#------------------------------------------------------------------------------ #$Date: 2021-07-17 09:18:46 +0300 (Sat, 17 Jul 2021) $ #$Revision: 267616 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243870.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_2243870 loop_ _publ_author_name 'Thiruvalluvar, Aravazhi Amalan' 'Sridharan, M.' 'Rajendra Prasad, K. J.' 'Zeller, M.' _publ_section_title ; Synthesis and crystal structure of 1-hydroxy-8-methyl-9H-carbazole-2-carbaldehyde ; _journal_coeditor_code YY2001 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989021007210 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac 'C14 H11 N O2' _chemical_formula_moiety 'C14 H11 N O2' _chemical_formula_sum 'C14 H11 N O2' _chemical_formula_weight 225.24 _chemical_name_common 9H-carbazole _chemical_name_systematic ; 1-Hydroxy-8-methyl-9H-carbazole-2-carbaldehyde ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 105.817(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 28.290(5) _cell_length_b 3.9052(7) _cell_length_c 20.264(3) _cell_measurement_reflns_used 7327 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 31.25 _cell_measurement_theta_min 2.21 _cell_volume 2154.0(6) _computing_cell_refinement ; SAINT (Bruker, 2005) ; _computing_data_collection ; APEX2 (Bruker, 2005) ; _computing_data_reduction ; SAINT (Bruker, 2005) ; _computing_molecular_graphics ; PLATON (Spek, 2020) ; _computing_publication_material ; SHELXL2018/3 (Sheldrick, 2015), PLATON (Spek, 2020) and publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXTL (Sheldrick, 2008) ; _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker SMART APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_unetI/netI 0.0316 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 19760 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.282 _diffrn_reflns_theta_min 1.496 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_T_max 0.991 _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2005) ; _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_description needle _exptl_crystal_F_000 944 _exptl_crystal_size_max 0.750 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.305 _refine_diff_density_min -0.237 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 325 _refine_ls_number_reflns 5344 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.178 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0551 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+1.1713P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1334 _refine_ls_wR_factor_ref 0.1463 _reflns_number_gt 4453 _reflns_number_total 5344 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file yy2001sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2243870 _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 0.933 _shelx_estimated_absorpt_t_max 0.991 _shelx_hkl_file ; 0 0 1 -1.86 0.07 0 0 1 -1.75 0.10 0 0 -2 1202.34 20.73 0 0 2 1223.37 20.52 0 0 2 1171.98 22.96 0 0 3 -0.21 0.44 0 0 3 -0.27 0.37 0 0 -3 -0.44 0.31 0 0 4 1109.59 17.77 0 0 -4 1092.60 17.70 0 0 4 1047.88 20.23 0 0 5 0.14 0.57 0 0 5 0.80 0.66 0 0 -5 0.04 0.51 0 0 6 356.93 7.78 0 0 -6 371.20 6.65 0 0 6 372.76 6.92 0 0 -7 0.33 0.56 0 0 7 1.07 0.65 0 0 7 -0.37 0.60 0 0 8 1569.82 25.82 0 0 8 1563.26 29.44 0 0 -8 1570.62 25.50 0 0 -9 0.66 0.65 0 0 9 0.05 0.73 0 0 10 34.93 2.06 0 0 -10 38.15 1.93 0 0 -11 -1.19 0.58 0 0 -11 0.21 0.78 0 0 11 -0.60 0.71 0 0 12 5.81 1.19 0 0 -12 6.39 1.05 0 0 -12 7.30 1.28 0 0 -13 0.23 0.54 0 0 13 0.34 0.88 0 0 -13 0.01 0.72 0 0 -14 3.59 1.04 0 0 -14 2.79 0.83 0 0 14 2.19 1.13 0 0 15 1.06 1.07 0 0 -15 -0.75 0.74 0 0 -15 0.70 0.65 0 0 16 304.60 7.66 0 0 -16 293.51 6.96 0 0 -16 310.63 8.74 0 0 -17 2.52 0.88 0 0 17 1.84 1.26 0 0 -17 1.66 1.04 0 0 18 120.15 4.69 0 0 -18 125.28 5.00 0 0 -18 126.67 4.29 0 0 19 1.95 1.37 0 0 -19 3.22 0.65 0 0 -19 2.56 1.24 0 0 -20 253.57 8.13 0 0 20 250.73 7.46 0 0 -21 1.40 0.43 0 0 21 3.11 1.64 0 0 22 57.52 3.67 0 0 23 