#------------------------------------------------------------------------------ #$Date: 2018-05-15 18:58:16 +0300 (Tue, 15 May 2018) $ #$Revision: 207790 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/94/1549413.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_1549413 loop_ _publ_author_name 'Seye, Dame' 'Diop, Libasse' 'Diop, Cheikh Abdoul Khadir' 'Geiger, David K.' _publ_section_title ; Diisopropylammonium hydrogen phthalate ; _journal_coeditor_code LH5874 _journal_issue 5 _journal_name_full IUCrData _journal_page_first x180704 _journal_paper_doi 10.1107/S2414314618007046 _journal_volume 3 _journal_year 2018 _chemical_formula_iupac 'C6 H16 N +, C8 H5 O4 -' _chemical_formula_moiety 'C6 H16 N +, C8 H5 O4 -' _chemical_formula_sum 'C14 H21 N O4' _chemical_formula_weight 267.32 _chemical_name_common ; Diisopropylammonium hydrogen phthalate ; _chemical_name_systematic ; Diisopropylammonium hydrogen phthalate ; _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' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _cell_angle_alpha 90 _cell_angle_beta 93.192(9) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.160(3) _cell_length_b 14.876(5) _cell_length_c 12.549(5) _cell_measurement_reflns_used 5881 _cell_measurement_temperature 200.(2) _cell_measurement_theta_max 25.2856 _cell_measurement_theta_min 2.4964 _cell_volume 1520.9(10) _computing_cell_refinement ; SAINT (Bruker, 2013) ; _computing_data_collection ; APEX2 (Bruker, 2013) ; _computing_data_reduction ; SAINT (Bruker, 2013) ; _computing_molecular_graphics ; PLATON (Spek, 2009) and Mercury (Macrae et al., 2006) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 200.(2) _diffrn_detector_area_resol_mean 8.3330 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker Smart X2S benchtop' _diffrn_measurement_method \w _diffrn_radiation_type MoKa _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 12641 _diffrn_reflns_theta_full 25.35 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_min 2.50 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_correction_T_min 0.48 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2013) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 576 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.400 _refine_diff_density_max 0.229 _refine_diff_density_min -0.228 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 188 _refine_ls_number_reflns 2772 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0572 _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^)+(0.0729P)^2^+0.6120P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1492 _refine_ls_wR_factor_ref 0.1640 _reflns_number_gt 2240 _reflns_number_total 2772 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lh5874sup1.cif _cod_data_source_block I _cod_database_code 1549413 _shelx_hkl_file ; -1 0 0 2076.99 69.49 -1 0 0 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56.89 