#------------------------------------------------------------------------------ #$Date: 2018-01-13 08:33:57 +0200 (Sat, 13 Jan 2018) $ #$Revision: 205185 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/86/1548677.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_1548677 loop_ _publ_author_name 'Shafer, Sarah K.' 'Lynch, Will E.' 'Padgett, Clifford W.' _publ_section_title ; 2-Chloro-4-nitropyridine N-oxide ; _journal_coeditor_code TK4042 _journal_issue 1 _journal_name_full IUCrData _journal_page_first x180016 _journal_paper_doi 10.1107/S2414314618000160 _journal_volume 3 _journal_year 2018 _chemical_formula_iupac 'C5 H3 Cl N2 O3' _chemical_formula_moiety 'C5 H3 Cl N2 O3' _chemical_formula_sum 'C5 H3 Cl N2 O3' _chemical_formula_weight 174.54 _chemical_name_systematic '2-Chloro-4-nitropyridine N-oxide' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 5.9238(14) _cell_length_b 9.735(2) _cell_length_c 22.444(8) _cell_measurement_reflns_used 2672 _cell_measurement_temperature 176(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 2.1 _cell_volume 1294.3(6) _computing_cell_refinement ; CrystalClear (Rigaku, 2009) ; _computing_data_collection ; CrystalClear (Rigaku, 2009) ; _computing_data_reduction ; CrystalClear (Rigaku, 2009) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015a) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015b) ; _diffrn_ambient_temperature 176 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Rigaku XtalLab mini CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1107 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 11029 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.459 _diffrn_reflns_theta_min 1.815 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.540 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (REQAB;Rigaku, 1998) ; _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method "'not measured" _exptl_crystal_description Prism _exptl_crystal_F_000 704 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.330 _refine_diff_density_min -0.331 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 1484 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.064 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0496 _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^)+(0.0560P)^2^+0.2450P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1204 _refine_ls_wR_factor_ref 0.1316 _reflns_number_gt 1088 _reflns_number_total 1485 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file tk4042sup1.cif _cod_data_source_block I _cod_original_cell_volume 1294.3(5) _cod_database_code 1548677 _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 0.838 _shelx_estimated_absorpt_t_max 0.958 _shelx_hkl_file ; 0 0 -2 0.93 0.58 0 0 2 0.06 0.98 0 0 -3 3.65 1.85 0 0 3 1.68 1.85 0 0 3 -0.52 1.62 0 0 -3 0.29 0.93 0 0 -4 7973.35 185.36 0 0 4 6786.14 158.21 0 0 4 6438.41 146.51 0 0 -4 6309.32 143.91 0 0 -5 -1.91 4.57 0 0 5 1.85 5.33 0 0 5 -0.64 1.62 0 0 -5 0.52 1.85 0 0 -6 349.41 21.07 0 0 6 298.06 14.76 0 0 -7 2.37 5.44 0 0 7 1.22 4.98 0 0 -8 5125.75 131.98 0 0 8 4437.12 112.71 0 0 8 4725.81 125.73 0 0 -9 7.29 11.75 0 0 9 1.10 9.44 0 0 9 1.68 1.39 0 0 -10 1365.68 99.05 0 0 10 1065.71 58.23 0 0 10 1228.72 65.01 0 0 -11 -0.23 3.76 0 0 11 5.62 4.75 0 0 11 1.68 1.51 0 0 -12 3.36 5.04 0 0 12 2.66 4.46 0 0 12 -0.06 1.62 0 0 -13 -2.32 4.86 0 0 13 -4.52 4.28 0 0 13 2.89 1.79 0 0 -14 92.27 18.99 0 0 14 81.22 12.39 0 0 14 72.59 18.35 0 0 -15 -1.97 6.25 0 0 15 1.68 4.69 0 0 15 -0.58 1.68 0 0 -16 15.92 9.20 0 0 16 2.37 4.98 0 0 16 5.50 2.03 0 0 -17 2.20 6.66 0 0 17 -0.41 1.74 0 0 -18 206.77 24.14 0 0 18 178.06 20.96 0 0 18 163.76 22.92 0 0 -19 -4.34 8.39 0 0 -20 484.05 55.69 0 0 20 436.59 50.19 0 0 -21 -7.18 7.70 0 0 21 6.83 7.64 0 0 -22 138.52 20.55 0 0 22 119.02 19.22 0 0 -23 3.07 8.80 0 0 23 1.85 7.06 0 0 -24 251.52 42.61 0 0 24 199.19 35.14 0 0 -25 7.29 13.14 0 0 25 -4.40 7.24 0 0 -26 57.71 19.91 0 0 26 42.89 15.86 0 0 -27 12.85 13.31 0 0 27 2.95 9.49 0 0 -28 224.26 33.00 0 0 28 209.15 61.53 0 0 29 5.15 10.07 0 1 0 3.07 1.10 0 1 0 -0.12 0.93 0 -1 0 -1.27 0.98 0 1 0 2.78 1.45 0 -1 0 0.41 0.98 0 1 1 -0.06 0.64 0 -1 -1 0.81 0.98 0 1 -1 -0.06 0.81 0 1 1 0.69 0.69 0 1 -1 1.74 1.16 0 -1 1 0.46 1.22 0 1 -1 -0.41 0.81 0 -1 1 0.35 0.41 0 -1 -1 0.41 0.81 0 1 -2 1.22 1.45 0 1 2 0.52 0.93 0 -1 -2 0.29 1.16 0 1 2 0.35 1.51 0 -1 2 1.56 2.37 0 1 -2 0.98 0.98 0 -1 2 0.41 0.52 0 -1 -2 0.00 1.74 0 1 -3 0.58 1.27 0 -1 -3 1.45 1.91 0 1 3 1.33 2.08 0 -1 3 -1.45 2.14 0 1 -3 0.64 0.58 0 -1 3 1.27 1.10 0 -1 -3 -0.29 1.91 0 1 -4 5.96 3.94 0 -1 -4 22.23 5.62 0 1 4 1.68 3.82 0 -1 4 5.90 4.11 0 1 -4 0.87 0.46 0 -1 4 4.92 1.33 0 -1 -4 0.29 2.14 0 1 -5 -0.17 3.36 0 -1 -5 1.33 2.95 0 1 5 -0.41 2.84 0 -1 5 -1.33 2.89 0 1 -5 -0.12 0.52 0 -1 5 0.12 0.52 0 -1 -5 3.36 2.43 0 1 -6 2.37 1.97 0 -1 -6 4.57 4.69 0 1 6 2.08 3.24 0 -1 6 0.00 3.30 0 1 -6 0.29 0.87 0 -1 6 -0.23 0.52 0 1 -7 5.67 3.18 0 -1 -7 0.93 3.59 0 1 7 -0.87 3.30 0 -1 7 -2.03 3.36 0 -1 7 0.46 0.87 0 -1 -7 0.17 2.14 0 1 -8 -3.76 3.94 0 -1 -8 -0.58 3.59 0 1 8 -1.33 3.36 0 -1 8 -0.81 3.94 0 -1 -8 -0.06 2.08 0 1 -9 1.97 2.60 0 -1 -9 -0.35 4.05 0 1 9 -1.91 3.53 0 -1 9 0.17 3.94 0 -1 9 0.64 0.81 0 -1 -9 -0.64 2.03 0 -1 -10 49.55 10.42 0 1 10 -1.85 3.88 0 -1 10 10.42 6.83 0 -1 10 -0.29 1.10 0 -1 -10 30.45 5.44 0 1 -11 -1.97 4.80 0 -1 -11 0.46 4.80 0 1 11 0.46 3.82 0 -1 11 2.03 4.28 0 -1 11 -0.29 1.10 0 -1 -11 3.13 3.53 0 1 -12 1.79 4.05 