0.90 1.63 0 0 24 11.77 2.58 0 0 25 -0.49 1.75 0 1 0 0.06 0.66 0 1 0 -0.92 0.56 0 1 0 -0.35 0.58 0 -1 1 209.26 4.48 0 1 1 207.30 4.22 0 1 -1 206.08 4.38 0 1 1 213.45 4.85 0 1 1 212.60 4.26 0 1 -1 205.60 4.49 0 1 2 1478.96 23.61 0 1 -2 1423.96 23.76 0 1 -2 1468.27 27.28 0 1 2 1447.27 27.09 0 1 2 1461.65 23.57 0 -1 2 1463.70 23.87 0 1 3 529.20 9.14 0 1 3 536.89 9.27 0 1 -3 528.26 9.57 0 -1 3 544.24 9.70 0 1 3 525.00 10.92 0 1 4 90.74 2.44 0 1 4 85.30 3.10 0 1 -4 88.10 2.66 0 -1 -4 90.36 2.37 0 -1 4 91.59 2.79 0 -1 -5 55.27 1.75 0 1 5 49.78 2.48 0 1 -5 54.61 2.11 0 1 5 52.96 1.89 0 -1 5 52.54 2.20 0 1 6 94.98 3.46 0 1 6 93.62 2.67 0 -1 -6 93.61 2.37 0 -1 6 93.23 2.98 0 1 -6 96.15 2.95 0 1 7 20.53 1.47 0 1 7 21.92 1.86 0 -1 7 21.23 1.65 0 1 -7 22.29 1.54 0 -1 -7 22.53 1.20 0 1 -7 21.90 0.81 0 1 8 47.28 2.07 0 1 8 47.98 2.73 0 1 -8 47.26 2.20 0 1 -8 47.55 1.49 0 -1 -8 52.29 1.77 0 -1 8 47.30 2.31 0 1 9 16.41 1.96 0 -1 -9 16.84 1.20 0 1 -9 16.11 0.84 0 1 9 16.96 1.53 0 -1 9 15.50 1.60 0 1 -9 16.10 1.60 0 1 10 87.44 3.90 0 -1 10 85.36 3.26 0 1 -10 83.86 3.07 0 -1 -10 84.54 2.47 0 1 -10 85.43 2.50 0 1 10 82.14 2.90 0 1 11 18.73 1.69 0 -1 11 15.92 1.76 0 1 -11 14.24 0.90 0 1 11 14.38 2.07 0 1 -11 18.71 1.72 0 -1 -11 18.53 1.34 0 1 -12 5.28 0.55 0 -1 -12 6.97 1.01 0 -1 12 7.27 1.39 0 1 12 6.41 1.30 0 1 -12 7.71 1.38 0 1 12 6.77 1.61 0 -1 13 10.05 1.61 0 1 13 11.44 1.51 0 -1 -13 13.07 1.31 0 1 13 9.83 1.91 0 1 -13 12.60 1.60 0 1 -13 9.44 0.74 0 1 14 104.30 4.73 0 -1 -14 99.47 3.14 0 -1 14 99.78 4.06 0 1 14 97.90 3.75 0 1 -14 100.62 3.79 0 1 -14 98.73 3.25 0 1 15 22.58 2.17 0 -1 15 20.82 2.23 0 -1 -15 22.62 1.79 0 1 -15 18.95 2.02 0 1 -15 18.21 1.08 0 1 16 88.97 3.84 0 -1 -16 86.47 4.97 0 -1 -16 91.92 3.30 0 1 -16 92.03 3.82 0 -1 16 90.15 4.07 0 -1 17 11.31 2.00 0 1 17 11.34 1.89 0 1 -17 11.82 1.86 0 -1 -17 11.29 2.32 0 -1 18 51.01 3.38 0 1 18 49.34 3.21 0 -1 -18 48.11 3.64 0 1 -18 46.31 2.95 0 -1 -19 8.37 1.92 0 1 -19 7.79 1.75 0 1 19 7.18 1.82 0 -1 19 8.69 1.96 0 1 -20 34.11 2.75 0 1 20 29.28 2.76 0 -1 20 35.79 3.18 0 -1 -20 34.96 2.90 0 1 -21 22.18 2.64 0 -1 21 21.30 2.64 0 -1 -21 19.51 2.06 0 1 21 22.37 2.60 0 1 22 1.29 1.60 0 -1 -22 4.01 0.71 0 -1 22 3.50 1.82 0 -1 23 37.43 3.62 0 -1 -23 24.50 2.31 0 1 23 29.91 3.18 0 -1 24 0.48 1.96 0 1 24 0.02 1.75 0 -1 -24 -1.31 0.57 0 -1 25 9.60 2.55 0 -1 -25 7.25 0.77 0 1 25 11.72 2.45 0 2 0 124.03 3.69 0 2 0 124.33 3.64 0 2 0 124.08 3.60 0 2 1 26.74 1.85 0 2 -1 28.25 1.37 0 2 1 24.36 1.71 0 2 1 28.55 1.66 0 -2 1 24.43 1.89 0 2 -1 25.85 1.83 0 -2 2 90.39 3.38 0 2 2 87.77 3.29 0 2 -2 89.73 3.19 0 2 2 91.47 3.06 0 2 2 90.44 2.99 0 2 -2 92.75 2.69 0 2 -3 12.58 1.55 0 2 -3 16.04 0.81 0 -2 3 10.14 1.56 0 2 3 13.67 1.42 0 2 3 11.91 1.30 0 2 3 13.33 1.66 0 2 -4 64.93 2.88 0 2 4 63.41 3.15 0 2 4 70.95 2.69 0 2 4 73.71 2.55 0 -2 4 65.07 3.07 0 2 5 56.19 2.39 0 2 -5 54.95 2.70 0 2 5 48.47 2.96 0 -2 5 55.12 2.82 0 2 6 2.11 0.86 0 2 -6 2.96 1.12 0 -2 6 2.69 1.22 0 -2 -6 4.41 0.99 0 2 7 67.05 3.54 0 2 7 73.72 2.76 0 -2 -7 74.88 2.63 0 -2 7 71.27 3.25 0 2 -7 73.01 3.14 0 -2 8 41.99 2.63 0 -2 -8 44.08 2.05 0 2 -8 40.64 2.53 0 2 8 44.65 2.30 0 2 8 40.54 2.94 0 -2 -9 2.13 0.84 0 2 9 1.08 1.33 0 2 9 2.17 0.97 0 2 -9 2.30 1.17 0 -2 9 2.37 1.26 0 2 -10 15.99 1.94 0 2 10 13.64 2.16 0 2 10 12.41 1.45 0 -2 10 13.58 1.90 0 -2 -10 15.81 1.39 0 2 11 59.24 2.82 0 -2 -11 61.63 2.35 0 2 11 56.42 3.82 0 2 -11 59.90 3.18 0 -2 11 59.51 3.33 0 -2 12 119.57 4.71 0 -2 -12 127.88 3.59 0 2 12 124.18 4.20 0 2 -12 125.71 4.69 0 2 12 120.50 5.51 0 2 -13 51.68 3.19 0 2 13 50.22 3.73 0 -2 13 51.46 3.25 0 2 13 49.96 2.88 0 2 14 0.64 1.70 0 -2 14 1.97 1.61 0 2 14 0.12 1.18 0 2 -14 0.09 1.10 0 2 -15 11.36 2.01 0 2 15 12.85 1.90 0 -2 15 10.31 1.98 0 2 15 12.23 2.39 0 2 -16 27.51 2.79 0 -2 16 26.47 2.85 0 2 16 24.14 2.52 0 2 -17 65.73 3.78 0 2 17 59.86 3.58 0 -2 17 64.87 3.95 0 -2 18 83.99 4.60 0 2 -18 82.16 4.25 0 -2 -18 76.13 5.18 0 2 18 75.42 3.97 0 -2 -19 22.35 3.21 0 2 -19 23.99 2.92 0 