2.20 5 5 4 99.79 3.70 5 5 4 100.29 3.80 6 5 4 8.10 0.70 6 5 4 9.20 0.80 7 5 4 81.79 3.20 7 5 4 84.59 3.30 8 5 4 -0.20 0.60 8 5 4 -0.50 0.70 9 -6 -4 26.90 1.90 9 -6 -4 32.10 2.10 8 -6 -4 -0.80 0.70 8 -6 -4 -0.20 0.80 8 -6 -4 -0.30 0.70 7 -6 -4 3.00 0.80 7 -6 -4 2.80 0.80 7 -6 -4 2.50 0.70 6 -6 -4 27.00 1.50 6 -6 -4 27.10 1.70 6 -6 -4 28.60 1.60 5 -6 -4 -0.10 0.40 5 -6 -4 0.00 0.50 5 -6 -4 -0.20 0.50 -5 6 4 -0.60 0.60 4 -6 -4 0.10 0.40 4 -6 -4 -0.10 0.40 -4 6 4 -0.30 0.50 3 -6 -4 110.39 3.90 3 -6 -4 108.39 4.00 -3 6 4 63.29 2.50 2 -6 -4 454.15 15.40 2 -6 -4 449.46 15.30 -2 6 4 287.17 10.70 -2 6 4 334.77 10.60 1 -6 -4 24.30 1.10 -1 6 4 17.30 0.90 0 -6 -4 17.60 0.90 0 6 4 15.10 0.80 -1 -6 -4 173.58 6.00 1 6 4 194.18 6.80 2 6 4 4.80 0.50 2 6 4 5.70 0.50 3 6 4 35.60 1.50 3 6 4 35.50 1.60 4 6 4 0.00 0.40 4 6 4 0.30 0.40 5 6 4 3.30 0.60 5 6 4 3.50 0.70 6 6 4 0.80 0.60 6 6 4 0.50 0.50 7 6 4 2.90 0.70 7 6 4 1.60 0.70 7 6 4 1.10 0.50 8 6 4 2.30 0.90 8 6 4 2.70 0.80 8 6 4 3.00 0.80 8 -7 -4 0.20 0.80 8 -7 -4 1.10 0.80 8 -7 -4 0.10 0.80 7 -7 -4 38.90 2.00 7 -7 -4 44.10 2.10 7 -7 -4 41.70 2.20 6 -7 -4 75.49 3.00 6 -7 -4 78.29 3.10 6 -7 -4 79.59 3.20 5 -7 -4 8.20 0.80 5 -7 -4 8.50 0.80 5 -7 -4 9.00 0.80 -5 7 4 5.60 0.90 4 -7 -4 5.20 0.60 4 -7 -4 5.50 0.60 -4 7 4 3.40 0.70 3 -7 -4 3.00 0.40 3 -7 -4 4.70 0.60 -3 7 4 1.30 0.50 2 -7 -4 90.49 3.30 2 -7 -4 94.19 3.40 1 -7 -4 78.59 2.90 -1 7 4 56.49 2.20 0 -7 -4 601.44 20.40 0 7 4 540.95 18.40 -1 -7 -4 309.87 10.60 1 7 4 320.27 11.00 2 7 4 8.20 0.70 2 7 4 8.40 0.60 3 7 4 27.00 1.30 3 7 4 25.80 1.20 4 7 4 -0.60 0.40 4 7 4 -0.10 0.40 5 7 4 11.40 1.00 5 7 4 11.70 0.90 6 7 4 24.90 1.40 6 7 4 26.90 1.50 7 7 4 30.00 1.80 7 7 4 29.40 1.70 8 7 4 0.70 0.70 8 7 4 0.40 0.80 8 -8 -4 14.00 1.30 8 -8 -4 17.70 1.70 8 -8 -4 14.20 1.50 7 -8 -4 -0.10 0.70 7 -8 -4 -0.80 0.70 7 -8 -4 -0.50 0.80 6 -8 -4 7.70 0.90 6 -8 -4 5.90 0.70 6 -8 -4 5.60 0.80 5 -8 -4 25.00 1.40 5 -8 -4 23.80 1.50 -5 8 4 11.10 1.10 4 -8 -4 22.20 1.30 4 -8 -4 19.80 1.20 -4 8 4 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2.00 7 -8 5 34.00 2.00 7 -8 5 35.50 1.80 8 7 -5 8.90 1.40 8 7 -5 13.20 1.50 7 7 -5 60.79 3.10 7 7 -5 65.99 3.10 6 7 -5 1.80 1.00 5 7 -5 3.20 0.90 -5 -7 5 2.10 0.80 4 7 -5 74.69 3.20 -4 -7 5 54.89 2.40 3 7 -5 31.00 1.70 -3 -7 5 27.80 1.40 -2 -7 5 80.99 3.10 -1 -7 5 96.19 3.60 -1 -7 5 102.59 3.60 0 -7 5 273.87 9.40 0 -7 5 272.97 9.40 1 -7 5 39.30 1.60 1 -7 5 38.00 1.70 2 -7 5 3.70 0.60 2 -7 5 3.90 0.50 3 -7 5 121.99 4.50 3 -7 5 124.69 4.40 4 -7 5 13.40 1.00 4 -7 5 16.00 1.20 4 -7 5 15.90 1.20 5 -7 5 15.50 1.30 5 -7 5 16.20 1.30 5 -7 5 19.10 1.10 6 -7 5 6.00 0.90 6 -7 5 4.70 0.90 6 -7 5 5.70 0.70 7 -7 5 29.20 1.80 7 -7 5 30.90 1.60 7 -7 5 31.30 1.80 8 -7 5 6.80 0.90 8 -7 5 6.00 1.00 8 -7 5 7.70 1.00 8 6 -5 -0.90 1.10 8 6 -5 -0.90 1.00 7 6 -5 124.59 5.20 7 6 -5 133.89 5.10 6 6 -5 43.10 2.40 5 6 -5 0.30 0.80 -5 -6 5 0.70 0.60 4 