#------------------------------------------------------------------------------ #$Date: 2018-11-23 05:56:32 +0200 (Fri, 23 Nov 2018) $ #$Revision: 212135 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/27/2242749.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_2242749 loop_ _publ_author_name 'Ben-Yahia, Ali' 'El Bakri, Youness' 'Lai, Chin-Hung' 'Essassi, El Mokhtar' 'Mague, Joel T.' _publ_section_title ; Crystal structure, DFT calculations and Hirshfeld surface analysis of 3-(4-methylphenyl)-6-nitro-1H-indazole ; _journal_coeditor_code FF2156 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 1857 _journal_page_last 1861 _journal_paper_doi 10.1107/S205698901801647X _journal_volume 74 _journal_year 2018 _chemical_absolute_configuration unk _chemical_formula_iupac 'C14 H11 N3 O3' _chemical_formula_moiety 'C14 H11 N3 O3' _chemical_formula_sum 'C14 H11 N3 O3' _chemical_formula_weight 269.26 _chemical_name_systematic ; 3-(4-Methylphenyl)-6-nitro-1H-indazole ; _space_group_crystal_system monoclinic _space_group_IT_number 7 _space_group_name_Hall 'P -2yc' _space_group_name_H-M_alt 'P 1 c 1' _symmetry_space_group_name_Hall 'P -2yc' _symmetry_space_group_name_H-M 'P 1 c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 96.681(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.1447(14) _cell_length_b 11.8380(12) _cell_length_c 7.4252(8) _cell_measurement_reflns_used 1994 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 24.8 _cell_measurement_theta_min 3.37 _cell_volume 1234.9(2) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_molecular_graphics ; DIAMOND (Brandenburg & Putz, 2012) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 180(2) _diffrn_detector_area_resol_mean 8.333 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method \w-\f _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1105 _diffrn_reflns_av_unetI/netI 0.1621 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 25051 _diffrn_reflns_theta_full 30.500 _diffrn_reflns_theta_max 30.534 _diffrn_reflns_theta_min 1.720 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2016) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 560 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.457 _refine_diff_density_min -0.317 _refine_ls_abs_structure_details ; Flack x determined using 891 quotients [(I^+^)-(I^-^)]/[(I^+^)+(I^-^)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack 0.6(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 363 _refine_ls_number_reflns 6667 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 0.939 _refine_ls_R_factor_all 0.1992 _refine_ls_R_factor_gt 0.0639 _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^)+(0.0622P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1152 _refine_ls_wR_factor_ref 0.1584 _reflns_number_gt 2803 _reflns_number_total 6667 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ff2156sup1.cif _cod_data_source_block I _cod_database_code 2242749 _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_hkl_file ; 0 0 1 -1.17 1.43 0 0 1 0.00 0.77 0 0 -1 -1.04 0.76 0 0 -1 -0.11 0.47 0 0 -1 1.54 1.15 0 0 -1 0.04 1.18 0 0 1 -1.17 0.81 0 0 -2 64.11 3.12 0 0 -2 63.51 5.40 0 0 2 60.13 3.26 0 0 2 65.21 3.24 0 0 2 60.06 3.00 0 0 2 64.38 2.89 0 0 2 69.69 5.15 0 0 -2 65.86 4.26 0 0 3 1.78 1.95 0 0 3 0.19 1.86 0 0 3 -0.61 1.67 0 0 3 -1.48 3.13 0 0 3 -1.28 1.65 0 0 -3 -2.40 1.75 0 0 -3 -0.52 1.29 0 0 -3 -3.93 3.02 0 0 -3 -0.54 3.29 0 0 4 16.65 2.64 0 0 -4 9.89 4.03 0 0 4 18.48 2.37 0 0 -4 21.95 4.21 0 0 4 17.80 2.47 0 0 4 17.61 2.45 0 0 4 19.27 4.16 0 0 -5 2.51 3.67 0 0 -5 -0.46 1.14 0 0 5 7.45 4.26 0 0 -5 -0.99 3.55 0 0 5 0.79 2.17 0 0 5 -0.71 2.25 0 0 5 0.49 2.16 0 0 5 -1.25 2.26 0 0 6 11.54 5.05 0 0 6 11.29 3.21 0 0 6 10.17 2.94 0 0 6 11.95 2.93 0 0 -6 7.41 4.45 0 0 7 -0.89 3.16 0 0 7 -0.88 3.02 0 0 7 4.00 5.70 0 0 -7 -2.39 4.90 0 0 8 -1.10 6.23 0 0 8 7.13 3.20 0 0 8 9.85 3.99 0 0 -8 -0.01 5.26 0 0 8 14.63 3.93 0 0 -9 -5.89 5.75 0 0 9 2.98 3.98 0 0 -10 -2.31 6.57 0 0 10 1.36 4.37 0 -1 0 0.67 0.53 0 1 0 0.39 0.51 0 -1 0 -0.39 0.52 0 -1 0 0.46 0.64 0 1 0 -0.37 0.70 0 1 0 0.21 0.53 0 1 0 -0.79 0.49 0 -1 0 0.40 0.61 0 1 0 -0.06 0.49 0 1 0 0.15 0.33 0 -1 0 -1.03 0.52 0 -1 0 -0.15 0.18 0 1 1 0.17 1.55 0 -1 1 1.42 1.09 0 -1 -1 -0.66 0.64 0 1 1 1.17 2.17 0 -1 1 1.80 1.02 0 1 1 -0.38 1.29 0 -1 -1 0.28 1.06 0 -1 -1 -0.66 1.55 0 1 1 -1.25 1.15 0 -1 -1 -1.03 1.11 0 1 -1 -0.57 0.92 0 1 1 0.75 1.05 0 1 1 1.23 1.43 0 -1 1 -0.31 0.91 0 1 1 0.69 1.13 0 1 -1 -0.30 0.81 0 -1 1 1.49 1.60 0 -1 1 -0.66 0.98 0 -1 -1 -0.11 1.26 0 -1 -1 -0.67 0.65 0 -1 -1 2.40 1.29 0 1 2 181.38 6.78 0 1 2 173.41 6.66 0 -1 -2 166.86 9.10 0 1 2 174.78 6.70 0 1 2 182.84 6.68 0 -1 -2 183.42 6.31 0 1 -2 182.45 6.30 0 -1 -2 182.66 6.74 0 -1 2 169.87 7.36 0 1 -2 176.33 7.46 0 -1 2 175.73 6.26 0 -1 2 173.22 