2 19 22.38 2.66 0 -2 19 24.18 2.94 0 2 20 0.96 1.62 0 -2 20 0.31 1.88 0 2 -20 1.50 1.41 0 -2 -20 1.93 0.95 0 2 21 56.46 3.73 0 -2 -21 64.81 4.55 0 -2 21 61.32 4.45 0 2 -21 60.63 3.98 0 2 22 49.06 3.49 0 -2 22 45.31 4.04 0 -2 -22 42.19 3.47 0 2 -22 41.27 3.40 0 -2 23 2.04 2.08 0 -2 -23 2.50 1.07 0 2 -23 2.17 1.65 0 -2 24 7.49 2.76 0 -2 -24 7.54 0.97 0 3 0 -1.13 1.04 0 -3 0 -2.81 1.09 0 3 0 1.35 0.42 0 3 -1 2.35 1.21 0 3 1 3.73 0.68 0 -3 1 1.59 1.37 0 3 1 1.26 1.25 0 3 2 45.39 2.40 0 -3 2 38.80 2.98 0 3 -2 41.12 2.72 0 3 2 43.30 2.67 0 3 2 41.39 2.60 0 3 -2 41.03 1.83 0 3 3 17.83 1.56 0 -3 3 15.98 2.10 0 3 3 14.51 1.83 0 3 3 13.76 1.81 0 3 -3 15.15 2.07 0 3 4 24.10 1.97 0 3 -4 19.47 2.17 0 3 4 20.82 2.17 0 -3 4 20.44 2.42 0 3 4 23.47 2.04 0 3 -5 26.30 2.33 0 -3 5 27.80 2.75 0 3 5 29.59 2.28 0 3 5 27.43 2.25 0 3 5 28.53 2.18 0 3 -6 25.85 2.49 0 3 6 31.32 2.62 0 -3 6 31.12 2.84 0 3 6 27.80 2.29 0 3 7 51.81 3.52 0 -3 -7 57.41 2.85 0 -3 7 56.35 3.43 0 3 -7 55.33 3.30 0 3 7 58.34 2.99 0 -3 8 3.48 1.60 0 -3 -8 2.12 1.16 0 3 -8 2.97 1.47 0 3 8 1.23 1.35 0 3 8 3.01 1.40 0 3 9 4.39 1.35 0 -3 9 3.65 1.72 0 -3 -9 4.14 1.30 0 3 -9 3.27 1.50 0 3 9 1.19 1.57 0 3 10 1.33 1.40 0 3 -10 2.12 1.40 0 3 10 1.15 1.18 0 -3 10 0.22 1.49 0 -3 -10 1.53 1.21 0 -3 11 0.22 1.52 0 3 11 -0.01 0.98 0 3 -11 2.42 1.53 0 3 11 0.25 1.23 0 3 12 2.23 1.40 0 3 -12 5.00 1.82 0 -3 12 3.83 1.92 0 3 12 2.82 1.31 0 3 13 26.07 2.63 0 3 13 30.30 2.61 0 -3 13 23.62 2.81 0 3 -13 24.91 2.79 0 -3 14 4.08 1.95 0 3 14 2.64 1.61 0 3 14 8.59 1.88 0 3 -14 3.56 1.72 0 -3 15 4.01 1.90 0 3 15 4.41 1.60 0 3 -15 2.87 1.68 0 -3 16 2.73 1.94 0 3 16 3.94 1.37 0 3 -16 4.56 1.82 0 3 -17 0.78 1.34 0 -3 -17 -0.41 1.56 0 -3 17 1.57 1.74 0 -3 -18 -1.80 0.88 0 3 -18 0.44 1.55 0 -3 18 0.85 1.66 0 -3 19 2.11 2.18 0 -3 -19 0.59 1.33 0 3 -19 1.10 1.49 0 3 -20 8.41 2.32 0 -3 -20 5.24 1.41 0 -3 20 6.35 2.45 0 -3 -21 2.47 0.93 0 3 -21 1.87 1.54 0 -3 21 1.72 2.38 0 4 0 28.69 2.73 0 -4 0 27.29 2.92 0 4 1 50.51 3.33 0 -4 -1 52.45 3.50 0 4 -1 55.24 3.50 0 -4 1 48.12 3.52 0 -4 -2 5.04 1.77 0 -4 2 9.83 2.22 0 4 2 9.81 2.04 0 4 -2 9.44 2.14 0 -4 -3 27.09 2.52 0 -4 3 27.42 3.08 0 4 3 27.27 1.86 0 4 -3 27.69 2.68 0 4 3 25.64 2.56 0 -4 4 8.45 2.12 0 4 4 7.33 1.93 0 4 4 8.51 0.92 0 4 -4 8.96 2.10 0 -4 5 45.58 3.53 0 4 5 45.99 3.09 0 4 -5 45.91 3.41 0 4 5 45.79 2.79 0 4 5 53.84 3.32 0 4 6 -0.21 1.37 0 4 -6 -1.12 1.39 0 -4 6 0.76 1.52 0 4 6 1.65 0.62 0 -4 7 5.61 2.07 0 4 7 5.72 1.02 0 4 7 2.97 1.67 0 4 -7 2.65 1.71 0 -4 -7 3.14 1.55 0 4 8 4.58 0.86 0 -4 8 1.19 1.86 0 4 8 1.27 1.45 0 4 -8 1.57 1.59 0 4 9 29.71 2.34 0 -4 9 26.31 3.02 0 4 -9 27.23 2.93 0 4 -10 8.31 2.31 0 -4 10 7.25 2.33 0 -4 11 6.37 2.23 0 4 -11 2.77 1.73 0 -4 12 0.70 1.93 0 4 -12 -0.04 1.39 0 4 -13 -0.97 1.45 0 -4 13 -2.23 1.37 0 -4 -14 -1.82 1.43 0 -4 14 0.39 2.01 0 4 -14 0.58 1.77 0 4 -15 5.87 2.10 0 -4 -15 2.38 1.48 0 -4 15 4.13 2.14 0 -4 16 3.72 2.31 0 -4 -16 5.20 1.46 0 4 -16 3.64 2.06 0 5 0 -0.74 1.77 0 5 1 0.03 1.96 0 5 -1 2.98 2.06 0 -5 1 4.77 1.97 0 -5 2 0.37 1.96 0 5 2 -2.43 1.91 0 5 -2 0.17 2.00 0 5 -3 2.65 2.22 0 -5 3 4.05 2.13 0 5 3 0.93 1.95 0 5 -4 5.08 2.37 0 -5 4 4.87 2.14 0 5 -5 17.52 3.03 0 -5 5 16.00 2.89 0 -5 6 28.25 3.60 0 5 -6 29.59 3.72 0 5 -7 2.41 2.21 0 -5 7 4.65 2.31 -1 0 26 68.36 4.56 -1 0 25 -0.54 1.73 -1 0 24 -0.69 1.67 -1 0 23 1.40 1.86 -1 0 22 18.78 2.52 -1 0 21 0.99 1.35 1 0 -21 0.53 0.42 -1 0 20 9.29 1.99 1 0 -20 10.88 1.66 -1 0 19 1.90 1.39 1 0 -19 -0.55 0.49 1 0 -19 0.45 1.19 1 0 -18 4.15 1.40 -1 0 18 6.33 1.65 1 0 -18 2.45 0.84 1 0 -17 1.02 1.09 1 0 -17 1.92 0.81 -1 0 17 1.70 1.23 1 0 -16 29.93 2.38 -1 0 16 31.61 2.56 1 0 -16 34.64 2.27 -1 0 15 -0.18 1.00 1 0 -15 -0.06 0.77 1 0 -15 1.41 0.73 -1 0 14 3.36 1.22 1 0 -14 2.94 1.07 1 0 -14 2.39 0.97 -1 0 13 0.48 0.87 1 0 -13 -1.34 0.62 1 0 -12 6.12 1.08 -1 0 12 6.50 1.21 -1 0 11 0.22 0.80 -1 0 11 0.09 0.64 1 0 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4.34 0.59 -36 1 11 2.32 0.69 -36 1 10 6.67 1.12 -36 -1 10 