0 -1 -12 -2.49 4.75 0 1 12 -1.16 3.76 0 -1 12 0.23 3.88 0 -1 12 0.23 1.10 0 -1 -12 1.33 2.26 0 1 -13 8.16 3.99 0 -1 -13 -1.27 4.69 0 1 13 1.10 3.99 0 -1 13 -0.52 4.05 0 -1 13 0.29 1.04 0 1 -14 0.41 4.98 0 -1 -14 -0.75 4.92 0 1 14 -1.16 4.28 0 -1 14 1.45 4.46 0 -1 14 -0.06 1.04 0 1 -15 2.14 3.59 0 -1 -15 7.93 8.10 0 1 15 4.52 5.15 0 -1 15 3.24 5.04 0 1 15 1.45 1.62 0 -1 15 -0.29 1.10 0 1 -16 4.98 3.82 0 -1 -16 -0.29 6.02 0 1 16 0.00 5.04 0 -1 16 2.60 5.09 0 1 16 0.35 2.20 0 1 -17 2.84 6.83 0 -1 -17 -3.36 6.08 0 1 17 -2.78 5.44 0 -1 17 -1.74 5.27 0 1 17 -0.41 2.72 0 1 -18 -3.01 6.77 0 -1 -18 6.77 9.44 0 -1 18 6.31 8.86 0 1 18 -0.52 2.95 0 1 -19 -2.43 7.41 0 -1 -19 -0.12 6.60 0 1 19 -0.46 5.62 0 -1 19 4.23 6.71 0 1 19 0.41 2.66 0 1 -20 -0.12 7.64 0 -1 -20 1.04 7.00 0 1 20 -2.08 6.02 0 -1 20 1.56 6.95 0 1 20 -0.23 1.97 0 1 -21 3.07 7.76 0 -1 -21 5.04 8.10 0 1 21 5.38 7.06 0 -1 21 5.90 10.07 0 1 -22 -2.66 7.53 0 -1 -22 5.33 10.25 0 1 22 -0.75 6.31 0 -1 22 0.75 6.66 0 1 -23 -3.01 8.05 0 -1 -23 2.14 7.64 0 1 23 -2.60 7.24 0 -1 23 -2.84 6.95 0 1 -24 13.26 13.55 0 -1 -24 13.14 12.50 0 1 24 3.42 7.70 0 -1 24 2.72 8.28 0 1 -25 8.80 13.14 0 -1 -25 13.78 12.16 0 1 25 4.63 7.87 0 -1 25 -4.57 7.18 0 1 -26 -4.80 8.45 0 -1 -26 11.69 12.04 0 1 26 2.89 8.80 0 -1 26 -1.56 7.76 0 1 -27 0.23 9.26 0 -1 -27 -1.22 8.86 0 1 27 -1.56 9.09 0 -1 27 0.17 8.97 0 1 -28 4.46 10.07 0 -1 -28 1.22 11.00 0 1 28 3.99 9.73 0 -1 28 -0.81 9.44 0 1 -29 0.29 10.54 0 -1 -29 -1.74 11.23 0 -2 0 1255.92 35.25 0 -2 0 1209.79 34.27 0 -2 -1 24.08 3.94 0 -2 1 25.18 4.11 0 2 1 41.91 11.52 0 -2 1 43.18 7.12 0 -2 1 20.49 5.90 0 -2 -1 26.51 7.81 0 2 -2 84.80 14.59 0 -2 -2 69.58 5.21 0 2 2 88.57 19.91 0 -2 2 70.28 7.76 0 -2 2 65.24 5.85 0 -2 -2 59.05 7.06 0 2 -3 4127.72 101.59 0 -2 -3 3471.45 83.53 0 2 3 3879.26 99.05 0 -2 3 3424.10 86.25 0 -2 3 3311.50 82.78 0 -2 -3 3231.50 82.49 0 2 -4 24.25 7.64 0 -2 -4 16.61 3.42 0 2 4 24.20 6.19 0 -2 4 20.72 5.56 0 -2 4 18.18 5.33 0 -2 -4 16.03 4.57 0 2 -5 114.39 9.78 0 -2 -5 111.09 8.68 0 2 5 113.00 9.44 0 -2 5 97.77 10.13 0 -2 5 94.59 5.85 0 -2 -5 85.38 8.22 0 2 -6 20.03 7.12 0 -2 -6 13.89 4.52 0 2 6 13.84 4.63 0 -2 6 13.08 4.57 0 -2 6 11.29 3.13 0 -2 -6 9.55 4.57 0 2 -7 4.34 3.07 0 -2 -7 4.80 3.18 0 2 7 1.85 3.47 0 -2 7 3.94 5.67 0 -2 -7 -1.39 2.95 0 2 -8 137.77 44.63 0 -2 -8 117.40 23.50 0 2 8 102.58 9.78 0 -2 8 95.86 13.37 0 -2 8 85.90 5.79 0 -2 -8 98.81 10.25 0 2 -9 3581.43 185.36 0 -2 -9 3612.81 135.63 0 2 9 3278.62 160.12 0 -2 9 3185.43 123.59 0 -2 9 2827.68 133.31 0 -2 -9 2993.59 113.46 0 2 -10 86.95 25.76 0 -2 -10 64.66 10.07 0 2 10 80.17 11.87 0 -2 10 63.62 12.10 0 -2 10 58.18 8.63 0 -2 -10 68.94 10.94 0 2 -11 650.65 41.68 0 -2 -11 623.04 38.50 0 2 11 