6 -5 1.70 0.80 -4 -6 5 1.30 0.60 3 6 -5 1.60 0.70 -3 -6 5 2.70 0.50 -2 -6 5 8.30 0.80 -1 -6 5 59.49 2.30 -1 -6 5 61.99 2.30 0 -6 5 786.92 26.70 0 -6 5 789.32 26.70 1 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2 13 -0.10 0.90 4 -2 -13 -0.70 1.20 -4 2 13 -0.50 0.90 -4 2 13 0.60 0.80 3 -2 -13 22.50 2.10 -3 2 13 15.60 1.50 -3 2 13 14.40 1.60 2 -2 -13 0.70 1.00 -2 2 13 2.90 0.80 -2 2 13 1.60 0.80 1 -2 -13 0.20 0.90 -1 2 13 0.30 0.80 -1 2 13 1.60 0.90 0 -2 -13 0.90 0.70 0 2 13 0.70 0.80 0 2 13 2.00 0.90 1 2 13 -0.70 0.90 1 2 13 0.70 0.90 2 2 13 -0.80 0.80 2 2 13 -0.20 0.90 2 2 13 1.00 1.00 3 2 13 0.30 1.00 3 2 13 0.60 1.00 3 2 13 0.90 0.90 4 2 13 8.70 1.10 4 2 13 11.00 1.30 4 2 13 10.40 1.30 5 -3 -13 -0.80 1.20 -5 3 13 0.50 0.70 -5 3 13 0.50 0.90 4 -3 -13 9.70 1.40 -4 3 13 5.60 0.90 -4 3 13 3.90 1.10 3 -3 -13 15.10 1.50 -3 3 13 14.00 1.50 -3 3 13 13.60 1.40 2 -3 -13 -0.90 0.90 -2 3 13 0.30 0.80 -2 3 13 1.20 0.80 1 -3 -13 0.50 0.80 -1 3 13 0.70 0.80 -1 3 13 0.20 0.80 0 -3 -13 0.80 0.70 0 3 13 0.40 0.80 0 3 13 0.90 0.80 -1 -3 -13 2.50 0.60 1 3 13 0.30 0.90 1 3 13 1.10 0.90 2 3 13 -0.30 0.90 2 3 13 -0.30 0.90 3 3 13 5.90 1.20 3 3 13 7.30 1.20 3 3 13 9.20 1.00 4 3 13 5.30 1.10 4 3 13 4.90 1.20 4 -4 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0 6 13 1.20 0.80 0 6 13 0.60 0.90 1 6 13 7.60 1.20 1 6 13 7.50 1.10 2 6 13 -0.80 0.90 2 6 13 1.60 1.00 3 6 13 9.00 1.30 3 6 13 5.90 1.10 -3 7 13 5.90 1.10 -3 7 13 6.90 0.90 -2 7 13 20.00 1.50 -2 7 13 17.70 1.70 -1 7 13 1.50 0.90 -1 7 13 0.50 0.80 0 7 13 2.00 0.80 0 7 13 0.70 0.90 1 7 13 1.60 0.90 1 7 13 1.90 1.00 2 7 13 -0.40 0.90 2 7 13 0.10 1.00 -2 8 13 3.90 0.90 -2 8 13 5.50 1.00 -1 8 13 1.70 0.90 -1 8 13 1.30 0.80 0 8 13 1.10 0.80 0 8 13 1.60 1.00 1 8 13 4.40 1.00 1 8 13 6.30 1.20 0 9 13 2.30 0.90 2 6 -14 2.60 1.00 -2 -6 14 4.20 0.90 -1 -6 14 5.60 1.40 -1 -6 14 5.10 1.00 0 -6 14 0.90 1.00 0 -6 14 0.20 0.90 1 -6 14 2.60 1.00 -3 -5 14 0.60 0.80 2 5 -14 10.40 1.30 -2 -5 14 16.40 1.60 -2 -5 14 12.00 1.40 1 5 -14 3.50 0.90 -1 -5 14 1.70 0.90 -1 -5 14 2.10 0.90 0 -5 14 0.50 0.90 0 -5 14 0.60 0.70 0 -5 14 0.80 1.00 1 -5 14 2.30 0.80 1 -5 14 0.60 1.00 1 -5 14 0.20 0.90 3 4 -14 1.00 1.10 -3 -4 14 0.30 0.80 -3 -4 14 0.80 0.90 2 4 -14 7.00 1.10 -2 -4 14 10.20 1.10 -2 -4 14 5.50 1.10 1 4 -14 0.80 0.90 -1 -4 14 0.90 0.90 -1 -4 14 0.40 0.80 0 -4 14 19.90 1.60 0 -4 14 21.50 1.70 1 -4 14 0.00 1.00 1 -4 14 1.60 0.80 1 -4 14 -0.20 0.90 2 -4 14 1.30 1.00 2 -4 14 2.90 0.80 2 -4 14 0.50 1.00 3 3 -14 -0.10 1.10 -3 -3 14 1.00 1.00 -3 -3 14 -0.20 0.80 2 3 -14 7.40 1.20 -2 -3 14 8.80 1.10 -2 -3 14 6.50 1.10 1 3 -14 2.20 1.00 -1 -3 14 2.30 0.90 -1 -3 14 3.50 1.00 0 -3 14 -0.60 0.90 0 -3 14 1.40 0.80 1 -3 14 -0.70 0.90 1 -3 14 -0.70 1.00 1 -3 14 2.60 0.80 2 -3 14 3.80 0.90 2 -3 14 3.70 1.10 2 -3 14 1.80 1.00 -4 -2 14 2.20 0.80 3 2 -14 -0.90 1.10 -3 -2 14 -0.10 0.90 -3 -2 14 -1.30 0.80 2 2 -14 8.40 1.30 -2 -2 14 