 17 0.75 0.00 -2 2 17 0.52 0.00 0 2 17 0.19 0.00 2 2 17 0.02 0.00 4 2 17 -0.02 0.00 6 2 17 -0.05 0.00 -17 3 17 -0.04 0.00 -15 3 17 0.07 0.00 -13 3 17 0.29 0.00 -11 3 17 0.54 0.00 -9 3 17 0.58 0.00 -7 3 17 0.21 0.00 -5 3 17 -0.36 0.00 -3 3 17 -0.72 0.00 -1 3 17 -0.69 0.00 1 3 17 -0.48 0.00 3 3 17 -0.35 0.00 5 3 17 -0.30 0.00 -14 4 17 0.03 0.00 -12 4 17 0.36 0.00 -10 4 17 0.52 0.00 -8 4 17 0.20 0.00 -6 4 17 -0.39 0.00 -4 4 17 -0.70 0.00 -2 4 17 -0.57 0.00 0 4 17 -0.31 0.00 2 4 17 -0.22 0.00 -11 5 17 -0.17 0.00 -9 5 17 -0.20 0.00 -7 5 17 -0.14 0.00 -5 5 17 0.01 0.00 -3 5 17 0.14 0.00 -1 5 17 0.13 0.00 -18 0 18 -0.44 0.00 -16 0 18 -0.64 0.00 -14 0 18 -0.84 0.00 -12 0 18 -0.95 0.00 -10 0 18 -0.72 0.00 -8 0 18 -0.01 0.00 -6 0 18 0.85 0.00 -4 0 18 1.23 0.00 -2 0 18 0.91 0.00 0 0 18 0.34 0.00 2 0 18 0.01 0.00 4 0 18 0.00 0.00 6 0 18 0.06 0.00 -17 1 18 -0.22 0.00 -15 1 18 -0.28 0.00 -13 1 18 -0.32 0.00 -11 1 18 -0.24 0.00 -9 1 18 0.01 0.00 -7 1 18 0.31 0.00 -5 1 18 0.42 0.00 -3 1 18 0.27 0.00 -1 1 18 0.04 0.00 1 1 18 -0.08 0.00 3 1 18 -0.08 0.00 5 1 18 -0.04 0.00 -18 2 18 0.07 0.00 -16 2 18 0.22 0.00 -14 2 18 0.44 0.00 -12 2 18 0.68 0.00 -10 2 18 0.66 0.00 -8 2 18 0.19 0.00 -6 2 18 -0.54 0.00 -4 2 18 -0.99 0.00 -2 2 18 -0.89 0.00 0 2 18 -0.50 0.00 2 2 18 -0.23 0.00 4 2 18 -0.15 0.00 -15 3 18 0.23 0.00 -13 3 18 0.46 0.00 -11 3 18 0.52 0.00 -9 3 18 0.14 0.00 -7 3 18 -0.49 0.00 -5 3 18 -0.87 0.00 -3 3 18 -0.72 0.00 -1 3 18 -0.35 0.00 1 3 18 -0.13 0.00 3 3 18 -0.07 0.00 -14 4 18 -0.03 0.00 -12 4 18 -0.20 0.00 -10 4 18 -0.34 0.00 -8 4 18 -0.29 0.00 -6 4 18 -0.02 0.00 -4 4 18 0.24 0.00 -2 4 18 0.29 0.00 0 4 18 0.18 0.00 -9 5 18 -0.22 0.00 -7 5 18 0.09 0.00 -5 5 18 0.31 0.00 -3 5 18 0.23 0.00 -17 1 19 0.40 0.00 -15 1 19 0.53 0.00 -13 1 19 0.64 0.00 -11 1 19 0.55 0.00 -9 1 19 0.07 0.00 -7 1 19 -0.65 0.00 -5 1 19 -1.09 0.00 -3 1 19 -0.91 0.00 -1 1 19 -0.38 0.00 1 1 19 -0.01 0.00 3 1 19 0.04 0.00 -16 2 19 0.32 0.00 -14 2 19 0.40 0.00 -12 2 19 0.35 0.00 -10 2 19 0.03 0.00 -8 2 19 -0.46 0.00 -6 2 19 -0.73 0.00 -4 2 19 -0.59 0.00 -2 2 19 -0.21 0.00 0 2 19 0.03 0.00 2 2 19 0.07 0.00 -15 3 19 -0.05 0.00 -13 3 19 -0.27 0.00 -11 3 19 -0.43 0.00 -9 3 19 -0.31 0.00 -7 3 19 0.10 0.00 -5 3 19 0.50 0.00 -3 3 19 0.57 0.00 -1 3 19 0.36 0.00 1 3 19 0.15 0.00 -12 4 19 -0.34 0.00 -10 4 19 -0.21 0.00 -8 4 19 0.24 0.00 -6 4 19 0.60 0.00 -4 4 19 0.55 0.00 -2 4 19 0.28 0.00 -16 0 20 0.45 0.00 -14 0 20 0.45 0.00 -12 