6.16 0 1 2 171.86 9.62 0 -1 2 165.44 6.18 0 -1 -2 177.11 6.63 0 -1 -2 175.28 6.28 0 -1 2 178.51 8.45 0 -1 2 176.94 6.32 0 -1 3 145.87 5.62 0 -1 -3 142.11 5.84 0 1 3 143.27 6.08 0 1 -3 143.27 7.16 0 -1 -3 146.33 8.93 0 -1 3 135.25 5.37 0 -1 3 137.51 8.04 0 1 3 133.04 8.92 0 -1 3 144.42 5.37 0 1 3 143.59 5.97 0 1 3 144.51 6.11 0 1 3 136.41 6.10 0 1 -3 149.89 5.34 0 -1 4 7.44 1.98 0 -1 4 0.74 1.94 0 1 4 2.57 2.35 0 -1 4 5.61 2.00 0 1 4 2.64 2.25 0 1 4 2.92 2.31 0 -1 -4 5.61 3.81 0 -1 -4 6.97 2.09 0 -1 -4 0.46 3.09 0 1 4 1.90 4.10 0 1 4 5.27 2.50 0 -1 4 -0.10 3.32 0 1 -4 3.23 1.22 0 1 -4 5.26 3.63 0 -1 -5 5.03 1.93 0 1 5 6.73 4.62 0 1 5 0.93 2.53 0 1 -5 3.98 1.37 0 -1 5 2.19 2.21 0 -1 5 0.97 3.42 0 1 5 3.55 2.45 0 -1 5 4.08 2.22 0 -1 5 4.64 2.24 0 1 -5 -1.31 3.66 0 -1 -5 1.48 4.14 0 1 5 3.15 2.44 0 -1 -5 4.28 3.66 0 1 5 2.70 2.52 0 1 -6 20.33 5.14 0 -1 6 26.03 3.33 0 1 6 33.46 3.89 0 -1 6 24.00 3.10 0 1 6 24.60 3.85 0 -1 -6 24.76 5.40 0 -1 6 20.56 5.26 0 1 6 22.47 3.62 0 -1 6 30.27 3.33 0 1 6 21.92 5.87 0 -1 7 -3.95 4.64 0 1 7 -4.28 3.02 0 1 7 3.35 3.52 0 -1 7 1.42 2.67 0 1 7 -0.35 5.38 0 -1 -7 0.21 4.56 0 1 -7 -5.70 4.78 0 1 7 1.76 2.97 0 -1 7 3.40 2.99 0 -1 7 2.23 3.14 0 -1 8 3.48 2.87 0 -1 8 -1.15 3.41 0 1 8 0.21 3.59 0 1 8 5.88 3.31 0 1 8 2.22 3.65 0 -1 -8 3.95 5.29 0 1 -8 -2.80 4.99 0 -1 8 -1.91 3.50 0 -1 8 -12.50 5.38 0 -1 -9 1.61 6.07 0 -1 9 1.13 3.84 0 1 -9 -5.66 5.53 0 1 9 4.46 4.29 0 -1 -10 13.32 7.44 0 1 10 -0.83 4.55 0 -1 10 1.97 4.30 0 2 0 -1.05 1.13 0 2 0 -1.65 1.31 0 -2 0 1.49 1.63 0 2 0 0.27 1.29 0 2 0 -0.73 1.32 0 -2 0 1.45 1.64 0 2 0 -3.34 1.49 0 -2 0 0.13 1.51 0 -2 0 -0.62 1.56 0 -2 0 -0.34 0.71 0 -2 0 2.38 1.60 0 2 0 1.44 1.92 0 -2 1 2101.18 65.07 0 2 -1 2082.53 65.01 0 -2 -1 2136.38 65.27 0 2 1 2096.82 67.82 0 -2 1 2104.31 68.44 0 2 -1 2145.98 65.19 0 -2 -1 2059.82 65.20 0 2 1 2104.38 65.21 0 -2 -1 2096.79 81.15 0 -2 -1 2082.34 67.83 0 -2 -1 2083.87 67.09 0 2 -1 2155.10 67.12 0 2 1 2097.48 67.14 0 2 1 2086.84 65.31 0 2 1 2105.42 67.21 0 -2 1 2064.05 67.05 0 2 1 1999.16 81.06 0 -2 1 2073.18 68.60 0 -2 -1 2058.46 67.80 0 -2 1 2131.14 65.19 0 2 2 150.05 6.10 0 2 2 159.71 6.57 0 2 -2 158.85 5.75 0 2 2 146.70 6.37 0 -2 2 150.94 5.91 0 2 2 155.63 6.54 0 -2 2 145.39 5.86 0 -2 -2 159.57 6.29 0 -2 -2 129.35 8.67 0 2 -2 148.22 5.77 0 -2 2 151.06 5.79 0 -2 2 154.66 7.62 0 -2 2 150.53 5.90 0 -2 -2 161.13 6.44 0 2 2 147.95 6.62 0 2 2 168.25 6.11 0 2 2 148.55 8.93 0 2 -3 1.72 3.08 0 2 3 2.41 2.55 0 -2 3 7.10 1.87 0 2 3 9.83 4.19 0 -2 3 5.08 2.05 0 -2 3 5.55 1.99 0 2 3 8.78 2.64 0 -2 -3 5.85 2.36 0 -2 -3 1.26 3.55 0 -2 3 7.92 1.93 0 2 3 9.09 2.64 0 2 3 8.01 2.64 0 -2 3 6.40 3.14 0 2 3 11.16 2.16 0 2 3 6.48 1.97 0 2 -3 5.96 1.83 0 -2 -4 57.31 3.95 0 2 4 53.51 4.27 0 2 -4 57.47 5.25 0 -2 -4 61.38 6.34 0 2 4 56.31 4.63 0 -2 4 48.22 3.47 0 2 4 61.16 6.39 0 -2 4 59.50 5.72 0 2 -4 47.40 2.64 0 -2 4 56.83 3.65 0 -2 4 54.49 3.54 0 -2 4 47.47 3.32 0 2 4 58.36 4.26 0 2 4 54.65 4.17 0 -2 5 28.55 4.82 0 -2 5 36.63 3.04 0 -2 -5 31.94 3.27 0 2 -5 29.85 4.93 0 -2 -5 35.13 5.85 0 2 5 32.63 3.77 0 -2 5 33.69 3.05 0 2 5 25.49 3.73 0 2 5 26.86 5.68 0 -2 5 34.93 3.13 0 -2 5 32.34 3.14 0 2 5 29.80 3.64 0 2 5 33.59 3.62 0 -2 6 2.41 2.79 0 2 6 0.40 3.05 0 -2 6 4.05 2.68 0 -2 -6 3.42 4.29 0 -2 6 7.78 2.55 0 -2 6 2.14 4.43 0 2 6 4.96 3.16 0 2 6 5.09 3.44 0 2 6 4.64 5.73 0 2 -6 10.43 5.03 0 2 7 -0.24 3.45 0 2 7 -6.96 5.93 0 -2 7 -10.20 4.49 0 2 7 2.79 3.76 0 -2 -7 0.71 4.90 0 -2 7 4.60 3.17 0 2 7 3.25 3.34 0 -2 7 0.69 3.08 0 -2 7 -0.47 2.55 0 2 -7 2.13 4.80 0 2 8 2.84 4.15 0 -2 8 12.63 3.74 0 -2 -8 12.55 5.95 0 2 -8 14.70 5.97 0 2 8 11.58 3.75 0 -2 8 13.14 3.80 0 -2 8 10.15 3.10 0 2 9 7.01 4.50 0 -2 -9 1.95 5.76 0 -2 9 7.51 4.05 0 2 9 8.96 4.02 0 -2 10 6.29 4.48 0 -2 -10 -6.90 6.14 0 2 10 11.50 5.07 0 -3 0 -0.21 0.90 0 -3 0 -0.85 2.44 0 -3 0 -2.02 2.41 0 3 0 3.40 2.19 0 -3 0 1.07 2.18 0 -3 0 -2.97 2.31 0 3 0 3.14 2.60 0 3 0 -2.06 2.22 0 -3 0 -0.05 2.34 0 3 0 -1.91 1.89 0 3 0 0.35 1.76 0 3 0 -1.22 2.29 0 3 1 144.23 6.76 0 -3 1 147.64 6.42 0 3 1 151.18 6.45 0 3 -1 156.22 6.33 0 -3 -1 150.05 6.81 0 3 1 144.82 7.04 0 -3 -1 152.05 6.51 0 3 -1 160.21 5.58 0 3 1 151.50 6.73 0 -3 1 153.50 6.59 0 3 -1 158.39 5.63 0 -3 -1 148.31 6.39 0 3 -1 158.01 6.44 0 -3 1 145.07 6.21 0 3 -1 156.19 6.29 0 -3 1 150.22 6.18 0 -3 -1 150.28 8.31 0 -3 1 143.57 6.01 0 3 1 152.38 6.63 0 -3 -1 150.04 6.80 0 -3 1 147.74 6.31 0 3 2 20.76 3.33 0 -3 -2 25.23 3.28 0 -3 -2 19.68 4.13 0 -3 2 18.46 2.62 0 3 2 19.26 2.65 0 3 -2 16.61 2.55 0 3 2 20.69 2.84 0 -3 2 20.05 2.62 0 3 2 23.80 4.09 0 -3 -2 21.84 2.79 0 -3 2 20.29 1.68 0 3 2 20.81 3.31 0 3 2 18.65 3.17 0 3 2 19.85 2.87 0 -3 -2 18.02 2.39 0 -3 2 16.50 2.58 0 -3 2 18.06 1.42 0 -3 -2 18.56 2.22 0 -3 3 80.08 4.39 0 -3 -3 80.85 7.47 0 -3 3 75.59 4.36 0 -3 -3 84.08 4.84 0 3 3 87.76 4.95 0 3 -3 84.79 4.17 