8.33 0.73 36 -1 -10 4.50 2.56 36 -1 -9 25.35 3.44 -36 1 9 24.03 2.20 -36 -1 9 24.92 1.72 36 -1 -8 -2.59 2.01 -36 1 8 2.78 0.66 -36 -1 8 3.37 0.59 -36 1 7 4.07 0.68 36 -1 -7 1.77 2.08 -36 -1 7 3.19 0.67 -36 1 6 4.83 1.08 -36 -1 6 5.81 0.82 -36 1 5 7.12 1.02 -36 -1 5 4.67 0.64 -36 -1 4 2.54 0.56 -36 1 4 2.12 0.65 -36 -1 3 0.38 0.56 -36 1 3 3.42 0.78 -36 1 2 3.94 0.87 -36 -1 2 2.64 0.71 -37 0 12 5.43 0.70 37 0 -12 7.55 2.56 -37 0 11 2.18 0.57 37 0 -11 -3.02 1.87 -37 0 10 19.03 1.74 -37 0 9 -0.81 0.66 -37 0 8 4.03 0.74 -37 0 7 2.38 0.61 -37 0 6 32.96 2.48 -37 0 5 0.40 0.64 -37 0 4 10.21 1.18 -37 0 3 0.18 0.62 37 -1 -8 4.53 2.39 -37 1 8 6.86 0.88 -37 -1 8 8.99 0.70 -37 1 7 4.92 0.92 -37 -1 7 5.75 0.73 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 47120 _shelx_res_file ; TITL oobf-mea in P2(1)/c Z=8 shelx.res created by SHELXL-2018/3 at 12:39:35 on 19-Jun-2021 CELL 0.71073 28.2898 3.9052 20.2642 90.000 105.817 90.000 ZERR 8.00 0.0048 0.0007 0.0034 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 112 88 8 16 MERG 2 FMAP 2 PLAN 20 SIZE 0.100 0.190 0.750 ACTA BOND $H HTAB CONF REM Instructions for potential hydrogen bonds EQIV $1 x, y-1, z HTAB C14 O3_$1 EQIV $2 x, -y+1/2, z+1/2 HTAB N1 O4_$2 HTAB O1 O2 EQIV $3 x, y+1, z HTAB N2 O2_$3 HTAB O3 O4 L.S. 8 TEMP 23.00 WGHT 0.061200 1.171300 FVAR 0.34865 C1 1 0.606950 0.878215 0.799342 11.00000 0.04451 0.02660 = 0.02606 -0.00148 0.01917 0.00129 AFIX 137 H1A 2 0.586381 0.993978 0.822872 11.00000 -1.50000 H1B 2 0.636607 1.007032 0.804205 11.00000 -1.50000 H1C 2 0.614950 0.654265 0.818701 11.00000 -1.50000 AFIX 0 C2 1 0.580259 0.845991 0.724751 11.00000 0.02842 0.01574 = 0.02829 0.00152 0.01605 -0.00168 C3 1 0.533057 0.970664 0.697481 11.00000 0.02978 0.01673 = 0.04107 0.00115 0.02125 0.00034 AFIX 43 H3 2 0.517561 1.081062 0.726518 11.00000 -1.20000 AFIX 0 C4 1 0.507674 0.937059 0.627778 11.00000 0.02123 0.01963 = 0.04433 0.00579 0.01199 0.00166 AFIX 43 H4 2 0.475869 1.021909 0.611961 11.00000 -1.20000 AFIX 0 C5 1 0.529353 0.780025 0.582674 11.00000 0.02031 0.01934 = 0.03097 0.00668 0.00526 -0.00077 AFIX 43 H5 2 0.512575 0.758554 0.536525 11.00000 -1.20000 AFIX 0 C6 1 0.577248 0.653100 0.607728 11.00000 0.01912 0.01691 = 0.02178 0.00476 0.00679 -0.00180 C7 1 0.601790 0.686209 0.678046 11.00000 0.02076 0.01569 = 0.02187 0.00420 0.00960 0.00021 C8 1 0.692294 0.230329 0.617673 11.00000 0.01883 0.01928 = 0.01817 0.00149 0.00594 -0.00150 C9 1 0.652847 0.408709 0.629860 11.00000 0.01811 0.01717 = 0.01701 0.00262 0.00659 -0.00279 C10 1 0.610093 0.475178 0.576461 11.00000 0.01816 0.01722 = 0.01734 0.00344 0.00611 -0.00245 C11 1 0.606425 0.367825 0.508865 11.00000 0.02266 0.02261 = 0.01767 0.00271 0.00406 -0.00335 AFIX 43 H11 2 0.578573 0.416290 0.473378 11.00000 -1.20000 AFIX 0 C12 1 0.645109 0.189606 0.496799 11.00000 0.02683 0.02183 = 0.01577 -0.00028 0.00674 -0.00645 AFIX 43 H12 2 0.643093 0.114554 0.452561 11.00000 -1.20000 AFIX 0 C13 1 0.688001 0.117568 0.550218 11.00000 0.02149 0.02034 = 0.01988 -0.00036 0.00890 -0.00386 C14 1 0.726874 -0.082090 0.536187 11.00000 0.02757 0.02143 = 0.02377 0.00039 0.01329 -0.00229 AFIX 43 H14 2 0.722444 -0.163999 0.491820 11.00000 -1.20000 AFIX 0 C15 1 0.882084 0.816034 0.684387 11.00000 0.03824 0.02365 = 0.01792 -0.00251 0.00835 -0.00288 AFIX 137 H15A 2 0.902174 0.905029 0.726989 11.00000 -1.50000 H15B 2 0.860603 0.642822 0.693463 11.00000 -1.50000 H15C 2 0.862872 0.997972 0.658394 11.00000 -1.50000 AFIX 0 C16 1 0.914381 0.662846 0.644126 11.00000 0.03003 0.01767 = 0.01597 0.00298 0.00531 -0.00266 C17 1 0.964916 0.643144 0.668582 11.00000 0.03299 0.02162 = 0.01813 0.00285 -0.00007 -0.00550 AFIX 43 H17 2 0.979856 0.730010 0.711994 11.00000 -1.20000 AFIX 0 C18 1 0.994708 0.497721 0.630771 11.00000 0.02441 0.02619 = 0.02652 0.00638 0.00053 -0.00187 AFIX 43 H18 2 1.028583 0.491116 0.649516 11.00000 -1.20000 AFIX 0 C19 1 0.974403 0.364522 0.566193 11.00000 0.02264 0.02373 = 0.02319 0.00613 0.00619 0.00312 