0 20 0.34 0.00 -10 0 20 -0.02 0.00 -8 0 20 -0.61 0.00 -6 0 20 -1.01 0.00 -4 0 20 -0.85 0.00 -2 0 20 -0.31 0.00 0 0 20 0.10 0.00 2 0 20 0.14 0.00 -15 1 20 0.20 0.00 -13 1 20 0.14 0.00 -11 1 20 -0.03 0.00 -9 1 20 -0.27 0.00 -7 1 20 -0.39 0.00 -5 1 20 -0.30 0.00 -3 1 20 -0.08 0.00 -1 1 20 0.08 0.00 1 1 20 0.08 0.00 -14 2 20 -0.30 0.00 -12 2 20 -0.38 0.00 -10 2 20 -0.19 0.00 -8 2 20 0.29 0.00 -6 2 20 0.72 0.00 -4 2 20 0.75 0.00 -2 2 20 0.40 0.00 0 2 20 0.06 0.00 -13 3 20 -0.31 0.00 -11 3 20 -0.11 0.00 -9 3 20 0.36 0.00 -7 3 20 0.73 0.00 -5 3 20 0.68 0.00 -3 3 20 0.33 0.00 -1 3 20 0.05 0.00 -8 4 20 0.18 0.00 -6 4 20 -0.04 0.00 -15 1 21 -0.22 0.00 -13 1 21 -0.18 0.00 -11 1 21 0.01 0.00 -9 1 21 0.41 0.00 -7 1 21 0.77 0.00 -5 1 21 0.74 0.00 -3 1 21 0.33 0.00 -1 1 21 -0.06 0.00 -12 2 21 0.01 0.00 -10 2 21 0.35 0.00 -8 2 21 0.60 0.00 -6 2 21 0.54 0.00 -4 2 21 0.22 0.00 -2 2 21 -0.05 0.00 -9 3 21 0.07 0.00 -7 3 21 -0.23 0.00 -5 3 21 -0.38 0.00 -12 0 22 0.13 0.00 -10 0 22 0.39 0.00 -8 0 22 0.66 0.00 -6 0 22 0.64 0.00 -4 0 22 0.28 0.00 -11 1 22 0.20 0.00 -9 1 22 0.30 0.00 -7 1 22 0.26 0.00 -5 1 22 0.10 0.00 -8 2 22 -0.39 0.00 17 5 0 -0.15 0.00 -21 1 1 -0.04 0.00 18 4 1 -0.12 0.00 -8 8 1 -0.18 0.00 20 0 2 0.11 0.00 14 6 2 -0.04 0.00 -13 7 3 0.05 0.00 6 8 3 0.11 0.00 15 5 4 -0.09 0.00 -16 6 4 0.10 0.00 -13 7 4 0.15 0.00 16 4 5 -0.05 0.00 -16 6 5 0.00 0.00 -13 7 5 0.01 0.00 -8 8 5 0.18 0.00 -16 6 6 -0.07 0.00 -13 7 6 -0.09 0.00 17 1 7 -0.11 0.00 -21 3 7 0.13 0.00 -16 6 7 -0.03 0.00 -13 7 7 -0.04 0.00 2 8 7 0.05 0.00 16 2 8 0.00 0.00 -21 3 8 -0.29 0.00 14 4 8 0.06 0.00 -16 6 8 0.00 0.00 10 6 8 0.29 0.00 -6 8 8 0.02 0.00 0 8 8 -0.09 0.00 -21 3 9 0.04 0.00 -11 7 11 -0.01 0.00 3 7 11 0.25 0.00 -22 0 12 0.04 0.00 1 7 12 0.10 0.00 -14 6 13 -0.18 0.00 -7 7 13 0.07 0.00 -21 1 15 0.13 0.00 7 3 16 0.02 0.00 -16 4 17 -0.11 0.00 -13 5 17 -0.12 0.00 -19 1 18 -0.16 0.00 -17 3 18 0.08 0.00 2 4 18 0.11 0.00 -11 5 18 -0.27 0.00 -17 1 20 0.20 0.00 -16 2 20 -0.17 0.00 -10 4 20 0.30 0.00 -14 2 21 -0.18 0.00 -11 3 21 0.26 0.00 -13 1 22 0.05 0.00 -3 1 22 -0.05 0.00 -10 2 22 -0.11 0.00 -6 2 22 -0.49 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 90522) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.189 0.250 19 3 ' ' 2 0.500 0.311 0.750 20 3 ' ' 3 0.500 0.689 0.250 19 3 ' ' 4 0.000 0.811 0.750 20 3 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL n1e_a C 2/c R = 0.06 CELL 16.9184 6.5230 17.2645 90.00 111.82 90.00 SPGR C2/c # Solvent Accessible Volume = 77 # Electrons Found in S.A.V. = 11 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.034 0.213 0.282 ! 