0 3 3 80.81 5.37 0 3 3 77.38 5.34 0 -3 3 82.11 4.42 0 3 3 81.90 7.69 0 3 3 84.64 4.78 0 -3 3 80.27 4.62 0 3 3 92.29 5.64 0 3 3 83.52 5.18 0 -3 3 87.57 5.88 0 3 4 21.75 5.31 0 -3 4 35.61 2.99 0 -3 -4 32.31 3.44 0 -3 4 26.63 2.81 0 3 4 29.95 3.82 0 -3 4 27.29 2.82 0 -3 4 26.25 3.97 0 3 4 23.19 3.40 0 -3 -4 29.67 5.45 0 -3 4 27.22 2.94 0 3 4 22.45 3.60 0 3 4 27.90 3.16 0 3 5 28.71 3.96 0 -3 -5 28.74 3.53 0 -3 5 20.90 4.32 0 -3 5 26.99 3.11 0 -3 5 26.06 2.97 0 3 5 28.41 3.99 0 3 5 27.13 6.07 0 3 5 32.76 3.90 0 -3 5 25.22 3.06 0 -3 5 26.39 3.08 0 3 -5 26.64 2.01 0 -3 6 27.70 3.32 0 3 6 20.38 4.07 0 3 6 29.52 4.24 0 3 6 9.58 6.32 0 3 6 33.56 4.68 0 -3 6 20.52 5.20 0 -3 6 28.48 3.57 0 -3 6 31.52 3.61 0 3 7 1.61 3.77 0 3 7 1.19 3.51 0 -3 7 4.99 3.30 0 -3 7 2.45 2.74 0 -3 -7 8.02 5.09 0 -3 7 2.58 3.21 0 -3 7 -5.11 4.59 0 3 7 7.42 4.17 0 3 8 10.17 4.75 0 -3 -8 11.47 5.66 0 3 8 15.33 4.34 0 -3 8 10.83 3.89 0 -3 -9 1.60 5.83 0 3 9 0.36 4.55 0 3 9 -1.67 3.89 0 -3 9 5.41 4.02 0 -3 10 2.73 4.20 0 3 10 -7.84 4.49 0 -3 -10 0.82 6.19 0 -4 0 56.92 4.62 0 4 0 50.59 3.85 0 4 0 52.77 4.11 0 4 0 52.37 4.17 0 -4 0 56.94 4.57 0 -4 0 53.55 4.36 0 -4 0 46.25 3.96 0 4 0 50.48 3.89 0 4 1 50.56 4.09 0 -4 -1 41.00 4.67 0 -4 -1 50.31 3.94 0 -4 1 43.80 3.74 0 -4 1 50.22 3.97 0 -4 -1 48.83 4.13 0 4 -1 41.31 3.10 0 -4 1 40.25 3.69 0 4 -1 61.39 3.46 0 -4 1 48.98 3.93 0 -4 1 53.06 3.99 0 -4 1 47.88 4.05 0 -4 -1 49.81 4.00 0 4 1 46.03 4.22 0 4 1 48.08 4.08 0 -4 -1 44.68 3.97 0 4 1 48.15 4.09 0 4 -1 39.74 3.89 0 4 -1 42.60 3.53 0 -4 -1 47.42 4.04 0 4 2 4.91 2.70 0 4 2 9.15 2.66 0 -4 2 6.92 2.66 0 -4 -2 4.94 2.32 0 -4 -2 10.26 2.81 0 4 -2 5.26 2.59 0 -4 2 3.08 2.09 0 -4 2 6.50 1.94 0 -4 2 9.29 2.81 0 -4 2 5.25 2.56 0 -4 -2 3.99 2.77 0 -4 -2 5.76 2.68 0 4 2 6.08 3.09 0 4 2 7.97 2.89 0 4 2 5.94 3.03 0 -4 -2 3.65 3.86 0 -4 -3 52.66 2.84 0 4 3 77.82 4.78 0 4 3 38.27 4.26 0 -4 3 51.85 4.14 0 4 3 51.51 4.52 0 -4 -3 52.56 6.10 0 -4 -3 51.57 2.88 0 -4 -3 49.99 4.08 0 4 3 53.56 5.91 0 -4 3 50.71 3.96 0 4 -3 49.74 3.75 0 4 3 51.02 4.31 0 -4 3 47.31 3.95 0 4 3 50.17 4.49 0 -4 -3 49.53 4.40 0 4 -4 11.29 2.19 0 4 4 12.00 3.30 0 4 4 11.80 4.83 0 -4 -4 14.25 4.88 0 -4 -4 16.49 3.28 0 -4 4 14.78 3.45 0 -4 4 14.40 2.70 0 4 4 13.66 3.68 0 4 4 13.59 3.24 0 4 4 13.50 3.72 0 -4 4 18.24 2.84 0 -4 4 18.44 2.92 0 -4 5 19.82 3.16 0 4 5 21.73 3.95 0 -4 5 17.82 4.08 0 -4 -5 19.65 3.59 0 -4 5 16.86 2.96 0 -4 5 19.30 3.01 0 4 5 14.91 5.87 0 4 -5 19.02 2.11 0 4 5 11.11 3.81 0 4 5 13.34 4.00 0 -4 5 12.85 3.03 0 -4 6 2.17 2.66 0 4 6 8.83 4.29 0 -4 6 2.53 2.98 0 -4 6 10.47 4.57 0 4 6 1.77 3.56 0 4 6 7.99 3.86 0 -4 6 2.66 3.05 0 -4 -6 0.44 2.82 0 -4 7 6.22 5.32 0 -4 7 4.32 3.24 0 -4 7 6.11 2.99 0 -4 7 0.46 3.22 0 4 7 4.06 3.76 0 4 7 4.66 4.44 0 -4 8 2.54 3.62 0 4 8 5.73 4.76 0 4 8 4.11 3.97 0 -4 -8 4.41 5.52 0 -4 8 3.41 3.82 0 -4 9 4.49 4.16 0 -4 -9 10.31 6.57 0 4 9 6.24 4.59 0 4 9 -7.80 4.65 0 -4 -10 10.00 7.09 0 4 10 4.40 5.43 0 5 0 1.17 2.16 0 5 0 2.22 2.42 0 5 0 0.32 3.09 0 5 0 1.74 2.79 0 -5 0 -1.10 0.75 0 5 0 2.01 2.86 0 -5 0 -0.77 2.84 0 -5 0 -1.43 3.02 0 -5 0 2.41 2.98 0 -5 0 -2.72 2.74 0 -5 1 92.18 5.47 0 -5 -1 94.93 5.95 0 5 -1 98.95 4.88 0 -5 -1 98.26 7.49 0 -5 1 89.28 5.24 0 -5 1 93.20 5.49 0 -5 -1 93.37 5.59 0 -5 -1 84.30 5.72 0 -5 -1 89.54 6.23 0 -5 1 86.59 6.13 0 5 -1 87.91 5.65 0 5 1 83.44 5.91 0 5 1 88.75 5.24 0 -5 -1 85.93 5.58 0 5 1 90.09 6.06 0 5 -1 99.56 5.93 0 5 1 80.00 5.63 0 5 1 91.28 5.77 0 -5 1 87.88 5.82 0 -5 -2 -0.34 3.97 0 -5 2 1.85 2.76 0 5 2 3.86 3.40 0 -5 2 0.16 2.76 0 -5 -2 4.69 2.73 0 -5 2 4.19 2.29 0 -5 2 1.38 2.63 0 -5 2 3.62 2.74 0 5 -2 4.38 2.93 0 -5 -2 2.68 3.09 0 5 2 4.30 2.81 0 -5 -2 5.05 2.93 0 5 2 2.61 3.15 0 5 2 4.29 3.45 0 -5 2 2.73 2.88 0 5 2 1.19 2.92 0 -5 -2 6.79 2.81 0 -5 -3 37.09 3.09 0 -5 3 37.83 3.68 0 -5 -3 43.79 4.14 0 -5 -3 28.61 5.43 0 5 3 35.20 4.34 0 -5 -3 37.82 3.20 0 5 3 37.22 4.17 0 -5 -3 43.07 4.39 0 -5 3 41.24 3.79 0 5 3 26.17 4.15 0 5 3 39.64 4.63 0 5 -3 40.90 3.67 0 -5 3 29.37 3.47 0 5 3 38.39 3.93 0 5 4 1.42 3.67 0 -5 4 9.47 2.98 0 -5 4 9.28 2.87 0 5 4 7.51 3.21 0 5 4 2.51 3.15 0 5 -4 4.92 2.53 0 -5 4 3.16 2.76 0 5 4 4.30 3.39 0 -5 4 6.57 2.94 0 -5 -4 7.12 3.33 0 -5 -4 3.40 4.57 0 5 5 2.38 4.02 0 -5 -5 1.53 3.16 0 -5 5 0.26 2.78 0 -5 5 2.66 2.87 0 5 5 -0.25 3.47 0 5 -5 0.22 0.82 0 -5 5 0.13 3.41 0 5 5 0.55 3.40 0 5 6 2.10 4.11 0 -5 6 0.18 3.13 0 -5 -6 2.55 3.24 0 5 6 -2.24 4.25 0 5 6 -0.82 3.84 0 -5 6 -2.44 3.99 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15.32 7.61 -17 6 -2 20.83 8.59 17 -6 3 10.24 7.58 17 6 3 13.09 7.24 -17 6 -3 11.75 8.34 -17 -6 -3 5.37 7.25 -17 7 4 -0.40 6.54 -17 -7 4 -4.71 5.86 -17 -7 4 -2.11 5.48 -17 7 3 9.58 7.06 -17 -7 3 -9.67 5.83 -17 -7 3 3.06 6.08 -17 -7 2 13.01 6.84 -17 7 2 -1.92 6.92 -17 7 1 -1.42 7.40 17 -7 -1 3.13 6.13 -17 -7 1 -7.41 5.99 17 -7 0 0.21 6.67 -17 7 