560.58 35.89 0 -2 11 519.19 34.21 0 -2 11 460.61 23.85 0 -2 -11 523.24 32.24 0 2 -12 25.01 10.42 0 -2 -12 11.00 7.06 0 2 12 23.97 8.16 0 -2 12 12.91 7.64 0 -2 -12 17.95 5.50 0 2 -13 88.28 30.80 0 -2 -13 72.47 12.45 0 2 13 61.01 11.00 0 -2 13 55.86 11.17 0 -2 -13 52.56 8.68 0 2 -14 368.97 46.43 0 -2 -14 316.93 22.98 0 2 14 268.42 20.78 0 -2 14 249.49 21.07 0 -2 -14 271.49 18.70 0 2 -15 672.25 46.25 0 -2 -15 646.31 40.00 0 2 15 570.94 36.18 0 -2 15 576.96 37.57 0 -2 -15 564.34 33.11 0 2 -16 567.64 64.83 0 -2 -16 502.40 35.14 0 2 16 481.51 34.67 0 -2 16 438.27 32.42 0 -2 -16 397.28 27.26 0 2 -17 776.21 96.38 0 -2 -17 752.07 56.96 0 2 17 658.87 51.17 0 -2 17 632.82 49.78 0 2 -18 362.26 41.04 0 -2 -18 367.47 40.75 0 2 18 332.39 38.73 0 -2 18 292.10 34.67 0 2 18 337.31 40.23 0 2 -19 618.64 67.27 0 -2 -19 606.83 64.60 0 2 19 524.81 58.29 0 -2 19 494.53 55.57 0 2 19 570.65 64.25 0 2 -20 1083.94 53.02 0 -2 -20 991.61 76.64 0 2 20 909.76 42.61 0 -2 20 862.06 43.36 0 2 20 940.09 86.48 0 2 -21 19.10 9.15 0 -2 -21 28.13 14.01 0 2 21 58.23 14.53 0 -2 21 11.98 8.57 0 2 21 3.94 3.88 0 2 -22 3.99 8.39 0 -2 -22 -1.74 7.47 0 2 22 0.41 6.83 0 -2 22 3.01 7.00 0 2 22 -3.13 3.94 0 2 -23 165.73 24.78 0 -2 -23 158.44 24.37 0 2 23 117.16 19.45 0 -2 23 154.62 21.42 0 2 -24 -2.08 9.96 0 -2 -24 6.71 10.36 0 2 24 1.91 7.24 0 -2 24 4.40 8.91 0 2 -25 6.77 10.30 0 -2 -25 -0.93 7.18 0 2 25 2.03 7.87 0 -2 25 11.87 11.75 0 2 -26 10.01 10.71 0 -2 -26 7.35 8.86 0 2 26 6.71 9.67 0 -2 26 12.10 12.39 0 2 -27 2.55 8.91 0 -2 -27 18.35 14.36 0 2 27 1.45 9.49 0 -2 27 2.20 8.63 0 2 -28 69.93 23.15 0 -2 -28 54.70 19.62 0 2 28 40.29 14.70 0 -2 28 23.04 16.32 0 -3 0 0.00 1.56 0 -3 0 -0.64 3.07 0 -3 0 -0.46 3.24 0 -3 -1 1.51 2.08 0 -3 1 -0.23 1.68 0 3 1 -0.64 3.13 0 -3 1 0.12 3.24 0 -3 1 0.29 3.07 0 -3 -1 -0.75 3.13 0 -3 -2 1.10 1.56 0 3 2 -1.79 2.89 0 -3 2 -0.58 3.47 0 -3 2 0.41 2.43 0 -3 -2 -0.93 3.30 0 3 -3 0.00 1.68 0 -3 -3 0.52 1.62 0 3 3 3.42 2.37 0 -3 3 2.78 3.53 0 -3 3 -0.35 2.20 0 -3 -3 -0.64 3.65 0 3 -4 -0.17 2.72 0 -3 -4 3.76 2.84 0 3 4 4.92 2.26 0 -3 4 2.84 3.88 0 -3 4 1.97 1.68 0 -3 -4 2.78 3.94 0 3 -5 -1.79 2.95 0 -3 -5 0.17 2.03 0 3 5 -0.75 3.13 0 -3 5 2.37 4.28 0 -3 5 2.55 2.72 0 -3 -5 -2.43 3.65 0 3 -6 -0.46 3.59 0 -3 -6 0.81 2.32 0 3 6 -1.04 3.59 0 -3 6 -2.37 4.11 0 -3 6 -0.64 1.56 0 -3 -6 2.95 3.82 0 3 -7 2.49 3.42 0 -3 -7 3.70 3.94 0 3 7 1.68 3.70 0 -3 7 2.03 4.23 0 -3 7 0.41 0.69 0 -3 -7 3.42 3.82 0 -3 -8 3.24 4.23 0 3 8 -2.78 4.57 0 -3 8 2.66 1.91 0 -3 -8 2.08 3.82 0 3 -9 -0.93 4.23 0 -3 -9 -0.58 2.78 0 3 9 31.32 11.52 0 -3 9 1.04 4.52 0 -3 9 0.41 0.41 0 -3 -9 3.36 4.23 0 3 -10 7.00 3.30 0 -3 -10 0.81 3.13 0 3 10 -2.14 4.80 0 -3 10 11.17 7.64 0 -3 10 1.10 1.10 0 -3 -10 2.95 3.99 0 