1.51 eA-3 ) ; _shelx_fab_checksum 16007 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' '-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 0.44150(6) 0.32631(17) 0.28986(6) 0.0333(3) Uani d 1 . . O O2 0.42054(9) 0.1572(2) 0.54805(7) 0.0545(4) Uani d 1 . . C C6 0.30515(9) 0.5396(2) 0.39219(8) 0.0252(3) Uani d 1 . . C C2 0.41732(8) 0.3534(2) 0.35542(8) 0.0264(3) Uani d 1 . . C C3 0.43558(8) 0.2261(2) 0.42109(8) 0.0276(3) Uani d 1 . . H H3 0.468878 0.106836 0.424213 0.033 Uiso calc 1 . . C C7 0.36773(9) 0.5477(2) 0.34683(9) 0.0311(3) Uani d 1 . . H H7A 0.335662 0.575102 0.286885 0.037 Uiso calc 1 . . H H7B 0.407869 0.662711 0.369541 0.037 Uiso calc 1 . . C C5 0.35360(9) 0.4640(2) 0.48148(8) 0.0296(3) Uani d 1 . . H H5A 0.392750 0.573764 0.513085 0.036 Uiso calc 1 . . H H5B 0.312185 0.439501 0.508610 0.036 Uiso calc 1 . . C C4 0.40447(9) 0.2706(2) 0.48729(8) 0.0299(3) Uani d 1 . . C C1 0.49293(9) 0.1495(3) 0.29054(9) 0.0316(4) Uani d 1 . . H H1A 0.463346 0.022376 0.295832 0.038 Uiso calc 1 . . H H1B 0.548105 0.157036 0.338214 0.038 Uiso calc 1 . . C C8 0.23173(9) 0.3930(3) 0.34703(10) 0.0350(4) Uani d 1 . . H H8A 0.201336 0.441546 0.289903 0.052 Uiso calc 1 . . H H8B 0.192439 0.388104 0.376769 0.052 Uiso calc 1 . . H H8C 0.254452 0.255480 0.345518 0.052 Uiso calc 1 . . C C9 0.26825(12) 0.7527(3) 0.39343(10) 0.0429(4) Uani d 1 . . H H9A 0.314317 0.847356 0.423877 0.064 Uiso calc 1 . . H H9B 0.227197 0.745890 0.421145 0.064 Uiso calc 1 . . H H9C 0.239567 0.801562 0.336078 0.064 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 0.0318(5) 0.0481(7) 0.0280(5) 0.0114(5) 0.0202(4) 0.0110(5) O2 0.0716(9) 0.0690(9) 0.0366(6) 0.0442(7) 0.0362(6) 0.0280(6) C6 0.0289(7) 0.0247(7) 0.0238(7) 0.0061(6) 0.0121(6) 0.0007(5) C2 0.0206(6) 0.0374(8) 0.0251(7) 0.0023(6) 0.0130(5) 0.0031(6) C3 0.0255(7) 0.0352(8) 0.0259(7) 0.0101(6) 0.0141(6) 0.0058(6) C7 0.0341(8) 0.0309(8) 0.0319(7) 0.0035(6) 0.0163(6) 0.0082(6) C5 0.0342(8) 0.0323(8) 0.0244(7) 0.0065(6) 0.0134(6) -0.0016(6) C4 0.0291(7) 0.0393(8) 0.0237(7) 0.0107(6) 0.0124(6) 0.0056(6) C1 0.0259(7) 0.0468(9) 0.0274(7) 0.0067(6) 0.0160(6) 0.0036(6) C8 0.0247(7) 0.0441(9) 0.0355(8) 0.0049(6) 0.0106(6) -0.0037(7) C9 0.0584(11) 0.0332(9) 0.0406(9) 0.0173(8) 0.0223(8) 0.0045(7) 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 C2 O1 C1 . . 