7.70 1.10 -2 -2 14 9.40 1.20 1 2 -14 3.50 1.00 -1 -2 14 4.00 1.00 -1 -2 14 3.50 0.90 0 -2 14 4.10 1.00 0 -2 14 4.50 0.90 1 -2 14 24.90 1.90 1 -2 14 27.10 1.90 1 -2 14 24.70 1.80 2 -2 14 1.00 1.00 2 -2 14 -0.90 1.00 2 -2 14 0.60 0.90 4 1 -14 -0.40 1.20 -4 -1 14 -0.30 0.90 -4 -1 14 -0.70 0.80 3 1 -14 3.80 1.30 -3 -1 14 6.40 1.00 -3 -1 14 4.20 1.10 2 1 -14 -0.20 1.00 -2 -1 14 -0.70 0.80 -2 -1 14 0.40 0.90 1 1 -14 2.90 0.90 -1 -1 14 2.40 0.90 -1 -1 14 2.50 1.00 0 -1 14 9.00 1.10 0 -1 14 6.90 1.10 1 -1 14 0.70 1.00 1 -1 14 1.80 1.00 1 -1 14 1.20 0.90 2 -1 14 3.00 1.10 2 -1 14 4.70 1.10 2 -1 14 5.00 1.10 3 -1 14 1.40 1.10 3 -1 14 3.10 1.00 3 -1 14 -0.20 1.00 4 0 -14 6.10 1.50 -4 0 14 3.00 0.90 -4 0 14 2.30 1.00 3 0 -14 -1.40 1.10 -3 0 14 0.40 0.80 -3 0 14 1.30 1.00 2 0 -14 1.80 1.10 -2 0 14 1.50 0.90 -2 0 14 0.10 0.90 1 0 -14 18.20 1.70 -1 0 14 19.00 1.70 -1 0 14 24.60 1.70 0 0 -14 24.70 1.70 0 0 14 40.50 2.40 0 0 14 47.50 2.40 1 0 14 1.00 0.90 1 0 14 3.30 1.00 2 0 14 21.20 1.80 2 0 14 21.80 1.90 2 0 14 22.90 1.80 3 0 14 3.50 1.00 3 0 14 3.20 1.10 3 0 14 5.70 1.10 4 -1 -14 -0.90 1.30 -4 1 14 1.20 0.80 -4 1 14 -0.30 0.90 3 -1 -14 5.50 1.30 -3 1 14 5.40 1.00 -3 1 14 6.10 1.10 2 -1 -14 -0.90 0.90 -2 1 14 1.20 0.90 -2 1 14 0.60 0.90 1 -1 -14 2.00 0.90 -1 1 14 2.90 1.00 -1 1 14 2.80 0.90 0 -1 -14 6.90 1.00 0 1 14 7.60 1.10 0 1 14 7.70 1.10 1 1 14 2.30 1.00 1 1 14 1.00 1.00 2 1 14 3.00 1.00 2 1 14 5.90 1.10 2 1 14 3.60 1.10 3 1 14 -0.70 1.00 3 1 14 1.30 1.00 3 1 14 1.00 0.90 -4 2 14 2.10 0.90 3 -2 -14 -0.70 1.10 -3 2 14 1.50 0.90 -3 2 14 0.00 0.80 2 -2 -14 7.20 1.30 -2 2 14 8.70 1.10 -2 2 14 9.60 1.20 1 -2 -14 3.20 1.00 -1 2 14 4.60 1.00 -1 2 14 5.40 1.00 0 -2 -14 3.30 0.90 0 2 14 6.20 1.00 0 2 14 6.00 1.00 -1 -2 -14 19.70 1.40 1 2 14 24.20 1.90 1 2 14 25.50 1.90 2 2 14 3.00 1.00 2 2 14 0.50 1.00 3 -3 -14 -0.60 1.10 -3 3 14 0.60 0.90 -3 3 14 1.10 0.80 2 -3 -14 7.80 1.30 -2 3 14 9.80 1.10 -2 3 14 8.00 1.10 1 -3 -14 2.10 0.90 -1 3 14 3.90 0.90 -1 3 14 3.10 1.00 0 -3 -14 -0.20 0.80 0 3 14 2.20 0.90 0 3 14 1.10 0.90 -1 -3 -14 2.10 0.70 1 3 14 0.10 0.90 1 3 14 1.10 1.00 2 3 14 4.10 1.10 2 3 14 5.00 1.10 3 -4 -14 -0.10 1.10 -3 4 14 1.90 1.00 -3 4 14 1.90 0.80 2 -4 -14 6.50 1.20 -2 4 14 6.70 1.10 -2 4 14 10.20 1.10 1 -4 -14 -2.50 0.80 -1 4 14 1.60 1.00 -1 4 14 2.20 0.90 0 -4 -14 12.10 1.20 0 4 14 24.20 1.70 0 4 14 21.00 1.80 1 4 14 1.40 0.90 1 4 14 2.30 1.00 2 4 14 -0.50 1.00 2 4 14 2.40 1.10 -3 5 14 0.90 0.80 2 -5 -14 10.10 1.20 -2 5 14 15.30 1.70 -2 5 14 15.50 1.50 -1 5 14 2.90 1.00 -1 5 14 4.60 0.90 0 5 14 2.00 1.00 0 5 14 0.70 0.90 1 5 14 0.30 1.00 1 5 14 0.70 1.00 -2 6 14 4.30 0.90 -1 6 14 6.30 1.20 -1 6 14 5.20 0.90 0 6 14 0.90 0.90 0 6 14 1.80 1.00 1 6 14 1.60 1.00 1 1 -15 1.50 0.90 -1 -1 15 1.40 0.90 -1 -1 15 -0.60 0.90 0 1 -15 3.20 0.90 0 -1 15 1.80 1.00 1 0 -15 1.40 0.90 -1 0 15 1.20 0.90 -1 0 15 1.10 1.00 0 0 -15 2.00 0.80 0 0 15 0.90 0.90 0 0 15 0.60 1.00 1 -1 -15 0.50 1.00 -1 1 15 2.20 1.00 -1 1 15 1.10 0.90 0 -1 -15 1.50 0.90 0 1 15 1.40 1.00 0 1 15 2.80 1.