0 0.51 7.24 -17 -7 0 2.30 6.52 -17 7 -1 9.44 7.76 17 -7 1 -0.44 6.59 -17 -7 -1 1.06 6.70 17 7 1 -2.19 6.03 17 -7 2 -0.18 6.47 -17 -7 -2 6.87 7.44 17 7 2 -8.54 6.12 -17 7 -2 -10.14 7.22 -17 -8 3 -2.61 6.27 -17 8 3 -9.17 6.47 -17 -8 2 6.47 6.42 -17 8 2 3.23 7.15 -17 8 1 5.51 7.67 -17 -8 1 9.95 6.86 17 -8 -1 -3.25 6.26 17 -8 0 1.34 6.62 -17 8 0 -15.19 6.60 -17 -8 0 10.15 7.06 17 -8 1 -3.45 6.35 -17 8 -1 0.78 7.49 -17 -8 -1 -1.37 6.83 -17 9 1 5.00 7.69 -17 -9 1 -2.96 6.72 -18 0 5 -3.82 6.03 -18 0 5 -2.42 6.23 -18 0 4 3.84 6.15 -18 0 4 18.15 7.15 -18 0 3 -6.01 5.99 -18 0 3 7.75 6.21 -18 0 2 -1.58 6.25 -18 0 1 7.20 6.52 18 0 0 23.45 7.08 -18 0 0 5.67 6.80 18 0 0 27.10 4.01 18 0 1 -1.46 5.00 18 0 1 5.42 6.49 -18 0 -1 2.04 7.09 18 0 2 18.54 7.20 -18 0 -2 26.35 8.09 18 0 3 4.13 6.85 -18 0 -3 -8.37 6.92 -18 -1 5 -1.57 6.05 -18 1 5 5.17 6.25 -18 -1 5 3.13 6.41 -18 1 5 3.75 6.27 -18 1 4 15.19 6.89 -18 1 4 5.33 6.20 -18 -1 4 8.70 6.24 -18 -1 4 12.51 6.78 -18 -1 3 -6.35 6.04 -18 -1 3 -0.05 6.20 -18 1 3 -4.65 6.40 -18 -1 2 0.10 6.00 -18 1 2 -2.40 6.34 -18 1 1 -8.90 5.83 -18 -1 1 6.26 6.65 -18 1 0 -6.22 6.17 -18 -1 0 0.74 6.22 18 -1 0 1.20 3.53 18 1 0 2.06 5.84 18 -1 0 -6.55 5.29 -18 -1 -1 0.58 6.88 18 1 1 -0.64 4.86 -18 1 -1 3.03 7.13 18 1 1 -11.73 5.02 18 -1 1 1.79 4.94 18 -1 1 1.30 6.06 -18 1 -2 -1.62 7.24 -18 -1 -2 4.86 7.02 18 1 2 5.70 5.98 18 -1 2 -6.84 5.80 18 1 2 -5.08 6.23 18 -1 3 -5.49 6.26 -18 -1 -3 1.16 7.04 18 1 3 -5.21 6.37 -18 1 -3 -0.85 6.96 -18 2 5 1.89 6.45 -18 -2 5 6.22 6.37 -18 2 5 3.12 6.27 -18 -2 5 0.46 5.72 -18 -2 4 3.86 6.29 -18 2 4 3.25 5.96 -18 -2 4 -3.71 6.24 -18 2 4 0.67 6.19 -18 2 3 -8.65 5.88 -18 -2 3 1.12 5.90 -18 -2 3 -7.75 5.74 -18 -2 2 11.74 6.48 -18 2 2 -8.56 6.32 -18 2 1 -3.78 6.60 -18 -2 1 13.61 6.89 -18 -2 0 -3.39 6.30 -18 2 0 4.67 6.89 18 2 0 4.04 6.04 18 -2 0 14.21 6.78 18 -2 0 11.22 4.07 18 -2 1 0.25 5.06 18 -2 1 9.92 6.35 -18 -2 -1 -0.36 6.65 -18 2 -1 -9.19 6.25 18 2 1 -5.93 5.41 18 2 2 11.67 7.01 18 -2 2 20.81 7.59 -18 -2 -2 13.31 7.58 -18 2 -2 7.51 7.57 18 2 2 23.96 6.03 -18 -2 -3 44.20 9.20 18 -2 3 57.54 9.95 18 2 3 45.41 8.91 -18 2 -3 30.05 8.94 -18 -3 5 -4.27 5.91 -18 -3 5 12.06 6.37 -18 3 5 2.54 6.81 -18 3 5 12.89 6.97 -18 3 4 0.17 6.37 -18 -3 4 0.66 5.99 -18 -3 4 -0.26 6.02 -18 3 4 -0.03 6.44 -18 3 3 -6.85 5.95 -18 -3 3 -14.43 4.92 -18 -3 3 -5.18 5.81 -18 3 2 -6.40 5.92 -18 -3 2 0.35 6.29 -18 -3 1 3.31 6.19 -18 3 1 -0.81 7.11 18 -3 0 0.02 3.88 18 -3 0 8.44 6.04 -18 -3 0 -1.78 6.26 -18 3 0 6.06 7.26 -18 3 -1 2.06 7.22 18 -3 1 -5.37 4.95 18 -3 1 -1.37 6.40 18 3 1 3.69 5.95 -18 -3 -1 -3.77 6.58 -18 -3 -2 7.47 7.59 18 -3 2 2.31 6.86 -18 3 -2 7.14 7.80 18 3 2 9.90 6.75 18 3 3 -1.65 6.67 -18 3 -3 0.88 7.48 -18 -3 -3 13.17 7.77 18 -3 3 -5.27 6.75 -18 4 5 -1.45 6.61 -18 -4 5 -12.11 5.52 -18 4 5 -1.83 6.85 -18 -4 5 4.85 6.25 -18 4 4 2.99 6.70 -18 -4 4 -2.33 6.07 -18 -4 4 -4.76 5.67 -18 -4 3 0.07 6.10 -18 4 3 -3.05 6.23 -18 -4 3 0.26 6.10 -18 -4 2 -12.10 5.57 -18 4 2 -0.83 6.58 -18 -4 1 5.76 6.43 -18 4 1 0.20 6.95 -18 -4 0 4.40 6.44 18 -4 0 -0.24 5.81 -18 4 0 3.33 7.14 18 -4 1 0.81 6.11 18 -4 1 11.28 5.46 -18 4 -1 4.62 7.27 18 4 1 6.75 6.19 18 4 1 5.66 4.38 -18 -4 -1 -6.59 6.25 -18 -4 -2 -1.62 7.23 18 4 2 3.74 6.62 18 -4 2 -0.98 6.82 -18 4 -2 18.27 8.36 -18 5 4 0.24 6.62 -18 -5 4 2.16 6.19 -18 -5 4 -5.22 6.14 -18 -5 3 11.13 6.13 -18 -5 3 13.36 6.88 -18 5 3 1.85 6.53 -18 -5 2 1.10 6.35 -18 5 2 7.91 7.12 -18 -5 1 -9.40 5.63 -18 5 1 4.04 7.31 -18 5 0 -1.90 7.06 18 -5 0 0.01 6.34 -18 -5 0 5.52 6.86 18 -5 1 -7.83 5.80 18 5 1 0.78 5.83 -18 5 -1 5.61 7.58 -18 -5 -1 -10.51 6.25 18 -5 2 9.74 6.96 -18 -5 -2 5.22 7.18 -18 5 -2 -8.25 7.20 18 5 2 10.50 6.67 -18 -6 4 0.48 6.08 -18 -6 4 -3.98 5.95 -18 6 4 2.92 6.78 -18 6 3 3.41 6.81 -18 -6 3 1.44 6.43 -18 6 2 -0.64 7.11 -18 -6 2 4.01 6.70 -18 -6 1 -2.28 6.24 -18 6 1 3.23 7.33 -18 6 0 -1.30 7.28 -18 -6 0 -0.81 6.55 18 -6 0 -1.64 5.82 -18 6 -1 6.75 8.06 18 -6 1 9.22 7.35 -18 -6 -1 -2.35 6.91 -18 -7 3 -0.89 6.50 -18 7 3 3.23 7.01 -18 -7 2 3.31 6.84 -18 7 2 -9.41 6.65 -18 -7 1 -5.21 6.74 -18 7 1 10.68 8.09 18 -7 0 19.65 7.44 -18 -7 0 12.09 7.64 -18 7 0 10.01 8.08 -19 0 4 8.14 7.05 -19 0 4 -9.57 6.24 -19 0 3 -4.81 6.34 -19 0 2 5.71 6.69 -19 0 1 -4.37 6.32 -19 0 0 9.19 7.04 -19 0 -1 -10.42 6.51 19 0 1 -12.07 5.91 -19 0 -2 86.78 11.50 19 0 2 63.13 9.66 -19 -1 4 -5.00 6.13 -19 -1 4 6.63 6.75 -19 1 4 2.32 6.69 -19 1 3 0.55 6.68 -19 -1 3 4.51 6.73 -19 -1 2 -0.32 6.26 -19 1 2 7.83 6.94 -19 1 1 8.54 6.97 -19 -1 1 3.44 6.74 -19 1 0 2.91 7.23 -19 -1 0 5.01 7.10 -19 -1 -1 0.78 7.18 -19 1 -1 9.14 7.81 19 -1 1 -0.70 6.31 19 1 1 3.93 6.33 -19 -1 -2 4.70 7.67 19 1 2 -6.29 6.16 -19 1 -2 10.89 8.09 19 -1 2 -3.31 6.47 -19 -2 4 -2.88 6.18 -19 -2 4 -8.50 6.04 -19 2 4 2.13 6.65 -19 -2 3 -11.13 5.59 -19 2 3 2.85 6.92 -19 2 2 -11.24 6.50 -19 -2 2 -2.70 6.56 -19 