117.88(10) ? C9 C6 C8 . . 108.50(12) ? C9 C6 C5 . . 110.31(11) ? C8 C6 C5 . . 109.89(12) ? C9 C6 C7 . . 109.84(12) ? C8 C6 C7 . . 110.15(11) ? C5 C6 C7 . . 108.15(11) ? C3 C2 O1 . . 125.39(13) ? C3 C2 C7 . . 123.44(12) ? O1 C2 C7 . . 111.17(11) ? C2 C3 C4 . . 120.14(13) ? C2 C3 H3 . . 119.9 ? C4 C3 H3 . . 119.9 ? C2 C7 C6 . . 112.86(11) ? C2 C7 H7A . . 109.0 ? C6 C7 H7A . . 109.0 ? C2 C7 H7B . . 109.0 ? C6 C7 H7B . . 109.0 ? H7A C7 H7B . . 107.8 ? C4 C5 C6 . . 114.46(11) ? C4 C5 H5A . . 108.6 ? C6 C5 H5A . . 108.6 ? C4 C5 H5B . . 108.6 ? C6 C5 H5B . . 108.6 ? H5A C5 H5B . . 107.6 ? O2 C4 C3 . . 121.41(13) ? O2 C4 C5 . . 119.97(12) ? C3 C4 C5 . . 118.59(12) ? O1 C1 C1 . 2_655 107.24(10) ? O1 C1 H1A . . 110.3 ? C1 C1 H1A 2_655 . 110.3 ? O1 C1 H1B . . 110.3 ? C1 C1 H1B 2_655 . 110.3 ? H1A C1 H1B . . 108.5 ? C6 C8 H8A . . 109.5 ? C6 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? C6 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? C6 C9 H9A . . 109.5 ? C6 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? C6 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 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 C2 . 1.3507(16) ? O1 C1 . 1.4423(17) ? O2 C4 . 1.2284(17) ? C6 C9 . 1.527(2) ? C6 C8 . 1.532(2) ? C6 C5 . 1.5336(19) ? C6 C7 . 1.5340(19) ? C2 C3 . 1.3454(19) ? C2 C7 . 1.496(2) ? C3 C4 . 1.4543(18) ? C3 H3 . 0.9500 ? C7 H7A . 0.9900 ? C7 H7B . 0.9900 ? C5 C4 . 1.5096(19) ? C5 H5A . 0.9900 ? C5 H5B . 0.9900 ? C1 C1 2_655 1.505(3) ? C1 H1A . 0.9900 ? C1 H1B . 0.9900 ? C8 H8A . 0.9800 ? C8 H8B . 0.9800 ? C8 H8C . 0.9800 ? C9 H9A . 0.9800 ? C9 H9B . 0.9800 ? C9 H9C . 0.9800 ? 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 _geom_hbond_publ_flag C3 H3 O2 5_656 0.95 2.46 3.391(2) 168 yes 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 C1 O1 C2 C3 . . . . -1.6(2) ? C1 O1 C2 C7 . . . . 177.57(12) ? O1 C2 C3 C4 . . . . -178.91(13) ? C7 C2 C3 C4 . . . . 2.0(2) ? C3 C2 C7 C6 . . . . -28.0(2) ? O1 C2 C7 C6 . . . . 152.85(12) ? C9 C6 C7 C2 . . . . 170.39(13) ? C8 C6 C7 C2 . . . . -70.16(15) ? C5 C6 C7 C2 . . . . 49.95(16) ? C9 C6 C5 C4 . . . . -170.57(13) ? C8 C6 C5 C4 . . . . 69.86(16) ? C7 C6 C5 C4 . . . . -50.42(16) ? C2 C3 C4 O2 . . . . -179.70(15) ? C2 C3 C4 C5 . . . . -1.5(2) ? C6 C5 C4 O2 . . . . -154.38(15) ? C6 C5 C4 C3 . . . . 27.4(2) ? C2 O1 C1 C1 . . . 2_655 177.15(12) ?