3 -11 1.39 3.53 0 -3 -11 13.72 6.89 0 3 11 5.62 4.75 0 -3 11 2.43 4.86 0 -3 11 -0.17 0.69 0 -3 -11 18.41 7.35 0 3 -12 6.83 4.17 0 -3 -12 2.72 3.94 0 3 12 -1.79 4.52 0 -3 12 -1.56 4.86 0 -3 -12 4.75 5.21 0 3 -13 1.33 2.95 0 -3 -13 3.07 4.11 0 3 13 2.78 4.80 0 -3 13 -2.37 5.15 0 -3 -13 0.06 3.76 0 3 -14 3.70 3.65 0 -3 -14 0.69 4.28 0 3 14 6.02 5.33 0 -3 14 -2.32 5.27 0 -3 -14 2.37 3.94 0 3 -15 -0.75 5.79 0 -3 -15 3.42 4.92 0 3 15 2.26 5.09 0 -3 15 4.80 6.08 0 -3 -15 1.79 3.99 0 3 -16 2.26 5.44 0 -3 -16 -2.49 5.21 0 3 16 3.88 5.33 0 -3 16 -0.69 5.50 0 -3 -16 0.98 3.76 0 3 -17 -1.56 6.54 0 -3 -17 1.74 5.50 0 3 17 -0.46 5.21 0 -3 17 6.89 6.95 0 -3 -17 1.27 3.94 0 3 -18 5.73 5.73 0 -3 -18 11.58 9.26 0 3 18 -0.75 5.15 0 -3 18 2.43 6.54 0 -3 -18 2.14 4.34 0 3 -19 3.42 7.81 0 -3 -19 4.17 6.48 0 3 19 0.46 5.90 0 -3 19 0.12 6.48 0 3 -20 4.80 3.47 0 -3 -20 2.14 6.08 0 3 20 2.08 6.14 0 -3 20 0.93 6.43 0 3 -21 5.62 8.45 0 -3 -21 2.08 6.77 0 3 21 2.49 6.31 0 -3 21 8.39 10.19 0 3 21 -2.55 4.40 0 3 -22 2.89 7.00 0 -3 -22 0.17 6.83 0 3 22 5.85 10.30 0 -3 22 0.29 7.35 0 3 22 -2.14 5.04 0 3 -23 0.69 6.43 0 -3 -23 11.87 10.42 0 3 23 1.33 6.71 0 -3 23 0.06 7.29 0 3 23 3.94 4.63 0 3 -24 10.19 14.53 0 -3 -24 0.29 6.48 0 3 24 4.86 7.41 0 -3 24 11.35 9.73 0 3 -25 6.48 10.48 0 -3 -25 -0.58 6.60 0 3 25 6.25 8.22 0 -3 25 2.55 7.93 0 3 -26 -2.49 9.44 0 -3 -26 -1.22 7.18 0 3 26 2.26 8.91 0 -3 26 -1.04 8.05 0 3 -27 -7.99 10.59 0 -3 -27 -4.23 7.35 0 3 27 -4.52 9.49 0 -3 27 -1.45 8.34 0 3 -28 0.00 9.32 0 -3 -28 12.33 12.27 0 3 28 8.63 14.30 0 -3 28 3.76 9.20 0 -4 0 389.70 19.97 0 4 1 2452.28 81.45 0 -4 1 2115.49 62.58 0 -4 1 1792.66 54.24 0 -4 -1 1875.15 57.37 0 -4 -2 195.95 11.52 0 -4 2 186.28 12.04 0 4 2 241.16 35.66 0 -4 2 214.24 16.56 0 -4 2 168.51 34.79 0 -4 -2 174.76 17.02 0 4 -3 34.21 12.33 0 -4 -3 23.04 4.34 0 4 3 48.05 12.62 0 4 -4 1934.60 100.78 0 -4 -4 1634.68 80.64 0 4 4 1939.92 100.49 0 -4 4 1680.18 87.24 0 -4 4 1693.55 86.89 0 -4 -4 1479.95 78.03 0 4 -5 31.32 9.96 0 -4 -5 32.13 5.90 0 4 5 35.48 9.96 0 -4 5 31.95 7.81 0 -4 5 22.87 5.50 0 -4 -5 32.42 9.61 0 4 -6 142.29 34.79 0 -4 -6 113.92 10.54 0 4 6 155.54 42.03 0 -4 6 130.48 15.22 0 -4 6 111.84 19.51 0 -4 -6 111.95 13.26 0 4 -7 4.11 4.05 0 -4 -7 0.58 2.43 0 4 7 12.04 6.77 0 -4 7 3.82 6.95 0 -4 7 1.27 1.56 0 -4 -7 3.53 4.86 0 4 -8 137.83 46.25 0 -4 -8 104.31 10.65 0 4 8 109.06 13.37 0 -4 8 110.04 14.18 0 -4 8 84.23 20.49 0 -4 -8 105.93 13.08 0 4 -9 1413.55 68.54 0 -4 -9 1259.92 53.72 0 4 9 1299.57 57.60 0 -4 9 1189.30 56.38 0 -4 9 1035.89 47.87 0 -4 -9 1136.50 52.97 0 4 -10 55.75 21.01 0 -4 -10 43.88 8.34 0 4 10 50.83 11.06 0 -4 10 49.73 14.59 0 -4 10 28.83 7.12 0 -4 -10 40.41 11.17 0 4 -11 1031.78 52.74 0 -4 -11 924.23 