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 78238 _shelx_res_file ; scan_0m_a.res created by SHELXL-2014/7 TITL scan_0m_a.res in P2(1)/c REM Old TITL scan_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.214, Rweak 0.011, Alpha 0.026, Orientation as input REM Formula found by SHELXT: C14 N3 O2 CELL 0.71073 8.1599 14.8757 12.5492 90.000 93.192 90.000 ZERR 4.000 0.0030 0.0053 0.0047 0.000 0.009 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O UNIT 56 84 4 16 OMIT 0 1 1 'obstructed' ACTA L.S. 10 BOND $H FMAP 2 PLAN 20 CONF HTAB HTAB O1 O3 HTAB O3 O1 EQIV $1 -x+1, y-1/2, -z+1/2 HTAB N1 O4_$1 HTAB N1 O2 SIZE 0.40 0.40 0.40 TEMP -73.000 WGHT 0.072900 0.612000 FVAR 0.58036 O1 4 0.511022 0.446407 0.353133 11.00000 0.02965 0.10330 = 0.08485 0.02795 0.00149 0.01249 H1O 2 0.511130 0.501681 0.284988 11.00000 0.10552 O2 4 0.343622 0.365840 0.442660 11.00000 0.06459 0.08188 = 0.10074 0.05012 0.00366 0.01972 O3 4 0.502767 0.550550 0.208416 11.00000 0.02951 0.09048 = 0.08699 0.02121 0.01174 -0.00795 O4 4 0.324265 0.611018 0.094988 11.00000 0.06140 0.11402 = 0.11072 0.07370 0.02362 0.00767 N1 3 0.519448 0.226053 0.538429 11.00000 0.03790 0.03780 = 0.03995 -0.00068 0.00052 0.00394 H1A 2 0.559218 0.186518 0.487850 11.00000 0.05888 H1B 2 0.472839 0.274721 0.497839 11.00000 0.06148 C1 1 0.665494 0.263025 0.603860 11.00000 0.04800 0.04894 = 0.04704 -0.00587 -0.00295 -0.00575 AFIX 13 H1 2 0.625681 0.309711 0.653596 11.00000 -1.20000 AFIX 0 C2 1 0.750442 0.189666 0.669258 11.00000 0.06258 0.11178 = 0.09152 0.04470 -0.03003 -0.01623 AFIX 137 H2A 2 0.780243 0.140475 0.622129 11.00000 -1.50000 H2B 2 0.676365 0.167007 0.721931 11.00000 -1.50000 H2C 2 0.849833 0.213920 0.706146 11.00000 -1.50000 AFIX 0 C3 1 0.778825 0.307288 0.529000 11.00000 0.05293 0.06133 = 0.07222 0.00169 0.00490 -0.01434 AFIX 137 H3A 2 0.820798 0.262050 0.480717 11.00000 -1.50000 H3B 2 0.870825 0.335101 0.570331 11.00000 -1.50000 H3C 2 0.718599 0.353517 0.487238 11.00000 -1.50000 AFIX 0 C4 1 0.385929 0.181113 0.596412 11.00000 0.04504 0.04407 = 0.05069 0.00581 0.00350 0.00017 AFIX 13 H4 2 0.435166 0.130156 0.639176 11.00000 -1.20000 AFIX 0 C5 1 0.262276 0.142989 0.513246 11.00000 0.05272 0.07927 = 0.07434 -0.00617 -0.00261 -0.01555 AFIX 137 H5A 2 0.214983 0.192032 0.469391 11.00000 -1.50000 H5B 2 0.174736 0.112014 0.549067 11.00000 -1.50000 H5C 2 0.317406 0.100349 0.467677 11.00000 -1.50000 AFIX 0 C6 1 0.308554 0.245779 0.671588 11.00000 0.06715 0.07858 = 0.06781 -0.00301 0.02715 -0.00157 AFIX 137 H6A 2 0.390315 0.264121 0.727540 11.00000 -1.50000 H6B 2 0.216331 0.216299 0.704200 11.00000 -1.50000 H6C 2 0.268801 0.298883 0.631811 11.00000 -1.50000 AFIX 0 C7 1 0.367636 0.425285 0.378004 11.00000 0.04228 0.04890 = 0.05205 0.00485 0.00052 0.01052 C8 1 0.355848 