AFIX 43 H19 2 0.994149 0.267196 0.541288 11.00000 -1.20000 AFIX 0 C20 1 0.923285 0.379533 0.539061 11.00000 0.02091 0.01712 = 0.01880 0.00390 0.00638 0.00078 C21 1 0.894087 0.529207 0.578137 11.00000 0.02058 0.01646 = 0.01664 0.00340 0.00517 -0.00042 C22 1 0.800915 0.276285 0.427185 11.00000 0.02136 0.01796 = 0.01661 0.00311 0.00682 0.00024 C23 1 0.842630 0.353377 0.479930 11.00000 0.02219 0.01739 = 0.01432 0.00159 0.00703 0.00040 C24 1 0.889996 0.265523 0.475733 11.00000 0.02062 0.01708 = 0.01712 0.00397 0.00635 0.00277 C25 1 0.896349 0.098469 0.417051 11.00000 0.02454 0.02252 = 0.02028 0.00236 0.00924 0.00447 AFIX 43 H25 2 0.927599 0.043979 0.413640 11.00000 -1.20000 AFIX 0 C26 1 0.855471 0.018118 0.365140 11.00000 0.03255 0.02204 = 0.01646 -0.00031 0.00932 0.00300 AFIX 43 H26 2 0.859196 -0.093655 0.326343 11.00000 -1.20000 AFIX 0 C27 1 0.807552 0.102095 0.369407 11.00000 0.02703 0.02024 = 0.01427 0.00116 0.00509 0.00008 C28 1 0.764897 -0.001007 0.316231 11.00000 0.03460 0.02334 = 0.01618 0.00030 0.00346 -0.00132 AFIX 43 H28 2 0.769894 -0.116522 0.278565 11.00000 -1.20000 AFIX 0 N1 3 0.647677 0.539058 0.690706 11.00000 0.01971 0.02181 = 0.01653 0.00131 0.00604 0.00194 N2 3 0.845270 0.510743 0.541731 11.00000 0.02038 0.02162 = 0.01486 -0.00052 0.00623 0.00020 O1 4 0.732678 0.168690 0.670244 11.00000 0.01874 0.03122 = 0.02028 -0.00058 0.00342 0.00468 O2 4 0.766037 -0.152039 0.579671 11.00000 0.02471 0.03010 = 0.03081 -0.00140 0.01232 0.00225 O3 4 0.756294 0.369683 0.433096 11.00000 0.01862 0.03179 = 0.01869 -0.00130 0.00512 -0.00133 O4 4 0.722032 0.053640 0.317240 11.00000 0.02779 0.03969 = 0.01930 -0.00107 0.00190 -0.00425 H1 2 0.669982 0.527235 0.729514 11.00000 0.03338 H1D 2 0.753011 0.035325 0.650783 11.00000 0.06457 H2 2 0.818714 0.600413 0.553055 11.00000 0.03135 H3A 2 0.734429 0.288319 0.395189 11.00000 0.06323 HKLF 4 REM oobf-mea in P2(1)/c Z=8 REM wR2 = 0.1463, GooF = S = 1.178, Restrained GooF = 1.178 for all data REM R1 = 0.0551 for 4453 Fo > 4sig(Fo) and 0.0693 for all 5344 data REM 325 parameters refined using 0 restraints END WGHT 0.0612 1.1713 REM Instructions for potential hydrogen bonds HTAB C14 O3_$1 HTAB N1 O4_$2 HTAB O1 O2 HTAB N2 O2_$3 HTAB O3 O4 REM Highest difference peak 0.305, deepest hole -0.237, 1-sigma level 0.062 Q1 1 0.5931 0.5618 0.5866 11.00000 0.05 0.30 Q2 1 0.5892 0.6975 0.6418 11.00000 0.05 0.30 Q3 1 0.6270 0.3863 0.6010 11.00000 0.05 0.29 Q4 1 0.9114 0.4586 0.5584 11.00000 0.05 0.29 Q5 1 0.9795 0.4289 0.6011 11.00000 0.05 0.28 Q6 1 0.9495 0.4519 0.5471 11.00000 0.05 0.27 Q7 1 0.5543 0.7193 0.5972 11.00000 0.05 0.26 Q8 1 0.9098 0.3643 0.5019 11.00000 0.05 0.26 Q9 1 0.5575 0.8894 0.7198 11.00000 0.05 0.26 Q10 1 0.8995 0.5272 0.6200 11.00000 0.05 0.25 Q11 1 0.9402 0.6660 0.6509 11.00000 0.05 0.25 Q12 1 0.8660 0.3359 0.4720 11.00000 0.05 0.25 Q13 1 0.8265 0.3788 0.4484 11.00000 0.05 0.24 Q14 1 0.5275 0.9283 0.6125 11.00000 0.05 0.24 Q15 1 0.6214 0.2269 0.5087 11.00000 0.05 0.23 Q16 1 0.6295 0.6644 0.6871 11.00000 0.05 0.23 Q17 1 0.8986 0.7478 0.6612 11.00000 0.05 0.23 Q18 1 0.6317 0.3435 0.5015 11.00000 0.05 0.23 Q19 1 0.9490 0.0624 0.4144 11.00000 0.05 0.23 Q20 1 0.8759 0.1312 0.3902 11.00000 0.05 0.23 ; _shelx_res_checksum 82743 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.60695(8) 0.8782(6) 0.79934(10) 0.0305(4) Uani d 1 . . H H1A 0.586381 0.993978 0.822872 0.046 Uiso calc 1 . . H H1B 0.636607 1.007032 0.804205 0.046 Uiso calc 1 . . H H1C 0.614950 0.654265 0.818701 0.046 Uiso calc 1 . . C C2 0.58026(7) 0.8460(5) 0.72475(10) 0.0225(4) Uani d 1 . . C C3 0.53306(7) 0.9707(5) 0.69748(11) 0.0269(4) Uani d 1 . . H H3 0.517561 1.081062 0.726518 0.032 Uiso calc 1 . . C C4 0.50767(7) 0.9371(5) 0.62778(11) 0.0278(4) Uani d 1 . . H H4 0.475869 1.021909 0.611961 0.033 Uiso calc 1 . . C C5 0.52935(6) 0.7800(5) 0.58267(10) 0.0239(4) Uani d 1 . . H H5 0.512575 0.758554 0.536525 0.029 Uiso calc 1 . . C C6 0.57725(6) 0.6531(5) 0.60773(9) 0.0190(3) Uani