2 1 -3.57 7.17 -19 -2 1 2.91 6.90 -19 -2 0 -0.08 6.83 19 -2 0 1.40 5.96 -19 2 0 0.69 6.98 19 -2 1 10.91 6.61 19 2 1 15.13 6.78 -19 -2 -1 8.23 7.53 -19 2 -1 3.11 7.83 -19 2 -2 -0.31 7.89 -19 -2 -2 -6.67 6.92 19 2 2 8.93 6.97 19 -2 2 3.23 7.08 -19 -3 4 4.62 6.72 -19 -3 4 4.11 6.76 -19 3 4 2.22 6.95 -19 3 3 -5.49 6.61 -19 -3 3 -9.30 5.97 -19 -3 2 -4.03 6.23 -19 3 2 7.08 7.28 -19 3 1 -0.39 7.11 -19 -3 1 -2.84 6.39 19 -3 0 9.56 6.73 -19 3 0 5.13 7.49 -19 -3 0 -1.66 6.84 -19 -3 -1 0.41 6.89 19 -3 1 -0.38 6.39 19 3 1 -3.88 5.87 -19 3 -1 -5.90 7.74 -19 -4 3 12.58 7.02 -19 4 3 -5.70 6.88 -19 -4 2 0.55 6.65 -19 4 2 10.86 7.56 -19 -4 1 -6.96 6.28 -19 4 1 2.97 7.36 -19 4 0 -3.65 7.18 19 -4 0 9.45 6.54 -19 -4 0 -3.21 6.59 19 -4 1 -4.32 5.86 -19 4 -1 8.53 7.88 -19 -4 -1 -13.11 6.32 -19 5 2 1.41 7.44 -19 -5 2 -4.21 6.45 -19 -5 1 -7.28 6.12 -19 5 1 8.28 7.78 -19 5 0 -3.78 7.17 -19 -5 0 -9.68 6.16 19 -5 0 4.15 6.83 -20 0 2 21.83 8.23 -20 0 1 -13.20 6.51 -20 -1 2 -3.81 6.58 -20 1 2 -3.67 7.30 -20 -1 1 4.87 6.91 -20 1 1 10.82 7.49 -20 1 0 -11.29 6.67 -20 -1 0 -4.63 6.81 -20 2 2 -4.88 6.86 -20 -2 2 6.11 7.29 -20 -2 1 6.52 7.41 -20 2 1 7.14 7.66 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 11280 _shelx_res_file ; JTM_ElBakri_b.res created by SHELXL-2014/7 TITL JTM_ElBakri_b.res in Pc REM Old TITL nabil7n REM SHELXT solution in Pc REM R1 0.167, Rweak 0.010, Alpha 0.011, Orientation as input REM Flack x = 0.292 ( 1.939 ) from Parsons' quotients REM Formula found by SHELXT: C30 N7 O3 CELL 0.71073 14.1447 11.8380 7.4252 90.000 96.681 90.000 ZERR 4.000 0.0014 0.0012 0.0008 0.000 0.007 0.000 LATT -1 SYMM X, -Y, 1/2+Z SFAC C H N O UNIT 56 44 12 12 TEMP -93.00 L.S. 5 BOND $H LIST 4 FMAP 2 PLAN 5 OMIT 1 0 0 OMIT -1 0 0 OMIT 1 1 0 OMIT -1 1 0 OMIT 2 1 0 OMIT -2 1 0 EQIV $1 x, -y, z+1/2 HTAB N2 O5_$1 HTAB C2 O4_$1 EQIV $2 x-1, -y+1, z-1/2 HTAB C4 O6_$2 EQIV $3 x, -y+1, z-1/2 HTAB N4 O2_$3 HTAB C16 O1_$3 EQIV $4 x+1, -y, z+1/2 HTAB C18 O3_$4 CONF ACTA 61 WGHT 0.062200 FVAR 0.34589 O1 4 0.464994 0.769361 0.474011 11.00000 0.04943 0.02759 = 0.06692 -0.00715 -0.00564 -0.01246 O2 4 0.545460 0.619744 0.557937 11.00000 0.03543 0.03782 = 0.06749 -0.00097 -0.02314 -0.00624 O3 4 -0.202236 0.375060 -0.094310 11.00000 0.02396 0.03001 = 0.03554 0.00366 -0.00534 -0.00130 N1 3 0.229322 0.276633 0.235719 11.00000 0.01565 0.02648 = 0.03247 0.00072 -0.00234 0.00029 AFIX 3 H2A 2 0.351844 0.244281 0.361256 11.00000 -1.20000 AFIX 0 N2 3 0.317926 0.303872 0.314122 11.00000 0.02748 0.01200 = 0.03311 0.00357 -0.00403 -0.00116 N3 3 0.474444 0.666775 0.479666 11.00000 0.03188 0.02595 = 0.03603 -0.00288 0.00646 -0.01186 C1 1 0.331939 0.417760 0.322417 11.00000 0.02294 0.02447 = 0.02372 0.00212 0.00297 0.00144 C2 1 0.408433 0.480526 0.398544 11.00000 0.01808 0.03419 = 0.02513 0.00690 0.00146 0.00729 AFIX 43 H2 2 0.465446 0.445928 0.452296 11.00000 -1.20000 AFIX 0 C3 1 0.397755 0.595380 0.392458 11.00000 0.02166 0.01888 = 0.02798 -0.00010 -0.00002 -0.00950 C4 1 0.314609 0.649663 0.312113 11.00000 0.02457 0.01510 = 0.02955 0.00090 -0.00054 0.00186 AFIX 43 H4 2 0.310633 0.729774 0.311512 11.00000 -1.20000 AFIX 0 C5 1 0.239614 0.586216 0.234944 11.00000 0.01873 0.02412 = 0.02282 -0.00081 -0.00002 0.00018 AFIX 43 H5 2 0.183437 0.621596 0.179016 11.00000 -1.20000 AFIX 0 C6 1 0.247311 0.466653 0.240007 11.00000 0.01576 0.01841 = 0.01994 0.00024 0.00192 0.00109 C7 1 0.184840 0.372828 0.191953 11.00000 0.01871 0.02080 = 0.01611 0.00211 0.00061 -0.00014 C8 1 0.085304 0.374947 0.109112 11.00000 0.01931 0.02564 = 0.01745 -0.00039 0.00207 0.00266 C9 1 0.049134 0.462868 -0.000292 11.00000 0.02557 0.02469 = 0.02367 0.00290 0.00604 -0.00509 AFIX 43 H9 2 0.090422 0.522336 -0.026891 11.00000 -1.20000 AFIX 0 C10 1 -0.046811 0.466795 -0.073177 11.00000 0.02353 0.02371 = 0.02943 -0.00015 -0.00307 -0.00091 AFIX 43 H10 2 -0.070182 0.527693 -0.148981 11.00000 -1.20000 AFIX 0 C11 1 -0.106665 0.380823 -0.033014 11.00000 0.02001 0.01869 = 0.02287 -0.00285 0.00283 -0.00117 C12 1 -0.072060 0.291635 0.078434 11.00000 0.03109 0.02271 = 0.02869 0.00372 -0.00356 -0.00386 AFIX 43 H12 2 -0.113511 0.232415 0.105369 11.00000 -1.20000 AFIX 0 C13 1 0.022874 0.289566 0.149783 11.00000 0.02938 0.02308 = 0.02095 0.00322 -0.00187 -0.00013 AFIX 43 H13 2 0.045862 0.229334 0.227378 11.00000 -1.20000 AFIX 0 C14 1 -0.240365 0.461599 -0.216251 11.00000 0.03532 0.04200 = 0.04063 0.01355 -0.01228 -0.00021 AFIX 137 H14A 2 -0.209174 0.458627 -0.327298 11.00000 -1.50000 H14B 2 -0.229078 0.535602 -0.158581 11.00000 -1.50000 H14C 2 -0.308963 0.449851 -0.246409 11.00000 -1.50000 AFIX 0 O4 4 0.520984 -0.269204 0.087852 11.00000 0.04223 0.02756 = 0.06674 -0.00535 -0.00081 -0.00995 O5 4 0.443656 -0.120053 -0.012132 11.00000 0.02884 0.04548 = 0.05269 0.00129 -0.00864 -0.00432 O6 4 1.175588 0.126594 0.713804 