45.67 0 4 11 991.21 44.52 0 -4 11 840.87 47.58 0 -4 11 736.67 30.91 0 -4 -11 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0.52 8.57 -7 2 -8 -0.12 8.68 -7 -2 8 -1.74 10.07 -7 -2 -8 -1.04 9.26 7 2 -9 2.78 7.35 7 -2 -9 -3.01 8.80 7 -2 9 4.63 10.25 7 2 9 6.71 8.91 -7 2 9 2.66 9.90 -7 -2 9 0.93 9.55 -7 2 -9 12.68 12.97 -7 -2 -9 18.41 15.17 7 2 -10 -3.82 6.77 7 -2 -10 11.11 10.48 7 -2 10 25.99 17.60 7 2 10 8.39 9.49 -7 2 10 24.43 18.06 -7 -2 10 16.27 12.62 -7 2 -10 6.54 9.49 -7 -2 -10 23.85 13.60 7 2 -11 0.58 6.43 7 -2 -11 0.00 7.76 7 -2 11 0.41 9.20 -7 2 11 3.01 10.77 -7 -2 -11 4.46 9.44 7 -3 0 3.36 8.45 -7 3 0 -1.04 8.68 -7 -3 0 2.66 10.13 -7 3 1 4.80 9.55 -7 3 -1 9.26 14.36 -7 -3 1 22.11 11.81 -7 -3 -1 18.58 15.28 -7 3 2 73.86 18.47 -7 3 -2 41.39 14.65 -7 -3 2 73.00 19.16 -7 -3 -2 57.60 18.29 7 3 3 3.24 7.99 -7 3 3 6.08 9.90 -7 3 -3 7.47 5.04 -7 -3 3 8.45 11.06 -7 -3 -3 10.19 12.74 7 3 4 140.32 24.66 -7 3 4 164.75 25.59 -7 3 -4 154.10 35.66 -7 -3 4 152.65 26.98 -7 -3 -4 132.91 22.58 7 3 5 8.63 9.20 -7 3 5 8.45 11.23 -7 3 -5 -2.72 9.78 -7 -3 5 12.68 10.42 -7 -3 -5 15.98 11.29 7 -3 6 82.49 22.75 7 3 6 87.58 21.01 -7 3 6 119.25 25.01 -7 3 -6 97.31 21.59 -7 -3 6 107.73 24.60 -7 -3 -6 96.09 22.06 7 3 7 2.55 3.99 -7 3 7 -9.32 9.09 -7 3 -7 -0.12 8.97 -7 -3 7 7.35 10.65 -7 -3 -7 -2.37 10.01 7 -3 -8 0.46 8.10 7 -3 8 4.52 10.54 7 3 8 3.07 8.28 -7 3 8 21.36 14.41 -7 3 -8 3.47 9.20 -7 -3 8 16.73 15.17 -7 -3 -8 4.46 10.59 7 -3 -9 10.77 10.07 7 -3 9 12.79 14.47 7 3 9 8.57 9.78 -7 3 9 -0.23 10.07 -7 3 -9 16.56 14.18 -7 -3 9 15.51 12.79 -7 -3 -9 15.57 15.69 7 -4 0 1.85 7.99 -7 4 0 2.08 10.07 -7 -4 0 -2.95 8.91 7 4 1 4.86 8.16 -7 4 1 14.70 6.14 -7 4 -1 -1.51 10.07 -7 -4 1 8.63 10.25 -7 -4 -1 9.32 10.77 7 -4 -2 -2.08 7.70 7 4 2 2.55 8.16 -7 4 2 11.46 13.60 -7 4 -2 1.10 6.71 -7 -4 2 -1.51 9.84 -7 -4 -2 2.66 10.01 7 -4 -3 5.73 9.03 7 4 3 -2.20 8.10 -7 4 3 8.34 9.90 -7 4 -3 1.51 7.76 -7 -4 3 -5.15 9.32 -7 -4 -3 -1.22 8.51 7 4 4 29.00 14.18 -7 4 4 42.37 19.22 -7 4 -4 36.93 16.79 -7 -4 4 34.44 18.47 -7 -4 -4 34.73 15.57 7 4 5 21.36 14.47 -7 4 5 41.22 20.90 -7 4 -5 30.45 17.71 -7 -4 5 25.70 14.82 -7 -4 -5 17.13 12.04 7 -4 -6 -1.22 8.80 7 4 6 1.56 8.91 -7 4 6 0.41 10.36 -7 4 -6 0.93 5.50 -7 -4 6 0.41 9.20 -7 -4 -6 -5.38 8.51 7 -4 -7 -1.56 9.38 7 4 7 9.90 13.43 -7 4 7 0.17 9.61 -7 4 -7 8.74 7.12 -7 -4 7 -5.44 9.73 -7 -4 -7 2.20 9.09 7 5 0 26.98 18.06 -7 5 0 3.18 10.30 -7 -5 0 3.76 9.90 7 -5 -1 -0.93 9.84 7 5 -1 3.24 8.68 7 5 1 9.38 10.65 -7 5 1 44.28 22.81 -7 5 -1 9.09 11.29 -7 -5 1 9.49 11.35 -7 -5 -1 12.91 11.58 -7 5 -2 27.15 15.17 -7 -5 2 39.25 20.09 -7 -5 -2 41.39 21.19 -7 5 3 6.60 9.67 -7 5 -3 4.28 10.07 -7 -5 3 12.74 16.38 -7 -5 -3 2.95 10.19 