d 1 . . C C7 0.60179(6) 0.6862(5) 0.67805(9) 0.0187(3) Uani d 1 . . C C8 0.69229(6) 0.2303(5) 0.61767(9) 0.0186(3) Uani d 1 . . C C9 0.65285(6) 0.4087(4) 0.62986(8) 0.0171(3) Uani d 1 . . C C10 0.61009(6) 0.4752(5) 0.57646(8) 0.0173(3) Uani d 1 . . C C11 0.60642(6) 0.3678(5) 0.50886(9) 0.0213(4) Uani d 1 . . H H11 0.578573 0.416290 0.473378 0.026 Uiso calc 1 . . C C12 0.64511(7) 0.1896(5) 0.49680(9) 0.0213(4) Uani d 1 . . H H12 0.643093 0.114554 0.452561 0.026 Uiso calc 1 . . C C13 0.68800(6) 0.1176(5) 0.55022(9) 0.0199(4) Uani d 1 . . C C14 0.72687(7) -0.0821(5) 0.53619(10) 0.0230(4) Uani d 1 . . H H14 0.722444 -0.163999 0.491820 0.028 Uiso calc 1 . . C C15 0.88208(8) 0.8160(5) 0.68439(9) 0.0265(4) Uani d 1 . . H H15A 0.902174 0.905029 0.726989 0.040 Uiso calc 1 . . H H15B 0.860603 0.642822 0.693463 0.040 Uiso calc 1 . . H H15C 0.862872 0.997972 0.658394 0.040 Uiso calc 1 . . C C16 0.91438(7) 0.6628(5) 0.64413(9) 0.0214(4) Uani d 1 . . C C17 0.96492(7) 0.6431(5) 0.66858(9) 0.0256(4) Uani d 1 . . H H17 0.979856 0.730010 0.711994 0.031 Uiso calc 1 . . C C18 0.99471(7) 0.4977(5) 0.63077(10) 0.0270(4) Uani d 1 . . H H18 1.028583 0.491116 0.649516 0.032 Uiso calc 1 . . C C19 0.97440(7) 0.3645(5) 0.56619(9) 0.0232(4) Uani d 1 . . H H19 0.994149 0.267196 0.541288 0.028 Uiso calc 1 . . C C20 0.92328(6) 0.3795(5) 0.53906(9) 0.0187(3) Uani d 1 . . C C21 0.89409(6) 0.5292(5) 0.57814(8) 0.0179(3) Uani d 1 . . C C22 0.80092(6) 0.2763(5) 0.42718(9) 0.0183(3) Uani d 1 . . C C23 0.84263(6) 0.3534(4) 0.47993(8) 0.0176(3) Uani d 1 . . C C24 0.89000(6) 0.2655(5) 0.47573(8) 0.0180(3) Uani d 1 . . C C25 0.89635(7) 0.0985(5) 0.41705(9) 0.0218(4) Uani d 1 . . H H25 0.927599 0.043979 0.413640 0.026 Uiso calc 1 . . C C26 0.85547(7) 0.0181(5) 0.36514(9) 0.0232(4) Uani d 1 . . H H26 0.859196 -0.093655 0.326343 0.028 Uiso calc 1 . . C C27 0.80755(7) 0.1021(5) 0.36941(9) 0.0206(4) Uani d 1 . . C C28 0.76490(7) -0.0010(5) 0.31623(9) 0.0254(4) Uani d 1 . . H H28 0.769894 -0.116522 0.278565 0.030 Uiso calc 1 . . N N1 0.64768(5) 0.5391(4) 0.69071(8) 0.0191(3) Uani d 1 . . N N2 0.84527(5) 0.5107(4) 0.54173(7) 0.0187(3) Uani d 1 . . O O1 0.73268(5) 0.1687(4) 0.67024(6) 0.0238(3) Uani d 1 . . O O2 0.76604(5) -0.1520(4) 0.57967(7) 0.0276(3) Uani d 1 . . O O3 0.75629(5) 0.3697(4) 0.43310(7) 0.0230(3) Uani d 1 . . O O4 0.72203(5) 0.0536(4) 0.31724(7) 0.0298(3) Uani d 1 . . H H1 0.6700(9) 0.527(7) 0.7295(13) 0.033(6) Uiso d 1 . . H H1D 0.7530(11) 0.035(9) 0.6508(16) 0.065(9) Uiso d 1 . . H H2 0.8187(8) 0.600(6) 0.5531(12) 0.031(6) Uiso d 1 . . H H3A 0.7344(11) 0.288(9) 0.3952(16) 0.063(9) Uiso d 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 C1 0.0445(12) 0.0266(10) 0.0261(10) 0.0013(9) 0.0192(9) -0.0015(8) C2 0.0284(9) 0.0157(9) 0.0283(9) -0.0017(7) 0.0160(8) 0.0015(7) C3 0.0298(10) 0.0167(9) 0.0411(11) 0.0003(7) 0.0213(9) 0.0011(8) C4 0.0212(9) 0.0196(9) 0.0443(12) 0.0017(7) 0.0120(8) 0.0058(8) C5 0.0203(8) 0.0193(9) 0.0310(10) -0.0008(7) 0.0053(7) 0.0067(7) C6 0.0191(8) 0.0169(8) 0.0218(8) -0.0018(6) 0.0068(6) 0.0048(7) C7 0.0208(8) 0.0157(8) 0.0219(8) 0.0002(6) 0.0096(7) 0.0042(7) C8 0.0188(8) 0.0193(9) 0.0182(8) -0.0015(7) 0.0059(6) 0.0015(6) C9 0.0181(7) 0.0172(8) 0.0170(8) -0.0028(6) 0.0066(6) 0.0026(6) C10 0.0182(7) 0.0172(8) 0.0173(8) -0.0025(6) 0.0061(6) 0.0034(6) C11 0.0227(8) 0.0226(9) 0.0177(8) -0.0034(7) 0.0041(6) 0.0027(7) C12 0.0268(9) 0.0218(9) 0.0158(8) -0.0064(7) 0.0067(7) -0.0003(7) C13 0.0215(8) 0.0203(9) 0.0199(8) -0.0039(7) 0.0089(6) -0.0004(7) C14 0.0276(9) 0.0214(9) 0.0238(9) -0.0023(7) 0.0133(7) 0.0004(7) C15 0.0382(10) 0.0237(10) 0.0179(8) -0.0029(8) 0.0083(7) -0.0025(7) C16 0.0300(9) 0.0177(9) 0.0160(8) -0.0027(7) 0.0053(7) 0.0030(7) C17 0.0330(10) 0.0216(9) 0.0181(8) -0.0055(8) -0.0001(7) 0.0028(7) C18 0.0244(9) 0.0262(10) 0.0265(9) -0.0019(7) 0.0005(7) 0.0064(8) C19 0.0226(8) 0.0237(10) 0.0232(9) 0.0031(7) 0.0062(7) 0.0061(7) C20 0.0209(8) 0.0171(8) 0.0188(8) 0.0008(7) 0.0064(6) 