11.00000 0.02295 0.02957 = 0.04114 -0.00388 -0.00824 -0.00146 N4 3 0.664765 0.195088 0.257149 11.00000 0.01964 0.02367 = 0.03384 0.00131 -0.00335 0.00691 AFIX 3 H4A 2 0.627743 0.254352 0.214505 11.00000 -1.20000 AFIX 0 N5 3 0.753291 0.223070 0.338696 11.00000 0.02646 0.02079 = 0.02727 -0.00094 -0.00088 -0.00488 N6 3 0.513314 -0.167007 0.075802 11.00000 0.02708 0.03737 = 0.03221 -0.00377 0.00274 -0.00976 C15 1 0.652789 0.082677 0.238898 11.00000 0.01557 0.01976 = 0.02349 -0.00481 0.00326 0.00092 C16 1 0.575410 0.019159 0.156710 11.00000 0.02603 0.02008 = 0.02370 -0.00393 0.00136 -0.00525 AFIX 43 H16 2 0.518629 0.052761 0.099872 11.00000 -1.20000 AFIX 0 C17 1 0.589152 -0.095782 0.165846 11.00000 0.02236 0.02763 = 0.02093 -0.01027 0.00360 -0.00865 C18 1 0.669988 -0.150578 0.251554 11.00000 0.03266 0.02202 = 0.02942 -0.00200 0.01340 -0.00579 AFIX 43 H18 2 0.672985 -0.230683 0.257401 11.00000 -1.20000 AFIX 0 C19 1 0.745150 -0.085242 0.327270 11.00000 0.02736 0.01897 = 0.02570 0.00497 0.00450 0.00441 AFIX 43 H19 2 0.801339 -0.119816 0.384763 11.00000 -1.20000 AFIX 0 C20 1 0.737609 0.032007 0.318352 11.00000 0.02371 0.01677 = 0.01514 -0.00010 0.00248 0.00309 C21 1 0.797355 0.125184 0.379435 11.00000 0.02604 0.01398 = 0.02337 0.00171 0.00195 -0.00076 C22 1 0.896002 0.124443 0.466213 11.00000 0.02225 0.01269 = 0.02232 -0.00159 0.00218 -0.00160 C23 1 0.957746 0.037964 0.429784 11.00000 0.02732 0.02580 = 0.02825 -0.00253 0.00070 -0.00194 AFIX 43 H23 2 0.934811 -0.021277 0.350096 11.00000 -1.20000 AFIX 0 C24 1 1.051767 0.036120 0.506790 11.00000 0.02688 0.03230 = 0.02693 -0.00217 0.00747 0.00307 AFIX 43 H24 2 1.092893 -0.023157 0.478710 11.00000 -1.20000 AFIX 0 C25 1 1.085187 0.121025 0.624543 11.00000 0.02060 0.03153 = 0.01804 0.00138 -0.00492 -0.00287 C26 1 1.024796 0.207685 0.666743 11.00000 0.03213 0.02958 = 0.01812 -0.00184 0.00231 -0.00954 AFIX 43 H26 2 1.047862 0.265228 0.749626 11.00000 -1.20000 AFIX 0 C27 1 0.931116 0.209884 0.587780 11.00000 0.02963 0.02039 = 0.02858 -0.00075 0.00515 -0.00035 AFIX 43 H27 2 0.890308 0.269478 0.615897 11.00000 -1.20000 AFIX 0 C28 1 1.240633 0.042391 0.667538 11.00000 0.02429 0.05421 = 0.05423 -0.01036 -0.00479 0.00416 AFIX 137 H28A 2 1.248287 0.048355 0.538394 11.00000 -1.50000 H28B 2 1.215908 -0.032616 0.692569 11.00000 -1.50000 H28C 2 1.302425 0.053539 0.739843 11.00000 -1.50000 AFIX 0 HKLF 4 REM JTM_ElBakri_b.res in Pc REM R1 = 0.0639 for 2803 Fo > 4sig(Fo) and 0.1992 for all 6667 data REM 363 parameters refined using 2 restraints END WGHT 0.0622 0.0000 REM Highest difference peak 0.457, deepest hole -0.317, 1-sigma level 0.066 Q1 1 0.0227 0.4601 0.1608 11.00000 0.05 0.46 Q2 1 1.0612 0.2040 0.4753 11.00000 0.05 0.44 Q3 1 0.9613 0.2173 0.4177 11.00000 0.05 0.44 Q4 1 -0.0426 0.2842 -0.0621 11.00000 0.05 0.41 Q5 1 1.0226 0.0355 0.6644 11.00000 0.05 0.41 ; _shelx_res_checksum 55065 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, 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 0.4650(5) 0.7694(5) 0.4740(8) 0.0490(17) Uani d 1 O O2 0.5455(5) 0.6197(5) 0.5579(8) 0.0492(19) Uani d 1 O O3 -0.2022(4) 0.3751(4) -0.0943(6) 0.0305(14) Uani d 1 N N1 0.2293(4) 0.2766(6) 0.2357(7) 0.0253(17) Uani d 1 H H2A 0.3518 0.2443 0.3613 0.030 Uiso d 1 N N2 0.3179(4) 0.3039(6) 0.3141(7) 0.0248(15) Uani d 1 N N3 0.4744(5) 0.6668(7) 0.4797(9) 0.0311(16) Uani d 1 C C1 0.3319(5) 0.4178(7) 0.3224(9) 0.0237(18) Uani d 1 C C2 0.4084(5) 0.4805(7) 0.3985(9) 0.0259(19) Uani d 1 H H2 0.4654 0.4459 0.4523 0.031 Uiso calc 1 C C3 0.3978(6) 0.5954(7) 0.3925(9) 0.0231(17) Uani d 1 C C4 0.3146(6) 0.6497(6) 0.3121(9) 0.0234(18) Uani d 1 H H4 0.3106 0.7298 0.3115 0.028 Uiso calc 1 C C5 0.2396(5) 0.5862(6) 0.2349(9) 0.0221(18) Uani d 1 H H5 0.1834 0.6216 0.1790 0.026 Uiso calc 1 C C6 0.2473(5) 0.4667(7) 0.2400(8) 0.0180(17) Uani d 1 C C7 0.1848(6) 0.3728(6) 0.1920(9) 0.019(2) Uani d 1 C C8 0.0853(6) 0.3749(7) 0.1091(9) 0.021(2) Uani d 1 C C9 0.0491(4) 0.4629(5) -0.0003(8) 0.0244(14) Uani d 1 H H9 0.0904 0.5223 -0.0269 0.029 Uiso calc 1 C C10 -0.0468(4) 0.4668(5) -0.0732(9) 0.0260(14) Uani d 1 H H10 -0.0702 0.5277 -0.1490 0.031 Uiso calc 1 C C11 -0.1067(6) 0.3808(6) -0.0330(9) 0.0205(19) Uani d 1 C C12 -0.0721(4) 0.2916(5) 0.0784(8) 0.0281(15) Uani d 1 H H12 -0.1135 0.2324 0.1054 0.034 Uiso calc 1 C C13 0.0229(4) 0.2896(5) 0.1498(8) 0.0248(14) Uani d 1 H H13 0.0459 0.2293 0.2274 0.030 Uiso calc 1 C C14 -0.2404(5) 0.4616(6) -0.2163(10) 0.0406(18) Uani d 1 H H14A -0.2092 0.4586 -0.3273 0.061 Uiso calc 1 H H14B -0.2291 0.5356 -0.1586 0.061 Uiso calc 1 H H14C -0.3090 0.4499 -0.2464 0.061 Uiso calc 1 O O4 0.5210(5) -0.2692(5) 0.0879(8) 0.0461(16) Uani d 1 O O5 0.4437(4) -0.1201(5) -0.0121(8) 0.0434(18) Uani d 1 O O6 1.1756(4) 0.1266(4) 0.7138(6) 0.0322(14) Uani d 1 N N4 0.6648(4) 0.1951(6) 0.2571(7) 