0.567110 0.175679 11.00000 0.03781 0.03987 = 0.06002 0.00414 0.01175 -0.00101 C9 1 0.218731 0.473234 0.325516 11.00000 0.02911 0.03324 = 0.04227 -0.00152 0.00004 0.00062 C10 1 0.213982 0.532714 0.237377 11.00000 0.02832 0.03275 = 0.04455 -0.00044 0.00319 -0.00010 C11 1 0.060482 0.566843 0.200791 11.00000 0.03677 0.05124 = 0.05277 0.01232 -0.00278 0.00517 AFIX 43 H11 2 0.055126 0.605719 0.140639 11.00000 -1.20000 AFIX 0 C12 1 -0.081710 0.546269 0.248433 11.00000 0.02879 0.06842 = 0.06568 0.00412 -0.00537 0.00473 AFIX 43 H12 2 -0.183330 0.570885 0.221803 11.00000 -1.20000 AFIX 0 C13 1 -0.076085 0.489613 0.335237 11.00000 0.02621 0.07070 = 0.06628 0.00260 0.00989 -0.00783 AFIX 43 H13 2 -0.173548 0.475513 0.369756 11.00000 -1.20000 AFIX 0 C14 1 0.072541 0.453411 0.371755 11.00000 0.03810 0.04919 = 0.04930 0.00703 0.00621 -0.00412 AFIX 43 H14 2 0.074686 0.413397 0.430816 11.00000 -1.20000 AFIX 0 HKLF 4 REM scan_0m_a.res in P2(1)/c REM R1 = 0.0572 for 2240 Fo > 4sig(Fo) and 0.0702 for all 2772 data REM 188 parameters refined using 0 restraints END WGHT 0.0729 0.6116 REM Instructions for potential hydrogen bonds HTAB O1 O3 HTAB O3 O1 HTAB N1 O4_$1 HTAB N1 O2 REM Highest difference peak 0.229, deepest hole -0.228, 1-sigma level 0.045 Q1 1 0.2820 0.5490 0.2131 11.00000 0.05 0.23 Q2 1 0.3616 0.6500 0.1467 11.00000 0.05 0.19 Q3 1 0.0999 0.5485 0.2650 11.00000 0.05 0.18 Q4 1 0.6003 0.5492 0.1676 11.00000 0.05 0.17 Q5 1 -0.0237 0.5740 0.2381 11.00000 0.05 0.17 Q6 1 0.2307 0.3678 0.4811 11.00000 0.05 0.15 Q7 1 0.0184 0.4699 0.3059 11.00000 0.05 0.15 Q8 1 0.1584 0.5386 0.1673 11.00000 0.05 0.15 Q9 1 0.8255 0.2364 0.7438 11.00000 0.05 0.14 Q10 1 0.1592 0.4525 0.3385 11.00000 0.05 0.14 Q11 1 0.6061 0.4391 0.3272 11.00000 0.05 0.14 Q12 1 0.2972 0.6289 0.0426 11.00000 0.05 0.14 Q13 1 0.2307 0.5162 0.2968 11.00000 0.05 0.14 Q14 1 0.1989 0.6165 0.1219 11.00000 0.05 0.13 Q15 1 0.4087 0.5651 0.2493 11.00000 0.05 0.13 Q16 1 0.4442 0.6286 0.0804 11.00000 0.05 0.13 Q17 1 0.1442 0.4862 0.3576 11.00000 0.05 0.13 Q18 1 -0.1946 0.5023 0.3667 11.00000 0.05 0.13 Q19 1 0.1627 0.1385 0.5482 11.00000 0.05 0.13 Q20 1 -0.0567 0.5325 0.3033 11.00000 0.05 0.13 ; _shelx_res_checksum 49617 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 O O1 0.51102(17) 0.44641(14) 0.35313(15) 0.0727(6) Uani d 1 H H1O 0.511(4) 0.502(2) 0.285(3) 0.106(11) Uiso d 1 O O2 0.3436(2) 0.36584(14) 0.44266(17) 0.0824(6) Uani d 1 O O3 0.50277(17) 0.55055(13) 0.20842(16) 0.0687(5) Uani d 1 O O4 0.3243(2) 0.61102(16) 0.09499(18) 0.0947(8) Uani d 1 N N1 0.51945(19) 0.22605(11) 0.53843(13) 0.0386(4) Uani d 1 H H1A 0.559(3) 0.1865(17) 0.4879(19) 0.059(7) Uiso d 1 H H1B 0.473(3) 0.2747(18) 0.4978(19) 0.061(7) Uiso d 1 C C1 0.6655(3) 0.26303(15) 0.60386(16) 0.0482(5) Uani d 1 H H1 0.6257 0.3097 0.6536 0.058 Uiso calc 1 C C2 0.7504(3) 0.1897(2) 0.6693(2) 0.0899(11) Uani d 1 H H2A 0.7802 0.1405 0.6221 0.135 