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 47683 _shelx_res_file ; TITL x792cout_a.res in Pbca x792cout.res created by SHELXL-2017/1 at 16:52:40 on 29-Sep-2017 REM Old TITL x792cout_a.res in Pbca REM SHELXT solution in Pbca REM R1 0.142, Rweak 0.004, Alpha 0.014, Orientation as input REM Formula found by SHELXT: C6 N O3 Cl CELL 0.71073 5.9241 9.735 22.444 90 90 90 ZERR 8 0.0093 0.0155 0.0337 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O Cl UNIT 40 24 16 24 8 L.S. 11 PLAN 20 SIZE 0.08 0.18 0.34 TEMP 173.15 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.056000 0.245000 FVAR 0.47947 CL1 5 0.849703 0.412408 0.700784 11.00000 0.03336 0.03499 = 0.03013 0.00165 -0.00521 0.00859 O1 4 1.006050 0.447132 0.583472 11.00000 0.02230 0.02841 = 0.04175 -0.00177 0.00680 0.00700 O2 4 0.131040 0.720446 0.673425 11.00000 0.03307 0.04525 = 0.03975 -0.00134 0.00902 0.00935 O3 4 0.103124 0.765563 0.579227 11.00000 0.02551 0.03004 = 0.04254 0.00484 -0.00689 0.00126 N1 3 0.813928 0.506225 0.592370 11.00000 0.02103 0.01745 = 0.03066 -0.00238 0.00316 -0.00145 N2 3 0.200085 0.713764 0.622051 11.00000 0.02086 0.02485 = 0.03596 -0.00061 0.00117 -0.00172 C1 1 0.712601 0.502997 0.647298 11.00000 0.02612 0.02124 = 0.02485 -0.00134 -0.00370 -0.00093 C2 1 0.511730 0.570334 0.657474 11.00000 0.02346 0.02582 = 0.02546 -0.00124 0.00213 -0.00269 AFIX 43 H2 2 0.445346 0.569168 0.695020 11.00000 -1.20000 AFIX 0 C3 1 0.411601 0.639086 0.611189 11.00000 0.01983 0.02246 = 0.03077 -0.00304 -0.00059 -0.00160 C4 1 0.508329 0.641838 0.555408 11.00000 0.02527 0.02467 = 0.02573 0.00171 -0.00326 -0.00172 AFIX 43 H4 2 0.438517 0.688058 0.524175 11.00000 -1.20000 AFIX 0 C5 1 0.709411 0.575167 0.546810 11.00000 0.02793 0.02687 = 0.02236 0.00033 0.00255 -0.00499 AFIX 43 H5 2 0.776304 0.576716 0.509329 11.00000 -1.20000 AFIX 0 HKLF 4 REM x792cout_a.res in Pbca REM R1 = 0.0496 for 1088 Fo > 4sig(Fo) and 0.0718 for all 1484 data REM 100 parameters refined using 0 restraints END WGHT 0.0557 0.2458 REM Highest difference peak 0.330, deepest hole -0.331, 1-sigma level 0.089 Q1 1 0.8614 0.3896 0.6599 11.00000 0.05 0.33 Q2 1 0.2244 0.7362 0.7173 11.00000 0.05 0.32 Q3 1 0.8385 0.4199 0.7484 11.00000 0.05 0.32 Q4 1 0.4196 0.6042 0.5821 11.00000 0.05 0.31 Q5 1 0.9165 0.4570 0.5862 11.00000 0.05 0.30 Q6 1 0.7292 0.5413 0.5730 11.00000 0.05 0.30 Q7 1 0.5652 0.5149 0.6392 11.00000 0.05 0.30 Q8 1 0.7481 0.5126 0.6273 11.00000 0.05 0.29 Q9 1 0.5036 0.6554 0.6421 11.00000 0.05 0.29 Q10 1 0.3487 0.4998 0.6985 11.00000 0.05 0.29 Q11 1 0.9885 0.4549 0.5162 11.00000 0.05 0.29 Q12 1 0.5512 0.5726 0.5504 11.00000 0.05 0.29 Q13 1 -0.0675 0.6968 0.7021 11.00000 0.05 0.29 Q14 1 0.1560 0.7037 0.6607 11.00000 0.05 0.27 Q15 1 0.3925 