0.0039(6) C21 0.0206(8) 0.0165(8) 0.0166(8) -0.0004(6) 0.0052(6) 0.0034(6) C22 0.0214(8) 0.0180(8) 0.0166(8) 0.0002(7) 0.0068(6) 0.0031(6) C23 0.0222(8) 0.0174(8) 0.0143(8) 0.0004(7) 0.0070(6) 0.0016(6) C24 0.0206(8) 0.0171(8) 0.0171(8) 0.0028(6) 0.0064(6) 0.0040(6) C25 0.0245(9) 0.0225(9) 0.0203(8) 0.0045(7) 0.0092(7) 0.0024(7) C26 0.0325(10) 0.0220(9) 0.0165(8) 0.0030(8) 0.0093(7) -0.0003(7) C27 0.0270(9) 0.0202(9) 0.0143(8) 0.0001(7) 0.0051(6) 0.0012(7) C28 0.0346(10) 0.0233(10) 0.0162(8) -0.0013(8) 0.0035(7) 0.0003(7) N1 0.0197(7) 0.0218(8) 0.0165(7) 0.0019(6) 0.0060(6) 0.0013(6) N2 0.0204(7) 0.0216(8) 0.0149(7) 0.0002(6) 0.0062(5) -0.0005(6) O1 0.0187(6) 0.0312(8) 0.0203(6) 0.0047(5) 0.0034(5) -0.0006(5) O2 0.0247(7) 0.0301(8) 0.0308(7) 0.0022(6) 0.0123(6) -0.0014(6) O3 0.0186(6) 0.0318(8) 0.0187(6) -0.0013(5) 0.0051(5) -0.0013(5) O4 0.0278(7) 0.0397(9) 0.0193(6) -0.0043(6) 0.0019(5) -0.0011(6) 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 C1 H1A . . 109.5 ? C2 C1 H1B . . 109.5 ? H1A C1 H1B . . 109.5 ? C2 C1 H1C . . 109.5 ? H1A C1 H1C . . 109.5 ? H1B C1 H1C . . 109.5 ? C3 C2 C7 . . 115.79(17) ? C3 C2 C1 . . 122.54(17) ? C7 C2 C1 . . 121.68(17) ? C2 C3 C4 . . 122.71(18) ? C2 C3 H3 . . 118.6 ? C4 C3 H3 . . 118.6 ? C5 C4 C3 . . 120.74(17) ? C5 C4 H4 . . 119.6 ? C3 C4 H4 . . 119.6 ? C4 C5 C6 . . 118.62(18) ? C4 C5 H5 . . 120.7 ? C6 C5 H5 . . 120.7 ? C5 C6 C7 . . 119.64(17) ? C5 C6 C10 . . 133.48(17) ? C7 C6 C10 . . 106.86(15) ? N1 C7 C2 . . 128.29(17) ? N1 C7 C6 . . 109.21(15) ? C2 C7 C6 . . 122.50(16) ? O1 C8 C9 . . 119.60(15) ? O1 C8 C13 . . 122.58(16) ? C9 C8 C13 . . 117.81(16) ? N1 C9 C8 . . 128.95(16) ? N1 C9 C10 . . 109.92(15) ? C8 C9 C10 . . 121.13(16) ? C11 C10 C9 . . 120.79(16) ? C11 C10 C6 . . 133.37(16) ? C9 C10 C6 . . 105.84(15) ? C12 C11 C10 . . 118.20(16) ? C12 C11 H11 . . 120.9 ? C10 C11 H11 . . 120.9 ? C11 C12 C13 . . 121.50(16) ? C11 C12 H12 . . 119.3 ? C13 C12 H12 . . 119.3 ? C8 C13 C12 . . 120.56(16) ? C8 C13 C14 . . 119.52(16) ? C12 C13 C14 . . 119.89(16) ? O2 C14 C13 . . 124.09(17) ? O2 C14 H14 . . 118.0 ? C13 C14 H14 . . 118.0 ? C16 C15 H15A . . 109.5 ? C16 C15 H15B . . 109.5 ? H15A C15 H15B . . 109.5 ? C16 C15 H15C . . 109.5 ? H15A C15 H15C . . 109.5 ? H15B C15 H15C . . 109.5 ? C17 C16 C21 . . 115.81(17) ? C17 C16 C15 . . 123.33(17) ? C21 C16 C15 . . 120.86(16) ? C16 C17 C18 . . 122.89(17) ? C16 C17 H17 . . 118.6 ? C18 C17 H17 . . 118.6 ? C19 C18 C17 . . 120.89(18) ? C19 C18 H18 . . 119.6 ? C17 C18 H18 . . 119.6 ? C18 C19 C20 . . 118.34(18) ? C18 C19 H19 . . 120.8 ? C20 C19 H19 . . 120.8 ? C19 C20 C21 . . 119.64(16) ? C19 C20 C24 . . 133.72(17) ? C21 C20 C24 . . 106.64(15) ? N2 C21 C16 . . 128.23(16) ? N2 C21 C20 . . 109.32(15) ? C16 C21 C20 . . 122.43(16) ? O3 C22 C23 . . 119.39(15) ? O3 C22 C27 . . 122.90(16) ? C23 C22 C27 . . 117.71(16) ? N2 C23 C22 . . 128.21(16) ? N2 C23 C24 . . 110.28(15) ? C22 C23 C24 . . 121.50(16) ? C23 C24 C25 . . 120.38(16) ? C23 C24 C20 . . 105.83(15) ? C25 C24 C20 . . 133.78(16) ? C26 C25 C24 . . 118.57(16) ? C26 C25 H25 . . 120.7 ? C24 C25 H25 . . 120.7 ? C25 C26 C27 . . 121.34(17) ? C25 C26 H26 . . 119.3 ? C27 C26 H26 . . 119.3 ? C22 C27 C26 . . 120.48(16) ? C22 C27 C28 . . 118.85(17) ? C26 C27 C28 . . 120.62(17) ? O4 C28 C27 . . 124.41(18) ? O4 C28 H28 . . 117.8 ? C27 C28 H28 . . 117.8 ? C9 N1 C7 . . 108.16(14) ? C9 N1 H1 . . 124.4(16) ? C7 N1 H1 . . 127.5(16) ? C23 N2 C21 . . 107.92(15) ? C23 N2 H2 . . 123.7(15) ? C21 N2 H2 . . 128.2(15) ? C8 O1 H1D . . 104.5(18) ? C22 O3 H3A . . 105.7(19) ? 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 C1 C2 . 1.500(3) ? C1 H1A . 0.9600 ? C1 H1B . 0.9600 ? C1 H1C . 0.9600 ? C2 C3 . 1.387(3) ? C2 C7 . 1.404(2) ? C3 C4 . 1.405(3) ? C3 H3 . 0.9300 ? C4 C5 . 1.376(3) ? C4 H4 . 0.9300 ? C5 C6 . 1.402(2) ? C5 H5 . 0.9300 ? C6 C7 . 1.411(2) ? C6 C10 . 1.438(2) ? C7 N1 . 1.378(2) ? C8 O1 . 1.354(2) ? C8 C9 . 1.393(2) ? C8 C13 . 1.409(2) ? C9 N1 . 1.378(2) ? C9 C10 . 