Uiso calc 1 H H2B 0.6764 0.167 0.7219 0.135 Uiso calc 1 H H2C 0.8498 0.2139 0.7061 0.135 Uiso calc 1 C C3 0.7788(3) 0.30729(17) 0.5290(2) 0.0621(6) Uani d 1 H H3A 0.8208 0.2621 0.4807 0.093 Uiso calc 1 H H3B 0.8708 0.3351 0.5703 0.093 Uiso calc 1 H H3C 0.7186 0.3535 0.4872 0.093 Uiso calc 1 C C4 0.3859(2) 0.18111(14) 0.59641(17) 0.0466(5) Uani d 1 H H4 0.4352 0.1302 0.6392 0.056 Uiso calc 1 C C5 0.2623(3) 0.1430(2) 0.5132(2) 0.0690(7) Uani d 1 H H5A 0.215 0.192 0.4694 0.104 Uiso calc 1 H H5B 0.1747 0.112 0.5491 0.104 Uiso calc 1 H H5C 0.3174 0.1003 0.4677 0.104 Uiso calc 1 C C6 0.3086(3) 0.24578(19) 0.6716(2) 0.0703(7) Uani d 1 H H6A 0.3903 0.2641 0.7275 0.105 Uiso calc 1 H H6B 0.2163 0.2163 0.7042 0.105 Uiso calc 1 H H6C 0.2688 0.2989 0.6318 0.105 Uiso calc 1 C C7 0.3676(3) 0.42528(14) 0.37800(17) 0.0478(5) Uani d 1 C C8 0.3558(2) 0.56711(13) 0.17568(18) 0.0456(5) Uani d 1 C C9 0.2187(2) 0.47323(12) 0.32552(14) 0.0349(4) Uani d 1 C C10 0.2140(2) 0.53271(12) 0.23738(15) 0.0352(4) Uani d 1 C C11 0.0605(2) 0.56684(14) 0.20079(17) 0.0471(5) Uani d 1 H H11 0.0551 0.6057 0.1406 0.057 Uiso calc 1 C C12 -0.0817(2) 0.54627(16) 0.24843(19) 0.0546(6) Uani d 1 H H12 -0.1833 0.5709 0.2218 0.066 Uiso calc 1 C C13 -0.0761(2) 0.48961(17) 0.33524(19) 0.0541(6) Uani d 1 H H13 -0.1735 0.4755 0.3698 0.065 Uiso calc 1 C C14 0.0725(2) 0.45341(14) 0.37176(17) 0.0454(5) Uani d 1 H H14 0.0747 0.4134 0.4308 0.054 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 0.0296(8) 0.1033(14) 0.0849(12) 0.0125(8) 0.0015(8) 0.0280(11) O2 0.0646(11) 0.0819(13) 0.1007(14) 0.0197(9) 0.0037(10) 0.0501(11) O3 0.0295(8) 0.0905(13) 0.0870(12) -0.0079(7) 0.0117(8) 0.0212(10) O4 0.0614(11) 0.1140(17) 0.1107(15) 0.0077(11) 0.0236(11) 0.0737(14) N1 0.0379(8) 0.0378(9) 0.0399(8) 0.0039(7) 0.0005(7) -0.0007(7) C1 0.0480(11) 0.0489(12) 0.0470(11) -0.0057(9) -0.0030(9) -0.0059(9) C2 0.0626(16) 0.112(2) 0.092(2) -0.0162(16) -0.0300(15) 0.0447(19) C3 0.0529(13) 0.0613(15) 0.0722(15) -0.0143(11) 0.0049(11) 0.0017(12) C4 0.0450(11) 0.0441(11) 0.0507(11) 0.0002(9) 0.0035(9) 0.0058(9) C5 0.0527(13) 0.0793(18) 0.0743(16) -0.0156(12) -0.0026(12) -0.0062(14) C6 0.0672(15) 0.0786(18) 0.0678(15) -0.0016(13) 0.0272(13) -0.0030(14) C7 0.0423(11) 0.0489(12) 0.0521(11) 0.0105(9) 0.0005(9) 0.0048(10) C8 0.0378(10) 0.0399(10) 0.0600(12) -0.0010(8) 0.0118(9) 0.0041(10) C9 0.0291(9) 0.0332(9) 0.0423(10) 0.0006(7) 0.0000(7) -0.0015(7) C10 0.0283(9) 0.0327(9) 0.0445(10) -0.0001(7) 0.0032(7) -0.0004(7) C11 0.0368(10) 0.0512(12) 0.0528(11) 0.0052(9) -0.0028(9) 0.0123(10) C12 0.0288(10) 0.0684(15) 0.0657(14) 0.0047(9) -0.0054(9) 0.0041(11) C13 0.0262(9) 0.0707(15) 0.0663(13) -0.0078(9) 0.0099(9) 0.0026(12) C14 0.0381(10) 0.0492(11) 0.0493(11) -0.0041(8) 0.0062(8) 0.0070(9) 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' N N 0.0061 0.0033 '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 C7 O1 