0.5690 0.6279 11.00000 0.05 0.27 Q16 1 0.2827 0.6452 0.6175 11.00000 0.05 0.27 Q17 1 0.4851 0.4196 0.6817 11.00000 0.05 0.27 Q18 1 0.2924 0.7199 0.6816 11.00000 0.05 0.26 Q19 1 0.8423 0.4168 0.7772 11.00000 0.05 0.25 Q20 1 -0.0340 0.8060 0.5891 11.00000 0.05 0.25 ; _shelx_res_checksum 41650 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy Cl Cl1 0.84970(12) 0.41241(8) 0.70078(3) 0.0328(3) Uani d 1 O O1 1.0061(3) 0.4471(2) 0.58347(8) 0.0308(5) Uani d 1 O O2 0.1310(3) 0.7204(2) 0.67343(9) 0.0394(6) Uani d 1 O O3 0.1031(3) 0.7656(2) 0.57923(8) 0.0327(5) Uani d 1 N N1 0.8139(3) 0.5062(2) 0.59237(9) 0.0230(5) Uani d 1 N N2 0.2001(4) 0.7138(2) 0.62205(9) 0.0272(5) Uani d 1 C C1 0.7126(4) 0.5030(3) 0.64730(10) 0.0241(6) Uani d 1 C C2 0.5117(4) 0.5703(3) 0.65747(11) 0.0249(6) Uani d 1 H H2 0.445346 0.569168 0.695020 0.030 Uiso calc 1 C C3 0.4116(4) 0.6391(3) 0.61119(11) 0.0244(6) Uani d 1 C C4 0.5083(4) 0.6418(3) 0.55541(11) 0.0252(6) Uani d 1 H H4 0.438517 0.688058 0.524175 0.030 Uiso calc 1 C C5 0.7094(4) 0.5752(3) 0.54681(11) 0.0257(6) Uani d 1 H H5 0.776304 0.576716 0.509329 0.031 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 Cl1 0.0334(4) 0.0350(4) 0.0301(4) 0.0086(3) -0.0052(3) 0.0017(3) O1 0.0223(10) 0.0284(11) 0.0418(12) 0.0070(9) 0.0068(8) -0.0018(8) O2 0.0331(12) 0.0453(14) 0.0397(12) 0.0094(10) 0.0090(9) -0.0013(10) O3 0.0255(10) 0.0300(11) 0.0425(12) 0.0013(9) -0.0069(8) 0.0048(9) N1 0.0210(12) 0.0174(11) 0.0307(11) -0.0014(10) 0.0032(8) -0.0024(9) N2 0.0209(12) 0.0248(12) 0.0360(13) -0.0017(10) 0.0012(9) -0.0006(10) C1 0.0261(14) 0.0212(13) 0.0249(12) -0.0009(12) -0.0037(10) -0.0013(10) C2 0.0235(14) 0.0258(14) 0.0255(13) -0.0027(12) 0.0021(10) -0.0012(10) C3 0.0198(13) 0.0225(13) 0.0308(14) -0.0016(11) -0.0006(11) -0.0030(10) C4 0.0253(14) 0.0247(14) 0.0257(14) -0.0017(11) -0.0033(10) 0.0017(10) C5 0.0279(14) 0.0269(14) 0.0224(13) -0.0050(12) 0.0026(10) 0.0003(11) 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' Cl Cl 0.1484 0.1585 '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 O1 N1 C1 121.0(2) O1 N1 C5 120.1(2) C5 N1 C1 118.9(2) O2 N2 O3 124.0(3) O2 N2 C3 117.9(2) O3 N2 C3 118.2(2) N1 C1 Cl1 116.0(2) N1 C1 C2 121.1(2) C2 C1 Cl1 122.9(2) C1 C2 H2 120.6 C3 C2 C1 118.7(2) C3 C2 H2 120.6 C2 C3 N2 119.0(2) C2 C3 C4 121.2(3) C4 C3 N2 119.7(2) C3 C4 H4 120.6 C5 C4 C3 118.7(2) C5 C4 H4 120.6 N1 C5 H5 119.4 C4 C5 N1 121.3(2) C4 C5 H5 119.4 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cl1 C1 1.697(3) O1 N1 1.291(3) O2 N2 1.225(3) O3 N2 1.228(3) N1 C1 1.372(4) N1 C5 1.371(3) N2 C3 1.469(4) C1 C2 1.378(4) C2 H2 0.9300 C2 C3 1.371(4) C3 C4 1.377(4) C4 H4 0.9300 C4 C5 1.370(4) C5 H5 0.9300 _cod_database_fobs_code 1548677