1.410(2) ? C10 C11 . 1.409(2) ? C11 C12 . 1.374(3) ? C11 H11 . 0.9300 ? C12 C13 . 1.417(2) ? C12 H12 . 0.9300 ? C13 C14 . 1.438(3) ? C14 O2 . 1.244(2) ? C14 H14 . 0.9300 ? C15 C16 . 1.505(3) ? C15 H15A . 0.9600 ? C15 H15B . 0.9600 ? C15 H15C . 0.9600 ? C16 C17 . 1.382(3) ? C16 C21 . 1.404(2) ? C17 C18 . 1.404(3) ? C17 H17 . 0.9300 ? C18 C19 . 1.380(3) ? C18 H18 . 0.9300 ? C19 C20 . 1.401(2) ? C19 H19 . 0.9300 ? C20 C21 . 1.417(2) ? C20 C24 . 1.440(2) ? C21 N2 . 1.379(2) ? C22 O3 . 1.350(2) ? C22 C23 . 1.392(2) ? C22 C27 . 1.410(2) ? C23 N2 . 1.379(2) ? C23 C24 . 1.408(2) ? C24 C25 . 1.410(2) ? C25 C26 . 1.371(3) ? C25 H25 . 0.9300 ? C26 C27 . 1.420(3) ? C26 H26 . 0.9300 ? C27 C28 . 1.439(2) ? C28 O4 . 1.237(2) ? C28 H28 . 0.9300 ? N1 H1 . 0.87(2) ? N2 H2 . 0.91(2) ? O1 H1D . 0.94(3) ? O3 H3A . 0.90(3) ? 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 C14 H14 O3 1_545 0.93 2.50 3.254(2) 138 yes N1 H1 O4 4_566 0.87(2) 2.00(2) 2.862(2) 174(2) yes O1 H1D O2 . 0.94(3) 1.74(3) 2.602(2) 151(3) yes N2 H2 O2 1_565 0.91(2) 1.97(2) 2.879(2) 173(2) yes O3 H3A O4 . 0.90(3) 1.78(3) 2.595(2) 150(3) 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 C7 C2 C3 C4 . . . . 0.8(3) ? C1 C2 C3 C4 . . . . -179.15(19) ? C2 C3 C4 C5 . . . . -0.9(3) ? C3 C4 C5 C6 . . . . 0.2(3) ? C4 C5 C6 C7 . . . . 0.5(3) ? C4 C5 C6 C10 . . . . 178.98(19) ? C3 C2 C7 N1 . . . . -179.66(18) ? C1 C2 C7 N1 . . . . 0.3(3) ? C3 C2 C7 C6 . . . . 0.0(3) ? C1 C2 C7 C6 . . . . 179.92(17) ? C5 C6 C7 N1 . . . . 179.06(16) ? C10 C6 C7 N1 . . . . 0.2(2) ? C5 C6 C7 C2 . . . . -0.6(3) ? C10 C6 C7 C2 . . . . -179.45(16) ? O1 C8 C9 N1 . . . . -0.6(3) ? C13 C8 C9 N1 . . . . 178.76(17) ? O1 C8 C9 C10 . . . . -179.52(16) ? C13 C8 C9 C10 . . . . -0.2(3) ? N1 C9 C10 C11 . . . . 179.77(16) ? C8 C9 C10 C11 . . . . -1.1(3) ? N1 C9 C10 C6 . . . . -0.63(19) ? C8 C9 C10 C6 . . . . 178.49(16) ? C5 C6 C10 C11 . . . . 1.2(4) ? C7 C6 C10 C11 . . . . 179.77(19) ? C5 C6 C10 C9 . . . . -178.36(19) ? C7 C6 C10 C9 . . . . 0.24(19) ? C9 C10 C11 C12 . . . . 1.6(3) ? C6 C10 C11 C12 . . . . -177.90(19) ? C10 C11 C12 C13 . . . . -0.8(3) ? O1 C8 C13 C12 . . . . -179.70(16) ? C9 C8 C13 C12 . . . . 1.0(3) ? O1 C8 C13 C14 . . . . 2.4(3) ? C9 C8 C13 C14 . . . . -176.92(16) ? C11 C12 C13 C8 . . . . -0.5(3) ? C11 C12 C13 C14 . . . . 177.38(17) ? C8 C13 C14 O2 . . . . -3.4(3) ? C12 C13 C14 O2 . . . . 178.69(18) ? C21 C16 C17 C18 . . . . -0.4(3) ? C15 C16 C17 C18 . . . . 179.59(18) ? C16 C17 C18 C19 . . . . -0.1(3) ? C17 C18 C19 C20 . . . . 0.3(3) ? C18 C19 C20 C21 . . . . 0.0(3) ? C18 C19 C20 C24 . . . . -178.91(19) ? C17 C16 C21 N2 . . . . 179.02(18) ? C15 C16 C21 N2 . . . . -0.9(3) ? C17 C16 C21 C20 . . . . 0.7(3) ? C15 C16 C21 C20 . . . . -179.26(17) ? C19 C20 C21 N2 . . . . -179.13(16) ? C24 C20 C21 N2 . . . . 0.0(2) ? C19 C20 C21 C16 . . . . -0.5(3) ? C24 C20 C21 C16 . . . . 178.64(16) ? O3 C22 C23 N2 . . . . 2.3(3) ? C27 C22 C23 N2 . . . . -177.78(17) ? O3 C22 C23 C24 . . . . -179.11(16) ? C27 C22 C23 C24 . . . . 0.8(3) ? N2 C23 C24 C25 . . . . 179.47(16) ? C22 C23 C24 C25 . . . . 0.6(3) ? N2 C23 C24 C20 . . . . -0.3(2) ? C22 C23 C24 C20 . . . . -179.20(16) ? C19 C20 C24 C23 . . . . 179.2(2) ? C21 C20 C24 C23 . . . . 0.18(19) ? C19 C20 C24 C25 . . . . -0.6(4) ? C21 C20 C24 C25 . . . . -179.59(19) ? C23 C24 C25 C26 . . . . -1.3(3) ? C20 C24 C25 C26 . . . . 178.46(19) ? C24 C25 C26 C27 . . . . 0.5(3) ? O3 C22 C27 C26 . . . . 178.33(17) ? C23 C22 C27 C26 . . . . -1.6(3) ? O3 C22 C27 C28 . . . . -4.1(3) ? C23 C22 C27 C28 . . . . 175.89(16) ? C25 C26 C27 C22 . . . . 1.0(3) ? C25 C26 C27 C28 . . . . -176.49(18) ? C22 C27 C28 O4 . . . . 0.3(3) ? C26 C27 C28 O4 . . . . 177.80(19) ? C8 C9 N1 C7 . . . . -178.24(18) ? C10 C9 N1 C7 . . . . 0.8(2) ? C2 C7 N1 C9 . . . . 179.03(18) ? C6 C7 N1 C9 . . . . -0.6(2) ? C22 C23 N2 C21 . . . . 179.13(17) ? C24 C23 N2 C21 . . . . 0.4(2) ? C16 C21 N2 C23 . . . . -178.75(18) ? C20 C21 N2 C23 . . . . -0.3(2) ? _cod_database_fobs_code 2243870