0.0262(15) Uani d 1 H H4A 0.6277 0.2544 0.2145 0.031 Uiso d 1 N N5 0.7533(4) 0.2231(6) 0.3387(7) 0.0252(17) Uani d 1 N N6 0.5133(5) -0.1670(8) 0.0758(8) 0.0323(17) Uani d 1 C C15 0.6528(5) 0.0827(6) 0.2389(9) 0.0195(16) Uani d 1 C C16 0.5754(5) 0.0192(6) 0.1567(9) 0.0234(18) Uani d 1 H H16 0.5186 0.0528 0.0999 0.028 Uiso calc 1 C C17 0.5892(6) -0.0958(7) 0.1658(9) 0.0236(17) Uani d 1 C C18 0.6700(6) -0.1506(7) 0.2516(10) 0.0273(19) Uani d 1 H H18 0.6730 -0.2307 0.2574 0.033 Uiso calc 1 C C19 0.7451(6) -0.0852(6) 0.3273(9) 0.0239(18) Uani d 1 H H19 0.8013 -0.1198 0.3848 0.029 Uiso calc 1 C C20 0.7376(5) 0.0320(7) 0.3184(8) 0.0185(17) Uani d 1 C C21 0.7974(6) 0.1252(6) 0.3794(9) 0.021(2) Uani d 1 C C22 0.8960(6) 0.1244(6) 0.4662(9) 0.019(2) Uani d 1 C C23 0.9577(5) 0.0380(5) 0.4298(9) 0.0273(14) Uani d 1 H H23 0.9348 -0.0213 0.3501 0.033 Uiso calc 1 C C24 1.0518(5) 0.0361(5) 0.5068(8) 0.0284(15) Uani d 1 H H24 1.0929 -0.0232 0.4787 0.034 Uiso calc 1 C C25 1.0852(6) 0.1210(7) 0.6245(9) 0.024(2) Uani d 1 C C26 1.0248(4) 0.2077(5) 0.6667(8) 0.0267(15) Uani d 1 H H26 1.0479 0.2652 0.7496 0.032 Uiso calc 1 C C27 0.9311(4) 0.2099(5) 0.5878(8) 0.0261(14) Uani d 1 H H27 0.8903 0.2695 0.6159 0.031 Uiso calc 1 C C28 1.2406(5) 0.0424(7) 0.6675(11) 0.0450(19) Uani d 1 H H28A 1.2483 0.0484 0.5384 0.067 Uiso calc 1 H H28B 1.2159 -0.0326 0.6926 0.067 Uiso calc 1 H H28C 1.3024 0.0535 0.7398 0.067 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 0.049(4) 0.028(5) 0.067(4) -0.012(4) -0.006(3) -0.007(3) O2 0.035(4) 0.038(4) 0.067(4) -0.006(3) -0.023(3) -0.001(3) O3 0.024(3) 0.030(3) 0.036(3) -0.001(2) -0.005(2) 0.004(2) N1 0.016(3) 0.026(5) 0.032(3) 0.000(3) -0.002(3) 0.001(3) N2 0.027(4) 0.012(3) 0.033(3) -0.001(3) -0.004(3) 0.004(3) N3 0.032(4) 0.026(4) 0.036(4) -0.012(4) 0.006(3) -0.003(4) C1 0.023(4) 0.024(5) 0.024(4) 0.001(4) 0.003(3) 0.002(3) C2 0.018(4) 0.034(6) 0.025(4) 0.007(4) 0.001(3) 0.007(3) C3 0.022(4) 0.019(4) 0.028(4) -0.009(4) 0.000(3) 0.000(3) C4 0.025(4) 0.015(4) 0.030(4) 0.002(4) -0.001(3) 0.001(3) C5 0.019(4) 0.024(5) 0.023(4) 0.000(4) 0.000(3) -0.001(3) C6 0.016(4) 0.018(4) 0.020(3) 0.001(4) 0.002(3) 0.000(3) C7 0.019(5) 0.021(6) 0.016(4) 0.000(3) 0.001(4) 0.002(3) C8 0.019(5) 0.026(6) 0.017(4) 0.003(3) 0.002(4) 0.000(3) C9 0.026(3) 0.025(3) 0.024(3) -0.005(3) 0.006(3) 0.003(3) C10 0.024(4) 0.024(3) 0.029(3) -0.001(3) -0.003(3) 0.000(3) C11 0.020(5) 0.019(5) 0.023(4) -0.001(3) 0.003(3) -0.003(3) C12 0.031(4) 0.023(4) 0.029(3) -0.004(3) -0.004(3) 0.004(3) C13 0.029(4) 0.023(3) 0.021(3) 0.000(3) -0.002(3) 0.003(3) C14 0.035(4) 0.042(4) 0.041(4) 0.000(3) -0.012(3) 0.014(4) O4 0.042(4) 0.028(5) 0.067(4) -0.010(4) -0.001(3) -0.005(3) O5 0.029(4) 0.045(5) 0.053(4) -0.004(3) -0.009(3) 0.001(3) O6 0.023(3) 0.030(3) 0.041(3) -0.001(2) -0.008(2) -0.004(2) N4 0.020(4) 0.024(4) 0.034(3) 0.007(3) -0.003(3) 0.001(3) N5 0.026(4) 0.021(4) 0.027(3) -0.005(3) -0.001(3) -0.001(3) N6 0.027(4) 0.037(5) 0.032(4) -0.010(4) 0.003(3) -0.004(3) C15 0.016(4) 0.020(5) 0.023(3) 0.001(4) 0.003(3) -0.005(3) C16 0.026(4) 0.020(5) 0.024(4) -0.005(4) 0.001(3) -0.004(3) C17 0.022(4) 0.028(5) 0.021(3) -0.009(4) 0.004(3) -0.010(3) C18 0.033(5) 0.022(4) 0.029(4) -0.006(4) 0.013(4) -0.002(4) C19 0.027(5) 0.019(4) 0.026(4) 0.004(4) 0.004(3) 0.005(3) C20 0.024(4) 0.017(4) 0.015(3) 0.003(4) 0.002(3) 0.000(3) C21 0.026(6) 0.014(6) 0.023(4) -0.001(4) 0.002(4) 0.002(3) C22 0.022(5) 0.013(5) 0.022(4) -0.002(3) 0.002(4) -0.002(3) C23 0.027(4) 0.026(4) 0.028(3) -0.002(3) 0.001(3) -0.003(3) C24 0.027(4) 0.032(4) 0.027(3) 0.003(3) 0.007(3) -0.002(3) C25 0.021(5) 0.032(6) 0.018(4) -0.003(4) -0.005(4) 0.001(3) C26 0.032(4) 0.030(4) 0.018(3) -0.010(3) 0.002(3) -0.002(3) C27 0.030(4) 0.020(3) 0.029(3) 0.000(3) 0.005(3) -0.001(3) C28 0.024(4) 0.054(5) 0.054(5) 0.004(3) -0.005(3) -0.010(4) 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 _geom_angle_publ_flag C11 O3 C14 117.2(5) ? C7 N1 N2 106.8(7) y N1 N2 C1 112.1(6) ? N1 N2 H2A 113.8 ? C1 N2 H2A 133.6 ? O1 N3 O2 123.0(9) ? O1 N3 C3 119.1(8) ? O2 N3 C3 117.9(8) ? N2 C1 C2 130.9(7) ? N2 C1 C6 106.0(7) ? C2 C1 C6 123.0(7) ? C3 C2 C1 116.3(8) ? C3 C2 H2 121.8 ? C1 C2 H2 121.8 ? C2 C3 C4 123.4(8) ? C2 C3 N3 119.0(8) ? C4 C3 N3 117.5(7) ? C5 C4 C3 119.6(7) ? C5 C4 H4 120.2 ? C3 C4 H4 120.2 ? C4 C5 C6 118.8(8) ? C4 C5 H5 120.6 ? C6 C5 H5 120.6 ? C1 C6 C5 118.8(8) ? C1 C6 C7 104.9(7) ? C5 C6 C7 136.1(7) ? N1 C7 C6 110.1(7) ? N1 C7 C8 121.5(7) ? C6 C7 C8 128.4(7) ? C9 C8 C13 118.1(7) ? C9 C8 C7 122.0(7) ? C13 C8 C7 119.7(7) ? C8 C9 C10 121.8(6) ? C8 C9 H9 119.1 ? C10 C9 H9 119.1 ? C11 C10 C9 118.9(6) ? C11 C10 H10 120.6 ? C9 C10 H10 120.6 ? O3 C11 C10 124.7(6) ? O3 C11 C12 115.0(6) ? C10 C11 C12 120.4(7) ? C13 C12 C11 119.9(6) ? C13 C12 H12 120.1 ? C11 C12 H12 120.1 ? C12 C13 C8 120.9(6) ? C12 