H1O 112.8(17) C8 O3 H1O 112.7(17) C4 N1 C1 118.04(15) C4 N1 H1A 109.7(15) C1 N1 H1A 107.7(15) C4 N1 H1B 108.6(15) C1 N1 H1B 107.0(14) H1A N1 H1B 105.0(19) C3 C1 C2 112.1(2) C3 C1 N1 108.24(17) C2 C1 N1 110.86(19) C3 C1 H1 108.5 C2 C1 H1 108.5 N1 C1 H1 108.5 C1 C2 H2A 109.5 C1 C2 H2B 109.5 H2A C2 H2B 109.5 C1 C2 H2C 109.5 H2A C2 H2C 109.5 H2B C2 H2C 109.5 C1 C3 H3A 109.5 C1 C3 H3B 109.5 H3A C3 H3B 109.5 C1 C3 H3C 109.5 H3A C3 H3C 109.5 H3B C3 H3C 109.5 N1 C4 C6 111.06(18) N1 C4 C5 107.78(17) C6 C4 C5 112.4(2) N1 C4 H4 108.5 C6 C4 H4 108.5 C5 C4 H4 108.5 C4 C5 H5A 109.5 C4 C5 H5B 109.5 H5A C5 H5B 109.5 C4 C5 H5C 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 C4 C6 H6A 109.5 C4 C6 H6B 109.5 H6A C6 H6B 109.5 C4 C6 H6C 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 O2 C7 O1 121.79(19) O2 C7 C9 118.10(19) O1 C7 C9 120.10(19) O4 C8 O3 121.6(2) O4 C8 C10 118.17(18) O3 C8 C10 120.20(19) C14 C9 C10 118.24(16) C14 C9 C7 113.74(17) C10 C9 C7 128.02(17) C11 C10 C9 117.81(17) C11 C10 C8 113.78(17) C9 C10 C8 128.41(16) C12 C11 C10 122.57(19) C12 C11 H11 118.7 C10 C11 H11 118.7 C11 C12 C13 119.40(18) C11 C12 H12 120.3 C13 C12 H12 120.3 C12 C13 C14 119.42(19) C12 C13 H13 120.3 C14 C13 H13 120.3 C13 C14 C9 122.54(19) C13 C14 H14 118.7 C9 C14 H14 118.7 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C7 1.267(3) O1 H1O 1.19(4) O2 C7 1.223(3) O3 C8 1.270(3) O3 H1O 1.20(4) O4 C8 1.220(3) N1 C4 1.501(3) N1 C1 1.513(2) N1 H1A 0.94(3) N1 H1B 0.95(3) C1 C3 1.506(3) C1 C2 1.510(3) C1 H1 1.0 C2 H2A 0.98 C2 H2B 0.98 C2 H2C 0.98 C3 H3A 0.98 C3 H3B 0.98 C3 H3C 0.98 C4 C6 1.510(3) C4 C5 1.520(3) C4 H4 1.0 C5 H5A 0.98 C5 H5B 0.98 C5 H5C 0.98 C6 H6A 0.98 C6 H6B 0.98 C6 H6C 0.98 C7 C9 1.526(3) C8 C10 1.517(3) C9 C14 1.387(3) C9 C10 1.415(3) C10 C11 1.405(3) C11 C12 1.369(3) C11 H11 0.95 C12 C13 1.376(3) C12 H12 0.95 C13 C14 1.382(3) C13 H13 0.95 C14 H14 0.95 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 O1 H1O O3 . 1.19(4) 1.20(4) 2.385(3) 173.(3) y N1 H1A O4 2_645 0.94(3) 1.83(3) 2.756(3) 169.(2) y N1 H1B O2 . 0.95(3) 1.83(3) 2.763(2) 166.(2) y C3 H3C O1 . 0.98 2.70 3.659(3) 166.1 y C3 H3A O4 2_645 0.98 2.69 3.392(4) 129.0 y C6 H6C O2 . 0.98 2.68 3.408(4) 131.8 y C12 H12 O3 1_455 0.95 2.58 3.401(2) 145.4 y C13 H13 O1 1_455 0.95 2.61 3.449(3) 147.9 y 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 C4 N1 C1 C3 -178.07(18) C4 N1 C1 C2 58.6(3) C1 N1 C4 C6 61.3(2) C1 N1 C4 C5 -175.11(19) O2 C7 C9 C14 10.5(3) O1 C7 C9 C14 -170.6(2) O2 C7 C9 C10 -168.8(2) O1 C7 C9 C10 10.1(3) C14 C9 C10 C11 -1.1(3) C7 C9 C10 C11 178.11(19) C14 C9 C10 C8 177.85(19) C7 C9 C10 C8 -2.9(3) O4 C8 C10 C11 -8.3(3) O3 C8 C10 C11 171.3(2) O4 C8 C10 C9 172.6(2) O3 C8 C10 C9 -7.7(3) C9 C10 C11 C12 1.5(3) C8 C10 C11 C12 -177.7(2) C10 C11 C12 C13 -0.4(4) C11 C12 C13 C14 -1.0(4) C12 C13 C14 C9 1.3(3) C10 C9 C14 C13 -0.2(3) C7 C9 C14 C13 -179.6(2) _cod_database_fobs_code 1549413