C13 H13 119.6 ? C8 C13 H13 119.6 ? O3 C14 H14A 109.5 ? O3 C14 H14B 109.5 ? H14A C14 H14B 109.5 ? O3 C14 H14C 109.5 ? H14A C14 H14C 109.5 ? H14B C14 H14C 109.5 ? C25 O6 C28 116.2(6) ? C15 N4 N5 112.5(6) ? C15 N4 H4A 131.8 ? N5 N4 H4A 115.3 ? C21 N5 N4 105.7(7) ? O4 N6 O5 122.7(9) ? O4 N6 C17 119.0(8) ? O5 N6 C17 118.3(8) ? N4 C15 C16 130.9(7) ? N4 C15 C20 106.7(6) ? C16 C15 C20 122.4(7) ? C17 C16 C15 114.1(8) ? C17 C16 H16 122.9 ? C15 C16 H16 122.9 ? C16 C17 C18 125.7(8) ? C16 C17 N6 117.1(8) ? C18 C17 N6 117.2(8) ? C19 C18 C17 118.3(7) ? C19 C18 H18 120.8 ? C17 C18 H18 120.8 ? C18 C19 C20 119.2(8) ? C18 C19 H19 120.4 ? C20 C19 H19 120.4 ? C19 C20 C15 120.1(8) ? C19 C20 C21 135.6(7) ? C15 C20 C21 104.3(7) ? N5 C21 C20 110.8(7) ? N5 C21 C22 120.0(7) ? C20 C21 C22 129.1(7) ? C23 C22 C27 118.1(7) ? C23 C22 C21 120.3(6) ? C27 C22 C21 121.6(6) ? C24 C23 C22 121.7(6) ? C24 C23 H23 119.2 ? C22 C23 H23 119.2 ? C25 C24 C23 119.5(6) ? C25 C24 H24 120.3 ? C23 C24 H24 120.3 ? O6 C25 C24 125.0(7) ? O6 C25 C26 114.7(7) ? C24 C25 C26 120.3(7) ? C27 C26 C25 120.0(6) ? C27 C26 H26 120.0 ? C25 C26 H26 120.0 ? C26 C27 C22 120.4(6) ? C26 C27 H27 119.8 ? C22 C27 H27 119.8 ? O6 C28 H28A 109.5 ? O6 C28 H28B 109.5 ? H28A C28 H28B 109.5 ? O6 C28 H28C 109.5 ? H28A C28 H28C 109.5 ? H28B C28 H28C 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O1 N3 1.222(8) ? O2 N3 1.233(9) ? O3 C11 1.377(9) ? O3 C14 1.431(7) ? N1 C7 1.323(9) y N1 N2 1.358(8) y N2 C1 1.363(10) y N2 H2A 0.9007 ? N3 C3 1.465(10) ? C1 C2 1.378(11) y C1 C6 1.404(10) y C2 C3 1.368(9) y C2 H2 0.9500 ? C3 C4 1.410(11) y C4 C5 1.370(10) y C4 H4 0.9500 ? C5 C6 1.420(10) y C5 H5 0.9500 ? C6 C7 1.438(10) y C7 C8 1.470(11) ? C8 C9 1.381(9) ? C8 C13 1.398(9) ? C9 C10 1.402(8) ? C9 H9 0.9500 ? C10 C11 1.378(9) ? C10 H10 0.9500 ? C11 C12 1.395(9) ? C12 C13 1.385(8) ? C12 H12 0.9500 ? C13 H13 0.9500 ? C14 H14A 0.9800 ? C14 H14B 0.9800 ? C14 H14C 0.9800 ? O4 N6 1.217(9) ? O5 N6 1.248(8) ? O6 C25 1.372(9) ? O6 C28 1.425(8) ? N4 C15 1.346(10) ? N4 N5 1.367(8) ? N4 H4A 0.9100 ? N5 C21 1.334(9) ? N6 C17 1.463(10) ? C15 C16 1.407(10) ? C15 C20 1.408(10) ? C16 C17 1.375(10) ? C16 H16 0.9500 ? C17 C18 1.401(12) ? C18 C19 1.380(11) ? C18 H18 0.9500 ? C19 C20 1.393(10) ? C19 H19 0.9500 ? C20 C21 1.431(10) ? C21 C22 1.467(12) ? C22 C23 1.392(9) ? C22 C27 1.407(9) ? C23 C24 1.385(8) ? C23 H23 0.9500 ? C24 C25 1.379(9) ? C24 H24 0.9500 ? C25 C26 1.394(9) ? C26 C27 1.385(7) ? C26 H26 0.9500 ? C27 H27 0.9500 ? C28 H28A 0.9800 ? C28 H28B 0.9800 ? C28 H28C 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 N2 H2A O5 2 0.90 2.11 3.005(9) 173 C2 H2 O4 2 0.95 2.41 3.201(10) 140 C4 H4 O6 2_464 0.95 2.60 3.329(9) 134 N4 H4A O2 2_564 0.91 2.15 3.043(9) 168 C16 H16 O1 2_564 0.95 2.39 3.171(10) 139 C18 H18 O3 2_655 0.95 2.61 3.340(10) 134 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 C7 N1 N2 C1 0.1(7) N1 N2 C1 C2 176.2(7) N1 N2 C1 C6 -1.4(7) N2 C1 C2 C3 -176.4(7) C6 C1 C2 C3 0.9(10) C1 C2 C3 C4 -0.7(10) C1 C2 C3 N3 176.7(6) O1 N3 C3 C2 179.9(7) O2 N3 C3 C2 -1.1(9) O1 N3 C3 C4 -2.5(9) O2 N3 C3 C4 176.5(6) C2 C3 C4 C5 -0.1(10) N3 C3 C4 C5 -177.6(6) C3 C4 C5 C6 0.8(10) N2 C1 C6 C5 177.6(6) C2 C1 C6 C5 -0.2(10) N2 C1 C6 C7 2.0(6) C2 C1 C6 C7 -175.8(6) C4 C5 C6 C1 -0.6(9) C4 C5 C6 C7 173.2(6) N2 N1 C7 C6 1.3(7) N2 N1 C7 C8 -177.9(6) C1 C6 C7 N1 -2.1(7) C5 C6 C7 N1 -176.5(7) C1 C6 C7 C8 177.0(6) C5 C6 C7 C8 2.6(11) N1 C7 C8 C9 -153.8(7) C6 C7 C8 C9 27.2(10) N1 C7 C8 C13 30.2(9) C6 C7 C8 C13 -148.8(7) C13 C8 C9 C10 -1.4(9) C7 C8 C9 C10 -177.4(6) C8 C9 C10 C11 0.5(9) C14 O3 C11 C10 3.6(9) C14 O3 C11 C12 -177.0(6) C9 C10 C11 O3 179.4(6) C9 C10 C11 C12 0.0(9) O3 C11 C12 C13 -179.2(6) C10 C11 C12 C13 0.2(9) C11 C12 C13 C8 -1.1(9) C9 C8 C13 C12 1.7(9) C7 C8 C13 C12 177.8(6) C15 N4 N5 C21 -2.4(7) N5 N4 C15 C16 -176.9(6) N5 N4 C15 C20 1.9(7) N4 C15 C16 C17 -179.6(6) C20 C15 C16 C17 1.8(9) C15 C16 C17 C18 1.8(10) C15 C16 C17 N6 -177.3(5) O4 N6 C17 C16 -176.7(7) O5 N6 C17 C16 4.0(9) O4 N6 C17 C18 4.2(9) O5 N6 C17 C18 -175.1(6) C16 C17 C18 C19 -3.2(11) N6 C17 C18 C19 175.8(6) C17 C18 C19 C20 0.9(10) C18 C19 C20 C15 2.4(10) C18 C19 C20 C21 179.5(7) N4 C15 C20 C19 177.2(6) C16 C15 C20 C19 -3.9(10) N4 C15 C20 C21 -0.7(6) C16 C15 C20 C21 178.2(5) N4 N5 C21 C20 1.8(7) N4 N5 C21 C22 178.7(6) C19 C20 C21 N5 -178.2(7) C15 C20 C21 N5 -0.7(7) C19 C20 C21 C22 5.3(12) C15 C20 C21 C22 -177.2(7) N5 C21 C22 C23 -147.3(7) C20 C21 C22 C23 28.9(10) N5 C21 C22 C27 32.7(10) C20 C21 C22 C27 -151.0(7) C27 C22 C23 C24 -1.4(10) C21 C22 C23 C24 178.7(6) C22 C23 C24 C25 0.9(9) C28 O6 C25 C24 5.4(9) C28 O6 C25 C26 -177.1(6) C23 C24 C25 O6 177.7(6) C23 C24 C25 C26 0.4(10) O6 C25 C26 C27 -178.7(5) C24 C25 C26 C27 -1.1(9) C25 C26 C27 C22 0.6(8) C23 C22 C27 C26 0.6(9) C21 C22 C27 C26 -179.5(6) _cod_database_fobs_code 2242749